WQ0012980_More Information Received_20200319

Initial Review
INITIAL REVIEW
Reviewer Thornburg, Nathaniel
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Date Paper Copy 3/19/2020
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Project Number* WQ0012980
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Biosolids Management Plan
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Division of Water Resources ! Division of Water Resources
Non -Discharge Branch I Non -Discharge Branch
1617 Mail Service Center I Att: Nathaniel Thornburg, P Floor, Office #942W
- =
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Signature
Submission Date 3/19/2020

SLOW -RELEASE
Milorganite
NITROGEN FERTILIZER
Milwaukee Metropolitan Sewerage District
Biosolids Management Plan
June 27, 2019

Biosolids Management Plan
Contents
Section
Topic
Page
1
Introduction
1
2
Biosolids Processing Facilities
7
3
Milorganite® Fertilizer
9
3.A
Production Process
9
3.13
Pathogen Reduction Demonstration
9
3.13.1
Primary Pathogen Reduction Demonstration: Heat Drying
9
3.B.1.a
Product Temperature
9
3.B.1.b
Moisture
10
3.B.1.c
Fecal Coliform — Heat Drying
10
3.13.2
Secondary Pathogen Reduction Demonstration: Recycling Bin Time and
Temperature
10
3.B.2.a
The Recycling Bins
10
3.B.2.b
Product Temperature in the Recycling Bins
11
3.B.2.c
Time in the Recycling Bins
11
3.B.2.d
Compliance Determination
11
3.B.2.e
Use of Time and Temperature
11
3.B.2.f
Fecal Coliform —Time and Temperature
12
3.13.3
Tertiary Pathogen Reduction Demonstration: Pathogen Analysis
12
3.0
Vector Attraction Reduction Demonstration
12
3.D
Sampling
12
3.D.1
Production Sample Point
12
3.D.2
Shipping Sample Point
13
3.D.3
Bagging Sample Point
13
3.F
Contingency Plan for Handling Noncompliant Product
14
3.F.1
Temperature Noncompliance
14
3.F.2
Pathogen Noncompliance
14
3.F.3
Moisture Noncompliance
14
3.F.4
Chemical Noncompliance
14
4
South Shore Filter Press Cake
24
4.A
Production Process
24
4.13
Pathogen Reduction Demonstration
24
4.0
Vector Attraction Reduction Demonstration
24
4.C.1
Digester Inlet Total Volatile Solids Sampling
24
4.C.1.a
Jones Island Primary Sludge Weekly Composite Analyzed for Volatile Solids
Once per Week
24
4.C.1.b
South Shore Primary Sludge Weekly Composite Analyzed for Volatile Solids
Once per Week
25
4.C.1.c
South Shore Waste Activated Sludge Daily Composite Analyzed for Volatile
Solids Three Times per Week
25

4.C.2
Digester Outlet Total Volatile Solids Sampling and Analysis
25
4.C.3
Volatile Solids Reduction Calculation
26
4.D
Sampling for Pathogens, Chemical Pollutants, and Nutrients
26
4.E
Contingency Plan for Noncompliant Cake
27
5
Jones Island Filter Press Cake
34
6
Quality Assurance and Quality Control
36
6.A
Product Quality
36
6.13
Product Temperature Data Quality Review
37
6.0
Laboratory Quality Assurance and Quality Control
37
Appendix 1
Standards for the Use or Disposal of Sewage Sludge 40 CFR 503 (Excerpts)
Appendix 2
Domestic Sewage Sludge Management, Wis. Adm. Code, Ch. NR 204 (Excerpts)
Appendix 3
Milwaukee Metropolitan Sewerage District Laboratory Certifications and
Accreditations
Appendix 4
Dioxin Toxic Equivalency Factors for Dioxins, Furans, and PCB congeners
Appendix 5
Milwaukee Metropolitan Sewerage District Central Laboratory Quality Manual
Appendix 6
Quality Control Requirement Summary Sheet Examples
Appendix 7
Sample Receiving Standard Operating Procedure
Appendix 8
Chain of Custody Templates
Appendix 9
Summary of Biosolids Analytical Methods, Holding Times, Preservation, and
Frequency of Analysis

Figures
Figure
Subject
Page
1-1
Jones Island Process Flow Diagram
3
1-2
South Shore Process Flow Diagram
4
3-1
Milorganite° Fertilizer Drying Process Flow Diagram
15
3-2
Milorganite® Fertilizer Pathogen Reduction Demonstration Hierarchy
16
3-3
Jones Island Sample Point Diagram
17
3-4
Milorganite° Fertilizer Production Sample Point
18
3-5
Milorganite® Fertilizer Shipping Sample Point
19
3-6
Milorganite® Fertilizer Bagging Sample Point
20
4-1
South Shore Cake Storage Bays
28
4-2
Digester Feed Sampling Locations
29
4-3
Digested Solids Samplers
32
5-1
Jones Island Filter Press Cake North Loadout
35
Tables
Table
Subject
Page
1-1
Applicable Land Application Regulations
5
1-2
Milorganite° Fertilizer Pollutant Limits
6
1-3
South Shore Filter Cake Pollutant Limits
6
2-1
Jones Island Biosolids Facilities
8
2-2
South Shore Biosolids Facilities
8
3-1
Pathogen Reduction Demonstration Hierarchy
21
3-2
Milorganite° Fertilizer Production Sampling and Analysis
22
3-3
Milorganite° Fertilizer Shipping Sampling and Analysis
23
3-4
Milorganite° Fertilizer Bagging Sampling and Analysis
23
4-1
South Shore Filter Cake Sampling and Analysis
33

I. Introduction
The Milwaukee Metropolitan Sewerage District (District) provides water reclamation services to
1.1 million people in 28 municipalities. The District owns two water reclamation facilities. The
Jones Island Water Reclamation Facility (Jones Island) is in Milwaukee. The South Shore Water
Reclamation Facility (South Shore) is in Oak Creek. Both Jones Island and South Shore have the
following wastewater treatment operations: preliminary, primary, secondary, and disinfection.
Both Jones Island and South Shore produce biosolids. Veolia Water Milwaukee LLC (Veolia)
operates these facilities for the District.
Figures 1-1 (p. 3) and 1-2 (p. 4) are schematic diagrams of the water reclamation facilities.
The primary biosolids management technique is the production of Milorganite° fertilizer, which
uses biosolids from both facilities. Since 1926, the District has nationally distributed
Milorganite° fertilizer. It is available in 32-pound bags and 5-pound bags for the retail market
and 50-pound bags for the professional landscaping market. Upon request, the District can
provide %-ton and 1-ton containers. Finally, Milorganite° fertilizer is available in bulk by truck
or railcar. The Milorganite° fertilizer production facility is at Jones Island.
Despite having two water reclamation facilities, solids processing is integrated. Four interplant
solids pipelines connect Jones Island and South Shore, which are approximately 10 miles apart.
Anaerobic digesters are located at South Shore. These digesters stabilize primary sludge from
both facilities. Primary sludge is pumped from Jones Island to South Shore. Digested primary
sludge from South Shore and waste activated sludge from South Shore are pumped to Jones
Island.
At Jones Island, the sludge from South Shore mixes with waste activated sludge from Jones
Island in equalization tanks. Thickening and pressing follow. The pressed sludge is mixed with
previously dried sludge and fed to a multi -pass heat drying system that uses horizontal rotary
drums. Pellet sizing follows drying. Storage follows sizing. From storage, the District ships
Milorganite° fertilizer in trucks or railcars to a bagging contractor or to customers of bulk
product.
If the District cannot use all biosolids to make Milorganite° fertilizer or if operating conditions
require solids removal, then the District, through Veolia, will produce filter cake at South Shore.
South Shore operates sludge thickeners and plate and frame presses to produce filter cake. The
District, through Veolia, operates the presses at least once per year to confirm functionality.
Contractors apply filter cake in bulk to agricultural land or, if land is unavailable, take it to a
landfill.
To be marketed and distributed without restriction, Milorganite° fertilizer must comply with
metals limits that allow unrestricted use and Class A requirements for pathogen reduction and
vector attraction reduction. As a Class B biosolids product, South Shore filter cake has less
stringent limits for pathogen indicators, but more stringent requirements regarding how and
where it is applied to land.
Table 1-1 (p. 5) identifies land application regulations that apply to Milorganite° fertilizer and
filter cake. Tables 1-2 (p.6) and 1-3 (p.6) identify the limits that apply.

The District implements and enforces an Industrial Waste Pretreatment Program to maintain
metals concentrations that comply with the applicable limits. The District achieves pathogen
reduction and vector attraction reduction through sludge processing, as fully described in this
Biosolids Management Plan.
A Wisconsin Pollutant Discharge Elimination System (WPDES) permit regulates operations of
the water reclamation facilities. This permit includes pollutant limits and sampling
requirements for biosolids. The WPDES permit effective April 1, 2019, Section 8.11, requires
the District to provide this Biosolids Management Plan.

W
JONES ISLAND WASTEWATER TREATMENT PLANT PROCESS FLOW
DIAGRAM
EXCEss FLOry nr�ERSIaN
-------------------------------------------------------------..._.....,...,...._�.-._...
CHLORINE
SCREW BAR GRIT PRIMARY AERATION 5ECCiVDARY CONTACT LAKE
RAW PUMPS SCREEN- CHAMBERS CLARIFIERS BASINS ""' CLARIFIERS HAS PLANTMICHIGAN
VASTEW4TER FIGH + EFFLUENT
LEVEL ��
M1
LOW
LEVEL
TC SOUTH 4 IRON SALTS SODIUM
SHORE LOOS HYPCCHLOR17E RI.;JI =ITF
ORI
INLINE PUMP I..... _. �? 7F_. �. ...._._._.. ��.�.�. �-_._._--.—. .——._._._._.—.—.—.—.—.—._._._._._._._._ a.
STATION I SCRERA NCS PRIMARY SOLIDS WASTE 0
ACT VA =D SOUTH SFDRE 0
I BIDSCLICS BC5OLID5 (p
I �
I
I PRIMARY WASTE BQ5CLILlS
TO LANDFILL DEBRIS SOLIDS RECEIVING
I PROCESSING SCREENING
POLYMERS INTERPLANT Q
I "CT
INLINETUNNEL IRON LIDS PUMPING
I SKIMMINGS
SYSTEM I H FROM 0
2LARIFIE4S FILTRATE ��Oy WAST
SLUDGE SCLIDSTO A
SKIMIM NOS THCRENING SOUTH SHORE fD (D
I PROCESSING GRAVTYBELTS u, h,
DUST Z N
SOLIDS TREATMENT PRIMARY SOLIDS 0
v
EOi BLEND EQIBLEND
FUEL HEAT SLUDGE TANK TANK �•
EQUALIZATION & L I
BLENDING TANKS Z
TURBINE
ELECTRICAL
ENERGY FUEL UU SB pp—t
BULK DR SLUDGE
PACKAGING CAKE FERRIC CHLORIDE
PCLVMER
HEAT DRIED MILORGANITE
FERTILIZER STORAGE DRYING DEWATERING
MILCRGANRE
PRCDDCTICN FILTRATE
LOST TO
FERTILIZER
PROCESSING
OR LANDFILL

SOUTH SHORE WASTEWATER TREATMENT PLANT PROCESS FLOW DIAGRAM
-- ExcEss F ow oivEasiGn
BAR GRIT PRIMARY AERATION 9EGONDRRY LAKE
RAW SCREENS CHAMBERS CLARIFIERS BASINS CLARIFIERS CHLORINE CONTACT BASIN PLANT MICHIGAN
;TEWATERscux saM EFFLUENT
70 JONES
IRON SALTS FOR P 9001UM O
REMOVAL N SOLIDS BISULFITE
GRIT
SODIUM
INLINE PUMP HYPOCHLORITE
STATION SCREENINGS PRIMARY SOLIDS WASTE BIOSOLIDS Ir
O
POLYMER y
SULIDSTO
TO LANDFILL PRIMARY THICKENING JONES ISLAND O
DEBRIS SOLI S n
PROCESSING SCREENING
INTERPLANT y CD
SOLIDS PUMPING
INLINE TUNNEL SKIMMINGS JONES N
SYSTEM r FROM ISLAND
.r
CLARIFIERS SOLIDS �
SKIMMINGS 0 METHANE
PROCESSING STORAGE
Imo.
PRIMARY SOLIDS ANAEROBIC
SOLIDS TREATMENT DIGESTION
CENTRATE to treatmert
1 POLYMER
UIGESTEU 610801ILl4 DIGESTED BIOSOLIUS ll� GBTs
METHANE GAS
STORAGE Digestors SLOWERRBOILERS
DEWATEREG
SOLIDS—[ S o
STORAGE O
a O
LAND APPLICATION ijiL
OR LANDFILL FILTER PRESS
FILTRATEtc4.t—t ELECTRIC ENGINES
GENERATORS

Table 1-1
Applicable Land Application Regulations
Product
Metals Limits
Pathogen Reduction
Vector Attraction Reduction
Federal
Wisconsin
Federal
Wisconsin
Federal
Wisconsin
Milorganite®
40 CFR 503.13(b)(3)
NR 204.07(5)(c)
40 CFR 503.32(a)(3)(7)
NR 204.07(6)(a)2c
40 CFR 503.33(b)(7)
NR 204.07(7)(g)
Fertilizer
and
Appendix B.B.2
"Class A Alternative 5"
40 CFR 503.32(a)(3)(1)
NR 204.07(6)(a)2a
"Class A Alternative 1"
40 CFR 503.32(a)(3)(6)
NR 204.07(6)(a)2a
"Class A Alternative 4"
Filter Cake
40 CFR 503.13(b)(1)
NR 204.07(5)(a)
40 CFR 503.32(b)(2)
NR 204.07(6)(b)1
40 CFR 503.33(b)(1)
NR 204.07(7)(a)
"Class B Alternative 1"

Table 1-2
Milorganite° Fertilizer Pollutant Limits
Pollutant
Limit
Arsenic
41 mg/kg
Cadmium
39 mg/kg
Copper
1,500 mg/kg
Lead
300 mg/kg
Mercury
17 mg/kg
Molybdenum
75 mg/kg
Nickel
420 mg/kg
Selenium
100 mg/kg
Zinc
2,800 mg/kg
PCBs
10 mg/kg
Moisture
10%
Fecal coliform
1,000 mpn/gTS
Enteric Viruses
1 pfu/4gTS
Helminth Ova
1/4gTS
Table 1-3
South Shore Filter Cake Pollutant Limits
Pollutant
Limit
Arsenic
75 mg/kg
Cadmium
85 mg/kg
Copper
4,300 mg/kg
Lead
840 mg/kg
Mercury
57 mg/kg
Molybdenum
75 mg/kg
Nickel
420 mg/kg
Selenium
100 mg/kg
Zinc
7,500 mg/kg
PCBs
10 mg/kg
Fecal coliform
2,000,000 mpn/gTS

2. Biosolids Processing Facilities
Both Jones Island and South Shore include facilities to process biosolids. At Jones Island, the
principal facilities are equalization and blending tanks, gravity belt thickeners, belt filter
presses, and gas -fired rotary drum driers with associated equipment. Jones Island has day
tanks for short-term (24 hours) finished product storage and silos for long-term finished
product storage. At South Shore, the principal facilities are dissolved air flotation thickeners,
anaerobic digesters, gravity belt thickeners, plate and frame presses, and a building for cake
storage. Both facilities have pumps for transferring solids between Jones Island and South
Shore using the Interplant Solids Pipeline. Tables 2-1 (p.8) and 2-2 (p. 8) summarize the
biosolids facilities at Jones Island and South Shore.

Table 2-1
Jones Island Biosolids Facilities*
Unit
Number
Size
Equalization Tanks
2
360,000 gallons each
Gravity Belt Thickeners
4
1200 max gpm each
Belt Filter Presses
24
55 gpm each
Dryers
12
Diameter: 8 feet
Length: 57.5 feet
Day Tanks
4
Diameter: 12 feet
Height: 60 feet
Capacity per tank: 175 tons
Storage Silos
12
Diameter: 26 feet
Height: 80 feet
Capacity per silo: 1,000 tons
Interplant Solids Pipeline Pumps
4
Pumps 1 and 4 pump to 14" lines, 1200 gpm
max, but pressure limited
Pumps 2 and 3 pump to 12" lines, 900 gpm
max, but pressure limited
*As identified by the Contract Compliance Office in June 2019
Table 2-2
South Shore Biosolids Facilities*
Unit
Number
Size
Dissolved air flotation thickeners
6
1,240 pounds/hour
Anerobic digesters
6
Digesters 6 and 8:
1.5 million gallons each
Digesters 9, 10, 11, and 12:
3 million gallons each
Storage Digesters
6
Digesters 1, 2, 3, 4, 5, and 7:
1.5 million gallons each
Gravity Belt Thickeners
3
2-meter width (1)
1-meter width (2)
Plate and Frame Presses
5
75' L x 12' W x 14' H, 151 plates
per press. In general, each press
can produce approximately 40
dry tons/24 hours of operation
Cake storage hanger bays
4
Dimensions of each bay = 84' W
x 170' L x 35' H.
1,700 wet tons of cake per bay
Interplant solids pipeline pumps
3 dual phase skids, 2
750-800gpm max. 400-450
pumps per skid. Each
typical. Pressure limited 200 psi
pump motor = 250 hp.
max, normal is 175 psi.
*As identified by the Contract Compliance Office in June 2019

3. Milorganite° Fertilizer
3.A Production Process
The Milorganite° fertilizer production process uses biosolids from the District's two water
reclamation facilities: Jones Island and South Shore. Milorganite° fertilizer production occurs at
Jones Island.
Generally, the steps in the production process are:
1. Waste activated sludge mixes with anaerobically digested sludge
2. Thickening
3. Dewatering
4. Mixing of dewatered sludge with previously heat -dried sludge
5. Multi -pass rotary drum drying
6. Screening
7. Sampling, including nutrients, metals, moisture, fecal coliform, and PCBs
8. Storage
9. Shipping to bagging contractor
10. Bagging
11. Shipping to distributors
Heat -drying occurs in twelve dryers in two groups of six. A recycling bin is at the end of each
group of six dryers. From the recycling bin, most pellets (60%-70%) return to the dryers. The
remaining pellets go to screens that separate pellets by size. Pellets that are larger than desired
return to the drying system.
Extensive product recycling occurs to produce a consistent product that complies with the
nutrient and pellet size guarantees required for commercial fertilizers. Three recycling systems
operate continuously: (1) from dryer to dryer, (2) from the recycling bin back to the dryers, and
(3) from screening back to the recycling bin. A fourth recycling system is available for special
conditions, such as low product temperature or conveyor failure. This fourth system operates
around individual dryers and returns product from the dryer outlet directly back to the dryer
inlet.
For the drying process, Figure 3-1 (p. 15) provides a process flow diagram.
3.13 Pathogen Reduction Demonstration
The District will demonstrate compliance with pathogen reduction demonstration requirements
according to the hierarchy indicated in Table 3-1 (p. 21) and in Figure 3-2 (p. 16).
3.13.1 Primary Pathogen Reduction Demonstration: Heat Drying
3.13.1.a Product Temperature
Each dryer contains a resistance temperature detector (RTD) at the end of its heated zone to
measure product temperature. Temperatures will be recorded every minute or whenever the
temperature changes, whichever is more frequent. According to the District's WPDES permit

effective April 1, 2019, the average temperature for each discrete fifteen -minute interval is
compared to the temperature required to demonstrate pathogen reduction (80°C/176°F).
Dryer Discharge Product temperature is visible to operators on their data display screens. If
product temperature falls below 1807, then automatic controls in each dryer recycle all
product leaving the dryer back to the inlet of the dryer. In addition, an alarm is initiated to
inform the operator that the temperature has dropped to or below 1807 and automatic
recycle has been initiated. The operators then take appropriate steps to increase the product
temperature.
3.13.1.1b Moisture
The District will collect daily 24-hour composite samples after pellet sizing and before storage
(WPDES Permit Sample Point 006). The District will analyze these samples for moisture. From
the 24-hour period represented by the sample, the District will hold product until the District
obtains results. If a result exceeds 10% moisture, then the District may re -analyze the original
sample or re -sample to confirm the moisture content. Product with a high moisture content
will be re -processed. If re -processing is not possible, then the District will manage this material
as a Class B product or ship it to a landfill for disposal.
3.B.1.c Fecal Coliform — Heat Drying
The District will collect one sample per week for fecal coliform after pellet sizing and before
storage (WPDES Permit Sample Point 006). If a result exceeds 1,000 MPN/gTS, then the
product will be re -processed. Before re -processing, the District may re -sample to confirm the
fecal coliform concentration. If product is already shipped, then the District would recall it and
re -process it. If re -processing is not possible, then product would be managed as a Class B
product or shipped to a landfill for disposal. All recent sample results are below or near the
level of detection, far below the limit, which indicates a minimal risk of fecal coliform problems.
3.13.2 Secondary Pathogen Reduction Demonstration: Recycling Bin Time and Temperature
3.B.2.a The Recycling Bins
As described above, a recycling bin follows each train of six dryers. After multi -pass drying,
product flows into the top of the recycling bin. From the bottom of the recycling bin, product
flows in two directions. Most product returns to the dryers for further multi -pass heat -drying.
The remaining product goes to screening. The bins have a capacity of 30 tons. The typical
operating range is 15 to 20 tons and retention times of 15 to 45 minutes. Detention time in the
bins varies according to how full they are. The bins are not heated. However, the large mass of
continuously arriving hot product usually maintains a temperature higher than 70°C (1587).
Product cools as it drops through the bin, making the temperature at the bottom of the bin the
lowest temperature.
Although the District operates two trains of dryers, the District has three recycling bins. One
bin serves only the north train of dryers. A second bin serves only the south train of dryers. A
third bin can be used by either train of dryers and is used when the primary bin for a train of
dryers is not operational.
10

3.B.2.b Product Temperature in the Recycling Bins
Three RTDs near the bottom of each bin provide product temperature. Temperatures are
recorded every minute or whenever the temperature changes, whichever is more frequent.
According to the District's WPDES permit effective April 1, 2019, the average temperature for
each discrete fifteen -minute interval is used to determine compliance.
Recycling bin temperature is continuously available to operators.
Temperature measurement at the recycling bins was fully operational beginning April 1, 2019.
3.B.2.c Time in the Recycling Bins
The District calculates detention time in a recycling bin using the rate of the mass entering the
recycle bin and the mass of the bin. Several weigh elements located on the recycle bin, recycle
product conveyors, and dryer feed system continuously measure the rate of the mass entering
the recycle bin and the mass of the recycle bin. The District continuously collects this
information and this information is continuously available to operators.
The District performed eleven tracer studies to determine how actual detention time compares
to the calculated detention time. The worst -case result found the ratio of the actual detention
time to the calculated detention time to be 0.73. In response, the District multiplies the
calculated detention time by 0.73 when determining compliance. Tracer study results are
available upon request.
3.B.2.d Compliance Determination
Using "Equation 2" from 40 CFR 503.32(a)(3)(ii)(A)7, the District will continuously calculate a
required temperature for the current detention time, based upon current bin mass, entering
mass flows, and the adjustment factor. To comply, the product temperature must be higher
than the required temperature.
3.B.2.e Use of Time and Temperature
If a fifteen minute in -drum product temperature is below the required temperature at any
individual dryer, then the District will use recycling bin time and temperature to demonstrate
pathogen reduction for the group of six dryers that includes the dryer with the low
temperature. Use of time and temperature will continue until 40 minutes after all in -drum
product temperatures are higher than the required temperature. 40 minutes is the worst -case
product travel time from the dryer farthest from the recycling bin to the outlet of the recycling
bin.
If time and temperature does not show compliance, then a gate from the recycle bin to
screening will automatically close, stopping product flow to screening and recycling all product
back to the dryers. In this configuration, all product will return to the dryers. This gate will
automatically reopen when time and temperature shows compliance. If this gate fails to close
or the temperature and time requirements are not achieved, then the District will segregate the
produced material. Depending upon the circumstances, the District will re -process it, sample it
for viruses and helminth ova, distribute it as a Class B Product, or dispose of it in a landfill.
11

3.13.2A Fecal Coliform —Time and Temperature
Fecal coliform analysis will occur as described above in sec. 3.13.1.c.
3.13.3 Tertiary Pathogen Reduction Demonstration: Pathogen Analysis
If both in -drum temperatures and time and temperature do not demonstrate compliance, then
the District will segregate product. For short-term product storage, the District has four "day
tanks." Each of these tanks has a capacity of approximately 175 tons. For long-term product
storage, the District has twelve silos and each silo has a capacity of approximately 1,000 tons.
The preferred approach to product management will be to re -process the segregated product.
If re -processing is not practical, then the preferred option will be to demonstrate Class A status
by sampling the segregated product for fecal coliform, enteric viruses, and helminth ova. If the
District proceeds with pathogen analysis, then the District will hold the segregated product until
the District receives the analytical results and the results comply. In this case, the District will
limit distribution of this product to Wisconsin or other states that accept this pathogen
reduction demonstration approach.
Alternatively, instead of pathogen testing, the District may decide to distribute the segregated
sludge as a Class B product or send it to a landfill for disposal, depending upon the availability
of land for bulk application, the availability of space in the silos for extended storage, and other
factors.
3.0 Vector Attraction Reduction Demonstration
The primary solids in Milorganite° fertilizer will be stabilized using anaerobic digestion.
Therefore, Milorganite° fertilizer will comply with the vector attraction reduction
demonstration requirements of 40 CFR 503.33(b)(7) and Wis. Adm. Code, sec. NR 204.07(g),
which require a solids concentration of 75% or greater (<25% moisture) for products with
stabilized primary solids. As noted above, the heat drying process reduces moisture to 10% or
less. The sampling point for moisture is after sizing and before short-term storage (WPDES
Permit Sample Point 006).
3.1) Sampling
Figure 3-3 (p. 17) provides a process flow diagram showing the locations of the production,
shipping, and bagging sample points.
3.D.1 Production Sample Point
The production sample point is Sample Point 006 in the WPDES permit. It is at Jones Island, in
Building 258, on the sixth floor. It is after sizing and before short-term storage. Product is
sampled as it is falling in a chute while product is on its way to the day tanks. Figure 3-4 (p. 18)
is a picture of the production sample point.
The sample point has a sampler that collects an aliquot for every four tons of production. A
scale on an upstream belt conveyor triggers the sampler. Daily composite samples are
collected from 5 am to 5 am whenever production is occurring.
Also, the sample point has a hatch for collecting grab samples.
12

Weekly composite samples are collected by combining daily samples in an amount proportional
to overall production for a seven-day period defined as Sunday through Saturday. Each weekly
sample is also analyzed for mercury and water extractable phosphorus. One weekly composite
sample per month is analyzed for total Kjeldahl nitrogen.
Table 3-2 (p. 22) shows the parameters for which sampling occurs, sample types, and the
frequency of analysis.
3.D.2 Shipping Sample Point
The shipping sample point is Sample Point 008 in the WPDES permit. It is at Jones Island, in
Building 259, on the third floor.
From storage in silos, Milorganite° fertilizer is shipped in bulk using trucks or railcars. Trucks
can hold up to 25 tons of product and railcars can hold up to 100 tons of product. The District
can load only one truck or one railcar at one time.
Composite samples are taken as described below. The composite sampler for shipping is
located just upstream of the loadout point, immediately after the addition of dust suppressant.
Figure 3-5 (p. 19) provides a picture of the composite sampler. Both railcars and trucks are
sampled at the same location.
Railcars are loaded at a rate of 30 to 40 tons/hour. When loading railcars, the composite
sampler is set to take an aliquot every 390 seconds. The sample duration for each aliquot is 4
seconds, which provides an aliquot weight of approximately 150 grams. Typically, filling a
railcar requires 3.5 hours. Therefore, each railcar load is sampled about 32 times. From the
roughly 4000-gram sample, 500 grams are used to perform an in-house sieve analysis for
particle size QA/QC. The remaining is sent to the MMSD Laboratory for additional analysis.
Trucks are loaded at a rate of 30 to 40 tons/hour. When loading trucks, the composite sampler
is set to take an aliquot every 150 seconds. The sample duration for each aliquot is 4 seconds
which provides an aliquot weight of about 150 grams. Typically, filling a truck requires 1 hour.
Therefore, each truckload is sampled approximately 24 times. Of the roughly 4000-gram
sample, 500 grams are used to perform an in-house sieve analysis for particle size QA/QC. The
remaining sample is sent to the MMSD Lab for additional analysis.
When loading either trucks or railcars, to grab the sample for fecal coliform, the District uses
the sampler to capture product from the conveyor.
Table 3-3 (p. 23) shows the parameters for which sampling occurs, sample types, and the
frequency of analysis.
3.D.3 Bagging Sample Point
Although some Milorganite° fertilizer is shipped in bulk to customers, most Milorganite°
fertilizer is bagged for retail distribution. The bagging contractor is Kinder Morgan, 1900 South
Harbor Drive, Milwaukee. Railcars transport product to the bagging facility, which is
approximately one mile south of the District's Jones Island facility. Based on customer demand,
product can be bagged in a variety of sizes: 5 pounds, 32 pounds, 50 pounds, % ton, and 1 ton.
13

Veolia staff will grab a sample from bagged product once per month. A random sealed retail
bag will be taken from the bagging conveyor, opened and sampled. Figure 3-6 (p. 20) shows
where sampling occurs. Typically, sampling will occur on the first Tuesday of the month. If
bagging is not occurring, then Veolia staff will visit on subsequent Tuesdays until a sample is
collected.
Table 3-4 (p. 23) shows the parameters for which sampling occurs, sample types, and the
frequency of analysis.
This location is WPDES Permit Sample Point 009.
3.F Contingency Plan for Handling Noncompliant Product
Management of noncompliant product will depend upon the type of noncompliance and the
options available at the time of the noncompliance. Beneficial reuse will always be preferred.
However, bulk land application may occur only if product complies with Class B requirements
and land is available. If land is unavailable or product does not comply with Class B
requirements, then the District will ship the product to a landfill.
Regarding results for pathogens, moisture, and chemical pollutants, analysts will constantly
monitor their results. If analysts identify unusually high results, then analysts will inform
operational staff. In addition, operational staff will monitor results as the results become
available to identify potential problems.
3.F.1 Temperature Noncompliance
If product does not comply with dryer discharge product temperature requirements, then the
District will use a secondary compliance method of time -temperature in the recycle bins, as
described in Section 3.13.2.e. above. If the time -temperature method in the recycle bins does
not comply, then the District will segregate and re -process the product to meet the applicable
standards. Alternatively, the District may land apply this product as a Class B sludge or ship it to
a landfill, depending on the issues and the conditions at the facility.
3.F.2 Pathogen Noncompliance
Noncompliant material will either be re -processed through the sludge drying cycle as described
in Section 3.13.1.c. above, land applied as a Class B sludge, or shipped to a landfill, depending on
the issues and the conditions at the facility.
3.F.3 Moisture Noncompliance
If a moisture concentration is greater than 10%, then this product will be segregated and
returned to the drying process, as allowed by facility conditions. If conditions do not allow re -
drying, then this material will be land applied as a Class B sludge or shipped to a landfill.
3.F.4 Chemical Noncompliance
Noncompliant material will either be land applied in bulk with loadings tracked or sent to a
landfill, depending on the magnitude of the problem, the availability of land, opportunities to
blend product to reduce concentrations, and other conditions.
14

