HomeMy WebLinkAboutNC0024252_Compliance Schedule_20171115CITY OF C O N O V E R PUBLIC WORKS DEPARTMENT
P.O. BOX 549 Phone 828-464-4808
CONOVER, NC 28613-0549
November 15, 2017
Mr. Ron Berry RECEIVCDINCDENWR
NCNR/Water Quality
NPDES Unit NOV 21 2017,
1617 Mail Service Center Water Quality
Raleigh, NC 27699-1617 Permitting Section
Dear Mr. Berry:
In order to comply with the NPDES permit issued and effective on
December 1, 2016 for the City of Conover Northeast Wastewater
Treatment Plant NCO024252 under section A.(6)COMPLIANCE SCHEDULE
FOR TOTAL COPPER, we wish to report on our present efforts to
assure clean sample collection and quality lab control. I feel
our past problem with higher than normal levels of copper were
few and sporadic and we have not conclusively identified the
cause. Since the issuance of our present permit we have been in
total compliance with the issued copper limit. We are concerned
with sample contamination and laboratory quality control and I
have attached some sample collections practice and procedure and
laboratory quality control statements with this correspondence.
Our samples are collected in single use, sterile FDA approved
bags which line our sampler jugs. The samples are then
transferred to single use food grade bottles for transportation
to the laboratory. All of our personnel collecting samples are
nonsmokers. Our samplers and lines are cleaned on a routine
basis to eliminate the possibility of contamination. We