Sludge CA Drying and Recycle System Schematic
Recycle Feed to Feed to dryer,
dryer in Dry Dry Tons/Day
Tons/Day (Typi I a I M assj
(Typica Mass)
18 I181818
180 180 —+I 188 � 196
Recycle Product
returning from
Recycle Bin, Dry Dryer? DryM MW Dryer10 Dryerl1
Tons/Day
jTypical Mass) • •
502�
4-- ------,__. .. A-. ..- -- ----
Dryer, Dryer2 Drysr3 07er4 DgwS
180 18 180 7 ISO 1 18 160 4'118
r
Temperature
Monitoring
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72
RECYCLE BIN 1•
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RECYCLE BIN 1 I a*
72
RECYCLE BIN 21 I
South Dryers and recycle
system are Mirror Image of
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Class B Land
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NO
W
L

Dewatered
Sludge
'M
Dryer Discharge
Sample ProductTemperature
and
Point010 Recycling Bin Time and
Temperature
Landfill
Sample
Point006
Railcarto
Bagging
Sample
Point009
Sample
Point008
Railcar Bulk
Distribution
Truckload
Bagged
Distribution
Truckload
Bulk
Distribution
3

Figure 3-4
Milorganite° Fertilizer Production Sample Point
18

Figure 3-5
Milorganite° Fertilizer Shipping Sample Point
19

Table 3-1
Pathogen Reduction Demonstration Hierarchy
Method
Parameters Measured
Sample Point
Citation
Heat Drying
Class A — Alternative 5
Fecal coliform
After screening
40 CFR 503.32(a)(3)(7)
and
Appendix B.B.2
NR 204.07(6)(a)2c
Product temperature
In -dryer at the
end of the heated
zone
Product moisture
After screening
Time and Temperature
Class A — Alternative 1
Fecal coliform
After screening
40 CFR 503.32(a)(3)(1)
NR 204.07(6)(a)2a
Temperature
Recycling bin
Time
Recycling bin
Pathogen Testing
Class A — Alternative 4
Fecal coliform
Enteric viruses
Helminth ova
Silo storage
40 CFR 503.32(a)(3)(6)
NR 204.07(6)(a)2a
21

Table 3-2
Milorganite® Fertilizer Production Sampling and Analysis
Parameter
Sample
Frequency
Sample Type
Analytical
Method
Laboratory
As, Cd, Cu, Fe, K, Mo, Ni, P, Pb, Se, Zn
Daily
24-hour mass -weighted composite
EPA 6010C
District
Al, B, Cr, Co
Monthly
24-hour mass -weighted composite
EPA 6010C
District
Hg
Weekly
Weekly mass -weighted composite
EPA 7471B
Contract
PCB Aroclors
Daily
24-hour mass -weighted composite
EPA 8082
Contract
Dioxin Toxic Equivalents: Dioxins, Furans, and PCB
congeners*
Monthly
24-hour mass -weighted composite
EPA 1668A
EPA 8290
Contract
Priority Pollutants - volatile organic compounds
Semi-annually
Grab
EPA 8260C
Contract
Priority Pollutants - Semi -volatile organic
compounds, pesticides, PCB Aroclors, metals,
cyanide
Semi-annually
24-hour mass -weighted composite
EPA 8270D
EPA 8081B
EPA 8082A
EPA 9012B
EPA 6010C
EPA 7471B
SM 4500
Contract
Nitrogen, ammonia
Monthly
24-hour mass -weighted composite
AOAC 2.065
District
Nitrogen, nitrate
Monthly
24-hour mass -weighted composite
AOAC 930.01
District
Nitrogen, total Kjeldahl
Monthly
Weekly mass -weighted composite
AOAC 955.04
District
Nitrogen, water insoluble
Monthly
24-hour mass -weighted composite
AOAC 945.01
District
Phosphorus, water extractable
Quarterly
Weekly mass -weighted composite
DNR/Penn State
District
Total volatile solids
Monthly
24-hour mass -weighted composite
SM 2540G
District
Moisture
Daily
24-hour mass -weighted composite
SM 2540G
District
Fecal Coliform
Weekly
Grab
EPA 1680
District
* Appendix 4 shows specific dioxin, furan, and PCB congeners and toxic equivalency factors
22

Table 3-3
Milorganite° Fertilizer Shipping Sampling and Analysis
Parameter
Sample
Frequency
Sample Type
Analytical
Method
Laboratory
Moisture
Monthly
Time composite
SM 254OG
District
Fecal Coliform
Monthly
Grab
EPA 1680
District
Table 3-4
Milorganite° Fertilizer Bagging Sampling and Analysis
Parameter
Sample
Frequency
Sample Type
Analytical
Method
Laboratory
Moisture
Monthly
Grab
SM 254OG
District
Fecal Coliform
Monthly
Grab
EPA 1680
District
23

4. South Shore Filter Press Cake
4.A Production Process
From both Jones Island and South Shore, all primary sludge is anaerobically digested at South
Shore. Also, when needed to control solids levels and when space in the digesters is available,
waste activated sludge from South Shore also goes to the digesters, after thickening using
dissolved air flotation thickeners. South Shore produces cake from the sludge produced by
digesters, using four plate and frame presses. A fifth press is present, but it is not operational.
Cake is typically in the range of 19% to 28% solids at the time of production.
The presses do not operate on a routine schedule. The presses will operate as needed to
reduce excess solids levels to the preferred level. The amount of sludge processed by the
presses during each run will vary. The presses will operate at least once per year to confirm
their functionality.
South Shore has four covered hanger bays for cake storage. Each hanger bay can store up to
1,700 wet tons of cake. Figure 4-1 (p. 28) shows pictures of the hanger bays. In the rare cases
where cake inventory exceeds the capacity of these hanger bays, the District will store cake in
on -site lagoons, which were originally constructed for liquid sludge. The District will cover any
cake stored in a lagoon.
A contractor will land apply cake as Class B biosolids. Land application of the cake depends
upon the availability of the contractor, the availability of agricultural land and the weather.
Therefore, land application is not always feasible each year. If space is insufficient to store
cake, then landfill disposal will occur.
4.13 Pathogen Reduction Demonstration
Sampling before land application will demonstrate a fecal coliform concentration less than
2,000,000 MPN/gTS as a geometric mean of seven samples.
4.0 Vector Attraction Reduction Demonstration
Sampling before and after digestion will demonstrate a total volatile solids reduction of at least
38%.
4.C.1 Digester Inlet Total Volatile Solids Sampling
Characterizing sludge being digested requires sampling three different sludges: Jones Island
primary sludge, South Shore primary sludge, and South Shore waste activated sludge. Figure 4-
2 (p. 29) shows these sampling locations. Volatile solids reduction calculations use results for
South Shore waste activated sludge, only when this sludge is being digested.
4.C.1.a Jones Island Primary Sludge Weekly Composite Analyzed for Volatile Solids Once per
Week
Samples are obtained by the Treatment Plant Operator 3 — Preliminary Treatment (TPO-3) in
the basement of the Preliminary Treatment Building (Building 203) from an in -line sample port.
Three times per 12-hour shift, the TPO-3 obtains a 166 ml grab sample from the in -line sample
port and adds it to a 1-liter bottle to obtain a 24-hour composite sample. The 1-liter bottle is
24

mixed and 145 ml aliquot is poured into a 1-liter bottle for the weekly composite sample. The
weekly composite sample will be stored in a refrigerator until the sample is complete.
The first aliquot of the weekly composite sample is obtained on Tuesday and subsequent daily
aliquots are added through Monday of the following week to create the weekly composite
sample. On Tuesday, the weekly composite sample is delivered to the MMSD Laboratory via
contract courier on ice for volatile solids analysis.
4.C.1.b South Shore Primary Sludge Weekly Composite Analyzed for Volatile Solids Once per
Week
Samples are obtained by the Treatment Plant Operator 4 — Primary Treatment on the lower
level Preliminary Treatment Building 303 from an in -line sample port. The automatic sampler
creates a time composite sample over 24-hours. This 24-hour composite sample is mixed and a
145 ml aliquot is poured into the 1-liter bottle for the weekly composite sample. The weekly
composite sample bottle is stored in a refrigerator until the sample is complete.
The first aliquot of the weekly composite is obtained on Tuesday and subsequent aliquots are
added through Monday of the following week to create weekly composite sample. On Tuesday,
the weekly composite sample is delivered to the MMSD Laboratory via contract courier on ice
for volatiles solids analysis.
4.C.1.c South Shore Waste Activated Sludge Daily Composite Analyzed for Volatile Solids
Three Times per Week
Manual grab time proportional samples are obtained by the Treatment Plant Operator 4 —
Secondary Treatment in the basement of the East Plant and West Plant pipe galleries, Buildings
332 and 331 respectively, from an in -line sample port. Three times per 12-hour shift, the TPO-4
obtains a grab sample from the in -line sample port independently from the East Plant sample
port and the West Plant sample port. After 24 hours, the daily composite sample fills a 1-liter
bottle.
Daily composite samples are started on Monday, Wednesday, and Saturday, at 5:00 a.m. and
are completed at 5:00 a.m. the following day. Samples are sent to the MMSD Laboratory for
analysis on Tuesday, Thursday, and Sunday. Samples are refrigerated during collection and
transported on ice by contract courier service to the MMSD Laboratory. At the MMSD
Laboratory, the two samples, East Plant and West Plant, are combined and analyzed for volatile
solids.
4.C.2 Digester Outlet Total Volatile Solids Sampling and Analysis
For South Shore digested sludge, a weekly composite sample is analyzed for volatile solids once
per week.
A six-inch line and an eight -inch line transports digested sludge from the digesters to the South
Shore wet well, from which this sludge is pumped to Jones Island. Only one line is in service at
any time. Each digested sludge line has an in -line time proportional composite sampler.
Samples are obtained by the Treatment Plant Operator 4 — Secondary Treatment in the
basement of Sludge Thickening Building 358 from an in -line sample port. The automatic
25

sampler creates a time composite sample over 24 hours. Aliquots from the daily composite
sample are used to prepare the weekly composite sample. This weekly composite sample is
stored in a refrigerator until the complete weekly composite sample is obtained. The first
aliquot is obtained on Tuesday and sampling continues through Monday of the following week
to create the weekly composite sample. On Tuesday, the weekly composite sample is sent to
the MMSD Laboratory via contract courier on ice for volatile solids analysis.
Figure 4-3 (p. 32) shows the digested sludge sampling locations.
4.C.3 Volatile Solids Reduction Calculation
Using the outlet volatile solids concentration and a weighted average for the inlet volatile solids
concentrations, a percent reduction is calculated using the Van Kleeck Method (For example,
see Control of pathogens and Vector Attraction in Sewage Sludge, U.S. Environmental
Protection Agency, 2003 Appendix Q.
Where:
%VSR — (V Sin — VSout) x 100
VSi, — VSin X VSout)
%VSR = volatile solids reduction
VSin = fractional volatile solids of raw biosolids fed to digester, kg/kg. For the District,
this value is a weighted average calculated based on daily flow and VS composite
data for JIPSD, SSPSD, and SSWAS.
VSout = fractional volatile solids of digested biosolids, kg/kg
The District will perform this calculation once per week, using weekly data.
4.D Sampling for Pathogens, Chemical Pollutants, and Nutrients
For pathogens, chemical pollutants, and nutrients, the sampling point is at South Shore,
Building 385, the hanger bays for cake storage. This location is Sample Point 005 in the WPDES
permit.
Before land application, the District will grab seven samples from locations throughout the
stored cake. The District will analyze each of these samples for fecal coliform. From each of
the seven samples, the District will mix equal masses from each grab sample into one
composite sample. The District will analyze the composite sample for arsenic, cadmium,
copper, lead, mercury, molybdenum, nickel, selenium, zinc, nitrogen — total Kjeldahl, nitrogen -
ammonia, phosphorus, water extractable phosphorus, potassium, and moisture. Once during
the permit term, the District will analyze cake for PCBs.
If the District intends one land application event involving cake from multiple runs of the
presses, then the District will sample each run separately.
Table 4-1 (p. 33) summarizes filter cake sampling frequency, sample analysis, and the
laboratory performing the analysis.
26

4.E Contingency Plan for Noncompliant Cake
The District will review sample results before land application. If any parameter does not
comply with the applicable limits, then landfill disposal will occur.
27

Figure 4-1
South Shore Cake Storage Bays
W.,

Figure 4-2
Digester Feed Sampling Locations
Figure 4-2A
Jones Island Primary Sludge Sample Location
v A. 8 n 6 ,l a 'it r
29

Figure 4-2B
South Shore Primary Sludge Sample Location
30

Figure 4-2C
South Shore East Plant Waste Activated Sludge Sampling Location
31

A
Figure 4-3
Digested Solids Samplers
fj
32

Table 4-1
South Shore Filter Cake Sampling and Analysis
Parameter
Sample
Sample Type
Analytical
Laboratory
Frequency*
Method
As, Cd, Cu, K, Mo, Ni, P, Pb, Se, Zn
Before land
Manual composite from seven grab
EPA 6010C
District
application
samples
Hg
Before land
Manual composite from seven grab
EPA 7471B
Contract
application
samples
PCB Aroclors
Once per permit
Manual composite from seven grab
EPA 8082
Contract
term
samples
Nitrogen, ammonia
Before land
Manual composite from seven grab
AOAC 2.065
District
application
samples
Nitrogen, total Kjeldahl
Before land
Manual composite from seven grab
AOAC 955.04
District
application
samples
Phosphorus, water extractable
Before land
Manual composite from seven grab
DNR/Penn State
District
application
samples
Total volatile solids
Before land
Grab
SM 2540G
District
application
Moisture
Before land
Manual composite from seven grab
SM 2540G
District
application
samples
Fecal Coliform
Before land
Seven grab samples
EPA 1680
District
application
*Filter cake production is unscheduled and unpredictable. To test equipment, production occurs at least once per year for one week or less.
Production may occur at other times if necessary to reduce solids levels. Production from each run is segregated during storage before land
application. The District samples each production run before land application. For example, if land application involves two production runs,
each run would be sampled separately. Land application occurs only after results are received and reviewed to confirm compliance.
33

5. Jones Island Filter Press Cake
At Jones Island, the District can send cake from belt filter presses out of the north side of the
dewatering and drying facility. The twelve north belt filter presses can dewater sludge to
approximately 18% solids. A series of three belt conveyers can divert cake from the normal
process path, bypassing the north dryers, and send the cake out the north side of the dewatering
and drying building. The cake drops into trucks for transport to a landfill.
The District would use this option only if equipment issues or chemical contamination prevent
beneficial reuse. Therefore, from this location, the District will send cake only to a landfill.
Figure 5-1 (p. 35) shows the truck loading chute. This location is Sample Point 010 in the WPDES
permit.
If this option is used, then the District will grab a sample of cake for moisture; arsenic, cadmium,
copper, lead, mercury, molybdenum, nickel, selenium, and zinc; and any other parameters
required by the landfill.
During a test run on February 21, 2019, pressed cake from the north belt filter presses was
discharged out the north side of the building into trucks destined for landfill. Approximately
131.3 wet tons at about 16% solids was generated over a 6-hour period. Samples were taken
before the test run of the equipment and analyzed to create a profile for the landfill. Also,
samples were taken during the February 21 test run and analyzed for PCBs to satisfy the
requirement in sec. 7.2.6.6 of the WPDES permit to analyze the filter press cake for total PCBs
once during 2019.
The District is planning to design and construct a similar system for the south side of the
dewatering and drying building.
34

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!A
mok
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mm
im

6. Quality Assurance and Quality Control
6.A Product Quality
As described above, the District will use sampling and analysis to evaluate compliance with the
applicable requirements. Samples move to the laboratory and results move from analysts to
process management staff according to the following steps.
1. When samples arrive, laboratory staff will thoroughly review them for proper
identification, documentation, proper preservation, proper containers, and compliance
with other requirements. The Chain of Custody will document this review. Any anomalies
will be addressed before analysis.
2. Before samples are shipped to other laboratories for analysis, laboratory staff will prepare
and ship the samples according to all applicable method and Chain of Custody procedures.
3. In all cases, analysts will have all required training completed and documented before
performing analyses.
4. All analytical results will be reviewed by a peer or supervisor for conformance to quality
assurance and quality control specifications.
Peer -reviewed results are then uploaded into the Laboratory Information Management
System (LIMS), an electronic repository of analytical data.
6. For moisture analysis, laboratory analysts will monitor daily results. Analysts will alert
laboratory management when a moisture content of a Milorganite° fertilizer sample
exceeds 10%. Laboratory management will inform the Contract Compliance Office of the
exceedance. The Contract Compliance Office will collaborate with Veolia to achieve
compliance. The response may include additional testing, segregation, reprocessing, or
other action.
7. Results from LIMS are automatically transferred to a Hach Water Information
Management Solution (WIMS) database, an electronic repository of analytical data, at
periodic intervals throughout the day. District and Veolia personnel use Hach WIMS for
operational and compliance information.
8. The Contract Compliance Office will review results as they become available, comparing
the results to permit and contract limits.
9. The laboratory will prepare and distribute monthly reports that contain analytical results,
including data qualifiers, detection limits, and comments. The Contract Compliance Office
and the Legal Services Department will review these reports before the District provides
the results to the Wisconsin Department of Natural Resources or other states.
W.

6.13. Product Temperature Data Quality Review
1. The temperature measuring devices installed in the dryers and recycle bins transmit the
measured temperatures on a real-time basis to displays that operators continuously
monitor.
2. Also, operators continuously monitor the recycle bin detention time and the required
temperature to demonstrate compliance with time and temperature requirements.
3. All the temperature monitoring devices are maintained by the Veolia maintenance
personnel per the equipment O&M manual.
4. The District's SCADA system stores this information and then the data is transferred to
Hach WIMS data management software as 15-minute averages.
5. The 15-minute average temperatures are compiled in graphs and sent to the Contract
Compliance and Veolia staff daily for review.
6. The Contract Compliance Office will notify and discuss with Veolia of any excursions or
abnormalities in the data.
7. Veolia staff will investigate any excursions or abnormalities in the data and document
them.
8. The District will compile the temperature data, along with the operation observation
notes, in monthly Milorganite° fertilizer compliance Reports.
6.0 Laboratory Quality Assurance and Quality Control
The MMSD Central Laboratory operates under a quality system that applies to all samples
received and analyzed at the laboratory. The Central Laboratory analyzes samples for fecal
coliform, nutrients, solids, metals, and physical characteristics. Contract laboratories analyze
organic contaminants and specialized inorganic parameters.
The MMSD Central Laboratory and the laboratories analyzing biosolids under contract will comply
with the hold times required by 40 CFR Part 503.8, 40 CFR Part 136, and the Wisconsin
Administrative Code, Chapter NR 219. The Central Laboratory and the laboratories under
contract will provide appropriate containers and preservatives to sample collectors.
Veolia Water Milwaukee or Contract Compliance Office staff sample Milorganite° fertilizer and
the District other biosolids. Personnel from the MMSD Central Laboratory do not collect samples.
However, after collection and receipt, Central Laboratory staff may send samples to a contract
laboratory for analyses the Central Laboratory does not perform.
The Central Laboratory is certified or accredited by the Wisconsin Department of Natural
Resources (DNR); the Wisconsin Department of Agriculture, Trade, and Consumer Protection; and
the Florida Department of Health, according to the NELAC Institute (TNI) Standard (National
Environmental Laboratory Accreditation Program (NELAP)). The laboratories receiving and
analyzing samples under contract for organic compounds and specialized inorganic parameters
operate under verifiable quality systems and are certified, at a minimum, by the Wisconsin DNR,
as applicable for the parameters analyzed. In most cases, contract laboratories are also
accredited to the TNI Standard (NELAP), a recognized national standard.
37

Quality assurance and quality control procedures for the Central Laboratory are summarized in a
comprehensive Quality Manual. The procedures in the Manual are complemented by Standard
Operating Procedures (SOPs) and Quality Control Summary Sheets. The following appendices
describe the Central Laboratory's quality system in more detail.
• Appendix 5: MMSD Central Laboratory Quality Manual
• Appendix 6: Quality Control Requirement Summary Sheet Examples
• Appendix 7: Sample Receiving Standard Operating Procedure
• Appendix 8: Chain of Custody Templates
• Appendix 9: Summary of Biosolids Analytical Methods, Holding Times, Preservation, and
Frequency of Analysis
Documents describing the quality systems of laboratories under contract can be procured and
submitted on request.
W.

Appendix 1
Standards for the Use and Disposal of Sewage Sludge
40 CFR 503 (Excerpts)
Sampling and Analysis (503.8)
Pollutant Limits (503.13)
Record Keeping (503.17
Pathogen Reduction (503.32)
Vector Attraction Reduction (503.33)
Appendix B.B.2

40 CFR 503.8 Sampling and analysis.
(a) Sampling. Representative samples of sewage sludge that is applied to the land, placed on a
surface disposal site, or fired in a sewage sludge incinerator shall be collected and analyzed.
(b) Methods. The materials listed below are incorporated by reference in this part. These
incorporations by reference were approved by the Director of the Federal Register in
accordance with 5 U.S.C. 552(a) and 1 CFR part 51. The materials are incorporated as they
exist on the date of approval and notice of any change in these materials will be published in
the Federal Register. They are available for inspection at the HQ Water Docket Center,
EPA/DC, EPA West, Room B102, 1301 Constitution Ave., NW., Washington, DC, and at the
National Archives and Records Administration (NARA). For information on the availability
of this material at NARA, call 202-741-6030, or go to:
hqp://www.archives.gov/federal register/code_of federal regulations/ibr locations.html.
Copies may be obtained from the standard producer or publisher listed in the regulation. The
methods in the materials listed below (or in 40 CFR part 136) shall be used to analyze
samples of sewage sludge.
(1) Enteric viruses. ASTM Designation: D 4994-89, "Standard Practice for Recovery of
Viruses From Wastewater Sludges", 1992 Annual Book of ASTM Standards: Section
11 - Water and Environmental Technology, ASTM, 1916 Race Street, Philadelphia,
PA 19103-1187.
(2) Fecal coliform. Part 9221 E. or Part 9222 D., "Standard Methods for the Examination
of Water and Wastewater", 18th Edition, 1992, American Public Health Association,
1015 15th Street, NW., Washington, DC 20005.
(3) Helminth ova. Yanko, W.A., "Occurrence of Pathogens in Distribution and Marketing
Municipal Sludges", EPA 600/1-87-014, 1987. National Technical Information
Service, 5285 Port Royal Road, Springfield, Virginia 22161 (PB 88-154273/AS).
(4) Inorganic pollutants. "Test Methods for Evaluating Solid Waste, Physical/Chemical
Methods", EPA Publication SW-846, Second Edition (1982) with Updates I (April
1984) and II (April 1985) and Third Edition (November 1986) with Revision I
(December 1987). Second Edition and Updates I and II are available from the
National Technical Information Service, 5285 Port Royal Road, Springfield, Virginia
22161 (PB-87-120-291). Third Edition and Revision I are available from
Superintendent of Documents, Government Printing Office, 941 North Capitol Street,
NE., Washington, DC 20002 (Document Number 955-001-00000-1).
(5) Salmonella sp. bacteria. Part 9260 D., "Standard Methods for the Examination of
Water and Wastewater", 18th Edition, 1992, American Public Health Association,
1015 15th Street, NW., Washington, DC 20005; or Kenner, B.A. and H.P. Clark,
"Detection and enumeration of Salmonella and Pseudomonas aeruginosa", Journal of
the Water Pollution Control Federation, Vol. 46, no. 9, September 1974, pp. 2163-
2171. Water Environment Federation, 601 Wythe Street, Alexandria, Virginia 22314.

(6) Specific oxygen uptake rate. Part 2710 B., "Standard Methods for the Examination of
Water and Wastewater", 18th Edition, 1992, American Public Health Association,
1015 15th Street, NW., Washington, DC 20005.
(7) Total, fixed, and volatile solids. Part 2540 G., "Standard Methods for the Examination
of Water and Wastewater", 18th Edition, 1992, American Public Health Association,
1015 15th Street, NW., Washington, DC 20005.
40 CFR 503.13 Pollutant limits.
(a) Sewage sludge.
(1) Bulk sewage sludge or sewage sludge sold or given away in a bag or other container
shall not be applied to the land if the concentration of any pollutant in the sewage
sludge exceeds the ceiling concentration for the pollutant in Table 1 of § 503.13.
(2) If bulk sewage sludge is applied to agricultural land, forest, a public contact site, or a
reclamation site, either:
(i) The cumulative loading rate for each pollutant shall not exceed the cumulative
pollutant loading rate for the pollutant in Table 2 of § 503.13; or
(ii) The concentration of each pollutant in the sewage sludge shall not exceed the
concentration for the pollutant in Table 3 of § 503.13.
(3) If bulk sewage sludge is applied to a lawn or a home garden, the concentration of each
pollutant in the sewage sludge shall not exceed the concentration for the pollutant in
Table 3 of § 503.13.
(4) If sewage sludge is sold or given away in a bag or other container for application to
the land, either:
(i) The concentration of each pollutant in the sewage sludge shall not exceed the
concentration for the pollutant in Table 3 of § 503.13; or
(ii) The product of the concentration of each pollutant in the sewage sludge and
the annual whole sludge application rate for the sewage sludge shall not cause
the annual pollutant loading rate for the pollutant in Table 4 of § 503.13 to be
exceeded. The procedure used to determine the annual whole sludge
application rate is presented in appendix A of this part.
(b) Pollutant concentrations and loading rates - sewage sludge -
(1) Ceiling concentrations.

TABLE 1 OF § 503.13 - CEILING CONCENTRATIONS
Pollutant Ceiling concentration
(milligrams per kilogram) 1
Arsenic 75 1
Cadmium E— 85 —:1
Copper 4300
Lead 840
Mercury C 57
Molybdenum C 75
Nickel � 420
Selenium 100
Zinc C 7500
1 Dry weight basis.
(2) Cumulative pollutant loading rates.
TABLE 2 OF § 503.13 - CUMULATIVE POLLUTANT LOADING RATES
Pollutant L2m
ulative pollutant loading rate
(kilograms per hectare)
Arsenic C 41
Cadmium C 39
Copper 1500
Lead 300
Mercury 17
Nickel 420
[Selenium ]� 100
[Zinc F-- - 2800

(3) Pollutant concentrations.
TABLE 3 OF § 503.13 - POLLUTANT CONCENTRATIONS
[Pollutant
Monthly average concentration
11 (milligrams per kilogram) 1
Arsenic
-� 41
J
FCadmium
] 39
Lcopper
]= 1500
[Lead
300
[Mercury
]C 17
—:1
[Nickel
]C 420
Selenium
100
[ Zinc�C 2800
1 Dry weight basis.
(4) Annual pollutant loading rates.
TABLE 4 OF § 503.13 - ANNUAL POLLUTANT LOADING RATES
Pollutant Annual pollutant loading rate
IL (kilograms per hectare per 365 day period)
Arsenic —1E 2.0
Cadmium IF 1.9
Copper
Lead
Mercury
Nickel
Seleniu
Zinc
75
15
0.85
21
5.0
140

40 CFR 503.17 Recordkeeping
(a) Sewage sludge.
(1) The person who prepares the sewage sludge in § 503.10(b)(1) or (e) shall develop the
following information and shall retain the information for five years:
(i) The concentration of each pollutant listed in Table 3 of § 503.13 in the sewage
sludge.
(ii) The following certification statement:
I certify, under penalty of law, that the information that will be used to
determine compliance with the Class A pathogen requirements in § 503.32(a)
and the vector attraction reduction requirement in [insert one of the vector
attraction reduction requirements in § 503.33(b)(1) through § 503.33(b)(8)]
was prepared under my direction and supervision in accordance with the
system designed to ensure that qualified personnel properly gather and
evaluate this information. I am aware that there are significant penalties for
false certification including the possibility of fine and imprisonment.
(iii) A description of how the Class A pathogen requirements in § 503.32(a) are
met.
(iv) A description of how one of the vector attraction reduction requirements in §
503.33 (b)(1) through (b)(8) is met.
40 CFR 503.32 Pathogens.
(a) Sewage sludge - Class A.
(1) The requirement in § 503.32(a)(2) and the requirements in either § 503.32(a)(3),
(a)(4), (a)(5), (a)(6), (a)(7), or (a)(8) shall be met for a sewage sludge to be classified
Class A with respect to pathogens.
(2) The Class A pathogen requirements in § 503.32 (a)(3) through (a)(8) shall be met
either prior to meeting or at the same time the vector attraction reduction
requirements in § 503.33, except the vector attraction reduction requirements in §
503.33 (b)(6) through (b)(8), are met.
(3) Class A - Alternative 1.
(i) Either the density of fecal coliform in the sewage sludge shall be less than
1000 Most Probable Number per gram of total solids (dry weight basis), or the
density of Salmonella sp. bacteria in the sewage sludge shall be less than three
Most Probable Number per four grams of total solids (dry weight basis) at the
time the sewage sludge is used or disposed; at the time the sewage sludge is
prepared for sale or give away in a bag or other container for application to the
land; or at the time the sewage sludge or material derived from sewage sludge
is prepared to meet the requirements in § 503.10 (b), (c), (e), or (f).

(ii) The temperature of the sewage sludge that is used or disposed shall be
maintained at a specific value for a period of time.
(A) When the percent solids of the sewage sludge is seven percent or
higher, the temperature of the sewage sludge shall be 50 degrees
Celsius or higher; the time period shall be 20 minutes or longer; and
the temperature and time period shall be determined using equation
(2), except when small particles of sewage sludge are heated by either
warmed gases or an immiscible liquid.
131, 700, 000
D = 100.1400r
Where,
D = time in days.
t = temperature in degrees Celsius.
(B) When the percent solids of the sewage sludge is seven percent or
higher and small particles of sewage sludge are heated by either
warmed gases or an immiscible liquid, the temperature of the sewage
sludge shall be 50 degrees Celsius or higher; the time period shall be
15 seconds or longer; and the temperature and time period shall be
determined using equation (2).
(C) When the percent solids of the sewage sludge is less than seven
percent and the time period is at least 15 seconds, but less than 30
minutes, the temperature and time period shall be determined using
equation (2).
(D) When the percent solids of the sewage sludge is less than seven
percent; the temperature of the sewage sludge is 50 degrees Celsius or
higher; and the time period is 30 minutes or longer, the temperature
and time period shall be determined using equation (3).
50, 070, 000
= 100.14001
Where,
D = time in days.
t = temperature in degrees Celsius.
(6) Class A - Alternative 4.
(i) Either the density of fecal coliform in the sewage sludge shall be less than
1000 Most Probable Number per gram of total solids (dry weight basis), or the

density of Salmonella sp. bacteria in the sewage sludge shall be less than three
Most Probable Number per four grams of total solids (dry weight basis) at the
time the sewage sludge is used or disposed; at the time the sewage sludge is
prepared for sale or give away in a bag or other container for application to the
land; or at the time the sewage sludge or material derived from sewage sludge
is prepared to meet the requirements in § 503.10(b), (c), (e), or (f).
(ii) The density of enteric viruses in the sewage sludge shall be less than one
Plaque -forming Unit per four grams of total solids (dry weight basis) at the
time the sewage sludge is used or disposed; at the time the sewage sludge is
prepared for sale or give away in a bag or other container for application to
the land; or at the time the sewage sludge or material derived from sewage
sludge is prepared to meet the requirements in § 503.10(b), (c), (e), or (f),
unless otherwise specified by the permitting authority.
(iii) The density of viable helminth ova in the sewage sludge shall be less than
one per four grams of total solids (dry weight basis) at the time the sewage
sludge is used or disposed; at the time the sewage sludge is prepared for sale
or give away in a bag or other container for application to the land; or at the
time the sewage sludge or material derived from sewage sludge is prepared to
meet the requirements in § 503.10 (b), (c), (e), or (f), unless otherwise
specified by the permitting authority.
(7) Class A - Alternative 5.
(i) Either the density of fecal coliform in the sewage sludge shall be less than
1000 Most Probable Number per gram of total solids (dry weight basis), or the
density of Salmonella, sp. bacteria in the sewage sludge shall be less than three
Most Probable Number per four grams of total solids (dry weight basis) at the
time the sewage sludge is used or disposed; at the time the sewage sludge is
prepared for sale or given away in a bag or other container for application to
the land; or at the time the sewage sludge or material derived from sewage
sludge is prepared to meet the requirements in § 503.10(b), (c), (e), or (f).
(ii) Sewage sludge that is used or disposed shall be treated in one of the Processes
to Further Reduce Pathogens described in appendix B of this part.
(b) Sewage sludge - Class B.
(1)
(i) The requirements in either § 503.32(b)(2), (b)(3), or (b)(4) shall be met for a
sewage sludge to be classified Class B with respect to pathogens.
(ii) The site restrictions in § 503.32(b)(5) shall be met when sewage sludge that
meets the Class B pathogen requirements in § 503.32(b)(2), (b)(3), or (b)(4) is
applied to the land.

(2) Class B - Alternative 1.
(i) Seven representative samples of the sewage sludge that is used or disposed
shall be collected.
(ii) The geometric mean of the density of fecal coliform in the samples collected
in paragraph (b)(2)(i) of this section shall be less than either 2,000,000 Most
Probable Number per gram of total solids (dry weight basis) or 2,000,000
Colony Forming Units per gram of total solids (dry weight basis).
40 CFR 503.33 Vector attraction reduction.
(a)
(b)
(1) One of the vector attraction reduction requirements in § 503.33 (b)(1) through (b)(10)
shall be met when bulk sewage sludge is applied to agricultural land, forest, a public
contact site, or a reclamation site.
(3) One of the vector attraction reduction requirements in § 503.33 (b)(1) through (b)(8)
shall be met when sewage sludge is sold or given away in a bag or other container for
application to the land.
(1) The mass of volatile solids in the sewage sludge shall be reduced by a minimum of 38
percent (see calculation procedures in "Environmental Regulations and Technology -
Control of Pathogens and Vector Attraction in Sewage Sludge", EPA-625/R-92/013,
1992, U.S. Environmental Protection Agency, Cincinnati, Ohio 45268).
(7) The percent solids of sewage sludge that does not contain unstabilized solids
generated in a primary wastewater treatment process shall be equal to or greater than
75 percent based on the moisture content and total solids prior to mixing with other
materials.
Appendix B to Part 503 - Pathogen Treatment Processes
B. Processes to Further Reduce Pathogens (PFRP)
2. Heat drying - Sewage sludge is dried by direct or indirect contact with hot gases to reduce the
moisture content of the sewage sludge to 10 percent or lower. Either the temperature of the
sewage sludge particles exceeds 80 degrees Celsius or the wet bulb temperature of the gas in
contact with the sewage sludge as the sewage sludge leaves the dryer exceeds 80 degrees
Celsius.

Appendix 2
Domestic Sewage Sludge Management
Wis. Adm. Code, Chapter NR 204 (Excerpts)
Metal Concentrations (NR 204.07(5))
Pathogen Reduction (NR 204.07(6))
Vector Attraction Reduction (NR 204.07(7))
Sludge Management Plan (NR 204.11)

NR 204.07 Land application of sludge
(5) METAL CONCENTRATIONS.
(a) Table 1 lists the ceiling concentrations of metal pollutants for sludge that is land
applied. Sludge may not be applied to land if the concentration of pollutants in the
sludge exceeds any of the ceiling concentration limits established in Table 1. Options
available if a ceiling concentration in sludge is exceeded include: retesting, mixing
with another sludge or other material and demonstration of compliance with Table 1,
landfilling or incinerating.
(b) Table 2 lists the cumulative metal pollutant loading limits for sites on which bulk
sludge is applied. If bulk sludge is applied to land and the sludge does not meet the
pollutant concentration limits in Table 3, then the limits in Table 2 shall apply to all
land application sites. Bulk sludge that does not meet the Table 3 concentration limits
may not be applied to sites where the cumulative pollutant loading limits in Table 2
have been reached. When bulk sludge that does not meet Table 3 limits is applied to
land, the permittee shall monitor and retain cumulative pollutant loadings records to
each site, and shall notify the department, in their annual report, when any site
reaches 90% of the allowable cumulative loading for any metal established in Table
2.
(c) Sludge shall meet all the pollutant concentration limits established in Table 3, to be
considered high quality. High quality sludge is exempt from the cumulative loading
limits specified in par. (b).
TABLE 1
CEILING CONCENTRATIONS
Ceiling concentration
Pollutant (milligrams per kilogram - ppm)
(dry weight)
Arsenic � 75
Cadmium 85
Copper C 4300
Lead
840
Mercury 57
Molybdenum 75
[Nickel 420
[Selenium 100

Zinc �C 7500
TABLE 2
LIFETIME CUMULATIVE METAL LOADINGS
Pollutant
Arsenic
Cadmium C
Copper C
Lead C
Mercury
Molybdenum Deleted
Nickel
SeleniumC
kg/ha lbs/ac
41 � 36
39 �C 34
1500 1339
300 268
17 15
Until EPA Revises
420 375
100 89
Note: The department strongly encourages permittees to produce sludge which meets the high
quality pollutant concentration limits set in Table 3.
TABLE 3
POLLUTANT CONCENTRATIONS
Monthly average concentration
Pollutant (milligrams per kilogram -
ppm) (dry weight)
Arsenic 7 41
FCadmium 1C 39
Copper 1500
[ Lead ] 300
L Mercury —1 17
[Molybdenum ] Deleted Until EPA Revises
Nickel 420
Selenium 100

(d)
Zinc 1 2800
1. Table 4 lists the maximum annual pollutant loading rates for sites where
bagged sludge that is not high quality is land applied. If bagged sludge does
not meet all of the pollutant concentrations in Table 3, the pollutant loading
requirements in Table 4 apply to all land application sites utilized, including
lawns and home gardens. To ensure that the annual pollutant loading rates in
Table 4 are not exceeded, the amount of sludge applied annually shall be less
than the annual sludge application rate calculated as follows:
ASAR = (APLR)/(C X 0.001)
Where:
ASAR = Annual sludge application rate in metric tons per hectare per 365-
day period calculated on a dry weight basis
APLR = Annual pollutant loading rate for a pollutant in kilograms per
hectare per 365-day period, as state in Table 4.
C = Pollutant concentration in milligrams per kilogram of total solids
calculated on a dry weight basis.
0.001 = A conversion factor.
2. When distributing bagged sludge that is subject to the Table 4 loading rates,
the permittee shall provide an information sheet to each person receiving the
bagged sludge or shall print instructions on the bag or container or label. The
label instructions or information sheet shall contain the following information,
at a minimum:
a. The name and address of the permittee who generated the sludge.
b. A statement that prohibits the use of the sludge except in accordance
with the instructions on the label or information sheet.
c. An annual sludge application rate as calculated in this subsection that
will ensure that the annual pollutant loading rate limits, established in
Table 4, are not exceeded.
d. The percentage content of nitrogen, phosphorus and potassium present
in the sludge.

TABLE 4
ANNUAL POLLUTANT LOADING RATES
Pollutant kg/ha E lbs/ac
Arsenic 2.0 E 1.78�
Cadmium
1.9 1.69
Copper
] 75 C 66.9
Lead
15 E 13.4
Mercury
0.85 F 0.76
CMolybdenurn
Deleted Until EPA Revises
[Nickel
21 �F 18.7
Elenium
—1 5.0 4.4
Zinc
140
F 125
(6) PATHOGEN DENSITIES AND TREATMENT PROCESSES. Sludge may not be land applied unless
the Class A pathogen requirements in par. (a) or the Class B pathogen requirements in par.
(b) are satisfied. These requirements are summarized in Tables 5 and 6. Bagged sludge and
exceptional quality sludge shall satisfy the Class A requirements in par. (a).
(a) One of the requirements in each subds. 1. And 2. Shall be met for sludge to be
classified as Class A. Class A requirements shall be met prior to or at the time of
meeting the vector attraction reduction requirements specified in sub. (7), unless the
process used to meet the vector requirements is one of either sub. (7) (f), (g) or (h).
Class A requirements are summarized in Table 5:
1. Pathogen or indicator organism densities. The required fecal coliform density
or salmonella density shall be satisfied immediately after the treatment
process in subd. 2. Is completed. If the material is bagged or distributed at that
time, no re -testing is required. If the material is bagged, distributed or land
applied at a later time, the sludge shall be retested and the requirements of
subd. 1. A. or b. satisfied at that time also, to ensure that regrowth of the
organisms has not occurred.
a. The sludge shall have a fecal coliform density equal to or less than
1,000 most probable number (MPN) per gram of total solids on a dry
weight basis. Compliance with this requirement shall be demonstrated
by calculating the geometric mean of at least 7 separate samples; or

b. The sludge shall have a salmonella density equal to or less than 3 MPN
per 4 grams of total solids on a dry weight basis; and
2. Pathogen treatment processes.
a. Satisfy the requirements as specified in 40 CFR 503.32 (a). 40 CFR
503.32 (a) as stated on January 1, 1996 is incorporated by reference; or
Note: Copies of this section are available for inspection in the offices of
the department of natural resources, secretary of state, and the legislative
reference bureau, Madison, Wisconsin, or may be purchased from the
superintendent of documents, U.S. government printing office,
Washington DC 20402.
c. Dry the sludge by direct or indirect contact with hot gases to reduce the
moisture content of the sludge to 10% or lower. Either the temperature
of the sewage sludge particles shall exceed 80' C or the wet bulb
temperature of the gas in contact with the sludge as the sludge leaves
the dryer shall exceed 80' C; or
(b) Either subd. 1. Or one of the requirements in subd. 2. Shall be met for the sludge to
be classified as Class B. The Class B requirements are summarized in Table 6:
1. Fecal coliform density. The sludge shall have a fecal coliform density of less
than or equal to 2,000,000 most probable number (MPN) or colony forming
units (CFU) per gram of total solids on a dry weight basis. Compliance with
this requirement shall be demonstrated by calculating the geometric mean of
at least 7 separate samples;
(7) VECTOR ATTRACTION REDUCTION. Sludge may not be land applied unless one of the 11
vector attraction reduction options in pars. (a) to (k) is satisfied. Paragraphs (a) to (i) are
processes which treat the sludge to reduce its attraction to vectors. Bagged sludge and
exceptional quality sludge shall satisfy one of the requirements in pars. (a) to (i). The
options are summarized in Table 7.
(a) The mass of volatile solids in the sludge shall be reduced by a minimum of 38%
between the time the sludge enters the digestion process and the time it either exits
the digester or a storage facility;
(g) Dry the sludge to 75% total solids when the sludge contains no unstabilized solids
from primary treatment;
NR 204.11 Sludge management plan
(1) GENERAL. The department may require the permittee to develop a sludge management
plan, submit the plan to the department for approval and operate in compliance with the
approved plan. The plan shall include a description of the facility's sludge management
program and how the permittee plans to operate the facility in compliance with the
requirements of this chapter.

Appendix 3
Milwaukee Metropolitan Sewerage District
Laboratory Certifications and Accreditations

State of Wisconsin
Department of Natural Resources
recognizes
Wisconsin Certification under NR 149
of
Milwaukee Metropolitan Sewerage District
Laboratory Id: 241325920
as a laboratory licensed to perform environmental sample analysis in
support of covered environmental programs (ch. NR149.02 Note) for the
parameter(s) specified in the attached Scope of Accreditation.
August 31, 2019
Expiration Date
August 1, 2018
" Issued on
Steven Geis, Chief
Environmental Science Services
Daniel L. Meyer, Secretary
Department of Natural Resources
This certiFcatedoes not guarantee validity of data generated, but indicates the methodology, equipment, quality
control practices, records, and proficiency of the laboratory have been reviewed and found to satisfy the
requirements ofch. NR 149, Wis. Adm. Code.

Scope of Accreditation
Milwaukee Metropolitan Sewerage District
250 West Seeboth Street
Milwaukee, WI 53204
Laboratory Id: 241325920
Expiration Date: 08/31/19
Issued Hate: 08/01/18
Wisconsin Certification underNR 149
Matrix: Aqueous (Non -potable Water)
Class: General Chemistry
Alkalinity by Colorimelry
Ammonia as N by Colorimerry
Ammonia as N by 1SE
Ammonia as N by Tilralion
Biochemical Oxygen Demand (SOT]) by S-d Assay
Carbonaceous Oxygen Demand (cBOD) by 3-d Assay
Chemical Oxygen Demand (COD) byCoiorimelry
Chloride by Colarimerry
Chlorophyll by Colorimerry
HEM (0i1&Grease, Hexane Ext. Material (HEM)) by
Grav-HEM
Hardness, Total as CaCO3 by 1CP
KjeldshI Nitrogen, Total by Calorimerry
Nitrate byColorimelry
Nitrite by Colorimelry
Organic Carbon, Total (TOC) by Comb•Ox
Phosphorus, Total byColorimefry
Residue, Non fiIto rahle (TSS) byGrav
Residue, Total byOrav
Residue, Volatile (TVS) by Gray
Residue, Volatile, NanfiIterable JVSS) by Grin
SOT -HEM (Silica Gel Treated HEM) by Gruv-HEAL
Sulfide by Tilralion
Class: Metals
Antimony by 1CP
Arsenic by 1CP
Beryllium by 1CP
Cadmium by 1CP
Calcium by ICP
Chromium (Total) by1CP
Cobalt by 1CP
Copper by 1CP
[run by 1CP
Lead by 1CP
Magnesium by 1CP
Manganese by 1CP
Molytrdenum by 1CP
Nicks) by 1CP
Selenium by 1CP
Silver by 1CP
Thallium by 1CP
Tin by1CP
Titanium by 1CP
Vanadium by 1CP
Zinc by 1CP
Page 1 of l
The laboratory named above is hereby licensed under eh. NR 149, W is. Adm. Code for the parameters listed in this attachment.
Analyte groups are defined and listed at http:: dnr.wi-Soy by searching keywords "Lab Certification:".

Scope of Accreditation
Milwaukee Metropolitan Sewerage District Laboratory Id: 241325920
250 West Seebotb Street Expiration Date: 08/31/19
Milwaukee, WI 53204 issued Date: 09/01/18
Wisconsin Certification under NR 149
Matrix: Solid (Waste, Soil & Tissue)
Class: General Chemistry
Ammonia as N by Tllrallon
Chloride byColorlmelry
Phosphorus, Total by 1CP
Residue, Total by Gran
Class: Metals
Aluminum by 1CP
Antimony by 1CP
Arsenic by 1CP
Barium by 1CP
Beryllium by1CP
Cadmium by 1CP
Calcium by ICP
Chromium (Total) by 1CP
Cobalt by ICP
Copper by 1CP
Iron by 1CP
Lead by 1CP
Magnesium by ICP
Manganese by 1CP
Molybdenum by 1CP
Nickel by 1CP
Potassium by 1CP
Selenium by 1CP
Silver by 1CP
Thallium by1CP
Tin by 1CP
Titanium by 1CP
Vanadium by ICP
Zinc by 1CP
Page 1 of I
The laboratory named above is hereby licensed under ch. NR 149, Wis. Adm. Code for the parameters listed in this attachment.
0 Analyte groups are defined and listed at http: dnr.wLgov by searching key wards "Lab Certifieatian:".

Wisconsin Department of Agriculture, Trade and Consumer Protection
2811 Agriculture Drim PO Box 8911. Madison, WI 53708-8911
License Number.115088-133
Expires: December 31, 2019
Statute: 93.12
Milk, Fond and Water Lab
Legal Name:
M M 8 D Lab Services Central Lab
250 W Seeboth St Mliwaukee WI 53204-1446
Certificate of Approval
Wisconsin Laboratory plumber 158
DFRS:
Enzymatic Substrate, Industry Supervisor
Doing Business As:
M M S C Lab Services Central Lab
Stardfard Water Tests:
Coiilert or Calilert 18, LTH or PA #allowed by 13GLB & EC OR EC+MUG, mFC agar (fecal conform, SWfR only),
Quanffray
This k yqr timm IM. FOU or Cans' as raquirad by law. NondransfwmlAe • anhj d 10 ravocaWn or suspension as provided by to
X-4mws des and w O&W.IdenlMkailonz
D. -BT-%s(o3nivffn b16.R.7(r OV15I
M M 8 Q Lab Servioes Central Lab
Alin: On W*den
250 W Ssebc4h St
PAMwaulee Wt 59204
DATCP Contact: [phone]
RR1cnmi� �I Yf
A;Fwl.. TicdC.11f1 Rw«umI
nnrrrnnrrnn�rrrnnnrNrunsurnamunN
rmrmun�ra�uimurd riurrrnnrnn�� ruun

ar! 1`I Lid
HEALTH
State of Florida
Department of Health, Bureau of Public Health Laboratories
This is to certify that
E571010
MILWAUKEE METROPOLFTAN SEWERAGE DISTRICT
250 WEST SEEBOTH STREET
MILWAUKEE. WI 53204-1446
has compiled with Florida Administrative Code 64E-1,
for the examination of environmental samples in the following categories
NON­POTAaLE WATER -GENERAL CHEMISTRY, NON -POTABLE WATER -METALS. NON -POTABLE WATER - MICROBIOLOGY, SOWdAND
CHEMICAL MATERIALS - GENERAL CHEMISTRY. SOLID AND CHEMICAL MATERIALS - METALS, SOLID AND CHEMICAL MATERIALS -
MICROBIOLOGY
Continued certification is c mUn ent upon successful on -going compliance with the NELAC Standards and FAG Rule 64E•1
regulations. Specific methods and analytes ceRffied are cited on the Laboratory Scope of Accreditation for this laboratory and
are on file at the Bureau of Pubiic health Laboratories, P. O. Box 210. Jacksolnnlle, Florida 32231. Clients and customers are
urged to verify with this agency the la3b6 atoryj'S1er'dfIcWbh Status In Florida for particular methods and analytes.
Date Issued: August 24, 2018
i
��W
Expiration Date: June 30, 2019
Patty A. L elfin; irn ski, MBA, MT(ASCP)
Chief Bureau of Public Health Laribratorles
OH Form 1697,7AM
NON -TRANSFERABLE E5710WZ OW24=8
Supersedes all previously Issued certificates

AIMIL
Rich scwt
Caletlle Philip, AMR MPH
Governor
St de
Surgeon General
Laboratory Scope ofAccredltadorr
Page t of 2
Attachment to Cert skate #: E571010-26, expiration date June 30, 2019. This listing of accredited
analytes should be used only when associated with a valid certificate.
State Laboratory ID. E571010
EPA Lab Code: W 101t019
(414) 2774384
E571010
Milwaukee Metropolitan Sewerage District
230 West Seebeth Street
Milwaukee, W1 $3204-14"
Matrix: Non -Potable Water
Certif atba
Asa"
Me11 wfftelt
Catgery
TYPI
Effective Hate
Antawks as N
SM e50WNH31)119th,
Gears! Chumimy
NELAP
1211/20"
20tk 21 it Ed jA SE
Attuiwtsy
EPA 2007
Meters
NELAP
8l312018
Arume
EPA 200.7
Metals
NELAP
IV317013
Beachpad oxygen demand
SM 5210 n
Gercral Chemisey
NELAP
7/112007
Cadmtvt
EPA 200 7
Meals
NELAP
IU312018
Chmmaao
EPA 2007
Metals
NELAP
813i2018
Cobalt
EPA 200.7
Mews
NELAP
W311019
Copper
EPA 200.7
Metals
NELAP
8/3/2018
Fecal enitfnrms
SM 9222 D
MKrobioSogy
NELAP
7/1/2007
Hexane Exhwlable MMcml - Silica Gel Treated
EPA 16MB
General Chemistry
NELAP
8131Y01a
(HEM-SGTy
Ldd
EPA 200.7
Meals
NELAP
BOWS
Mwtgartese
EPA 200.7
Mews
NELAP
8/3(2018
Moybdawtt
EPA 200 7
Mews
NELAP
SIMON
Nukes
EPA 200 7
Mews
NELAP
81)(2019
Nttrern as N
EPA 353.2
General Chemtstry
NELAP
7/1/2007
Nitrite n N
EPA 353.2
General Chemistry
NELAP
MOW
Oil & Crease
EPA 1664A
Gawel Chemtsny
NELAP
7/112007
lytosphorM tons
EPA 365 l
Grr eral Chemistry
NELAP
7/1/2007
Selemuns
EPA200.7
Metals
NELAP
8/3/2013
SiWef
EPA 200.7
Melats
NELAP
9/ 12018
Tin
EPA ".7
McW3
NELAP
8l312018
Timm
EPA 2007
Metals
NELAP
9007018
Tout mrtraL rote
EPA 353 2
General Chemistry
NELAP
7/1/2007
vamw1wri
EPA 200.7
!dents
NELAP
8/3/2018
lute
EPA 2001
Mews
NELAP
IM2018
Ciieuts and Cuatomas are urged to verify the laboratory's current eerdllestion stator with
the finvirenntettal Laboratory Certification Program, issue Date: 8f2412013 Expiration Date: 6/M019

Ride 3eoH Celeste Ph1Ap, MD, MPH
GDvemor Stata surgeon General
Laboratory Scope ojAccredhadon Pap 2 of 2
Attachment to Certificate A: E571010-26, expiration date June 30, 2019. This listing of rteeredited
analytes should be used only when anociated with a valid certifkate.
State Laboratory ID: E571010 EPA Lab Code: WIM19 [phone]
E571010
Willwanicee Mdrtspaiitan Sewe"Ce District
256 Wall Seeboth Street
Milwaukee, WI 53204-1446
Mod=: Solid and Chem lent Materials
Certlficatlen
Aealyte
Melhodfreeh
Catepry
Type
Eirective Date
Aluminum
EPA6010
Metals
NELAP
moll
Arsenic
EPA6010
Meals
NELAP
7M007
Cadmium
EPA6010
Mewls
NELAP
IM007
Calcium
EPA6010
Metals
NELAP
7MOD7
Chromium
EPA6010
me"
NELAP
7Nl2007
Cobalt
EPA6010
Metals
NELAP
7Nf2007
Copper
EPA 6D10
Mewls
NELAP
7MOD7
Wei eoldorms
EPA 16110
Microbiology
NELAP
tV31201S
Iron
EPA 6010
Metals
NELAP
7n/2007
Lead
EPA6010
Meals
NELAP
T1912OD7
Magnesium
EPA6010
Mewls
NELAP
7n=7
Manganese
EPA6010
Meals
NaAP
719720D7
Molybdenum
EPA6010
Metals
NELAP
7MOD7
Nickel
EPA6010
Meals
NELAP
7N72OD7
PH
EPA9045
GerffwC'hemistry
NELAP
711rM7
Phasplwrus, tDtal
EPA6010
Meals
NELAP
019WO
Ponutum
EPA6010
Meals
NELAP
7Nl2007
Residue -fixed
SM 2340 G
General Chemistry
NELAP
W112007
Residuatote]
SM 2540 G
Crcrerd Chemistry
NELAP
711f2OD7
Reslduo-rolelde
SM 2MO G
General Chemistry
NELAP
711=
Selermlm
EPA 6010
Metals
NELAP
7N12007
'11 Whom
EPA 6010
Metals
NELAP
7N12007
Zinc
EPA 6010
Metals
NELAP
7Nf2t.107
Clients and Customers are arZed to verify the laboratory's current etrlillatlan status with
the Enviroo mental LaboratoryCertifkation Proilmen. issue Date: V24f2019 Expiration Date: 613012019

Appendix 4
Dioxin Toxic Equivalency Factors for
Dioxins, Furans, and PCB Congeners
CAS Number
Congener
Toxic Equivalency Factor
EPA
Maine
1746-01-6
2,3,7,8 - Tetrachlorodibenzo-p-dioxin
1.0
1.0
40321-76-4
1,2,3,7,8 - Pentachlorodibenzo-p-dioxin
1.0
0.5
39227-28-6
1,2,3,4,7,8 - Hexachlorodibenzo-p-dioxin
0.1
0.1
57653-85-7
1,2,3,6,7,8 - Hexachlorodibenzo-p-dioxin
0.1
0.1
19408-74-3
1,2,3,7,8,9 - Hexachlorodibenzo-p-dioxin
0.1
0.1
35822-46-9
1,2,3,4,6,7,8 - Heptachlorodibenzo-p-dioxin
0.01
0.01
3268-87-9
1,2,3,4,6,7,8,9 - Octachlorodibenzo-p-dioxin
0.0001
0.001
51207-31-9
2,3,7,8 - Tetrachlorodibenzofuran
0.1
0.1
57117-41-6
1,2,3,7,8 - Pentachlorodibenzofuran
0.05
0.05
57117-31-4
2,3,4,7,8 - Pentachlorodibenzofuran
0.5
0.5
70648-26-9
1,2,3,4,7,8 - Hexachlorodibenzofuran
0.1
0.1
57117-44-9
1,2,3,6,7,8 - Hexachlorodibenzofuran
0.1
0.1
72918-21-9
1,2,3,7,8,9 - Hexachlorodibenzofuran
0.1
0.1
60851-34-5
2,3,4,6,7,8 - Hexachlorodibenzofuran
0.1
0.1
67562-39-4
1,2,3,4,6,7,8 - Heptachlorodibenzofuran
0.01
0.01
55673-89-7
1,2,3,4,7,8,9 - Heptachlorodibenzofuran
0.01
0.01
39001-02-0
1,2,3,4,6,7,8,9 - Octachlorodibenzofuran
0.0001
0.001
32598-13-3
3,3',4,4' - Tetrachlorobiphenyl
0.0001
0.0005
70362-50-4
3,4,4',5 - Tetra chlorobiphenyl
0.0001
57465-28-8
3,3',4,4',5 - Pentachlorobiphenyl
0.1
0.1
32598-14-4
2,3,3',4,4' - Pentachlorobiphenyl
0.0001
0.0001
31508-00-6
2,3',4,4',5 - Pentachlorobiphenyl
0.0001
0.0001
65510-44-3
2',3,4,4',5 - Pentachlorobiphenyl
0.0001
0.0001
74472-37-0
2,3,4,4',5 - Pentachlorobiphenyl
0.0005
0.0005
32774-16-6
3,3',4,4',5,5' - Hexachlorobiphenyl
0.01
0.01
38380-08-4
2,3,3',4,4',5 -Hexachlorobiphenyl
0.0005
0.0005
69782-90-7
2,3,3',4,4',5' - Hexachlorobiphenyl
0.0005
0.0005
52663-72-6
2,3',4,4',5,5' -Hexachlorobiphenyl
0.00001
0.00001
39635-31-9
2,3,3',4,4',5,5' - Heptachlorobiphenyl
0.0001
0.0001
35065-30-6
2,2',3,3',4,4',5 -Heptachlorobiphenyl
0.0001
69782-91-8
2,2',3,4,4',5,5' -Heptachlorobiphenyl
0.0001

Appendix 5
Milwaukee Metropolitan Sewerage District
Central Laboratory Quality Manual

Milwaukee Metropolitan Sewerage District
Central Laboratory
260 W. Seeboth Street
Milwaukee, WI 53204
QUALITY MANUAL
Version 11.0 January 2019
J
Alfredo Sotomayor —Labo to anager
[phone] f
Jessica Nanes — Laboratory Team Supervisor
[phone]
Richard Vincent — Laboratory Team Supervisor
[phone]
Kim Walden — Quality Assurance Specialist
[phone]
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or . ////q
Date
Date
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Date
jz312,019
Date

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TABLE OF CONTENTS
1.0 POLICY STATEMENT
2.0 GLOSSARY AND TERMS USED
Quality Manual
MMSD Central Laboratory
Revision: 11.0
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3.0 ORGANIZATION AND RESPONSIBILITIES
3.1 Organization Chart
3.2 Central Laboratory Organizational Structure and Relationships
3.3 Communication Processes within the Laboratory
3.4 Training
3.5 Laboratory Capabilities
4.0 QUALITY ASSURANCE OBJECTIVES
4.1 Precision
4.2 Accuracy
4.3 Representativeness
4.4 Completeness
4.5 Comparability
4.6 Detection limits
5.0
SAMPLE HANDLING
5.1
Sample Tracking
5.2
Sample Acceptance Policy
5.3
Sample Receipt Protocols
5.4
Storage Conditions
5.5
Chain of Custody
5.6
Sample Transport
5.7
Sample Disposal
6.0 CALIBRATION PROCEDURES AND FREQUENCY
6.1 Traceability of Calibration
6.2 Reference Standards
6.3 General Requirements
6.4 Analytical Support Equipment
6.5 Instrument Calibration
7.0 TEST METHODS AND STANDARD OPERATING PROCEDURES
7.1 Protocol Specifications
8.0 INTERNAL QUALITY CONTROL CHECKS
8.1 Laboratory Quality Control Samples
8.2 Method Detection Limits
8.3 Demonstration of Method Capability
9.0 DATA REDUCTION, REVIEW, REPORTING AND RECORDS
9.1 Data Reduction and Review
9.2 Control of Data
9.3 Records
9.4 Document Control System
9.5 Confidentiality
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10.0 REVIEW OF NEW WORK, CUSTOMER COMMUNICATIONS, AND COMPLAINTS
10.1 New Work
10.2 Customer Communications
10.3 Complaints
11.0 PERFORMANCE AND SYSTEM AUDITS
11.1 Internal Laboratory Audits
11.2 External Audits
11.3 Managerial Review
12.0 EQUIPMENT, MEASUREMENT TRACEABILITY, STANDARDS AND REAGENTS,
AND PREVENTATIVE MAINTENANCE
12.1 Equipment
12.2 Support Equipment
12.3 Glassware Cleaning
12.4 Measurement Traceability
12.5 Reference Materials
12.6 Documentation and Labeling of Standards and Reagents
12.7 Preventative Maintenance
13.0 SPECIFIC ROUTINE PROCEDURES USED TO EVALUATE DATA QUALITY
13.1 Laboratory Control Samples
13.2 Matrix Spikes/Matrix Spike Duplicates
13.3 Method Blanks
13.4 Estimation of Uncertainty
14.0 CORRECTIVE ACTION
15.0 PROCUREMENT
15.1 Subcontracting Laboratory Services
15.2 Purchasing Procedures
16.0 CERTIFICATIONS AND ACCREDITATIONS
APPENDICES
APPENDIX A — Demonstration of Capability Documentation
APPENDIX B — Deionized Water Monitoring Requirements
APPENDIX C — Laboratory Services Notification Form
APPENDIX D — Methods Available from MMSD Laboratory
APPENDIX E — Request for Analytical Services Form
APPENDIX F — Authorized Signatories MMSD Central Laboratory
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1.0 POLICY STATEMENT
This Quality Manual summarizes the policies and operational procedures associated with the Milwaukee
Metropolitan Sewerage District's (MMSD or District) Central Laboratory. Specific protocols for sample
handling and storage, chain -of -custody, laboratory analyses, data reduction, corrective action, and
reporting are described. All policies and procedures have been structured in accordance with the
applicable requirements of the Wisconsin Department of Natural Resources (WDNR), Wisconsin
Administrative Code, Chapter NR149, and the NELAC Institute's (TNI) 2009 Standard. Further details
on these policies and procedures may be contained in Standard Operating Procedures (SOPS) and related
documents. Departures from these documented policies and procedures or from standard specifications
are allowed only with the express permission of the Laboratory Manager or his designee.
Through the application of these policies and procedures, the laboratory assures that it is impartial and
that personnel are free from undue commercial, financial, or other pressures that might influence their
technical judgment. The laboratory is responsible for carrying out testing activities that meet the
requirements of the TNI Standard and WDNR Chapter NR 149, as applicable, and the needs of its clients.
This Quality Manual, SOPS, and related documentation describe the quality (management) system for
MMSD's Central Laboratory. Where the Quality Manual documents laboratory requirements, a separate
SOP or policy is not required unless further detail is needed. Other policies and procedures relating to
laboratory quality assurance/quality control (QA/QC) that augment the manual will be found in the
laboratory section of the MMSD SharePoint site.
The Central Laboratory is a part of the Milwaukee Metropolitan Sewerage District. Its responsibility is to
provide quality laboratory services that meet the District's need for environmental, product, and process
testing. The laboratory does not provide testing services for outside entities unless these are part of
District projects or initiatives.
The District's mission is to cost-effectively protect public health and the environment, and to
prevent pollution and enhance the quality of area waterways.
The goals of the Central Laboratory are:
• To produce data that is scientifically valid, defensible, and of known and documented quality in
accordance with standards developed by the WDNR and any applicable state or Environmental
Protection Agency (EPA) regulations or requirements;
• Provide prompt and professional service to clients;
• Maintain a working environment that fosters open communication with both clients and staff,
• Build continuous improvement mechanisms into all laboratory functions.
Each member of the staff plays a part in meeting these goals. If the laboratory is to achieve the objectives
of the management system, all team members must perform their work in a way that meets the
requirements of the Quality Manual and follow applicable policies and procedures.
The trained staff within the Central Laboratory provides analytical testing which includes wet chemistry,
microbiology, metals analysis, physical, and compositional testing. Most of the samples analyzed are
aqueous matrices or biosolids.
The objectives of this Quality Manual are to:
• Provide a consistent documented policy that will be applicable to daily laboratory operations;
• Ensure reliability of performance of all sections of the laboratory;
• Ensure compliance with all applicable state and federal regulations.
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The Quality Manual describes documentation needed so that the Central Laboratory achieves a uniform
total quality approach.
The Central Laboratory is committed to producing the highest quality data and professional laboratory
services for its clients. Because of this commitment, all personnel are directed to practice the policies
presented in this Quality Manual. Every time there is a revision, all laboratory employees sign a form,
kept with their training records, that states that they have read and understood the Quality Manual.
The Quality Manual is maintained current and up-to-date by the Quality Assurance Specialist (QAS) and
the Laboratory Manager.
The Central Laboratory is supports a proactive program for prevention and detection of improper,
unethical or illegal actions. Internal proficiency testing; analyst training; post -analysis data review by
Laboratory Team Supervisors and the QAS; and ethics policies and training both at the District and
laboratory level are part of the tools that are used to achieve this. In addition to ongoing surveillance, the
following are performed:
• All new employees have ethics as part of their documented orientation training.
• Externally developed courses and reviews as they are available, or internally created
presentations are offered to all laboratory staff annually. Training offered is documented.
• The QAS includes a review to detect improper practices in her annual systems review.
2.0 GLOSSARY AND TERMS USED
Quality control terms are generally defined within the section that describes the activity.
Glossary
Terms that are used in the TNI Standard are defined in section 3.0 of each of the reference modules.
These are the normative definitions for the laboratory. Method specific terms are defined in SOPS. Other
terms are defined in NR 149 and NR 219.
Acronyms
A list of acronyms used in this and other laboratory documents includes the following:
ANSI
American National Standards Institute
ASTM
American Society for Testing and Materials
°C
Degrees Celsius
CAS
Chemical Abstract Service
CCV
Continuing calibration verification
COC
Chain of custody
CHO
Chemical Hygiene Officer
CHP
Chemical Hygiene Plan
DO
Dissolved oxygen
DOC
Demonstration of Capability
EPA
Environmental Protection Agency
GW
Groundwater
JI or JIWRF
Jones Island Wastewater Reclamation Facility
ICP-OES
Inductively -coupled plasma optical emission spectroscopy
ICV
Initial calibration verification
IMAC
Internal Microbiology Analyst Certification
IW
Industrial waste Uncontrolled Document
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IWPP
Industrial Waste Pretreatment Program
LCS
Laboratory control sample
MDL
Method detection limit
MPN
Most probable number
MS
Matrix spike
MSD
Matrix spike duplicate
NELAP
National Environmental Laboratory Accreditation Program
NIST
National Institute of Standards and Technology
PT
Proficiency Test, Proficiency Testing
QA
Quality Assurance
QC
Quality Control
QAS
Quality Assurance Specialist
RL
Reporting Limit
RPD
Relative percent difference
RSD
Relative standard deviation
SS or SSWRF South Shore Wastewater Reclamation Facility
SOPS
Standard operating procedures
TNI
The NELAC Institute
UV
Ultraviolet
VOC
Volatile organic compound
WQP
Water Quality Protection Division
WDNR
Wisconsin Department of Natural Resources
WDATCP
Wisconsin Department of Agriculture, Trade, and Consumer Protection
WET
Whole effluent toxicity
3.0 ORGANIZATION AND RESPONSIBILITIES
3.1 Organization Chart
The Central Laboratory is part of the District's Water Quality Protection Division (WQP). The
relationship of the laboratory and the WQP to the organization is shown in Figure 3-1. An organization
chart for the laboratory is shown in Figure 3-2. The Human Resources Department maintains job
descriptions for all laboratory personnel.
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Figure 3-1
Milwaukee Metropolitan Sewerage District Organization Chart
Human Resources
Commission
Office of the Executive
Director
Information
Technology
Services
Legal Services Technical Services planning, Research, Water Quality
and 5ustainability I Protection
Engineering Research & Central
Services Laboratory
Capital Program
Business
Administration
Industrial Waste,
Water Quality
Research, &
Conveyance
System Monitoring
Office of Contract
Compliance
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Executive Director
Cost Center
Finance
Agency Services
,Accounting
Facilities
Management
Office of Graphics
Management a nd
Budget
Marketing &
Milorganikes
Office of Business
& Community
Engagement
Records
Management

Quality Manual
MMSD Central Laboratory
Revision: 11.0
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Figure 3-2:
MMSD CENTRAL LABORATORY ORGANIZATION CHART
Director of
Water Quality Protection
Laboratory Administrative
Manager Assistant
Laboratory Quality
LIMS Database Laboratory Team Laboratory Team
Project Assurance
Manager Analyst Supervisor Supervisor Specialist
Laboratory Laboratory Tech
Helper Chemistry (4)
Laboratory Tech
Chemistry (6)
Chemist (3)
Microbiologist
3.2 Central Laboratory Organizational Structure and Relationships
Each laboratory employee has an important role to play in achieving the objectives of the management
system. The quality of our data rests on the checks and balances created by our quality system and the
commitment to that system by all staff. The responsibilities of the key members of the organization, as
they relate to quality management, are outlined below.
During the summer months, the laboratory employs student interns that work with permanent staff to gain
knowledge of laboratory procedures and help meet the higher demand for analyses during the season.
One of the chemistry technicians is the laboratory's designated Chemical Hygiene Officer (CHO). The
responsibilities of the CHO are described in the MMSD Central Laboratory's Chemical Hygiene Plan (.
3.2.1 Laboratory Manager
Under the direction of the Director of Water Quality Protection Division, the Laboratory Manager
provides the overall management, strategic direction, and coordination of the laboratory functions and
their outcomes, in accordance with District policies and procedures. The Laboratory Manager's
responsibilities include:
Managing staff to ensure quality, accurate and on time completion of the laboratory functions.
Monitoring employee performance and reviewing implementation of training initiatives to ensure
compliance with established processes and procedures.
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• Monitoring and directing improvements in technical systems to ensure efficient and effective
flow of scientific data and reporting.
• Implementing and monitoring the laboratory's operations through key performance indicators to
ensure compliance with established processes and procedures.
• Directing development and monitoring of all SOPS and laboratory related functions to ensure they
are compatible with District needs and goals.
• Recommending improvements and coordinating staff training in laboratory processes and
functions.
• Monitoring the development of specifications, acquisitions, and implementation of all new
technologies utilized by the laboratory.
• Establishing and monitoring agreements with contract laboratories as necessary.
• Overseeing the maintenance and implementation of the current laboratory certifications and
accreditations, including WDNR, Wisconsin Department of Agriculture, Trade, and Consumer
Protection (WDATCP), and NELAP processes and procedures to ensure meeting established
guidelines and deadlines.
• Reviewing, at least annually, its management and quality systems to ensure continuing suitability
and effectiveness and to introduce any necessary changes or improvements.
• Planning, implementing, and monitoring the cost center's Operations and Maintenance budget to
ensure compliance with established policies and procedures.
• Ensuring organizational compliance with all local, state and federal regulatory agencies.
• Ensuring the training of new and current employees.
• Ensuring compliance with all safety and work rules and regulations, and the maintenance of
departmental housekeeping standards.
• Approving the Quality Manual and SOPS.
• Maintaining a working environment which encourages open, constructive problem solving and
continuous improvement.
3.2.2 Laboratory Quality Assurance Specialist
The QAS is not directly involved in day-to-day operations and reports directly to the Laboratory
Manager. The QAS serves as the focal point for QA/QC. She is responsible for auditing the
implementation of the Quality System and has sufficient authority to stop work as deemed necessary in
the event of serious QA/QC issues. The QAS specific functions and duties include:
• Maintaining laboratory certification through the proficiency testing program, timely submittal of
applications and other required paperwork, and auditing reports to ensure compliance with
established processes and procedures.
• Reviewing the quality of data reported to verify that it is documented as appropriate and as
required by the Quality Manual and applicable certification and accreditation requirements.
• Identifying analytical methods for use in the laboratory in accordance with state and federal
regulations and permits.
• Reviewing contract laboratory data and potential laboratories for use.
• Investigating, identifying, and recommending corrective action for significant quality problems in
the laboratory to ensure compliance with established processes and procedures.
• Working with MMSD staff and contractors to provide guidance on proper sampling and
preservation methods.
• Working with laboratory management to maintain, approve, and implement the Laboratory
Quality Manual.
• Approving laboratory SOPS.
• Providing Quality Systems training to all new personnel.
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Assisting in identifying appropriate resolution of complaints received from clients involving data
quality issues.
Monitoring data quality measures by statistical methods to verify that the laboratory routinely
meets stated quality goals.
Maintaining the laboratory Quality Systems records as appropriate, including laboratory SOPS,
analytical training records, data pertaining to certification and accreditation, method validation,
method detection limits (MDLs), proficiency testing, and analysts' demonstrations of capability
(DOCs).
3.2.3 Laboratory Team Supervisors
Under the direction of the Laboratory Manager, the Laboratory Team Supervisors are responsible for the
overall allocation of staff and resources of their respective teams to accomplish all the laboratory analysis
and operations assigned, in accordance with District policies and procedures. Their responsibilities
include:
• Establishing and supervising a system for scheduling daily work to meet customer needs,
including overtime and weekend work.
• Establishing and supervising a system to ensure the timely reporting of data per customer
requirements.
• Implementing and supervising a system to ensure that teams are adequately cross -trained for
coverage in all areas, weekend work, and special needs.
• Ensuring that all team members are adequately trained and have demonstrated capabilities for
which they are responsible and that such demonstration is documented.
• Ensuring that the quality of all data reported by the laboratory is documented.
• Reviewing data reports as assigned.
• Ensuring all sample acceptance criteria are verified and that samples are logged into the sample
tracking system, properly labeled and stored.
• Evaluating overall teams' performance and contributions of individual team members.
• Interacting with team members to ensure that assigned team processes are continually evaluated
and improved if necessary.
• Overseeing and directing teams on methods development and their implementation.
• Assisting in maintaining QA/QC systems.
• Administering District and department policies and handling personnel issues.
• Assisting in developing the annual laboratory budget and monitoring and assisting in purchasing
items required by teams.
• Recommending acquisitions of equipment and laboratory consumables, and overseeing the
selection, installation, and use of such items within the laboratory.
• Ensuring the training of new and current employees in the process and methods required to
achieve the District standards for quality, quantity, and safety, consistent with the District's
principles.
• Maintaining technical competency and remaining current in technology and changes in the
industry.
• Ensuring compliance with all required records, paperwork, and documents.
• Ensuring compliance with all safety and work rules and regulations.
• Ensuring the maintenance of departmental housekeeping standards.
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3.2.4 Laboratory Project Manager
Under the direction of the Laboratory Manager, the Laboratory Project Manager works with laboratory
staff and clients to direct laboratory projects in accordance with District policies and procedures. The
position's duties include:
• Serving as the primary laboratory customer contact and working with customers to define the
scope of service and reporting requirements.
• Coordinating requests for services with analytical staff.
• Providing feedback to management on changing customer needs.
• Coordinating activities with contract laboratories.
• Verifying or validating contract laboratory data.
• Preparing and distributing laboratory reports to customers and agencies.
• Enabling feedback necessary to ensure customer satisfaction.
• Maintaining the laboratory's final data report files.
3.2.5 Technical Staff
The technical staff is responsible for analyzing samples and identifying corrective actions. All personnel
are responsible for complying with all QA/QC requirements that pertain to their organizational and
technical functions. As documented in employee records, technical staff members have the experience
and education to fulfill their analytical functions and a general knowledge of laboratory operations, test
methods, QA/QC procedures, and records management.
The following sections briefly summarize the job duties of the laboratory technical staff. Complete job
descriptions are kept by MMSD Human Resources.
3.2.5.1 Chemist
The position's duties include:
• Reporting to the Team Supervisor in charge of their respective area.
• Performing analytical methods and data recording in accordance with documented procedures.
• Performing and documenting calibration and preventive maintenance.
• Implementing and performing data processing and data review procedures.
• Evaluating the preparation and maintenance of laboratory records.
• Evaluating instrument performance and overseeing the calibration, preventive maintenance, and
scheduling of repairs.
• Reporting nonconformance to Team Supervisors and the QAS as appropriate.
• Meeting the quality requirements defined in this Quality Manual and other supporting QA
policies and procedures.
3.2.5.2 Microbiologist
The position's duties include:
• Reporting to the Team Supervisor in charge of their respective area.
• Performing analytical methods and data recording in accordance with documented procedures.
• Performing microscopic examinations and interpreting them to District staff and customers.
• Implementing and performing data processing and data review procedures.
• Evaluating the preparation and maintenance of laboratory records.
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• Evaluating instrument performance and overseeing the calibration, preventive maintenance, and
scheduling of repairs.
• Reporting nonconformance to the Team Supervisors and QAS as appropriate.
• Meeting the quality requirements defined in this Quality Manual and other supporting QA
policies and procedures.
3.2.5.3 Laboratory Technician
The position's duties include:
• Reporting to the Team Supervisor in charge of their respective area.
• Performing analytical methods and data recording in accordance with documented procedures.
• Performing and document calibration and preventive maintenance.
• Performing data processing and data review procedures.
• Reporting nonconformance to the Team Supervisors and QAS as appropriate.
• Meeting the quality requirements defined in this Quality Manual and other supporting QA
policies and procedures.
3.2.5.4 Laboratory Helper
The position's duties include:
• Reporting to the Team Supervisor in charge of their respective area.
• Washing labware in mechanical dishwashers in accordance with established procedures.
• Preparing sample containers for sampling activities as needed.
• Maintaining inventory of supplies for labware cleaning area.
• Cleaning and maintaining mechanical dishwashers.
• Assisting all laboratory sections as directed.
3.2.6 Laboratory Information Management System (LIMS) Database Analyst
The position's duties include:
• Providing services to support the management of laboratory documentation and data.
• Designing, programming, and maintaining electronic data uploads from various sources into
LIMS and from LIMS to other databases.
• Performing queries of historical laboratory databases.
• Preparing and maintaining laboratory data reports and other data transmittals (electronic).
• Monitoring ongoing data transmittals and data archival activities.
3.2.7 LIMS Senior Systems Analyst
This position is part of the District's Information Technology Services (ITS) Department but works
closely with laboratory personnel. The position's duties include:
• Providing system and database analysis and design for the LIMS.
• Working with District ITS, contractors and other staff to integrate LIMS data into other databases
and reports outside of the laboratory.
• Taking the lead in electronic and hard copy report development for laboratory data; translating
customer requests for electronic and hard copy reports into LIMS deliverables.
• Developing, implementing, maintaining, and administering the LIMS.
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3.3 Communication Processes within the Laboratory
Effective communication between staff, management, customers, vendors and other involved parties can
and should occur daily to maintain an effective workplace. Many of these interactions are informal and
ad hoc. Management has an open-door policy and staff are encouraged to discuss any concerns and ideas
for improvement with their managers.
Formal processes to ensure that appropriate communication regarding management system updates,
progress reports, policies, procedures and other important information include, but are not limited to, the
following:
• The Laboratory Manager holds a weekly meeting with his staff to discuss workload, analytical
capacity, projected laboratory activities for the week, District initiatives affecting the laboratory,
and any concerns from staff and direct reports.
• Each Team Supervisor holds a monthly team meeting for discussing problems, new procedures,
administrative updates, new technology and other topics specific to operations. These meetings
are meant to be open forums and all staff are encouraged to participate in discussions.
• The Team Supervisors hold joint team meetings to discuss special topics and promote team cross -
communication.
• The Laboratory Manager holds "all hands" meetings as needed to discuss topics such as
assessment findings, new regulations or procedures, provide training, convey internal and global
communication, or to seek feedback and input from the entire laboratory staff.
• The QAS attends each of these meetings to provide QA/QC updates to staff as appropriate.
• The laboratory maintains a dedicated area on the MMSD SharePoint site where laboratory
information is posted and made available to all staff.
3.4 Training
3.4.1 Orientation and Technical Training of Staff
Training is an ongoing activity and is performed to maintain and develop proficiency, and to promote
improvement. Training can be external or internal. Examples of external training include seminars,
courses at academic institutions, vendor -sponsored instrument training, and classes conducted on or off -
site. Internal training includes on-the-job training and seminars given by experienced or trained MMSD
personnel. Laboratory employees are qualified and assigned duties based on experience and training
documented in their training file. Each new employee receives orientation and training in quality, ethics,
and health and safety.
The supervisors will perform periodic assessments to determine training needs. These should include the
input of employees and other managers.
3.4.2 Quality Orientation
Each newly hired MMSD Central Laboratory employee receives a quality systems orientation. The QAS
conducts this orientation within one month of the employee's report -to -work date. Attendance at QA
orientation is documented in the employee's training file. The QAS reviews, at a minimum, the following
topics with the new employee as they apply to the individual's assigned responsibilities:
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• MMSD Quality System and applicable documents including the MMSD Quality Manual.
• MMSD policies on ensuring data integrity, meeting client requirements, and ethics.
• Identification and documentation of nonconformance and corrective action procedures.
• Proper data recording practices.
• Key elements of QC as applied in the laboratory.
Ethics and fraud prevention are components of our employee orientation. This training includes review of
pertinent MMSD administrative documents, and discussions about data integrity, and data
misrepresentation. Employees are made aware of the legal and environmental repercussions that result
from data misrepresentation.
3.4.3 Quality Training
Continued training, consistent with requirements of the Quality Manual is provided regularly. Formal
training sessions may be conducted and documented by the QAS, Laboratory Manager, designee or
external trainers. The training sessions address relevant regulatory requirements, basic QC practices,
responsibilities of the technical and QA staff, and the reporting of nonconformance.
Quality issues are discussed regularly at biweekly team meetings and weekly management meetings.
Additional training as needed is also provided in special meetings.
All MMSD laboratory employees become familiar with the laboratory's quality programs by reading the
MMSD Laboratory Quality Manual, pertinent sections of the Wisconsin Codes, TNI Standard, and SOPS
pertaining to their positions.
3.4.4 Health and Safety Training
Each newly hired laboratory employee is required to receive health and safety training in accordance to
the Laboratory's CHP. The orientation is performed as soon as possible after the employee's report -to -
work date and before the employee handles chemicals. The Laboratory's CHO maintains documentation
of training completion and copies are also included in the employee's training file.
All laboratory staff is given periodic refresher training on various health and safety topics. Attendance
records for these are maintained by the Laboratory CHO. The District also offers general health and
safety training available to all employees. This may include cardio-pulmonary resuscitation (CPR), first
aid, fire safety and other pertinent topics. These training records are maintained by and reside in the
Human Resources Department.
3.4.5 Data Integrity and Ethics Training
Ongoing data integrity training is provided for all laboratory employees. This training may be presented
by either MMSD staff or contractors on site, or by webinars or interactive web -based seminars. Training
will always include management and staff discussion of how the specific material applies to daily work.
Documentation of training is recorded with a signature attendance sheet or form that demonstrates staff
have participated and understand their obligations related to data integrity.
3.4.6 Training Records
The QAS is responsible for setting up and maintaining training records for the entire laboratory. The
types of records in the training files may include documentation of technical (procedural) training, QA
training, proficiency demonstrations, professional development, and any other training related to job
performance. Initial or ongoing technical proficiency training records include documentation of the
ability to perform sample preparation or analysis using internally prepared laboratory control samples and
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when available, external standard reference materials. Personnel are required to demonstrate competency
in performing methods by successfully completing a DOC before conducting analysis independently on
client samples.
Information is filed in the employee's training file as training is completed.
3.4.7 Professional Development
This category includes courses and training relating to an individual's job duties or approved training
plan. This training can be college level courses funded by the District's tuition reimbursement program,
seminars, meetings, and internal courses available for District staff. Records of employee's professional
development training are kept by the Human Resources Department.
3.5 Laboratory Capabilities
The MMSD Central Laboratory provides chemical and microbiological environmental analyses as well as
process and product testing for the various fertilizer products produced at the District. The laboratory has
extensive experience serving the analytical needs of a variety of MMSD internal operations. The
following are the most common types of samples that are analyzed in the District laboratory:
• Wastewater influent, effluent, and samples from various stages of the wastewater treatment process;
• Groundwater;
• Surface water from Milwaukee's watersheds and harbors;
• Industrial wastewater samples from the District's Industrial Waste Pretreatment Program;
• Biosolids (sludge), Milorganite® (a fertilizer produced by the MMSD), and mixed liquors.
This list is not all inclusive and other sample matrices may be analyzed as needed.
Most samples are collected by contractors and MMSD staff who are not part of the laboratory. The
laboratory usually supplies containers and preservatives but does not take an active role in sampling for
most compliance testing.
The MMSD Central Laboratory is certified by the WDNR for analysis of environmental samples, the
WDATCP for microbiology analysis, and by the Florida Department of Health for the NELAP. Copies of
current certifications are posted electronically and in hard copy at the laboratory.
The MMSD Central Laboratory floor plan is shown in Figure 3-3. The 45,000 square foot, two -floor
facility, houses the MMSD Central Laboratory staff and management.
The design of the laboratory ensures data quality, safety, efficiency, automation, and security. Instrument
laboratories are separate from sample preparation laboratories to eliminate the potential for cross -
contamination. The reagent water systems provide water of required quality for all laboratory operations.
Laboratory facilities are designed and organized to facilitate testing of environmental samples.
Environmental conditions are monitored to ensure that conditions do not invalidate results or adversely
affect the required quality of any measurement.
Access to and use of areas affecting the quality of the environmental tests is controlled to authorized
personnel only.
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Figure 3-3
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The laboratory work spaces are adequate, and appropriately clean to support environmental testing and ensure
an unencumbered work area.
The laboratory is divided into two process teams. The Wet Chemistry and Microbiology team handles
glassware preparation, autochemistry, biochemical oxygen demand (BOD), microbiology, and solids. The
Metals and Milorganite team is responsible for metals analysis, oil and grease, sample receiving, nitrogen
analysis, total organic carbon (TOC), chemical oxygen demand (COD), chlorophyll, a variety of physical and
chemical tests on Milorganite, and some plant operation monitoring.
The laboratory operates seven days a week, 365 days a year. Analysts are cross -trained on those analyses that
are provided daily to meet wastewater treatment and production needs.
4.0 QUALITY ASSURANCE OBJECTIVES
The overall QA objective for MMSD's Central Laboratory is to develop and implement procedures for
laboratory analysis, chain -of -custody, and reporting that will provide results which are of known and
documented quality. Data Quality Indicators (DQI) are used as descriptors in interpreting the degree of
acceptability or utility of data. The principal DQIs are precision, accuracy, representativeness, comparability,
and completeness. DQIs are used as quantitative goals for the quality of data generated in the analytical
measurement process. This section summarizes how specific DQIs and QA objectives are met.
4.1 Precision
Precision describes how much random error there is in the measurement process or how reproducible an
analytical technique is. Precision is assessed through the calculation of relative percent differences (RPD) and
relative standard deviations (RSD) for replicate samples. Laboratory precision may be assessed through the
analysis of a matrix spike/matrix spike duplicates (MS/MSD), sample duplicate pairs, or examination of
precision between laboratory control samples (LCS). Laboratory staff monitors ongoing precision using
control charts.
4.2 Accuracy
Accuracy is the degree of agreement between an observed value and an accepted reference or true value.
Accuracy is assessed through the analysis of MS/MSD, QC check samples, and LCSs. It is further assessed by
the analysis of blanks and through the adherence to proper sample handling and preservation procedures and
holding times. Laboratory staff monitor ongoing accuracy using control charts.
4.3 Representativeness
Representativeness expresses the degree to which data accurately and precisely represent a characteristic of a
population, parameter variations at a sampling point, a process condition, or an environmental condition within
a defined spatial or temporal boundary. Lack of representativeness occurs when the sample collection method
does not extract the material from its natural setting in a way that accurately captures the desired qualities to be
measured. It can also occur when improper sub -sampling is done in the laboratory.
4.4 Completeness
Completeness is a measure of the amount of valid data obtained from submitted samples.
The laboratory completeness objective is to generate valid data for greater than 95% of the samples received.
This is measured by tracking the "Lab Services Notifications" for invalid or missing data.
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4.5 Comparability
Comparability is an expression of the confidence with which one data set can be compared to another.
Comparability can be determined by examining the specifications of the measurement system used, that is,
analytical methods, detection limits, holding time compliance, and rules for reporting data. Documentation of
these, and any deviations, is important in determining comparability of data.
4.6 Detection Limits
Method Detection Limit (MDL) is defined as the minimum concentration of a substance that can be measured
and reported with 99% confidence that the analyte concentration is greater than zero and is determined from
analysis of a sample in a given matrix containing the analyte. MDLs are determined, where appropriate,
annually in accordance with the procedure found in Title 40 CFR Part 136.
The Limit of Quantitation (LOQ) is the minimum concentration of an analyte that can be identified and
quantified within specified limits of precision and bias during routine analytical operating conditions. LOQs
are matrix, method, and analyte specific. In some cases, they may be instrument specific. At the Central
Laboratory, they are usually calculated as 10 times the standard deviation of the MDL, and in some
documented cases, as the concentration of the low-level quality control sample or the concentration of the
lowest calibration standard, depending upon the method and customer needs. In all cases, the MDL is less
than the LOQ.
The QAS maintains a standardized worksheet for MDL determinations. All MDLs are reviewed and approved
by the Team Supervisor and QAS before implementation. The QAS is responsible for updating the LIMS with
new MDLs and notifying the appropriate customers of these updates.
In some cases, calculation of an MDL is not appropriate (e.g. BOD and pH determination). In these cases, a
reporting limit not related to a statistical determination will be included in reports.
5.0 SAMPLE HANDLING
This section summarizes policies and practices for sample handling.
5.1 Sample Tracking
The laboratory tracks all samples using unique numbers generated by the LIMS. This process is known as
"sample log -in". Sample numbers may be assigned in the LIMS by laboratory or other MMSD staff who
perform sampling. This assignment may be performed prior to sample collection or when the sample arrives at
the laboratory. Each sample container label will contain a unique identification (ID) code.
5.2 Sample Acceptance Policy
Samples submitted to the laboratory for environmental analysis must meet the requirements of applicable
WDNR regulations and EPA guidelines. When samples are received that do not meet these requirements, the
laboratory documents the nature and substance of the variation. The requirements include:
Proper, full, and complete documentation, including the sample identification, the location, date and
time of collection, collector's name, preservation type, sample type and any special remarks
concerning the sample. In some cases (e.g. freshwater samples) the time of collection will be included
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in the LIMS as a test field for the sample. A chain of custody is submitted for each sample, but
multiple samples can be on a single form;
• Unique identification of samples using durable labels completed in indelible ink;
• Use of appropriate sample containers;
• Appropriate chemical and physical preservation as required by the methods;
• Receipt within holding times;
• Adequate sample volume.
Milorganite submitted for product testing (i.e. shipment testing) will be submitted with complete identification
(lot numbers and dates). Analyses must generally be completed within seven days to meet shipping
requirements.
5.3 Sample Receipt Protocols
Upon receipt, the condition of the sample, including any abnormalities or departures from standard conditions
is recorded. For samples requiring refrigeration on collection that arrive having ice in the cooler, the
laboratory may report the samples as "received on ice". If the samples are not received on ice or the ice has
melted, the laboratory must report the temperature. Generally, a calibrated pyrometer is used for this purpose.
For samples with a specified temperature of 4° C, a temperature ranging from just above the freezing
temperature of water to 6° C is considered acceptable. Samples that are hand -delivered to the laboratory
immediately after collection may not meet these criteria. In these cases, the samples will be considered
acceptable if there is evidence that the chilling process has begun, such as arrival on ice. Further detail on this
is provided in the sample receiving SOP.
Where applicable, chemical preservation will be verified using readily available techniques, such as pH. This
check will be made upon receipt of the sample, unless the integrity of the sample might be compromised by
this additional handling prior to analysis. In those cases, sample preservation will be verified prior to the
analysis. This verification is documented. The preservation status of subcontracted samples is verified by the
subcontract laboratory.
Where there is any doubt as to the sample's suitability for testing, the laboratory will consult its clients for
further instruction before proceeding. If the sample does not meet the sample receipt acceptance criteria, the
condition of the samples will be noted on the chain of custody form and in the LIMS. If the laboratory has to
make a pH adjustment, add some other preservative, or filter the sample, this will be documented.
5.4 Storage Conditions
Samples which require thermal preservation are stored under refrigeration within the specified preservation
temperature of the method and NR 219.04.
Refrigerator and freezer storage temperatures are monitored and documented on each day of use.
Samples are held securely, stored apart from standards, reagents, food, or potentially contaminating sources to
minimize cross -contamination. All portions of samples, including extracts, digestates, leachates, or any
sample products are maintained in accordance with regulatory requirements.
5.5 Chain of Custody (COC)
COC documents are used to establish an intact, continuous record of the physical possession of sample
containers and collected samples. The COC records account for all time periods associated with the samples
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until they arrive at the MMSD laboratory. The COC forms remain with the samples during transport or
shipment.
Access to all samples and sub -samples is controlled. The MMSD facility is maintained securely and is
restricted to authorized personnel only.
5.6 Sample Transport
Samples that are transported under the responsibility of the laboratory are handled safely and in accordance
with required transport and storage conditions. This includes moving bottles within the laboratory.
5.7 Sample Disposal
All samples, digestates, leachates, and extracts or other sample preparation products are disposed of in
accordance with Federal, State, and local laws and regulations.
6.0 CALIBRATION PROCEDURES AND FREQUENCY
6.1 Traceability of Calibration
Wherever applicable, calibration of analytical support equipment and instruments is traceable to national
standards of measurement.
6.2 Reference Standards
Reference standards of measurement (such as Class 1 or equivalent weights, or traceable thermometers) are
generally used for calibration only. Reference standards are subjected to in-service checks between
calibrations and verifications.
6.3 General Requirements
Each calibration is dated and labeled with, or traceable to, the method, instrument, analysis date, analyte name,
concentration, and response (or response factor). Sufficient information is recorded to permit reconstruction of
the calibration. Acceptance criteria for calibrations comply with method requirements or are established and
documented.
6.4 Analytical Support Equipment
Analytical support equipment includes: balances, ovens, refrigerators, freezers, incubators, water baths,
temperature measuring devices and volumetric dispensing devices if quantitative results are dependent on their
accuracy, as in standard preparation and dispensing or dilution into a specified volume. All such support
equipment is calibrated or verified at least annually, using NIST traceable references when available, over the
appropriate range of use. The results of the calibration or verification must be within the specifications
required of the application for which the equipment is used, or the equipment is removed from service until
repaired.
Mechanical volumetric dispensing equipment, including burettes (except Class A glassware), is checked for
accuracy quarterly.
Other volumetric glassware that is not class A is verified before use. The record of that verification is
maintained in the laboratory.
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Glass micro -liter syringes have a certificate attesting to their established accuracy. If the certificate of
accuracy for glass micro -liter syringes is not available, the accuracy of the syringe is demonstrated before use
and documented.
Prior to use on each day the equipment is in operation, balances, ovens, refrigerators, freezers, incubators, and
water baths are checked with NIST traceable references (where possible) in the expected use range. The
acceptability for use or continued use is determined by the analysis or application performed with the
equipment.
Additional information on the calibration of analytical support equipment may be found in SOPS or equipment
manuals.
6.5 Initial Instrument Calibration
Calibration procedures for laboratory instruments consist of an initial calibration and calibration verifications.
The SOP for each analysis performed in the laboratory describes the calibration procedures, frequency,
acceptance criteria, and the conditions that will require recalibration. Where appropriate, the initial calibration
is verified using an independently prepared calibration verification solution made from a second source.
Quantitation is always determined from the initial calibration unless the test method or applicable regulations
require quantitation from the continuing calibration. Unless stated otherwise in the reference method, the
minimum number of points for establishing the initial instrument calibration is three. The lowest calibration
standard shall be at or near the limit of quantitation. Any results obtained above the highest calibration
standard are diluted and reanalyzed. No data should be reported outside of the calibration range without the
review and approval of the Team Supervisor. In those rare cases, the data must be qualified.
If the initial calibration fails, the analysis procedure is stopped and evaluated. For example, a second standard
may be analyzed and evaluated, or a new initial calibration curve may be established and verified. In all cases,
the initial calibration must be acceptable before analyzing any samples.
When an initial instrument calibration is not performed on the day of analysis, a calibration verification check
standard is analyzed at the beginning and at the end of each batch. If a calibration check standard fails, and
routine corrective action procedures fail to produce a second consecutive calibration check within acceptance
criteria, a new initial calibration curve is constructed. The samples affected by the unacceptable check are
reanalyzed after a new calibration curve has been established, evaluated and accepted. Samples may be
reported with qualifiers (flagged) only if reanalysis is not possible because there is limited sample volume or
hold times have expired.
For ICP analysis, where single point calibration is allowed (with a zero and single point calibration), the
following apply:
a) For single point plus zero blank calibrations, the zero point and the single point standard are analyzed
prior to the analysis of samples and verified at the frequency required by the method.
b) The linearity of single point plus zero blank calibrations is determined by analysis of at least three
standards and one of them at a concentration of at least 10% above the calibration standard. The
resulting linear dynamic range is verified at least yearly.
6.6 Continuing Instrument Calibration
The validity of the initial calibration is verified prior to sample analysis by use of an initial calibration
verification (ICV) or a continuing calibration verification (CCV) standard. The ICV is usually is prepared
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from a source different than the one used to generate a calibration curve. The CCV and the calibration
standards share the same source. Corrective action is initiated for continuing instrument calibration
verification results that are outside of acceptance criteria. This is performed for all analytical systems that
have a calibration verification requirement. Calibration is verified for each compound, element, or other
discrete chemical species.
The calculations and associated statistics for calibration verification are included or referenced in the test
method SOP.
Sufficient raw data records are retained to allow reconstruction of the continuing instrument calibration
verification. Continuing instrument calibration verification records connect the continuing verification to the
initial instrument calibration.
7.0 TEST METHODS AND STANDARD OPERATING PROCEDURES
The laboratory SOPS that accurately reflect all laboratory activities including general procedures and specific
test methods. The QAS maintains a list of current SOPS on the District's SharePoint site accessible to all
laboratory personnel. Each SOP indicates its effective date and revision number, and includes the signatures
of the QAS, Laboratory Team Supervisor, and Laboratory Manager. SOPS must be approved by these
authorized personnel prior to use. Copies of the analytical methods are maintained in the individual
laboratories and are accessible to all analysts performing them.
Procedures for test methods describing how the analyses are actually performed in the laboratory are specified
in method SOPS. The SOPS for sample preparation and analysis are based on reference methods published by
EPA, Standard Methods, or other recognized references. Each method SOP includes or references:
i) Identification of the method;
ii) Applicable matrix or matrices ;
iii) MDL and LOQ;
iv) Scope and application, including analytes to be analyzed;
v) Summary of the method;
vi) Definitions (in the SOP or by reference);
vii) Interferences;
viii) Safety;
ix) Equipment and supplies;
x) Reagents and standards;
xi) Sample collection, preservation, shipment and storage;
xii) Quality control;
xiii) Calibration and standardization;
xiv) Procedure;
xv) Data analysis and calculations;
xvi) Method performance;
xvii) Pollution Prevention;
xviii) Data Assessment and acceptable criteria for QC measures;
xix) Corrective actions for out -of -control data;
xx) Contingencies for handling out -of -control data;
xii) Waste management;
xxii) References;
xxiii) Tables, diagrams, flowcharts and validation data
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QC acceptance criteria and corrective actions for each method are contained in the QC Requirements
Summary Sheets Manual, a separate document from the Quality Manual. MDLs, which are reviewed at least
annually, can be found by query in LIMS. A copy of the most recent limits can also be obtained from the
QAS.
SOPS for general laboratory procedures that are not analytical methods, as for example, sample receiving and
thermometer calibration, do not have to include all the sections listed above if they are not applicable to the
procedure.
7.1 Protocol Specifications
For certain analyses related to process control, method and customer -defined specifications are documented in
Protocol Specifications. These do not replace SOPS but rather serve to communicate certain expectations to
both the customer and the analysts. These are written documents that include some technical specifications
such as precision and accuracy goals, and turnaround times, deliverables and communication instructions.
8.0 QUALITY CONTROL VERIFICATION
Individual reference sheets for QA/QC requirements and corrective action for specific analytical methods are
compiled in the QC Requirements Summary Sheets Manual. These are used as a reference at the bench.
8.1 Quality Control Samples
The data acquired from QC analyses are used to estimate the quality of analytical data, determine the need for
corrective action in response to identified deficiencies, and interpret results after corrective action procedures
are implemented. Each method SOP includes a QC section which addresses the minimum QC requirements
for the procedure. The internal QC checks may differ slightly for each individual procedure but in general are
described below.
a) Method Blanks are performed at a frequency of one per batch of samples per matrix type per sample
preparation or test method. The results of these samples are used to determine batch acceptance.
b) Laboratory Control Samples (LCS) are analyzed at a minimum of I per batch of 20 or fewer samples per
matrix type per sample preparation method except for analytes for which spiking solutions are not
available or applicable, such as pH, BOD, and turbidity. The results of these samples are used to
determine batch acceptance.
c) Matrix Spikes (MS) are performed at a frequency of 1 in 20 samples per matrix type per sample
extraction or preparation method except for analytes for which spiking solutions are not available or
applicable such as, total suspended solids, total dissolved solids, total volatile solids, total solids, pH,
BOD and turbidity. Poor performance in a matrix spike generally indicates a problem with sample
composition, and not the laboratory analysis, and is reported to assist in data assessment.
d) Matrix Spike Duplicates (MSD) or Laboratory Duplicates are analyzed at a minimum of 1 in 20 samples
per matrix type per sample preparation or test method. Poor performance in the duplicates generally
indicates a problem with the sample composition and is reported to assist in data assessment.
8.2 Method Detection Limits
For analytes for which spiking is a viable option, detection limits are determined by an MDL study. This is
performed as described in 40 CFR Part 136, Appendix B. The method detection limit is determined for the
compounds of interest in each method in laboratory pure reagent water.
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An MDL study is not performed for any component for which spiking solutions are not available such as total
suspended solids, BOD, total dissolved solids, total volatile solids, total solids, pH, or microbiology
parameters. For these, the detection limit may be based on the signal to noise ratio from the analysis of a
standard, calculated based on manufacturer's guidance (such as the pH probe or analytical balance); or
established with guidance from regulators (e.g. BOD).
MDLs in used are reviewed at least annually for continuing applicability. MDL studies are performed
annually or whenever there is a significant change to an instrument or method. Once the study is performed,
reviewed and approved by the Team Supervisor and QAS, the limits are updated in LIMS and a change
notification is given to customers and analysts.
8.3 Demonstration of Method Capability
Prior to acceptance and use of any method, satisfactory initial demonstration of method performance, referred
to as "Initial Demonstration of Capability" or "IDOC" is required for every analyst performing a method.
Analysts also complete ongoing demonstrations of capability for all tests they perform.
The procedure and forms for the DOCs are contained in Appendix A. These demonstrations are performed
initially when the method is validated, each time there is a significant change in instrument type, personnel, or
test method, and annually as an ongoing demonstration of proficiency.
For microbiological analyses, candidate analysts are certified to perform tests after comparing generated test
results to those of a principal analyst, usually the laboratory Microbiologist.
8.4 Proficiency Testing
MMSD's Central Laboratory analyzes proficiency testing (PT) samples from a provider approved by NELAP
and the WDNR at least two times per year. The specific analytes and matrices analyzed are based on the
current scope of the laboratory services and availability of appropriate PT materials. The specific
requirements for the PT samples are contained in the standards for each certification. The QAS manages the
PT program. Team Supervisors are responsible for scheduling, reporting to the QAS raw data review, and
initiating corrective action, if necessary.
Within the constraints imposed by some certification programs, the laboratory analyzes PT samples following
the same procedures used to analyze routine samples.
The QAS is responsible for keeping records of study dates, results and submittals, including copies of any
electronic submittals sent to the PT provider.
If any PT sample results fail study acceptance criteria, Team Supervisors will work with the QAS to
investigate the cause of the failure and document any corrective action that is taken. Analysis of additional PT
samples will be completed in accordance with the guidelines established by applicable regulatory agencies.
9.0 DATA REDUCTION, REVIEW, REPORTING AND RECORDS
9.1 Data Reduction and Review
Data reduction is performed following documented procedures. Computer programs used for data reduction
are validated before use by performing manual calculations. All information used in the calculations (e.g. raw
data, calibration files) is recorded to enable reconstruction of final results.
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All data are reviewed by a second analyst or supervisor in accordance with laboratory procedures to ensure
that calculations are correct and to detect transcription errors. Spot checks are performed on computer
calculations to verify program validity. Errors detected in the review process are referred to analysts for
corrective action.
9.2 Control of Data
The laboratory assures that computers and software are protected and secure by locked access and control of
the laboratory environment.
The District ITS Department is responsible for maintenance and security of the network, desktops, servers and
stored electronic data.
Commercial off -the -shelf software (e.g. word processing, database and statistical programs) used within the
designed application range is considered sufficiently validated when in-house programming is not used.
The laboratory assures that computers, user -developed computer software, automated equipment, or
microprocessors used for the acquisition, processing, recording, reporting, storage, or retrieval of
environmental test data are:
a) Documented in sufficient detail and validated as being adequate for use;
b) Protected for integrity and confidentiality of data entry or collection, data storage, data transmission
and data processing;
c) Maintained to ensure proper functioning and are provided with the environmental and operating
conditions necessary to maintain the integrity of environmental test data;
d) Held secure, including the prevention of unauthorized access to, and the unauthorized amendment of,
computer records.
9.3 Records
Records provide the direct evidence and support for the necessary technical interpretations, judgments, and
decisions concerning laboratory results. These records provide the historical evidence needed for subsequent
reviews and analyses. Records should be legible, identifiable, and retrievable, and protected against damage,
deterioration, or loss. All records are maintained in accordance with the District's Records Retention Policy.
Original data records are retained for a minimum of five years. The laboratory follows applicable District
procedures and policies for records archival and disposal.
Any documentation errors are corrected by drawing a single line, in ink, through the error so that it remains
legible, and is initialed by the responsible individual, along with the date of change. The correction is written
adjacent to the error.
The laboratory complies with District policies on electronic signatures, records handling, and other applicable
records requirements.
Laboratory records include the following:
SOPS — Any revisions to laboratory procedures are written, dated, and distributed to all relevant individuals to
ensure implementation of changes. Current copies of all SOPS are maintained on the MMSD SharePoint site.
Equipment Maintenance Documentation — A history of the maintenance record of each equipment serves as an
indication of the adequacy of maintenance schedules and part inventory. As appropriate, the maintenance
guidelines of the equipment manufacturer are followed. When maintenance is necessary, it is documented in
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either standard forms or in hardcopy or electronic logbooks. Maintenance records from external services or
vendors are also kept on file.
Calibration Records — The frequency, conditions, standards, and records of calibration are recorded and
maintained.
Traceability of Standards and Reagents — The laboratory documents the identity, source, and purity of reagents
and standards, their lot number, and receipt and expiration dates. The laboratory maintains records that link
intermediate and working standards, and reagent solutions to their respective stocks or neat compounds.
Sample Mana eg ment — The laboratory maintains a record of all procedures to which a sample is subjected
while in the laboratory's possession. These include records pertaining to:
a) Sample preservation, appropriateness of sample container, and compliance with holding time
requirements;
b) Sample identification, receipt, including shipping receipts, COCs, assignment records, and disposal
records for Industrial Waste Pretreatment Program (IWPP) samples.
Original Data — The raw data and calculated results for all samples is maintained in laboratory notebooks, logs,
bench sheets, files, or other sample tracking or data entry forms. Instrumental output is stored in a computer
file or a hard copy report. Electronic raw data is maintained in archival systems by the District ITS
Department, or the LIMS database analyst.
C Data — The raw data and calculated results for all QC samples and standards are maintained in the same
manner as original data. Documentation allows correlation of sample results with associated QC data.
Final Report — A copy of any report issued by the laboratory and any supporting documentation.
9.4 Document Control System
A document control system is used to ensure that all staff has access to current policies and procedures at
all times. The QAS controls all laboratory quality documents. Documents which are managed by this system
include this Quality Manual, SOPS, Protocol Specifications, and policies used for QA. The system consists of
a document review, revision and approval system, and document control and distribution.
All quality documents are reviewed and approved by the QAS, the appropriate Laboratory Team Supervisor,
and the Laboratory Manager. Documents are revised whenever the activity described changes significantly.
Controlled documents are uniquely identified with: 1) date of issue, 2) revision number, 3) page number, 4)
total number of pages, or a mark to indicate the end of the document, and 5) the signatures of the issuing
authority (i.e., management). These forms are maintained by the LIMS Database Analyst on the MMSD
SharePoint laboratory site. Analysts are instructed to go to SharePoint to ensure that they are using the most
current version. All laboratory personnel are notified by e-mail of updates to those documents.
Documents are reviewed at least biannually to ensure that contents are suitable and in compliance with the
current quality systems requirements, and accurately describe current operations. All invalid or obsolete
documents are removed, or otherwise prevented from unintended use.
Forms and spreadsheets used for testing or QC purposes are also controlled. These may be created and
reviewed by either the QAS or the Team Supervisors. They are uniquely identified and filed electronically.
The QAS maintains a list of authorized signatories for document types commonly generated by and used at the
laboratory. The latest version of the list is included in Appendix F. Authorized signatories for personnel and
procurement records are referenced in established District -wide policies.
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9.5 Confidentiality
Access to all MMSD records is available to the public under Wisconsin state statutes. However, records
requests must be formally made in compliance with MMSD Administrative Policies Section 76 (Records).
Daily access to laboratory records and LIMS data is limited to MMSD personnel except with the permission of
the QAS or Laboratory Manager.
9.6 Reporting
Test reports, when generated for regulatory purposes, contain at least the following information:
• The name and location of the laboratory where the tests were performed, if the laboratory is not the
MMSD Central Laboratory. A laboratory ID number may be used in lieu of the full name and
location;
• Page numbers on the LIMS generated portion of the report;
• The name of the internal customer;
• Method ID — this can be a method citation or an OpSid;
• A unique identification, (generally a LIMS number or field ID, for each of the samples tested);
• Date of receipt of the samples by the laboratory;
• The name and signature of the person authorizing the report;
• Certification or accreditation number of the laboratory.
Since the MMSD Central Laboratory is an internal laboratory, these reports are generally considered as
backups or appendices for final reports prepared by staff outside of the laboratory.
Laboratory reports may be hard copy or electronic. Electronic copies of laboratory reports should be in pdf
format.
10.0 REVIEW OF NEW WORK, CUSTOMER COMMUNICATIONS AND COMPLAINTS
10.1 New Work
The review of all new work assures requirements are clearly defined, the laboratory has adequate resources
and capability, and the test method is applicable to the customer's needs. This process assures that all work
will be given adequate attention without shortcuts that may compromise data quality. Most requests for new
work will come through the Laboratory Project Manager, but requests may also come to the Laboratory Team
Supervisors or Laboratory Manager. In all cases, the decision to accept new work will be made after
consultation with the Laboratory Team Supervisors to determine whether the laboratory has the necessary
accreditations, resources, including time, equipment, deliverables, and personnel to meet the work request. If
the request includes analyses that are not routinely performed, the QAS will also review the request to ensure
that all certification or accreditation requirements are met.
The customer will be made aware of the results of the review if it indicates any potential conflict, deficiency,
lack of certification or accreditation, or inability of the laboratory to complete the work satisfactorily.
Specifications for new work are documented in the Request for Analytical Services (RAS) form by the
Laboratory Project Manager and made available to all staff involved with the work.
The review process is repeated when there are amendments to the original request by the client. Relevant
personnel are given copies of the amendments.
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10.2 Customer Communications
As an internal service organization, communication between the laboratory and the customers is key to
satisfactory performance. The laboratory collaborates with customers, both internal and external, in clarifying
their requests and in monitoring laboratory performance related to their work. Several mechanisms devised to
facilitate this communication will be described here.
While communication between all District staff is encouraged, the Laboratory Project Manager serves as the
primary laboratory customer contact and works with customers to define the scope of service and reporting
requirements.
The Laboratory Project Manager will use the Laboratory Services Notification, Client Disposition Form
(Appendix C) to document and notify when samples are lost or compromised.
The "IWPP Request for Data Verification Form" is used for requesting and documenting reviews of industrial
waste data.
10.3 Complaints
All customer complaints are documented by the person receiving the complaint and addressed by appropriate
personnel. If it is determined that a complaint has merit, a corrective action is initiated. See Section 14 for
corrective action procedures.
The Laboratory Project Manager solicits feedback from customers through an annual survey
11.0 PERFORMANCE AND SYSTEM AUDITS
11.1 Internal Laboratory Audits
The QAS performs annual internal audits to verify that laboratory operations continue to comply with the
requirements of the quality system. Where the audit findings cast doubt on the correctness or validity of the
laboratory's results, an immediate corrective action is initiated and any client whose work may have been
affected is notified.
The internal system audits include an examination of laboratory documentation on sample receiving, sample
log -in, sample storage, chain -of -custody procedures, sample preparation and analysis, and instrument
operating records. The annual review may be a single review covering the entire laboratory quality system or
a series of shorter reviews throughout the year, at the discretion of the QAS.
All investigations that result in findings of inappropriate activity are documented and include any management
decisions involved, corrective actions taken, and all appropriate notifications to clients. Clients are notified
promptly, in writing, when audit findings cast doubt on the validity of the data.
Audits are reviewed after completion to assure that corrective actions were implemented and effective. When
necessary, the QAS performs a follow-up audit.
11.2 External Audits and Assessments
The MMSD Central Laboratory will cooperate and assist with all external audits and assessments, whether
performed by clients or accreditation bodies. All external audits and assessment are fully documented and
tracked to closure.
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Management will ensure that all areas of the laboratory are accessible to auditors and assessors as applicable
and that appropriate personnel are available to assist in conducting the audit or assessment.
Any findings related to an external audit or assessment follow corrective action procedures. These are
performed within the timeframe specified by the accreditation body. The Laboratory Manager or designee will
follow up to verify that corrective actions have been implemented.
11.3 Managerial Review
Laboratory management performs an annual review of the quality system to ensure its continuing suitability
and effectiveness, and to introduce any necessary changes or improvements. This will include a general
review of the status and need for revision of SOPS and other controlled documents and data integrity
procedures. The review may consider reports from managerial and supervisory personnel, the outcome of
recent internal audits, assessments or audits by external bodies, the results of proficiency tests, any changes in
the volume and type of work undertaken, feedback from clients, corrective actions, and other relevant
information. The Laboratory Manager and other top management shall ensure that the integrity of the
management system is maintained when changes to it are planned and implemented.
12.0 EQUIPMENT, MEASUREMENT TRACEABILITY, STANDARDS AND REAGENTS, AND
PREVENTATIVE MAINTENANCE
12.1 Equipment
The Central Laboratory owns and maintains the necessary equipment to meet its accreditation requirements
and client needs. A current list of major analytical and support equipment in use is maintained by the QAS in
a dedicated database.
Equipment is operated only by authorized personnel. Up-to-date instructions on the use and maintenance of
equipment, including any relevant manuals provided by the manufacturer of the equipment, are readily
available for use by laboratory personnel.
All equipment, including hardware and software, are safeguarded from adjustments which would invalidate
the test results measures by limiting access to the equipment and using password protection where appropriate.
Equipment that has been subject to overloading, mishandling, giving suspect results, or been shown to be
defective or outside specifications is taken out of service, isolated to prevent its use, or clearly labeled as being
out of service until it has been shown to function properly. If it is shown that previous tests are affected, then
procedures for non -conforming work are followed.
All raw data records are retained to document equipment performance. These records include logbooks, data
sheets, or equipment computer files.
Records are maintained for all major equipment used for testing. The records include:
a) The name of the equipment;
b) The manufacturer's name, type identification, and serial number or other unique identification;
c) Date received and date placed in service (if available);
d) Current location, where appropriate;
e) Copy of the manufacturer's instructions, where available;
f) All routine and non -routine maintenance and repairs performed on the equipment:
g) Planned and required routine maintenance activities.
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Maintenance records of major equipment are kept in the laboratory where the instrument is used. Most major
equipment is under a service contract with the manufacturer or its representative, which includes routine
preventative maintenance as well as guaranteed service in the event of equipment failure.
12.2 Support Equipment
Certified professionals conduct regular maintenance of balances and fume hoods annually.
Maintenance on other support equipment, such as ovens, refrigerators, and thermometers is performed as
needed.
Records of maintenance to support equipment are kept in the laboratories where the equipment is located and
when practical, as electronic files in SharePoint.
For microbiology analyses, records for autoclaves used in the laboratory are required for the following:
• Initial performance of the autoclave functional properties (supplied by the installer);
• Temperature demonstration of sterilization via continuous monitoring device or maximum registering
temperature;
• For every cycle, record date, contents, maximum temperature reached, pressure, time in sterilization
mode, total run time, and analyst's initials;
• Quarterly check of autoclave timing device against a stopwatch; and
• Annual maintenance check to include a pressure check and calibration of temperature device.
12.3 Glassware Cleaning
Glassware is cleaned to meet the sensitivity of the method and to ensure that test results are not affected by
contamination. Glassware cleaning procedures are available in SharePoint and are posted in the dishwashing
area.
12.4 Measurement Traceability
Measurement quality assurance comes in part from traceability of standards to certified materials. All
equipment used that affects the quality of test results is calibrated prior to being put into service and on a
continuing basis. These calibrations are traceable to national standards of measurement where available.
Sections 12.5 and 12.6 describe how reference materials, standards, and reagents, are handled to provide
measurement traceability.
If traceability of measurements to SI units is not possible or not relevant, evidence for correlation of results
through inter -laboratory comparisons, proficiency testing, or independent analysis is provided.
12.5 Reference Materials
Reference materials are substances that have concentrations that are sufficiently well established to use for
calibration or calibration verification. Certified reference materials, where commercially available, are
traceable to national standards of measurement.
Purchased certified reference materials require a certificate of analysis (COA). Otherwise, purchased
reference materials are verified by comparison to another certified reference material, or DOC.
Reference standards and materials are stored in accordance with manufacturer's recommendations and
separately from working standards or samples.
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12.6 Documentation and Labeling of Standards and Reagents
Records are kept for all standards and reagents, including the identity of the manufacturer or vendor, the
manufacturer's COA or purity, the date of receipt, recommended storage conditions, and an expiration date
after which the material is not used unless it is verified.
All reagents, standards, gases, and other chemicals used for testing are labeled to indicate the receipt, opened,
and expiration dates. Expiration dates are only required when provided by the manufacturer or supplier or
required by the method.
Detailed records are maintained on reagent and standard working solutions. These records indicate traceability
to purchased stocks or neat compounds, reference to the method of preparation, date of preparation, expiration
date, and preparer's initials.
The expiration date will be that provided by the manufacturer or the expiration required by the method,
whichever occurs sooner. Commercial dehydrated powders and media used for microbiological testing are
assigned an expiration date of six months from the date the package is opened, or the manufacturer's
expiration date, whichever occurs sooner.
All containers of prepared reagents and standards bear a unique identifier and expiration date and are linked to
the documentation requirements above.
In methods where the purity of reagents is not specified, analytical reagent grade is used. Reagents of lesser
purity than those specified by the method are not used. The labels on the container are checked to verify that
the purity of the reagents meets the requirements of the method.
The quality of reagent water sources is monitored and documented to meet method specified requirements.
Requirements for laboratory reagent water can be found in Appendix B.
12.7 Preventative Maintenance
The laboratory has a routine preventative maintenance program that minimizes instrument failure and other
system malfunctions. Designated laboratory employees regularly perform routine scheduled maintenance and
repair of all instruments. All maintenance that is performed is documented. All laboratory instruments are
maintained in accordance with manufacturer's specifications.
13.0 SPECIFIC ROUTINE PROCEDURES USED TO EVALUATE DATA QUALITY
QC acceptance criteria on QC sample analyses are used to determine the validity of the data. Typically,
acceptance criteria are taken from published EPA methods. Where no EPA criteria exist or if adequate
historical data indicates that tighter limits are appropriate, laboratory generated acceptance criteria are
established. Laboratory generated acceptance criteria for accuracy are generally based on the historical mean
recovery plus or minus three standard deviations. Acceptance criteria for precision generally range from 0-20
% RPD.
Analytical data generated with QC samples that fall within prescribed acceptance criteria indicate the
laboratory was in control. Data generated with QC samples that fall outside the established acceptance criteria
indicate the laboratory was out of control for those tests. These data are considered suspect and the
corresponding samples are reanalyzed or reported with qualifiers.
13.1 Laboratory Control Samples (LCS)
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An LCS is analyzed with each batch of samples to verify that the accuracy of the analytical process is within
the expected performance of the method. The results of the laboratory control sample are compared to
acceptance criteria to determine usability of the data. Data generated with LCS samples that fall outside the
established acceptance criteria are judged to be out of control. These data are considered suspect and the
corresponding samples are reanalyzed or reported with qualifiers.
13.2 Matrix Spikes/Matrix Spike Duplicates
Results from MS/MSD analyses are primarily designed to assess data quality in a given matrix, and not
laboratory performance. In general, if the LCS results are within acceptance criteria, but individual percent
recovery in the matrix spike or matrix spike duplicate) falls outside the designated acceptance criteria and
there are no other assignable causes for the excursion, poor recovery is attributed to a matrix effect not a
laboratory performance problem. These results are reported with qualifiers and are not reanalyzed unless
specifically requested by the client.
13.3 Method Blanks
Method blanks are processed along with and under the same conditions, including all sample preparation steps,
as the associated samples in a preparation batch. Whenever a method blank contains analytes of interest above
the reporting limit of an analysis, the laboratory evaluates the nature of the interference and its effect on each
sample in that batch.
Generally, a sample in a batch is reanalyzed or qualified if the blank contamination exceeds the reporting limit
and is greater than 10% the amount measured in that sample. Each sample in the affected batch is assessed
against the above criteria to determine if the sample results are acceptable.
The laboratory follows the requirements of NR 149.48 (3) (d) when evaluating Wisconsin regulatory samples
associated with method blanks having detectable concentrations of analytes.
13.4 Estimation of Uncertainty
Estimation of uncertainty consists of the sum of the uncertainties of the numerous steps of the analytical
process, including, but not limited to variability in sample plans, spatial and temporal sampling, sample
heterogeneity, calibration or calibration check, extraction, and aliquoting.
The laboratory estimates uncertainty using the standard deviation calculated from routine quality control
samples. These estimates are provided as needed, on request. Information on uncertainty will be provided to
customers when the uncertainty affects compliance with a regulatory limit.
14.0 CORRECTIVE ACTION
Corrective action is the process of identifying, recommending, approving and implementing measures to
counter unacceptable procedures or out of control QC performance which can affect data quality.
Any QC sample result outside of acceptance limits requires corrective action. Once the problem has been
identified and addressed, corrective action may include the re -analysis of samples, or appropriately qualifying
the results. Analysts are responsible for the corrective actions specified in the QC Requirements Summary
Sheets Manual for the analyses they perform.
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Where a complaint, or any other circumstance, raises doubt concerning the laboratory's compliance with the
laboratory's policies or procedures, or with the quality of the laboratory's tests, the laboratory promptly
reviews the involved areas of activity and responsibility. Records of the subsequent actions are maintained.
SOP-LPROS-032 details the process for formal corrective action and root cause analysis.
Preventive action aims at minimizing or eliminating inferior data quality or other non-conformance through
scheduled maintenance and review before the non-conformance occurs. Preventive action includes, but is not
limited to: review of QC data, including control charts, to identify quality trends; discussion of QC topics in
regularly scheduled staff meetings; and annual managerial reviews.
All employees have the authority to recommend preventive action procedures; however, management is
responsible for implementing preventive action.
15.0 PROCUREMENT
15.1 Subcontracting Laboratory Services
No work is subcontracted to another laboratory without the client's express knowledge and permission. Any
subcontracted work is placed with a laboratory that has been approved by the Laboratory QAS and Laboratory
Manager for the tests to be performed. The following records of all subcontracted analyses are maintained:
• A copy of the subcontracted laboratory's scope of accreditation;
• A copy of the analytical report from the subcontracted laboratory;
• Any other specifications, correspondence or purchasing documentation related to the service.
15.2 Purchasing Procedures
All purchases will be made in accordance with MMSD's Procurement Policies and Guidelines.
The following persons are approved signatories for the Milwaukee Metropolitan Sewerage District Central
Laboratory, and thus have the authority to purchase goods:
• Laboratory Team Supervisor — Purchases under $1,000.
• Cost Center Manager (Laboratory Manager) — Purchases under - $2,999.99.
• Division Director (WQPT) — Purchases under $19,999.
• Executive Director— Purchases up to - $99,999.99
• Commission Resolution — $100,000.00 and up
MMSD only uses those outside support services and supplies that are of adequate quality to sustain confidence
in the laboratory's tests. Records of all suppliers for support services or supplies required for tests are
maintained.
16.0 CERTIFICATIONS AND ACCREDITATIONS
The Central Laboratory is certified to perform inorganic and microbiological analyses in non -potable water
and solids by the WDNR, and by the WDATCP to perform microbiological testing in potable water. The
Central Laboratory is accredited to the TNI Standard by the Florida Department of Health (DPH) to perform
inorganic and microbiological analyses of non -potable water and solids. Official copies of certificates and
scopes of accreditation are maintained by the QAS. Current copies of these documents are also posted in the
laboratory's SharePoint site.
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APPENDIX A
DEMONSTRATION OF CAPABILITY
DOCUMENTATION
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A demonstration of capability (DOC) must be on file for each analyst prior to performing any test
method. The DOC can be either an initial demonstration of capability (IDOL) or an ongoing,
continuing demonstration of capability (simply referred to as a DOC).
All demonstrations are documented through the use of the forms in appendix A. The coversheet certifies that
the demonstration of capability has been met and serves to bring together information about the test being
certified, the applicable SOP, the raw data, and the analyst who performed the procedure. The coversheet is
always associated with a datasheet, either a DOC spreadsheet for chemical tests or the Internal Microbiology
Analyst Certification (IMAC) form for microbiological tests.
An initial demonstration of capability (IDOC) is conducted whenever there is a significant change in
instrument type, personnel, or test method, or if insufficient data is available to complete an ongoing DOC
within one calendar year. The following steps are performed for the IDOC:
a) A quality control sample is prepared by the laboratory using stock standards that are independent from
those used in instrument calibration. In lieu of laboratory prepared standards, a QC sample may be
obtained from an outside source.
b) The analyse or analyses are diluted in a volume of clean matrix sufficient to prepare four aliquots at a
concentration that is approximately mid -scale on the calibration curve, usually the concentration of the
LCS.
c) The four aliquots are prepared and analyzed concurrently in accordance with the test method and are
not grouped with actual client samples.
d) Using all of the results, the mean recovery and the standard deviation are calculated for each parameter
of interest using the spreadsheets in this appendix.
e) The calculated percent recovery is compared to the corresponding acceptance criteria for accuracy in
the test method or to the laboratory -generated acceptance criteria. If all parameters meet the
acceptance criteria, the analysis of actual samples may begin. If any parameter does not meet the
acceptance criteria, the performance is unacceptable for that parameter.
f) When one or more of the tested parameters fail the acceptance criteria, the laboratory repeats the test
for all parameters that failed to meet the criteria. If repeated failure occurs, the laboratory will locate
and correct the source of the problem and repeat the test for all compounds of interest beginning with
step c).
A DOC must be completed annually using the existing results of quality control samples, such as the LCS. If
this annual requirement is not met for any reason, an IDOC is performed. The LCS results are extracted from
run files within the previous year and transferred to the DOC calculation spreadsheet for processing.
An DOC for the BOD test is handled similarly using existing glucose-glutamic acid (GGA) data from the past
year. The five-day length of the BOD test requires analysts to record GGA results for both the setup and
readout functions. Results are extracted from existing run files within the previous year and transferred to the
spreadsheet titled: `BOD DOC". If this annual requirement is not met for any reason, an IDOC is performed
and both setup and readout functions are carried out by the same analyst.
A separate spreadsheet for metals tests is used for both IDOC and DOC data, since metals are determined in
multi -element batches.
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Internal Microbiology Analyst Certification (IMAC) Program
Methods: SM 9222D (1997), SM 9223B (2004)
SOPS: LAB-028 and LAB-093
For microbiology analyses, the primary analysts and microbiologist perform an annual DOC using purchased
certified reference material quality control samples obtained from an approved provider. Four satisfactory
results on purchased QC samples are required annually for the following microbiological parameters: fecal
coliform by membrane filtration SM 9222D and E. coli by defined substrate Q-Tray analysis SM 9223B in
aqueous samples.
Once the primary analysts have approved DOCs, they certify all candidate analysts through the Internal
Microbiology Analyst Certification (IMAC) program. All analysts must perform an annual DOC (initial or
ongoing). The following steps are performed:
1. Primary microbiology analysts (PA) process an internal sample and establish an accepted reference
value for the sample. These results serve as the "known concentration" for the given sample.
2. The candidate analysts (CAs) must perform analysis on the same internal sample as the primary
analyst concurrently. The CA must produce satisfactory results according to the current SOPS with
four samples in duplicate to obtain an IDOC or one sample in duplicate to maintain an ongoing DOC.
3. The known concentration and CA's results are log -transformed (base 10).
4. The log difference between the CA's results and known concentration must be within the
microbiology laboratory's current IMAC control limits (acceptable range). The CA's results must be
within 20% log difference of the known concentration as a demonstration of accuracy.
5. The log difference of the CA's duplicate results must be within be within the microbiology
laboratory's current IMAC control limits as a demonstration of precision.
Example Calculations:
Fecal Coliform (FC) by SM 9222D (1997) Applicable SOP: LA13-028 Fecal Coliforrn by MF, Revision: 1.2
Sample ID: 1 Sample date: 1215117 PA CA lag PA CA lag acceptable CA CA lag
PA FC result: 3700 CA FC result: 3700 difference /o differenc range f difference Pass?
log(10) FC of result: 3.568 log(10) CA FC result: 3.568 0.000 0.000
CA FC duplicate result: 4800 0263 0.113 YES
log(10) CA dup result: 3.681 1 0.113 3.119
E. C'oN (Ec) by SM 9223B (2004) Applicable SOP: LAB -093 E. coli by defined substrate, Revision: 0.0
Sample ID: 1 Sample date: 1215117 PAICA log PAICA log acceptable CAICA log
PA Ec result: 4400 CA Ec result: 4200 difference /o differenc range f difference Pass's
log(10) Ec of result: 3.643 log(10) CA Ec result: 3.623 0.020 0.556
CA FC duplicate result: 3600 0.433 0.067 YES
log(10) CA dup result: 3.556 1 0.087 2.421
Yellow sections must be filled in Slue sections calculations: Do \ot Change
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Microbiology control limit criteria for IMAC
The microbiology laboratory's current IMAC control limits are set annually using the previous year's CA
duplicate results. Precision is demonstrated by duplicate analysis on all IMAC DOC samples analyzed.
Calculate precision criterion according to the following procedure:
1. Record duplicate analysis as D1 and D2.
2. Calculate the logarithm of each result (if < MDL use the MDL) as L1 and L2.
3. Calculate the range (Ring), defined as the absolute difference between Li and L2, for each pair of
transformed duplicate results.
4. Calculate the mean of the ranges (R) of the lab duplicates for all IMAC participants from the previous
year and multiply the result by 3.27 (see example in Table 9020: VII from Standard Methods for the
Examination of Water and Wastewater, 22nd ed. 2012).
5. Update annually repeating the procedure using the previous years' sets of duplicate results.
Table 9020: VII from Standard Methods for the Examination of Water and Wastewater, 22nd ed. 2012
TABLE 9020:VII_ CALCULATION OF PRECISION CRITERION
Duplicate Analyses
Sample No. Dl DZ
Ll
Logarithms of Counts
L2
Range of Logarithms (RI.,)
(LI - L2)
1
89
71
1.9494
1.8513
0.0981
2
38
34
1.5798
1.5315
0.0483
3
58
67
1.7634
1.8261
0.0627
14
7
6
0.8451
0.7782
0.0669
15
110
121
2.0414
2.0828
0.0414
Calculations:
I of Rjcl� = 0.0991 + 0.0483 + 0.0627 + ... + 0.0669 + 0.0414 = 0.718 89
R _ :SR,g-4.71889=0.0479
n 15
Precision cntenoa = 3.27 R = 327 (0.0479) = 0. 15 66
DOCs for total coliform and fecal coliform by most probable number (MPN) methods:
Methods: EPA Method 1680, SM 9221B (2006), SM 9221E (2006)
SOPS: LAB-031, LAB-090 and LAB-018
For biosolid samples by SM 9221B (2006) and EPA 1680, follow the DOC instructions from SOP-031
Quantification of Fecal and Total Coliform in Biosolids by MPN. For liquid samples by SM 9221 B and E
(2006), analysts will perform an annual DOC using purchased certified reference material QC samples
obtained from an approved provider. One satisfactory result on purchased QC samples is required annually.
DOC Requirements for readout of total & fecal coliforms by MPN method
A demonstration on capability (DOC) should be on file for all analysts that perform these analyses. For
determination of positive or negative tubes by checking for gas production in the inverted tubes, a DOC is not
required to determine presence or absence of gas. If transfer of positive tubes or speciation is required, the
analyst performing the transfer must have a current DOC.
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Reference DOC calculation spreadsheet - MMSD Microbiology
TMAC Event Results
Matnx: Aqueous
Candidate Analyst.
Approval date*:
Fecal Coliform (FC) by SM 9222D (1997) Applicable SOP. LAB-028 Fecal Coliform by MF, Revision:
Sample TD- Sample date:
PI inary Analyst (PA) Candidate Analyst (CA) PNCA log I P 11CA log acceptable CA CA log
PA FC result: CA k C result: difference /o differen range :h difference Pass?
log(10) FC of result: MI MI log(l0) CA FC result: *TUMl MUM! Wm
CA FC duplicate result: 0.000 #NUM!
lov(l0) (A dun result: #AUM, YNIMI #NLIMI
E. C'oH (Ec) by SM 9223B (2004) Applicable SOP: LAB-093 E. coli by defined substrate, Revision:
Sample II]:
Sample date:
Primly Analyst (PA)
Candidate Analyst (CA)
PA�C'A log
PA/C.4 log
acceptable
CA,CA log
PA Ec result:
CA Ec result:
difference
/ differen •
ranged
difference
Pass?
log(10) Fc of result: #N(iMl
log(10) CA Ec result: #NfUfMI
#NUMI #kNUMI
CA FC duplicate result:
0.000 #NUMI
log(10) CA dup result: #rj>j'[]M1
#NUM! ffNu g!
Yellow sect Ions must be filled in
Blue Sections calculHllons: Do Not Change
We, the undersiWaed LLRT 'f'tlrnt.
l_ The analyst identified above, using the cited test method(s), which is in use at this facility for the analysis of samples
under the DATCP, NELAP, or other required certifications, has met the Demonstration of Capability.
2 The procedure was performed by the analyst identified on this certification.
3_ The analyst has mead, understands and is using the latest version of the laboratory's quality documentation that relates to
the performance of this procedure. A copy of the latest test mcthod(s) and the SOPS required for this procedure arc
available on-
site-4- The data associated with the demonstration of capability are true, accurate, and comp] etc
5. All the raw data (including a copy of the certification form) necessary to reconstruct and validate these analyses have
been retained by the laboratory and the associated information is well organised and available for review by authorised
assessors.
Candidate Analyst (CA):
sion nOW
Primary Analyst (PA)*:
sdRna DAW
Team Supervisor:
sdgn.k_ Dam
Quality Assurance Specialist:
Date of expiration & 13 monthsfrone the approval dale above.
Adopted: 12/21/17
Revised 00/00100
3ign.4vc
DMO94
MQC7
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MMSD Central Laboratory
Demonstration of Capability
Analyst: I I Date
Method: IACIAC (16) 945.01 1 Method Reference:
Analyte: Applicable 50P:
SOP Version:
Instrument: Matrix:
Run numbers: Method Blanks:
Spike Concentration: Yellow sections must be Pilled in
Units:
9b Recovery Blue sections calculations: Do Not Change
Replicate 1 #DIV/0!
Replicate 2 #DIV/0
Replicate 3 #DIV/0!
Replicate 4 #DIV/01
Bean #kDiV/01 #DIV/01 Mean 96 Recovery
Standard Deviation #DIV/01 #DIV/01 RSD
Wes, the undyxj _td CERTIFY b�&L
1. The analyst identified above, using the cited test method(s), which is in use at this facility for the analysis of samples under
the WDNR, NELAP, or other required certifications, has met the Demonstration of Capability.
2. The procedure was performed by the analyst identified on this certification-
3- The analyst has read, understands and is using the latest version of the laboratory's quality documentation that relates to the
performance of this procedure. A copy of the latest test method(s) and the SOPS required for this procedure are available on -
site.
4. The data associated with the demonstration of capability are true, accurate, and complete-
5- All the raw data (including a copy of the certification form) necessary to reconstruct and validate these analyses have been
retained by the laboratory and the associated information is well organized and available for review by authorized assessors.
Analyst:
Team Supervisor:
Signar—
Siprtature
irm
Date
Quality Assurance Specialist:
sirnature Date
Date of expffwtion is 365 days from the above date highlighted m yellow
Adopted: 9/8/17 D000086
Revised: 01/23/18 Page 1 of 1
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MMSD Central Laboratory
Demonstration of Capability BOD
Analyst: Applicable SOP: LAB-076 Biochemical Oxygen Demand
Date: SOP Revision:
Method: 5M (20011 5210 B
Instrument ID: BOD Auto E2 2 Yellow sections must hefllIEd In
Matrix: Aqueous Blue sections caIculatlans: Do Not Change
Setup runs Readoutruns
GGA Value 198 GGA Value 198
Units: mg/L Units: mg/L
Method Method
%Recovery Blank(s) %Recovery Blank(s)
Replicate 1 0.0D% Replicate 1 O.OD%
Replicate 2 0.0D% Replicate 2 0.OD%
Replicate 3 0.0°% Replicate 3 0.0%
Replicate 4 0.0°% Replicate 4 0.0%
MEAN ttDIV/O! 0.0°% Mean %Recovery MEAN #DIV/O! 0.0% Mean %Recovery
Standard Deviation #DIV/0! #DIV/O! RSD tandard Deviation #DIV/0! #DIV/O! RSD
Run IDs: I Run IDs:
The sheet is only used for validation of continuing demonstration of capability. The analyst performing the setup on this
sheet will not perform the readout. The analyst performing the readout on this sheet will not perform the setup.
We the undersigned, CERTIFY that.
1. The analyst identified above, using the cited test met hod (s), which is in use at this facility far the analysis of samples
under the WDNR, NELAP, or other required certifications, has met the Demonstration of Capability.
2. The procedure was performed by the analyst identified on this certification.
3. The analyst has read, understands and is using the latest version of the laboratory's quality documentation that relates
to the performance of this procedure. A copy of the latest test met hod (s) and the 50Ps required for this procedure are
available on -site.
4. The data associated with the demonstration of capability are true, accurate, and complete.
S. All the raw data (including a copy of the certification form) necessary to reconstruct and validate these analyses have
been retained by the laboratory and the associated information is well organized and available far review by authorized
assessors.
Analyst:
si'a—,• ftm�.
Team Supervisor:
sg.xt Doe
Quality Assurance Specialist:
Spn�we n.ir
Date of e�Viretion it 365 days from the above date highlighted M yellow
Adopted:12/11/14
Revision 1.0, Revised! 6126118
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APPENDIX B
MMSD DEIONIZED WATER MONITORING
REQUIREMENTS
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DEIONIZED WATER MONITORING REQUIREMENTS
TEST
Chemical Tests:
MONITORING
FREQUENCY
Conductivity Monthly*
Total Organic Carbon Monthly
Heavy Metals, Single (Cd, Cr, Cu Ni, Annuallyt
Pb, and Zn)
Heavy Metals, Total Annuallyt
Total Residual Chlorine Monthly or with each use
Bacteriological Tests:
Heterotrophic Plate Count Monthly
Use Test For a new source
Water Quality TestTT Annually
MAXIMUM ACCEPTABLE
LIMITS
<2 µmhos/cm @ 25°C
<1.0 mg/L
<0.05 mg/L
<0.10 mg/L
<0.1 mg/L
<500 CFU/mL
Student's t < 2.78
0.8-3.0ratio
*Monthly if meter is in -line or has a resistivity indicator light; otherwise with each new batch of reagent water.
TOr more frequently if there is a problem.
TT'Ibis bacteriological quality test is not needed for type II or better
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APPENDIX C
LABORATORY SERVICES
NOTIFICATION FORM
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LAB SERVICES NOTIFICATION
SAMSD Client Disposition Form
PARTNERS FOR A CLEANER ENVIRONMENT
Sample Date:
Source Codes):
Customer, Project or Survey:
LIMS Numbers):
DP SI❑
Anal to/Parameter
Data Flag(s)
Applied
Estimated
Completion Date
Lao uommemsttxDianauon:
Samples qualified (flagged) and verified in LIMS: ❑
Initials:
Analyst:
Date:
Supervisor:
Date:
Client(s) Notified:
Date:
Original File: Lab Project Manager; Electronic Copies To: Lab Manager, QA Specialist, Lab Supervisors and Analyst
This form must be filled out whenever a sample is lost, data is unusable, and/or when the following laboratory qualifiers are
used, D4, H3, H4, IS, LA, M2, M3, M5, M7 and NU.
Lab Services Notification DDC 0013 Page 1 of 2
Revised. 5/09/17
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APPENDIX D
METHODS AVAILABLE FROM
MMSD CENTRAL LABORATORY
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OpSid*
Analyte Name
Current Method
1101
Ammonia (Milorganite)
AOAC (13) 2.065
1103
Nitrogen, Robertson (Milorganite)
AOAC 2.069 (13)
1102
Nitrogen, Total Modified (Milorganite)
AOAC 2.061 (13)
195
Alkalinity (Auto chemistry)
EPA 310.2
368
Aluminum (ICP)
SW846: 6010C/EPA 200.7
110
Ammonia (ISE)
SM 4500 NH3 D (1997)
ill
Ammonia (Manual)
SM 4500-NH3 C (1997)
192
Ammonia Nitrogen (Auto chemistry)
SM 4500-NH3G (1997)
389
Antimony (ICP)
SW846 6010C/EPA 200.7 Rev. 4.4
369
Arsenic (ICP)
SW846 6010C/EPA 200.7 Rev. 4.4
371
Barium (ICP)
SW846 6010C/EPA 200.7 Rev. 4.4
372
Beryllium (ICP)
SW846 6010C/EPA 200.7 Rev. 4.4
854
BOD- 20 Day Total
SM 5210 C (2001)
850
BOD- 5 Day Total
SM 5210 B (2001)
374
Cadmium (ICP)
SW846 6010C/EPA 200.7 Rev. 4.4
373
Calcium (ICP)
SW846 6010C/EPA 200.7 Rev. 4.4
198
Chloride (Auto chemistry)
SM 4500 CI-E (1997)
171
Chlorophyll A
SM 10200 H (1998)
376
Chromium (ICP)
SW846 6010C/EPA 200.7 Rev. 4.4
123
Citrate Insoluble Phosphorus (ICP)
SW846 6010C/EPA 200.7 Rev. 4.4
375
Cobalt (ICP)
SW846 6010C/EPA 200.7 Rev. 4.4
68
COD
SM 5220 D (1997)
481
Coliform - Total MPN (sludge)
SM 9221 B (2006)
482
Coliform- Fecal MPN (sludge)
EPA 1680
377
Copper (ICP)
SW846 6010C/EPA 200.7 Rev. 4.4
880
E-Coli QT
SM 9223 B (2004)
213
Coliform, Fecal MF
SM 9222 D (1997)
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OpSid*
Analyte Name
Current Method
211
Coliform, Fecal MPN
SM 9221 E (2006)
437
Hardness
SM 2340 B (1997)
731
HEM (SPE)
EPA 1664 B
378
Iron (ICP)
SW846 6010C/EPA 200.7 Rev. 4.4
388
Lead (ICP)
SW846 6010C/EPA 200.7 Rev. 4.4
383
Magnesium (ICP)
SW846 6010C/EPA 200.7 Rev. 4.4
384
Manganese (ICP)
SW846 6010C/EPA 200.7 Rev. 4.4
274
Milorganite pH
EPA 9045 D
385
Molybdenum (ICP)
SW846 6010C/EPA 200.7 Rev. 4.4
387
Nickel (ICP)
SW846 6010C/EPA 200.7 Rev. 4.4
189
Nitrate & Nitrite (Auto chemistry)
EPA 353.2
194
Nitrate Nitrogen (Auto chemistry)
EPA 353.2
193
Nitrite Nitrogen (Auto chemistry)
EPA 353.2
115
Nitrogen (%, Total)
AOAC (16) 955.04
114
Nitrogen (Nitrate)
AOAC (16) 930.0
112
Nitrogen (Organic - Calculated)
AOAC (10) 2.057
133
Nitrogen (Total, NCS)
AOAC (18) 993.13
747
Phosphorus - Total % DW (Calc.)
SW846 6010C/EPA 200.7 Rev. 4.4
196
Phosphorus - Total (Auto chemistry)
EPA 365.1
397
Phosphorus (ICP)
SW846 6010C/EPA 200.7 Rev. 4.4
748
Potassium - Total % DW (Calc.)
SW846 6010C/EPA 200.7 Rev. 4.4
380
Potassium (ICP)
SW846 6010C/EPA 200.7 Rev. 4.4
390
Selenium (ICP)
SW846 6010C/EPA 200.7 Rev. 4.4
732
SGT-HEM (SPE)
EPA 1664 B
200
Silica - Total (Auto chemistry)
USGS I - 2700 - 85
367
Silver (ICP)
SW846 6010C/EPA 200.7 Rev. 4.4
100
Solids (% Ash)
SM 2540 G (1997)
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OpSid*
Analyte Name
Current Method
97
Solids (% Moisture)
SM 2540 G (1997)
137
Solids (% Total)
SM 2540 G (1997)
145
Solids (% Volatile)
SM 2540 G (1997)
83
Solids (Suspended)
SM 2540 D (1997)
90
Solids (Suspended, Volatile)
SM 2540 E (1997)
80
Solids (Total Dissolved, Calculated)
Calculated value
79
Solids (Total Soluble)
SM 2540 C (1997)
75
Solids (Total)
SM 2540 B (1997)
254
Specific Gravity, Sludge
SM 2710 F (1997)
422
Strontium (ICP)
SW846 6010C/EPA 200.7 Rev. 4.4
187
Sulfate
SM (15) 426 C
394
Thallium (ICP)
SW846 6010C/EPA 200.7 Rev. 4.4
392
Tin (ICP)
SW846 6010C/EPA 200.7 Rev. 4.4
393
Titanium (ICP)
SW846 6010C/EPA 200.7 Rev. 4.4
746
TKN % DW (Calc.)
SM 4500-Norg-B (1997)
191
TKN Nitrogen (Auto chemistry)
EPA 351.2
877
Total Carbon
SM 5310 C (2001)
875
Total Dissolved Organic Carbon
SM 5310 C (2001)
876
Total Inorganic Carbon
SM 5310 C (2001)
874
Total Organic Carbon
SM 5310C (2000)
395
Vanadium (ICP)
SW846 6010C/EPA 200.7 Rev. 4.4
134
Water Insoluble Nitrogen
AOAC 2.061 (13)
396
Zinc (ICP)
SW846 6010C/EPA 200.7 Rev. 4.4
122
Phosphorus — Water Extractable
WDNR Guidance
*OPSID is a LIMS reference number. Many of these tests are available as soluble (rather than total) or dry weight (solids). See
Laboratory Project Manager for further information.
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APPENDIX E
REQUEST FOR ANALYTICAL
SERVICES FORM
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REQUEST FOR ANALYTICAL SERVICES
RAS: Click here to enter text. Date: 11/28/16 Rewsion: 1. Originator: Click here to enter text.
Customer: Click here to enter text. Charge Number: Click here to enter text. Billable To: Click here to enter text.
Project Name: Click here to enter text.
Name for Report Files: Click here to enter text.
Project Cornacts/Affiliations: Ciick here to enter text.
Project Description:
ampling dates: Click here to enter text. Sample frequency: Click here to enter text.
roject Instructions:
Requested Analytes:
Samnlp Tvnp• ChnmP an irpm Sni irrp r.Mp- r Iirk hprp to Pntpr Tp xt SItP rr AP- r'Iirk hp rP to PniPr TPxt
OPSID
Ana"
# of
samples
Grab or
Camp.
OPSID
Analyte
# of
samples
Grab or
Comp_
Sample matrix type: Choose an item. Turn around requirements/Due date: Click here to enter text.
Will samples include field blanks: Yes ❑ No ❑
Certification Requirements: WI DNR ❑ WIDATCP ❑ NELAC ❑ Not Required ❑ Other:
Chain of Custodies: Choose an item. Sample deliveryv[a: Click here to enter text.
nwu�srL L L-1 Ru 33Jcy LE d�
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REQUEST FOR ANALYTICAL SERVICES
Bottles needed:
Vaz M Nln I— !If .a' Il't h.k... I
e
a
2
0
m
o
m
0
Analytes in Bottle
m
a
u
Bottle types: P-Plastic, G-Glass, V-vial,
S-Sterile, AM -Amber, WP-Whirl Pack
Preservation: 1) H2SO4, 2] HCL,3) HND3,
4) Sodium ThiosuIfate, 5] On Ice Only, 6] None
Labels needed I l Bottles pre -labeled 171
Report Format:
Standard LIMS report ❑ Excel spreadsheet ❑ Other ❑ Lisr other. Click here to enter text.
Report sent to: Ciick here to enter text.
Copies to: Click here to enter text.
Number of reports frequency required: Click here to enter text.
Data Review:
Data review by: Click here to enter text. Report review by: Click here to enter text.
Additional Information:
Notes:
A[0 ?LLL 1lYJY11G 3j[y LEi.doa
Kr.wrb�i i i-S awnyrn >>I„V ie
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APPENDIX F
AUTHORIZED SIGNATORIES
MMSD CENTRAL LABORATORY
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Authorized Signatories
MMSD Central Laboratory
Document Type
Analyst
Reviewer
Analyst
Chemical
Hygiene Officer
Laboratory Data
Analyst
Laboratory
Manager
Laboratory
Project
Manager
Quality
Assurance
Specialist
Risk Manager
Coordinator
Team
Supervisor
Bench Sheets
X
X
C alibration of S upportE quipment
X
X
Chemical Hygiene Plan
X
X
X
Corrective Action Records
X
X
X
X
Demonstrations of Capability
X
X
X
Internal Microbiology Analyst C ertification
X
X
X
X
Instrument Maintenance Log Books
X
X
X
Linear Dynamic Range
X
X
X
Method Detection Limits
X
X
X
QC Requirements Summary Sheet Manual
X
Quality Manual
X
X
X
R e orts to Clients
X
X
X
X
X
Standard Operating Procedures
X
X
X
Standards and Reagent Verification
X
X
X
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Appendix 6
Quality Control Requirement Summary Sheet Examples

Metals (solids matrix)
Corrective Action Procedures
Method: SW 846 6010 C
sample
Description
Frequency
Criteria (Contr❑i Limitsi
Flagging Protocol /Corrective Action
ICV
Mid -point standard, run after
pnce, directly after calibration
9❑-110%Recovery
Correct problem and rerun ICV. Ifthat fails, the
(Initial Calibration
raIlbration ofthe instrument to
"Ilbration must be rerun and verified. Flagging
Verification)
erlfy the ar,'curacy of calibration_
(second source(.
(t 10% of the known concentration(
1s not appropriate.
LL-ICV
Low -point standard, run after
Correct problem and rerun LL-ICV. If that fails,
(Low Level Initial
calibration instrumentto
theccuracy
Gnce, directly after calibration
50-150%Recovery
the calibration most be rerun and verified.
Calibration Verification)
aof
verify the accurary of calibration.
(second scurcel-
If 50%of the known concentration)
Flagging is not appropriate.
Correct problem and reanalyze the CCV. If the
ccv
Mid -point standard con
Every 10samples;
CCV fails reanalyze all samples since the last
(Continuing Calibration
periodically throughout run to
once in each analytical
90 -110 %Recovery
successful CCV. Flagging is not appropriate. if
Verification)
verify the calibration.
sequence.
(*-10% of the known concentration)
reanalyzing sample does not solve the problem,
consult the Team Su pervisoc
ICS
Standards that verify that the
80-120%Recovery
(Interference check
interference correction factors are
At the beginning of a run
(±20%and/or ♦3xthe LOGof
Correct the problem and reanalyze the lCS.
solutions)
working correctly.
non -included elements)
areoble not appropriate.
lagging is
This sample verifies the MDL and
Correct problem, repeat CCR and reanalyze all
COB
(Continuing Calibration
may Indicate when there is drift in
Every l0 samples;
once in each analytical
13 times the MDT
samples s'mcethe last ...ssful CCB_ If
Blank)
the instrument calibration on the
low end of the calibration range.
sequence.
(Method Detection Limit]
wrrectiveaction is not possible, apply AO Flag to
affected results with a narrative explanation.
This standard is to verify the law
correct problem, repeat LL{CV and reanalyze all
LL{CV
end spectrum of the calibration
Once, during ordirectlyafter the
50-150%Recovery
samples since the successful LL-CCV. If corrective
(Low Level continuing
curve,runsomewhere between the
.
(±50%of the known concentration)
action is not possible, apply B9 qualifier to
Calibration Verification]
LOD and the LOG,
affected results.
A sample free of the analyte of
Investigate the problem and reanalyze the blank
interest and is processed in the
The highest of:
and all associated samples.
MIS
same man ner as the samples.
Every20 samples;
MDL (Method detection limit]❑r,
If reanalyzing is not possible, apply B3 qualifier
Method Blank)
Failure ofa method blank can
once in each analytical batch.
<_ 5 %of the Regulatory Limitor ,
<_1o%measured
to all samples in the associated batch thatare�
indicatecomaminationduring
concentraEion of the
MOL and where the blank is , 10%ofthefield
processing_
smple&_
a
sample concentration_
Mid -point standard that Is
Correct problem, repeat LCS, and reanalyze all
processed in the manner as the
samples in the associated batch. If corrective
LCs
analytical samples. This can verify
Every 20 samples;
action fails and reanalysis is not possible, apply
(Laboratory Control
the sample processing stages, and
once in each analytical batch
g0-120%Recovery
(± 20 %of the known concentration)
qualifiers,
Sample)
may indicate contamination from
(second source).
117 if the LCS was above controllimits,
ample prep or materials used to
BR ifthe LCSwas below control limits_
process samples.
Gualify a1I samples in the associated batch.
Review LCS and other run data_ If there is an
A sample that is spi ked with a
assignable cause, correct the problem and
knowncc—mrationofthe
Every 20 samples;
reanalyze; if not, lag the data. Forthespecific
Ms
aralyteto be determined. May
75-125%Recovery
analyte(&) in the parent, apply qualifier if
(Matrix Spike)
indicate 'mterferences in the
in in each analytical batch
1±25% of the known concentration)
acceptance criteria aren't met:
ample matrix or co ntamir ion
(second source).
Q2 if the MS is above limits,
during processing.
0,3 if the MS is below limits.
Qualify both parent and spike.
The same as a matrix spike, run in
duplicate, This sample verifies the
Follow the same Flagging protocol listed for MS
MSo
matrix sampleand also shows the
Every 20 samples;
75-125%Recovery and
s D
amples.lf the RPD exceeds control limits, apply
Matrix Spike Caplicate:
( pie pica e;
reproducibility between the MS/
repro ty
once in each analytical batch
<2D %relative percent difference (RPD)
qualifier parent spike
the Ds f both the t and k
Ml which verifies accurary and
(s cu dsource)_
from the MS_
samples.
precision.
D000017

Fecal Coliform - MPN Methods (Biosolids)
Corrective Action Procedures
Methods, EPA 1680
Sample
Description
Frequency
Criteria (Control Limits)
Flagging Protocol / Corrective Action
A sample of sterile peptone buffered
dilution water is processed in the same
ME
manner as the samples. Failure efa
Once each day of
5 ML(Method detection limit)
If target organisms are found in the blank 2 MDL, apply
(M"ncd Blank)
method blank may indicate
analysis.
M9 qualifier to all samples in the associated batch.
contamination during processing_
A sample that is spiked with a fare—
Review the other run data. Flag the data. For the
MS
con cenfraticn of the analyte to be
Every 20 samples;
Class A Biosolids: 30-424%Recovery
specific analyte(s) in the parent, apply qualifier if
acceptance criteria aren't met:
(Matrix Spike)
determined. May indicate
once in each analytical
Class eeigsglids: 8-709%Recovery
the MSisarw
interferences in the sample matrix or
during
batch.
(method criteria)
lldnt;
31 if the MSis limits.
contamination processing.
qualify bath parent and spike.
moan
Class A Biosolids: 30. 424 % Rewvery
The same as a matrix spike, run in
Class B Diosolids:8-709%Recovery and
MSD
du licate_This sam le verifies the
p
Ever 2n sam les;
y p
<_ 150 %relative percent difference (R PbJ for
Follow the sa—fl tocel listed for MS
agging pro
(Matrix Spike
trio sample and also shows the
ma
cei each analytical
Gass la aosBi-o and
samples. If the RPD exceeds control limits, apply the D2
Duplicate)
reproducibility between the MS/ MSD,
batch.
qualifier to bath the parent and spike samples.
which verifies accuracy and precision.
5125 %RPbfor Class B Biosolids from the MS
( method criteria).
,,-- „nns
DDCDD17

Appendix 7
Sample Receiving Standard Operating Procedure

SOP No.: LPROS-001
Revision: 6.4
Date: 12/7/18
Page 1 of 24
MMSD CENTRAL LABORATORY
STANDARD OPERATING PROCEDURE
Sample Receiving
Procedure
Number:
LPROS-001
1 Creation
Date:
9/1/02
Revision
Date:
12/7/18
Prepared
By:
Jessica Nanes
Reviewed
By:
Zach Vogel
Laboratory Manager Approval:
Quality Assurance Specialist Approval:
\
�;, -M Wddw
PROPRIETARY INFORMATION STATEMENT
This document has been prepared by MMSD solely for its use and the use of MMSD's
customers in evaluating its qualifications and capabilities in connection with a particular
project.
TABLE OF CONTENTS
1.0
Purpose
2.0
Scope and Applicability
3.0
Definitions
4.0
Requirements and Procedures
5.0
Quality Control
and Quality Assurance
6.0
References
7.0
Appendices
Appendix A
Required Containers, Preservation Techniques, and Holding Time for
Wastewater
Appendix A-1
Sampling and Holding Time Requirements for Chlorophyll Analysis
(SM20 Table 1060:1)
Appendix B
Abbreviated Procedure for Receiving Daily Production Samples into
LIMS
Appendix C
Instructions for Thermal Preservation Verification
Appendix D
Instructions for pH Verification, pH Adjustment and Preservation
Appendix E
Emailing the Daily Plant Data Report to Veolia on Weekends/Holidays
Appendix F
Printing Sample Labels
Appendix G
Filtering Samples for Soluble Analyses
Appendix H
SOP Editorial Changes and Revisions
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Page 2 of 24
1.0 PURPOSE
1.1 The purpose of this document is to define the acceptance criteria and procedures
for sample receiving in the MMSD Laboratory.
2.0 SCOPE AND APPLICABILITY
2.1 This Standard Operating Procedure (SOP) applies to all samples that are received at
the MMSD Central Laboratory for chemical and microbiological analysis. All
variances must be properly documented.
2.2 This document refers to the process commonly referred to as "sample receiving".
Prior to official sample receipt, samples must be logged into the Laboratory
Information Management System (LIMS). In the MMSD laboratory, sample log -in
refers to the process of assigning samples a unique identifier in the LIMS, and
entering pertinent sample information such as location, depth, matrix, date of
collection, etc. This process can be performed prior to sample collection or after
samples arrive at the lab. Samples can be logged in by the Sample Custodian with
information from the "sampling party", the Laboratory Project Manager, or the
sampling parties themselves, if they are MMSD employees and have access to the
LIMS.
2.3 Sample storage in the document refers to the central sample storage area.
Individual lab areas will follow these same requirements by default. However,
individual test methods may dictate different storage requirements which are
covered in their respective SOPS.
3.0 DEFINITIONS
3.1 Refer to the glossary in the Laboratory Quality Manual (LQM), current revision.
3.2 "Sample Custodian". the laboratory analyst assigned to the sample receiving area.
4.0 REQUIREMENTS AND PROCEDURES
4.1 The Sample Custodian will receive the samples that arrive in the lab. When the
samples are delivered to the lab, it is the job of the Sample Custodian to check all
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Revision: 6.4
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Page 3 of 24
documents that have been delivered with the sample. These include the chain of
custody (COC), any air bills or other delivery receipts, additional instruction sheets
or supplementary information included with the samples. The Custodian must check
that samples are properly labeled. The Sample Custodian should also document
sample condition as described in this SOP. Only after this is complete may the
sample be "received" into the LIMS database.
4.1.1 If the samples(s) do not meet the specified requirements as defined in this SOP, by
regulation or by other agreed upon conditions, the customer will be notified as soon
as possible.
4.1.2 Appendix A is a list of sampling and preservation methods for analytical samples
based on requirements NR219, Standard Methods, and the analytical methods used
in-house unless otherwise noted.
4.2 A COC should accompany all samples and have the following information:
• Sample identification (this is indicated by written description, and may
include a LIMS number or laboratory source code).
• Sample (Site) Location (this may be a site code) or other specific identifier.
• The source of the samples, and/or group taking the samples. This may be a
program identifier such as IWPP, WQ LISGS, etc.
• Name of the receiving laboratory.
• Sample information (this should be listed individually for each sample).
• Collection date and time (of each sample). Time may be optional if
provided to the tab in some other format.
• Number of bottles and/or type of sample.
• Sample collection type: grab or composite.
• Sample matrix (wastewater, sludge, soil, etc.) This need not be redundant.
If the matrix is implicit in the location (e.g. "effluent wastewater") or
sample identification (e.g. "Milorganite") a separate matrix description isn't
necessary.
• Requested tests.
• Sample Preservation (e.g., sulfuric acid, nitric acid, thiosulfate). Any
discrepancy must be documented on the COC and should be corrected by
hand on the label.
• Additional field or customer information may be included on a program or
project specific basis.
4.2.1 Signatures or initial of each person or party who has handled the sample, including
the date and time of indicated action. This will include the person who collected the
sample, couriers or person delivering the sample, and the sample custodian
receiving the sample for the lab.
422 COC documents shall be completed in ink.
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4.2.3 The laboratory may ask for additional information based on the sample matrix,
method, or other requirements for outsourced laboratory data.
4.3 Upon receipt, the Sample Custodian will review the sample label. The sample label
must be legible, and contain the following items:
+ Sample identification: this can consist of a LIMS number or site code or
other specific identifier.
Date and time the sample was collected (time may be optional on the label
if supplied to the lab in another format).
Required tests. Sample carboys from the plants do not need the required
tests on the label.
Sample preservative (if required).
4.4 If samples or the bottle labels do not match the COC, information is missing from the
chain of custody, there is no chain of custody, or if the sample bottles are not
labeled, the sample cannot be received in the laboratory until the issue is resolved.
The Sample Custodian should notify the customer or the Lab Project Manager.
Generally, when there are discrepancies, the COC is transmitted to the customer for
review and correction. If the sample is not for regulatory purposes, it is acceptable
for the Lab Project Manager or the Sample Custodian to create the proper
documentation based on conversations or other documentation with the customer.
Other documentation may be substituted for the COC, providing that this provides
adequate information.
4.4.1 Sample receiving issues are logged on the district SharePoint site at:
https://home.mmsd.com/district/Lists/SampleReceivingTeam. This log will state the
problem, date, lab contact, person notified of the problem, resolution, and status.
4.5 Upon receipt, the Sample Custodian will check the condition of the samples and
document any abnormalities or departures from standard conditions. If the sample
requires cooling and solid ice is still present in the cooler, the lab simply reports the
sample as "Received on Ice". If the ice has melted, the lab must report the
temperature of the melt water or of the temperature blank.
4,5.1 All samples that require cooling shall be considered acceptable if they meet one of
the following:
• They are collected the same day as they are received and are received on
ice;
• They are collected and delivered to the lab within 15 minutes;
• The arrival temperature of a representative sample container is within 20C
of the required temperature or method specified range. For samples with
a specified temperature of VC, samples with a temperature ranging from
just above the freezing temperature of water to 60C shall be acceptable.
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4.5.1.1 If samples that require cooling are not received on ice, or if the ice melted, the
temperature of the sample must be verified and recorded on the COC. Use the
temperature blank or a randomly selected sample and measure the temperature
with the pyrometer (Note: If the pyrometer is not available, a thermometer may be
used instead as long as it does not compromise the integrity of the sample).
4.5.1.2 Appendices C, D, and E contains instructions on thermal and chemical preservation
verification and reporting daily plant samples to plant personnel during weekends.
These instructions are also posted in the sample receiving area.
4.5.1.3 Samples that require thermal preservation are stored under refrigeration that is
within the specified preservation temperatures of the method and NR 219.04.
4.6 When pouring an aliquot of sample, whether for verification of pH (or other
preservation), compositing or simply obtaining the amount required for an analysis,
care must be taken to have a homogeneous sample. Smaller containers may be
shaken before pouring. However, carboys used for collecting wastewater may be
too large and bulky for this. It is recommended that these sample containers be
swirled vigorously for at least a half a minute or more. Look at the bottom to be
sure that solids and other material or layers are being incorporated. If not, mix
longer before pouring. If the container weight is an issue, the sample container may
be rolled on the counter rather than swirled.
4.7 When samples requiring chemical preservation arrive in the laboratory, each sample
shall be checked for evidence of proper preservation. In most cases this includes a
check of the pH. After the sample is checked for preservation, the Sample Custodian
shall check the pH verified section on the chain of custody for each sample bottle
that is verified and initial near the checkmarks or in a specified area on the COC. If
the standard forms are not used, the Sample Custodian should initial by the sample
preservative or indicate that the preservation has been checked in some manner for
each sample checked. If samples do not meet the requirements for pH, this shall be
noted on the COC and the Sample Custodian shall make adjustments.
4.7.1 In the cases where opening the sample bottle to take a pH in the receiving area may
compromise the integrity of the sample (e.g. volatile organic analysis, low level
mercury, oil and grease) the pH verification will not be performed in sample
receiving.
4.7.2 In some cases, samples are composited and aliquoted in the sample receiving area.
In those cases, the laboratory shall document the sample preservation using the
sample preservation report in LIMS. All pH adjustments shall be verified and
documented.
4.7.3 For convenience, the required pH verification and adjustment for BOD may be
performed in the sample receiving area rather than the BOD lab. The initial pH of
samples to be analyzed for BOD should be within the range of 6.0 to 8.0. If it is not
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Page 6 of 24
within this range, adjust the sample temperature to 20 ± 3°C, then adjust the pH to
7.0 to 7.2 before analysis using sulfuric acid (H2SO4) or sodium hydroxide (NaOH) of
such strength that it does not dilute the sample by more than 0.5%. Exceptions may
be justified with freshwater samples when the BOD is to be measured at in -situ pH
values. After the pH is verified, the Sample Custodian shall check the pH verified
section on the chain of custody for each sample bottle that is verified and initial near
the checkmarks or in a specified area on the COC. If pH adjustment is required, the
Sample Custodian shall record the sample temperature (between 17-23°C) and the
start and end pH in the BOD — pH Checks logbook, and mark the sample for
identification by the BOD analyst.
4.8 Some samples collected for soluble analyses are filtered in sample receiving, such as
groundwater samples and samples for special projects. Instructions for filtering
these samples are in Appendix G.
4.9 Once samples have been checked, the Sample Custodian should enter the required
information to receive the samples in LIMS. Appendix B contains a procedure for
this LIMS entry.
5.0 QUALITY CONTROL AND QUALITY ASSURANCE
5.1 Sample receiving protocol is based on NR149.46 and NR219.04.
5.2 The pyrometer used to measure the temperature of samples should be verified at
least every six months using a NIST certified thermometer over the full temperature
range that the IR thermometer will be used. This would include ambient (20-30' C),
iced (4° C), and frozen (0 to -50 C). Each day of use a single check of the IR should be
made by checking the temperature of a bottle of water at the temperature of
interest that contains a calibrated thermometer. Agreement between the two
should be within 0.5° C, or the device should be recalibrated.
5.3 Refrigeration units will be monitored daily to ensure proper temperature
requirements are being met. If variances are observed, they must be documented
and a Team Supervisor and/or the Quality Assurance Specialist must be made aware
of the situation and of the samples involved.
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6.0 REFERENCES
6.1 Wisconsin Department of Natural Resources, NR 149.46, Laboratory Certification
and Registration.
6_2 Wisconsin Department of Natural Resources, NR 219.04, Analytical Test Methods
and Procedures.
6_3 Standard Methods of Examination of Water and Wastewater, 201h-22"d Editions.
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Page 8 of 24
Appendix A REgUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIMES FOR WASTEWATER
Note: For reference only. Refer to analyte SOPS for official requirements.
Maximum holding
Parameter numberfname Container Preservation 2.3 time °
Table A—BACNWW Tmtr.
1-5 Coliform, total, fecal, and Z tali
PA, G
Cool, <I 0 -C, 0.0009% 8 hours uz3
NazSz03s
6. Fecal streptococai
PA, G
Cool, <I 0 -C, 0 0008% 8 hours 22
NazSz035
7 Enterococci
PA, G
Cool, <10 -C, 0.000s% 8 hours zz
Na25ZO36
8 mmoerefia
PA, G
Cool, <I 0 -C, 0.0009% 8 hours"
1VazSzO3s
TAblo A—Aquada Tmddly Tied
9-12 Toncity, acute and chronic
P, FP, G
Cool, 5:6 -C ra
36 hours
Table 1�7 wwrEa & Teft
I Acidity
P. FP, G
Cool, 56 °C is
14 days
2. Alkalinity
P, FP, G
Cool, 56 °C 18
14 days
4 Ammonia
P, FP, G
Cool, 56 °C 10, H2SO4 to pH
<2
28 days
9 Biochemical oxygen demand
P, FP, G
Cool, 56 °C
48 hours
11 Bromide
P. FP. G
Nonereautred
28 days
14 Biochemical oxygen demand, P, FP G Cool, 56 °C 18 48 hours
carbonaceous
15 Chemical oxygen demand R FP, G Cool, 56 °C 18, H2SO4to pH <2 28 days
16 Chloride P, FP, G Noneregwred 28 days
17 Chlorine, total residual P. G None regwred Analyze within 15
minutes
21 Color
P, FP, G
Cool, 56 °C is
48 hours
23-24 Cyanide, total or available (or CATC)
and free
P, FP, G
Cool, 56 °C 18, NaOH to pH
> 10 6, reducing agent if
oxidizer present
14 days
25 Fluoride
P
Noneregwred
28 days
27 Hardness
P, FP, G
HNO; or H2SO4 to pH <2
6 months
28 Hydrogen ion (pH)
P, FP, G
None required
Analyze within 15
minutes
31, 43 Kleldahl and organic N
P. FP, G
Cool, 56 °C 19, H2SO4to pH <2 28 days
38 Nitrate
P, FP, G
Cool, 56 °C A
48 hours
39 Nitrate-nitnte
P. FP, G
Cool, 56 °C la, H2SO4to pH <2 28 days
40 Nitrite
P, FP, G
Cool, 56 °C 19
48 hours
41 Oil and grease
G
Cool to 56 °C 18, HCl or
H2504ta pH <2
28 days
42 Organic Carbon
P, FP, G
Cool to 56 °C 18, HCI, H2SO4,
or H3PO4 to pH <2
28 days ..
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Appendix A REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIMES FOR WASTEWATER
Note: For reference only. Refer to analyte SOPS for official requirements.
Maximum holding
Parameter numberiname Container Preservation 2.3 time d
44.Orthophosphate
P, FP, G
Cool, to 56 °C lfia4
Filter within 15
minutes, Analyze
tanthin 48 hours
46. Oxygen, Dissolved (Probe or
G, Bottle and
Nonerequtred
Analyze within 15
Luminescence)
top
minutes
47. Oxygen, Dissolved Winkler
G, Bottle and
Fix on site and store in dark
8 hours
top
48 Phenols
G
Cool, 56 °C e, H2SO4to pH
28 days
<2
49 Phosphorous (elemental) G Cool, 56 °C's 48 hours
50 Phosphorous, total R FP, G Cool, 56'C ls, IW04to pH 28 days
<2
53. Residue, total
P, FP, G
Cool, 56 °C Is
7 days
54 Residue, Filterable S
P, FP, G
Cool, 56 °C e
7 days
55 Residue, Nonfilterable (TSS)
R FP, G
Cool, _<6 °C is
7 days
56. Residue, Settleable
P FP, G
Cool, 56 °C a
48 hours
57 ReslduG Volatile
P, FP, G
Cool, 56 °C sJ
7 days
61 Silica
P or Quartz
Cool, 56 °C 1
28 days
64 Specific conductance
P FP, G
Cool, 56 °C 19
28 days
65 Sulfate
P, FP, G
Cool, 56 °C a
28 days
66 Sulfide
P, FP, G
_
Cool, 56 °C 18, add nnc
acetate plus sodium hydroxide
to off >9
?days O
67 Sulfite P, FP, G None required Analyze within 15
minutes.
68 Surfactants P, FP, G Cool, 56 °C a 48 hours
69 Temperature P. FP, G None required Analyze
73 Turbidity P, FP, G Cool, 56 °C 18 48 hours
Table B—Metals:
10 Boron
P, FP, or uartz
HNO3to H <2
6 months
18. Chromium VI
R FP, G
Cool, 56 °C 18 pH = 9.3-9 721
28 days .
35 Mercury (CVAA)
P, FP, G
HNO3to pH <2
28 days
35 Mercury (CVAFS)
FP, G; and FP-
5 mUL 12N HCl or 5 mUL
90 days 17
lined can 11
BrCI 11
3, B-8, 12, 1 3, 19, 20, 22, 26, 29, 30, 32-34, P, FP, G H NO3 to pH <2, or at least 24 6 months
36, 37, 45, 47, 51, 52, 58-60, 62, 63, 70-72, hours prior to analysis is
74,75 Metals, except boron, chromium VI, and
mercury
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Appendix A REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIMES FOR WASTEWATER
Note: For reference only. Refer to analyte SOPS for official requirements.
Maximum holding
Parameter numberiname ContainerPreservation 2,3 time 0
Table C­Orpnia Tale:
3,4 Acrolein and acrylomtnle
G, FP -lined
Cool, 56 °C 18, 0.008%
l4 days'0
septum
Na2S203, pH to 4-510
119 Adsorbable Organic Halides (AOX)
G
Cool, <6 QC, 0.008%
Hold at least 3 days, but
Na25203HNO3to PH <2
not more than 6 months
114-119 AiXylated phenols
G
Cool, <6 °C, H2SO4to pH <2
28 days until extraction,
40 days after extraction
7,38 Beandines 11. n
G, FP -lined cap Cool, 56 °C 18, 0 008%
7 days until extraction.13
Na3S203s
29, 85-37, 63-65,107 Chlorinated
G, FP -lined cap
Cool, 56 °C 1s
7 days unti I extracti on,
hydrocarbons 11
40 days after extraction
120 Chlorinated Phenolics
Cool, <6 °C, 0 008% Na2S203,
30 days until acetylabon,
_
H2SO4to pH <2
30 days afteracetylahon.
15, 16, 21, 31, 87 Haloethers 11
G, FP -lined cap
_
Cool, 56 °C 18, 0 008%
7 days until extraction,
Na2S2035
40 days after extraction.
54, 55, 75, 79 Nitroaromatics and Isophorone 11 G, FP -lined cap
Cool, 56 °C 18, store in dark
7 days until extraction,
0 0080/6Na2S203s
40 days afterextractiom
82-84 Nitrosamrnes 11,14
G, FP -lined cap
Cool, 56 °C' store in dark,
7 days until extraction,
0 008°/, Na2S2031
40 days after extraction.
88-94 PCBs"
G, FP -lined cap
Cool, 56 °C m
1 year until extraction, I
v ear after extraction.
60.62, 66 72, 85, 86, 95-97, 102, 103
PCDDslPCDFs 11
Aqueous Samples- Field and Lab G Cool, <6 °C 18, 0 008% 1 year
Preservation Na2S2033, pH <9
Solids and Mixed -Phase Samples Field G Cool, 56 °C 18 7 days
Preservation
Tissue Samples Field Preservation G Cool, 56 °C 19 24 hours
Solids, Mixed -Phase, and Tissue Samples
G
Freeze, 5 -10 °C
1 year
Lab Preservation
23, 30, 44, 49, 53, 77, 80, 81, 98, 100, 112
G. FP -lined cap
Cool, 56 °C 1e, 0 008%
7 days until extraction,
Phenols 11
Na2S203
40 days after extraction.
14, 17, 48, 50-52 Phthalate esters it
G, FP -lined cap
Cool, 56 °C 18
7 daysuntil extraction,
40 days after extraction
1, 2, 5, 8.12, 32. 33. 58, 59, 74, 78, 99, 101
G. FP -lined cap
Cool, 56 °C 10, store in dark
7 daysuntil extraction,
Polynuclear aromatic hydrocarbons 11
0 008% 1423S2035
40 days after extraction
6, 57, 106 Purgeabl a aromatic hydrocarbons
G, FP -lined
Cool, 56 °C 18 0 008%
14 days 9
septum
NaaS203s, HCl to pH 2
13, 18-20, 22, 24-28, 34-37, 39-43, 4547, 56,
G, FP -lined
Cool, 56 °C 18, 0 008%
14 days
76, 104, 105, 108-111, 113 Purgeable
septum
Na2S2031
Halocarb ons
Table D-Pesticides Tests
1-70 Pesticides 11
G, FP -lined cap
Cool, 56 °C 18, pH 5-9-15
7 daysuntil extraction,
40 days afterextraction.
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Appendix A REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIMES FOR WASTEWATER
Note: For reference only. Refer to analyte SOPS for official requirements.
Maximum holding
Parameter numberiname ContainerPreservation 2,3 time 4
Table E—Radiological Tests.
1-5 Alpha. beta and radium P, FP, G HNOs to PH <2 6 months
Table H—Bacterial rests:
l E colt PA, G Cool, <10 IQ 0 0008% 8 hours."
Na2S203s
2. Enterococa PA, G Cool, <10 IQ 0 0008% 8 hours.32
Na2S203s
Tame H—Protozoan Tests:
8 0)ptosportalum
LDPE, field 1- l0 °C
filtration
96 hours 71
9.Mara&a LDPE, field 1-10 °C 96 hours7l
filtration
1 "F is for polyethylene; "FP" is fluoropolymer (polytetrafluoroethylene (PTFE), Teflon), or other
fluorupolyme , unless stated otherwise in thisTable F; "G" is glass, "PA is any plastic that is made of astenlizable
material (polypropylene or other autorlavable plastic), "LDPE' is lowdeasity polyethylene.
Except where noted in this table and the method for the parameter, preserve each grab sample within 15
mmutes of collection Fora composite sample collected with an automated sample (e g., using a 24-hour composite
sampler, refrigerate the sample at < 6 °C during collection unless specified otherwise in this table or in the
method(s) For a composite sample to be split into separate aliquots for preservation and/or analysis, maintain the
sample at < 6 Orp unless specified otherwise in this table or in the method(s), until collection, splitting and
preservation is completed Add the preservative to the sample container prior to sample collection when the
preservative will not compromise the integrity of a grab sample, a composite sample, or aliquot split from a
composite sample within 15 minutes of collection.
The temperature of the samples shall be documented upon receipt at the laboratory If the samples are skipped
in crushed or cube ice (not "blue ice parks) and solid ice is still present in the coolm the I ab may simply report the
samples as "received on ice". Iftheice has melted, the lab must reportthe either the temperature ofthe melt• water
or of atemperature blank A temperature blank is defined as an aliquot of deionized water, in an appropriate sample
container, which is transported along with the samples. Since shipping simply with "blue ice" packs does not insure
that samples aremaintaned at the appropriate temperatures, the sample collector must submit a temperature blank
when using these ice packs for shipping
3 When any sampleisto be shipped by common carrier orsentviathe U.S. Postal Service, it must comply
with the Department of Transportation Hazardous Materials Regulations (49 CFRpart 172) The person offering
such material for transportation is responsible for ensuring such compliance. For the preservation requirement; the
Office of Hazardous Materials, Materials Transportation Bureau, Department of Transportation has determined that
the Hazardous Materials Regulations do not apply to the following materials: Hydrochloric acid (HCI) in water
solutions at concentrations of0.04%by weight or less (pH about 1.96 or greater, Nitric acid (HNO3) in water
solutions at concentrations of0.15°roby weight or less (pH about 1.62 or greater), Sulfuric acid (H2SO�) in water
solutions at concentrations of 0 35% by weight or less (pH about 1.15 or greater), and Sodium hydroxide (Na0H) in
water solutions at concentrations of 0 080%by weight or less (pH about 12 30 orless)
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Appendix A REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIMES FOR WASTEWATER
Note: For reference only. Refer to analyte SOPS for official requirements-
4 Samples should be analyzed as soon as possible a$er collection. The times hsted are the maximum tunes that
samples may beheld before the start of analysis and still be considered valid. Samples may be held for longer
periods only if the permittee ormonitoring lab oratory has data on fil a to show that, for the specific types of samples
under study, the analyzes are stable for the longer time, and has received a variance from the EPA Regional
Administrator under s. NR219.05). For a grab sample, the holding time begins at the time of collection. For a
composite sample collected with an automated sampler (e.g., using a 24 -hour composite sampler), the holding time
begins atthe time of the end of collection of the composite sample. For a set of grab samples composnted in the field
or laboratory, the holding time begins at the time of collection of the last grab sample in the set. Some sampl es may
not be stable for the maximum time period given in the table. A perrmittee ormomtonng laboratory is obligated to
hold the sample for a shorter time if it knows that a shorter time is necessary to maintain sample stability See 40
CFR 136.3(e) for details.
s ASTM D7365-09a specifies treatment options for samples containing oxidants (e g., chlorine). Also, Section
9060A of Standard Methods for the Examination of Water and Wastewater (20th and 21st editions) addresses
deciilorin ation procedures.
6 Sample collection and preservation: Collect avolume of sample appropriate to the analytical method in a
bottle o fthe material specified. If the sample can be analyzed within 48 hours and sulfide is not present, adjust the
pH to >12 with sodium hydroxide solution (e g., 5 %wfv), refrigerate as specified, and analyze within 48 hours
Otherwise, to extend the holding time to 14 days and miti gate interference; treat the sample immediately using any
or all of the following techniques, as necessary, followed by adjustment of the sample pH to >12 and refrigeration as
specified.
There maybe interferences that are not mitigated by approved procedures Any procedure for removal or
suppression of an interference maybe employed, provided the laboratory demonstrates that it more accurately
measures cyanide. Particulate cyanide (e.g., ferric ferrocyanide) or a strong cyanide complex (e g., cobalt cyanide)
are more accurately measured if the laboratoryholds the sample at room temperature and pH > 12 fora minimum of
4 hours prior to analysis, and p erforms UV digestion or dissolution under alkaline (pH=12) conditions, if necessary.
Sulfur: To remove elemental sulfur (S8), filter the sample immediately If the filtration tune will exceed 15
minute; use a larger filter or a method that requires a smaller sample volume (e.g., EPA Method 335.4 or Lachat
Method 01). Adjust thepH of the filtrate to >12 with NaOH, refrigerate the filter and filtrate, and ship ortraisport to
the laboratory. Inthelaboratory, extract the filter with 100 mL of 5% NaOH solution foraminimum oft hours.
Filter the extract and discard the solids Combine the 5% NaOH—extracted filtrate with the initial filtrate, lower the
pH to approximately 12 with concentrated hydrochloric or sulfuric acid, and analyze the combined filtrate. Because
the detection limit for cyanide will b e increased by dilution by the filtrate from the sohd; test the sample with and
without the solids procedure if a low detection limit for cyanide is necessary Do notuse the solids procedure if a
higher cyanide concentration is obtained without it. Alternatively, analyze the filtrates from the sample and the
solids separatcl), add the amounts determined (in ger mg). and divide by the original sample volume to obtain the
cyanide con- centration
(1) Sulfide If the sample contains sulfide as determined bylead acetate paper, or if sulfide is known or
suspected to b e present immediately con- duct one of the volatihzahon treatments or the precipitation
treatmentas follows Volatilization—Headspace expelling. In a fume hood orwell— ventilated area,
transfer 075 liter of sampleto a4 4—L collapsible container (e g, CubitainerTM) Acidify with
concentrated hydrochloric acid to pH <2. Cap the container and shake vigorously for 30 seconds Remove
the cap and expel the headsp ace into the fume hood or open area by col- lapsing the container without
expelling the sample. Refill the headspace by expanding the container Repeat expelling a total of five
headsp ace volumes. Adjust the pH to > 12, refrigerate, and ship or transport to the lab oratory scaling to a
smaller or larger sample volume must maintain the air to sample volume ratio A larger volume of air will
result in too great a loss of cyaw de (> 101/61 Dynamic stripping: In a fume hoo d or well ventilated area,
transfer 0 75 liter of sample to a container of the material sp ecified and acidify with concentrated
hydrochloric acid to pH <2. Using a calibrated au sampling pump or flowmeter, purge the aadified
sample into the fume hood or open areaduwgh a flitted glass aerator at a flowrate of 2 25 Llmin for 4
minutes Must the pH to >12, refrigerate, and ship ortransportto the laboratory. Scalmgto asmaller or
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Appendix A REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIMES FOR WASTEWATER
Note: For reference only. Refer to analyte 5OPs for official requirements.
larger sample volume must maintain the air to sample volume ratio Alarger volume of air willresultin
too great a loss of cyanide (> 10%) Precipitation If the sampl a contains particulate matter that would be
removed by filtration, filter the sample prior to treatment to assure that cyanide associated with the
particulate matter is included in the measurement Ship or transport the filter to the laboratory In the
laboratory, extract the filter with I OD mL of 5% NaOH solution for a minimum of 2 hours Filter the
extract and discard the solid& Combine the 5% NaOH-extracted filtrate with the initial filtrate, lower the
pH to approximately 12 with concentrated hydrochloric orsulfuric acid, and analyze the combined filtrate.
Because the detection limit for cyanide will be increased by dilution by the filtrate fmm the solids, test the
sample with and without the solids procedure if a law detection hmit for cyanide is necessary Do not use
the solids procedure if a higher cyanide concentration is obtained withouttt. Alternatively, analyze the
filtrates from the sample and the solids separately, add the amounts determined (in g or mg), and divide
by the original sample volume to obtain the cyanide concentration. For removal. of sulfide by preapitation,
rase the pH of the sample to >12 with NaOH solution, then add approximately 1 mg of powdered
cadmium chlonde for each mL of sample For example, add approximately 500 mg to a 500-ml, sam- pie.
Cap and shake the container to mix Allow the precipitate to settle and test the sample with lead acetate
paper If necessary, add cadmium chloride but avoid adding an excess. Finally, filter through 0 45 micron
filter
Cool the sample as specified and ship or transport the filtrate and filter to the laboratory In the laboratory,
extract the filter with 100 mL o f 5% NaOH solution for a minimum of 2 hours. Filter the extract and
discard the solids Combine the 5% NaOH-extracted filtrate with the initial filtrate, lower the pH to
approximately 12 with concentrated hydrochloric or sulfuric acid, and analyze the combined filtrate
Because the detection linut for cyanide will be increased by dilution by the filtrate form the solids, test the
sample with and without the solids procedure if a low detection lint for cyanide is necessary Do not use
the solids procedure if a higher cyanide concentration is obtained without it. Alternatively, analyze the
filtrates from the sample and the solids separately, add the amounts determined (in g or mg), and divide by
the original sample volume to obtain the cyanide concentration. If a h gand- exchange method is used (e.g.,
ASTM D6888), it may be necessary to increase the ligand exchange reagent to offset any excess of
cadmium chlondt
(2) Sulfite, tlnosulfate,orthiocyanate lfsulfite,thiosulfate;orthiocyanateisknown orsuspected tobe
present, use UV digestion with a glass coil (Method Kelada701) or ltgand exchange (Method OIA-16 7)
to preclude cyanide loss or positive interference.
(3) Aldehyde If formaldehyde; acetaldehyde, or another water-soluble aldehyde is known or suspected to be
present; treat the sample with 20 mL of 3.5% ethyl enediamme solution per liter o f sampl e.
(4) Carbonate Carbonate interference is evidenced by noticeable effervescence upon acidification in the
distillation Bask a reduction in the pH of the absorber solution, and incomplete cyanide spike recovery.
When significant carbonate is present. adjust the pH to 12 using calcium hydroxide instead of sodium
hydroxide Allow the precipitate to settle and decant or filter the sample prior to analysis (also see
Standard Method4500-CN.B.3.d)
(5) Chlorine, hypochlorite, or other oxidant Treat a sample known or suspected to contain chlorine,
hypochlorite, or other oxidant as directed in footnote 57 For dissolved metals, filter grab samples within 15
minutes o f toll ection and before adding preservatives For a composite sample collected with an
automated sampler, filter the sample within 15 minutes after completion of collection and before adding
preservatives. If it is known or suspected that dissolved sample integrity wifi be compromised during
collection of a composite sample collected automatically over time (e.g, by interchange of ametal
between dissolved and suspended forums), collect arid filter grab samples to be comp osited (footnote 2) in
place of a composite sample collected automattcally
T For dissolved metals, filter grab samples within 15 minutes of collection and before adding preservatives
For a composite sample collected with an automated sampler, filter the sample within 15 minutes after completion
of collection and before adding preservatives. if it is known or cusp ected that dissolved sample integrity will be
compromised during collection of composite sample collected automatically overtime (e &. byinterchange of a
metal between dissolved and suspended forms), collect and filter grab samples to be comrposited (footnote 2) in
place of a composite sample collected automatically.
8 Guidance applies to samples to be analyzed by GC, LC, orGC1MS for specific compounds.
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Appendix A REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIMES FOR WASTEWATER
Note: For reference only. Refer to analyte SOPS for official requirements.
9 If the sample is not adjusted to pH < 2, then the sample must be analyzed within seven days of sampling.
to The p H adjustment is not required if acrolein will not b e measured S ample for acrolein receiving no pH
adjustment must be analyzed within 3 days afsampling
I When the extractable analytes of concern fall within a single chemical category, the speilied preservative
and maximum holding times should be observed for optimum safeguard of sample integrity (I.e , use all necessary
preservatives and hold forthe shortest time listed) When the analytes of concern fall within two or more chemical
categories, the sample may be preserved by cooling to <_ 6 cC, reducing residual chlorine with 0 008% sodium
thiosulfatq storing in the dark, and adjusting the pH to 6-9. samples preserved in this manner may be held for seven
days before extraction and for forty days after extraction. Exceptions to this optional preservation and holding time
procedure are noted in footnote 5 (regarding the requirement for tiuosulfate reduction), and footnotes 12, 13
(regarding the an aly sis o f b enndine)
" If 1,2-diphenylhydrazine is likely to be present adjust the pH of the sample to 4 0 f 0 2 to prevent
rearrangement to benzidine
13 Extracts may be stored up to 30 days at < 0 °C
14 For the analysis of diphenylmtrosamine, add 0.008% Na2S203 and adjust pH to 7-10 with NaOH within 24
hours of sampling.
u The pH adjustment may be performed upon receipt at the laboratory and may be omitted if the samples are
extracted within 72 hours of collection For the analysis of aldrin, add 0 0080/6 Na:i%C3
16 Place sufficient ice with the samples in the shipping container to ensure that ice is still present when the
samples arrive at the laboratory However, even if ice is present when the samples arnv4 immediately measure the
temperature of the samples and confirm that the preservation temperature maximum has not been exceeded In the
isolated cases where it can be documented that this holding temperature cannot be met, the permittee can be given
the option of on -ate testing or can request avanance The request for a variance should include supportive data
which show that the toxicity o f the effluent samples is not reduced because of the increased holding temperature.
Aqueous samples must notbe frozen. Hand -delivered samples used on the day of collection do not need to be cooled
to 0 to 6 °C pnor to test initiation.
it Samples collected for the determination of trace level mercury (<100 ng/Q using EPAMethod 1631 must
be collected in tightly -capped fluoropolymeror glassbottles and preserved with BrCI or HCl solution within 48
hours of sample collection. The time to preservation may be extended to 28 days if a sample is oxidized in the
sample bottle A sample collected for dissolved trace level mercury should be filtered in the laboratory within 24
hours of the time of collection However, if circumstances preclude overnight shipment, the sample should be
filtered in a designated clean area in the field in accordance with procedures given in Method 1669 If sample
integrity will not be maintained by shipment to and filtration in the laboratory, the sample must be filtered to a
den gnated clean area in the field within the time period necessary to maintain sample integrity A sample that has
been collected for determination of total or dissolved trace level mercury must be analyzed within 90 days of sample
collection.
1e Aqueous samples must be preserved at <_ 6 °C, and should not be frozen unless data demonstrating that
sample freezing does not adversely impact sample integrity is maintained on file and accepted as valid by the
regulatoryauthonty Also, for purposes of NPDES monitoring, the spea lication of "_< 6 °C" is used in place of the
"4 °C" and "< 4 °C" sample temperature requirements listed in some methods It is not necessary to measure the
sample temperature to three significant figures (11100th of 1 degree), rather, three sigrificant figures are specified so
that rounding down to 6 °C may not be used to meet the 56 °C requirement. The preservation temperature does not
apply to samples that are analyzed immediately (less than 15 minutes)
19 An aqueous sample may be collected and shipped without acid preservation. However, acid must be added
at least 24 hours before analysis to dissolve any metals that adsorb to the container walls If the sample must be
analyzed within 24 hours ofcollectinn, add the acid immediately (see footnote 2) Soil and sediment samples do not
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Appendix A REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIMES FOR WASTEWATER
Note: For reference only. Refer to analyte SOPS for official requirements.
need to bepreserved with and. The allowances in this footnote supersede thepresevation and holding time
requirements in the approved metals methods.
20 To achieve the 28-day holding time, use the ammomum sulfate buffer solution specified in EPA Method
218 6 The allowance in this footnote supersedes preservation and holding time requirements in the approved
hexavalent chromium methods, tint ess this supersession would compromise the measurement in which case
requirements in the metho d must be followed
11 Holding time is calculated from time of sample collection to elution for samples shipped to the laboratory in
bulk and calculated from the time of sample filtration to elution for samples filtered in the field.
' Sample analysis should begin as soon as possible after receipt; sample incubation must be started no later
than 8 hours from time of collection
23 For fecal cols form samples for sewage sludge (bicsolids) only, the holding time is extended to 24 hours for
the following sample types using either EPA Method 1680 (LTB-EC) or 1681 (A-1) Class A composted, Class B
aerobically digested, and Class B anaerobically digested.
24 The immediate filtration requirement in orthophosphate measurement is to assess the dissolved or bio-
available form of orthophosphorus (t e,that whi rh passes through a 0 45-micron filter), hence the requirement to
filter the sample immediately upon collection (f e., within 15 minutes of collection)
0 The sulfide method performed by the MMSD Laboratory, 40 CFR Part 425 Appendix A, has a
48 hour hold time.
Appendix A-1
Sampling and Holding Time Requirements for Chlorophyll Analysis (SM20 Table 1060:1)
• Container — Plastic or glass
• Minimum sample size — 500 mL
• Sample type — grab
• Samples must be filtered within 24-48 hours of collection
• Samples must be analyzed within 28 days of collection
• Unfiltered samples should be kept in the dark at 40C
• Filtered samples should be kept in the dark at -20°C
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Appendix B
Abbreviated Procedure for Receivine Daily Production Samples into LIMS
Daily Plant Samples (wastewater)
1. Be sure you are logged on to the computer in sample receiving with your own name and
password.
2. Open up LIMS —General User Client/Samples/Receive tab.
3. Click on the "Process, Milo, AgriLife and Special Samples" button under "Receive
Samples". The "Receive Process Samples" window opens.
4. In the "Receive Process Samples", in window 1, highlight the Source Codes of all samples
that were received, and click "View Samples."
5. In window 2, highlight the specific samples that were received.
6. In window 3, enter your name, the appropriate date and time, and the sample
temperature or the "On Ice" box. Click the "Received" button.
7. Pop-up boxes will appear for each source code asking for the sample time and flow
(flow for SC 513 & 557).
8. Write all LIMS numbers on each COC sheets, sign, date and time.
The source codes normally received on weekends include:
•
114 — SS
Influent
•
172 —JI
Primary effluent
•
166—JI
Low level influent
•
214 — SS
Primary effluent
•
514 — SS
Effluent
•
551— JI
Effluent
•
557 — JI
Effluent grab
•
513 — SS
Effluent grab
•
167—JI
High level influent
a
198—A
ISS Influent
•
175 — JI
Influent
Milorganite Production Samples
9. Go to the Samples, Receive tab, and click on the "Process, Milo, AgriLife and Special
Samples" button under "Receive Samples". The "Receive Process Samples" window
opens.
10. In the "Receive Process Samples", in window 1, highlight the Source Codes of all
Milorganite samples that were received, and click "View Samples."
11. In window 2, highlight the specific samples that were received.
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12. In window 3, enter your name, the appropriate date and time, and the sample
temperature (for room temperature, enter 20' C.). Click the "Received" button.
13. Go to the "Edit Sample" tab. In the "Select Sample #" tab, enter the LIMS number for
the Milorganite Daily Composite, Source Code 951, and click "Get".
14. In the "Survey ID" box, enter "DM" then the Sample Date in MMDD format, with no
spaces. (Ex: The May 15 sample would be "DM0515".)
15. Click the "Save Edits" button.
16. Pop-up boxes will appear for each source code asking for the sample time.
17. Write all LIMS numbers on each COC sheets, sign, date and time.
"Normal" WEEKEND Source codes
• 951-- Milorganite daily composite
• 986 — Greens grade Milorganite shipment (this does not show up on the report)
• 975 — Milorganite Meehan shipment
Logging In and Receiving Milorganite Shipments
1. Go to the "Log Individual' tab.
2. In the "Sample Info" window, click the drop -down arrow next to the "Use Template" list
box.
3. Highlight the appropriate template for the sample to be logged in. (i.e. "Milo Shipment
Classic 975" or "Milo Shipment GG 987".) and click "Get".
4. Enter your name, the collection date and time.
5. Enter the "MX" or shipment number in both the "Survey Number" and "Conn. Desc"
sections.
6. Enter the Customer Information. Click the "Cust. Info" box. Choose the Customer Name
from the "Consigned To" drop -down list box, or enter the information. Enter the
"Transportation Method": click the drop down arrow and choose or enter the
information (if a "Car Number" is available, it is entered here). Click "Accept".
7. Click "Create Now".
8. Write the LIMS number on the COC sheet.
9. Go to the "Receive" tab and click on the "Process, Milo, AgriLife and Special Samples"
button under "Receive Samples". The "Receive Process Samples" window opens.
10. In the "Receive Process Samples", in window 1, highlight the Source Codes from all
Milorganite samples that had LIMS numbers created and click "View Samples."
11. In window 2, highlight the specific samples.
12. In window 3, enter your name and the sample temperature (for room temperature,
enter 20° C.). Click the "Received" button.
13. Pop-up boxes will appear asking for the sample time. If the sample time has already
been entered, just press the "Enter" key or retype the time.
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Creating the Daily Sample Report
1. Go to the "Reports" tab. In box 1, make sure the month, day and year are correct in
both boxes.
2. In box 2, click the "Received Date(s)" button.
3. In box 3, in the "Sample Status Selection" window, select "Samples Received". In the
"Source Codes" window, select "Plant/Process/Milo".
In box 4, in the "Plant and Process only" box, click "Preview", and check the report for
accuracy. If the report is correct, close the Report preview and click "Print and Email".
Sign the report and staple it to the daily sample COCs.
Using the Flow Compositing Workbook
1. The Flow Compositing workbooks can be found at:
\\Fps04\home IablTechnicallReceivinglFlow Compositingl
2. Open the file for the current year, and go to the correct month spreadsheet to find the
correct date.
3. Enter the Low Level (I-Q, High Level (HL) and ISS figures from the A Daily Flow Sheet.
4. Write down the sample volumes needed to make the composite.
5. Save the spreadsheet and close the workbook.
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Appendix C
Instructions for Thermal Preservation Verification to be Posted in Sample Receiving
If samples that require cooling are not received on ice the temperature of the sample must be
verified and recorded on the COC. Use the temperature blank or a randomly selected sample
and measure the temperature with the pyrometer. (NOTE: If the pyrometer is not available,
use a thermometer and a temperature blank or pour off an aliquot of sample to check. Do not
place the thermometer directly into a sample bottle). The pyrometer should be held a set
distance from the sample to measure the temperature accurately and consistently. Refer to the
pyrometer user manual for more details. Document the temperature on the COC.
Measure the temperature if:
•*e Samples are not received on ice;
Examples should include:
➢ Samples collected on weekends but not delivered until Monday;
➢ Storm waters.
You do not have to measure and record the temperature if:
❖ Samples do not require thermal preservation (e.g. samples for metal analysis);
❖ Samples arrive the day they are collected and they are received on ice.
Examples should include:
➢ Freshwater samples;
➢ Daily plant samples;
➢ Ground waters.
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Appendix D
Instructions for PH Verification, pH Adjustment and Preservation
Samples that call for a specific sample pH and sample preservation should be verified and
adjusted according to the requirements of the analysis method. Record of verifications,
adjustments, and preservations depend on the sample type and analysis. The pH should be
verified using pH paper.
The pH should be verified if:
❖ Samples require chemical preservation (see Appendix A)
❖ Samples should be a specific pH for analysis (e.g. BOD samples)
The pH should not be verified if:
❖ Opening the bottle will compromise the sample integrity (e.g. VOCs, low level mercury,
oil and grease)
❖ Samples for BOD analysis come from natural waters (WQ BOD); BOD is measured with
in -situ pH values.
Verification of BOD: PH between 6-8 (Plant & IW; WQ are natural waters see abovel
If pH verification passes:
- Check the pH verified section of the COC and initial.
If PH verification fails:
- Warm sample to 17-23 "C, record final temperature in the log book.
- Pour off aliquot and take initial reading with pH probe, record in log book.
- Adjust pH to 7.0-7.2 with < 0.5% volume H2SO4 or NaOH accordingly (see chart below).
- Record final adjusted pH in log book.
- Initial the COC.
- Indicate sample has been adjusted on sample bottle for identification by BOD analyst.
Do not dilute the sample > 0.5% volume with preservative: 20 drops of acid/base = 1 mL.
If the sample is diluted > 0.5%, pour off a fresh sample and start again.
Volume of
Sample
Volume of
Preservative
Maximum # of drops
(approximate)
100 mL
0.5 mL
10
25
250 mL
1.25 mL
500 mL
2.5 mL
50
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SOP No.: LPROS-001
Revision: 6.4
Date: 12/7/18
Page 21 of 24
Verification of other samples (preserved before receipt)
Freshwater Samples: TP, NH3, TKN, TOC, NOS < pH 2 with H2SO4; metals < pH 2 with HNO3 j
If PH verification passes:
- Check the pH verified section for each
applicable sample on the COC and initial.
If PH verification fails:
- Initial the COC
- Preserve metals with HNO3
- Preserve all others with H2SO4
- Record in COC notes section
Plant: Ammonia probe, phosphorus, COD, TKN should be preserved to < pH 2 with H2SO4 C
If pH verification passes: If pH verification fails:
- Check the pH verified section for each - Initial the COC
applicable sample on the COC and initial. - Preserve with H2504
- Record in COC notes section
Industrial Waste: TP, Manual Ammonia < pH 2 with H2504
If pH verification passes:
- Check the pH verified section for each
applicable sample on the COC and initial.
If pH verification fails:
- Initial the COC
- Preserve with H2504
- Record in COC notes section
Preservation of other samples (preserved upon receipt)
Plant: Tuesday plant metals
Sample needs to be preserved with HNO3. Sample aliquot is split from unpreserved sample
carboy, preserved with HNO3 and verified with pH paper. Preservation and verification is
recorded in the preservation log book.
Industrial Waste: metals, mercury
When metals or mercury samples are received unpreserved, they are preserved with HNO3 and
verified with pH paper. Preservation and verification is recorded on the generated printout as
well as the preservation log book. In the metals digestion lab all metals samples are rechecked
for a pH of < 2 before aliquoting for digestion. The pH verification is documented on the metals
digestion runsheet. If a sample fails a verification it is noted in the metals preservation logbook
in sample receiving and is preserved with additional HNO3to a pH < 2.
Uncontrolled Document

SOP No.: LPROS-001
Revision: 6.4
Date: 12/7/18
Page 22 of 24
Appendix E
Emailing the Daily Plant Data Report to Veolia on Weekends/Holidays
1. In the LIMS General User client, click on "Results" and click on the "Daily Plant Data"
tab.
2. Check the date range for the report. It is set to go back 14 days from the current date.
3. Click the "Print Plant Report" button. The "rptPlantData" window will open.
4. Click on the email symbol ("J 3) in the task bar or right click on the report and select
"Sent to: Mail Recipient (as attachment)".
S. The "Send Object As" window will open. Select "PDF Format (*.pdf)".
6. An untitled email message with the report attached will open. Complete the email
message to Veolia MKE Shift Supervisors([e-mail]),
and click "Send".
Appendix F
Printine Sample Labels
1. In the LIMS General User client, click on "Samples" and click on the "Receive" tab.
2. Click the "Print Primary Labels" button.
3. Filter the list by selecting the sample status, sample type, and/or date range.
Enna Pnme Labels
i� Select sample(s) ftwn lit below.
iRpn` 150 1BUOB289 A
5114/15
451 15fA]B232 WASComp 5/14/15
6211 MOM SS 5/1�/15
15i1 15001i307 A5/15/15
700 15908308 55 5/15/15
Print Labels mWorSave lnf m thm
o ED
Fiter fist by usk0 the options below. A button that 6 Rdrcd in
ait Ater the ist, out A rat
Sam*Status•. ; C, I L° Rcvd Al
Fv-I-MIREZ
Save Info Phil • Save I ppte Faro
4. Select the sample from the list and click on the "Print + Save" button.
5. Select the label printer, usually'11PS01\LabelLab_3".
6. The label will print all tests listed under the LIMS number.
a. Use a marker to cross out any tests that are not required if the sample is split for
different analyses. Duplicate labels can be printed by following the steps above.
b. If there is an issue printing labels write the sample ID, sample collection
date/time, the required tests, and sample preservative (if applicable) on a label
or directly on the sample bottle.
Uncontrolled Document
5114/15
451 15fA]B232 WASComp 5/14/15
6211 MOM SS 5/1�/15
15i1 15001i307 A5/15/15
700 15908308 55 5/15/15
Print Labels mWorSave lnf m thm
o ED
Fiter fist by usk0 the options below. A button that 6 Rdrcd in
ait Ater the ist, out A rat
Sam*Status•. ; C, I L° Rcvd Al
Fv-I-MIREZ
Save Info Phil • Save I ppte Faro
4. Select the sample from the list and click on the "Print + Save" button.
5. Select the label printer, usually'11PS01\LabelLab_3".
6. The label will print all tests listed under the LIMS number.
a. Use a marker to cross out any tests that are not required if the sample is split for
different analyses. Duplicate labels can be printed by following the steps above.
b. If there is an issue printing labels write the sample ID, sample collection
date/time, the required tests, and sample preservative (if applicable) on a label
or directly on the sample bottle.
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SOP No.: LPROS-001
Revision: 6.4
Date: 12/7/18
Page 23 of 24
Appendix G
Filtering Samples for Soluble Analyses
Certain samples collected for soluble analyses that are not filtered in the field are filtered in the
sample receiving area, such as groundwater or special project samples. Freshwater samples are
filtered with chlorophyll analysis and are not described here.
Equipment and Supplies:
1. Filters, large pore >0.45 µm, 47 mm diameter, glass microfiber without organic binder.
2. Filters, fine pore 0.45 µm, 47 mm diameter.
3. Filtration apparatus with 47 mm membrane filter funnels.
4. Laboratory vacuum supply or vacuum pump.
5. Vacuum flask of adequate size to contain the sample to be filtered.
6. Vacuum tubing, Tygon E-3606 NSF or equivalent, 3/8" inside diameter.
Procedure:
1. Assemble filtration apparatus, beginning with the large pore filters.
2. Dispense the sample into the filtration apparatus and filter the sample through the glass
microfiber filter. If filtration time exceeds 5 minutes, select a smaller volume of sample
and process using a new filter. Once the filter becomes too clogged to continue filtration
replace with a fresh filter, disposing of the used filter. Continue dispensing sample
through filtration apparatus until entire sample has been filtered.
3. Replace vacuum flask with a clean flask, assemble filtration apparatus with a fine pore
0.45 µm filter.
4. Dispense the sample into the filtration apparatus and filter. If filtration time exceeds 5
minutes, select a smaller volume of sample and process using a new filter. Once the
filter becomes too clogged to continue filtration replace with a fresh filter, disposing of
the used filter. Continue dispensing sample through 0.45 µm filters until entire sample
has been filtered.
5. Transfer sample to appropriate container and preserve as specified by the test method.
Uncontrolled Document

SOP No.: LPROS-001
Revision: 6.4
Date: 12/7/18
Page 24 of 24
Appendix H
SOP Editorial Chanees and Revisions
SOP Revision Updates/Editorial Changes
Date: 11/13/18
Revision ID: 6.4
Reason for change: Update SOP in response to DNR assessment and for minor editorial changes.
Change: Updated Appendix A to add footnote about the MMSD sulfide method hold time and
Appendix D to revise the metals pH verification procedure.
Signatures
Updated "Water Quality" samples to "freshwater" samples throughout the document.
Minor editorial changes to wording in sections: 2.2, 3.2, 4.1, 4.2, 4.4.1, 4.5,
Appendices A, A-1, and D.
Added Appendix G: Filtering Samples for Soluble Analyses
Laboratory manager sig ure
QA Speclat4t signature
Uncontrolled Document

Appendix 8
Chain of Custody Templates

Milwaukee Metropolitan Sewerage District Central laboratory - Chain of Custody
(PIeaSe Print clearly)
Client
Project Name:
Project Conta ct:
Contact Pho ne Mum her;
6rab/[emposke I .�
I RdWq—hed ar:
Rely Irqul�ned 81Y_
WIrApilshed 09:
bate/Yme�
wre/n�„e:
�Dabl Tl roe:
Sample Type/
Wcation:
Date Needed:
Sampled By:
(PKM)
Sampled By:
(Srsna[ure]
-Matrix- GW.Gr MwHer, 5w=ylrytr water; WV&WaM weer, k-&cdse:5p•5pld
1=14 n ; NIAC; 5diy50y o.NNoi s•HeOFI:NNh5�0:; 7-her
INNSD
Horn Rr � way wweaaan
a
a
k
Cf(aettLvrsunaMs
LIMS M / Lab Commanls
�a
I
_ pn lCe7 _ TFS 1 N0, _
R-1a.8w10 4

CHAIN -OF -CUSTODY 1 Analytical Request Document
. .. la till3�J/flCat T e CMn-of-CUMody S a LE GAt. D00-MmT All r•r.vem Was must be o mplKW as ""iy
OIL
SAMPLE ID
'urmun kys er WY�wmerwm mu.i.aoa.a[rq vacex rrerso e.rny.�.mw�.�.ma.r..�s mrieemrgesbrsz oer mane,k .nr�..o.es .uwa �=ao o.n F-ALL-W20rev 08. 12.00-=7

TestAmerica Chicago
2417 Bond Strom
Attn: Sandra Fredhak
Unirersily Park, IL 60484
nhone 708.5U 5200 fax 70A 53A Si Ri
TestAmedca
Chain of Custody Record 7kE LEADER iH EMVIRONNENTALIESriNa
Client Canna of
Project Manger Both Sawn Site
Contact:
Ilntc•
COC No.
YgvrCompany Narm here MMS❑
T&Fan:414-22S.2171 Loh
Contact:
farrier:
of _ COCS
dress 26D W Seeboth
Ana is To around Time
E
i
Job No-
C *wt&Zip MilwaaukeC. WI
Calendar [ C ) Of WDrk Days (W) W
[phone] Phone
TATirdiiftwi f m H,mw
0 2 ys
O t week
d 2 days
0 I day
(4141 225-2266 FAX
SOG No
Prgeet Name:
57N'
P OO
58mpler
Sample identif"lion
Sample
Oate
Sanpk
Tiace
Sample
Type
Ustrix
v a
ems.
Sam k S ific Ndes
Preservation Uwd: 1= Im 2- HO; 3- H2SO4; 4-HNO& S-NaOH; 6- Oeher
srlNe Nawrd I& ngfkadsa
= Nniv H=Urrl = Ilfummohlr 0 skni I,". I4rrsrra v L= link- �
Semple Dkrm al fA fee may be assessedBf samples ere retained►an9w than I man
�Return TO Ckeni � Disposal By Leh � Archive For 6fpneh5
Softio lnstructiffOC Requirements& Comments:
Relinquished by
company
Daltr Time
Ruin ved by.
Company
Datdtime.
Relinquished by.
Company.
17aWd17me
Received by:
Company
DIWTimc:
Relinquished by.
CDmpanv
Drlefrime
Reaeisrd by:
Company:
Date Time
Forst Na CA-C-WI-002, Rv.3.1, dated OR212012

Appendix 9
Summary of Biosolids Analytical Methods, Holding Times,
Preservation, and Frequency of Analysis

Fre uenc
Parameter
parameter
Method
Hold Time
Preservation
Milorganite
Milorganite
Milorganite
South Shore
Category
Production
Shipping (Outfall
Bagging
Cake (Outfall
Outfall006
008)
(Outfall009
005
Nutrients
MangenTotal
AOAC (16) 955.04
NA
Monthly
al'
NA
Nitrogen, Total
AOAC (18) 993.13
NA
Daily
(Auto)NA
Every Shipment
Nitrogen,
AOAC (13) 2.065
NA
Monthly
Ammonia
NA
Per Run
Nitroe n
AOAC (16) 930.01
NA
Monthly
Nitro
NA
Nitrogen, Total
351.2
28 Days
NA
Quarterly
ICeldahl
Per Run
Nitrogen, Water
Calculated
NA
Monthly
Insoluble
NA
Phosphorus,
SW846:6010C
Daily
Total
28 Days
NA
Every Shipment
Per Run
Phosphorus,
Water
WDNR Guidance
NA
6 months
Monthly
Extractable
Per Run
Available P2O5
Calculated
NA
NA
Every Shipment
Insoluble
Calculated
NA
NA
Phosphorus
Every Shipment
Potassium,
SW846: 6010C
6 months
Daily
Total
NA
Per Run
8 Hours total
6 Hours
transport
Pathogens
Fecal Coliform
EPA 1680
time
<10°C
Weekly
Monthly
Monthly
Per Run
2 hours
processing
time
Metals
Aluminum
SW846: 6010C
6 months
NA
Monthly
Antinomy PP
SW846: 6010C
6 months
NA
2x/ ear
Arsenic
SW846: 6010C
6 months
NA
Daily
Per Run
Beryllium PP
SW846: 6010C
6 months
NA
2x/ ear
Boron
SW846: 6010C
6 months
NA
Monthly

Calcium
SW846: 6010C
6 months
NA
2x/year
Cadmium PP
SW846: 6010C
6 months
NA
Daily
Every Shipment
Per Run
Chromium PP
SW846: 6010C
6 months
NA
Monthly
Every Shipment
Cobalt
SW846: 6010C
6 months
NA
Monthly
Copper(PP)
SW846: 6010C
6 months
NA
Daily
Per Run
Iron
SW846: 6010C
6 months
NA
Daily
Every Shipment
Lead PP
SW846: 6010C
6 months
NA
Daily
Per Run
Magnesium
SW846: 6010C
6 months
NA
2x/year
Manganese
SW846: 6010C
6 months
NA
2x/year
Mercury PP
SW846 7471 B
28 days
NA
Weekly
Per Run
Molybdenum
SW846: 6010C
6 months
NA
Daily
Per Run
Nickel PP
SW846: 6010C
6 months
NA
Daily
Per Run
Selenium PP
SW846: 6010C
6 months
NA
Daily
Per Run
Sodium
SW846: 6010C
6 months
NA
2x/year
Silver PP
SW846: 6010C
6 months
NA
2x/year
Thallium PP
SW846: 6010C
6 months
NA
2x/year
Zinc PP
SW846: 6010C
6 months
NA
Daily
Per Run
H
pH
SW846:9045D
NA
NA
Weekly
PCB
Aroclors
EPA 8082
365 Days
4°C
Daily
Once per permit
TEQ
Dioxins,
Furans, PCB
Congeners
SW 846:8290, EPA
1668A
365 Days
4°C
Monthly
Solids
% Moisture
SM 2540 G 1997
7 Days
4°C
Daily
Every Shipment
Per Run
% Total
SM 2540 G 1997
7 Days
4°C
Monthly
Monthly
Per Run
% Volatile
SM 2540 G 1997
7 Days
4°C
Monthly
VOC
8260C
14 Days
4°C
2x/year
AL
Priority
SVOC Acid
Extractable
8270D
14 Days
4°C
2x/year
Pollutants
SVOC Base
neutral
8270D
14 Days
Extract; 40
Analyze
4°C
2x/year
Pesticides
8081 B
14 Days
Extract; 40
Analyze
4°C
2x/year
Cyanide PP
9012B
14 Days
4°C
2x/year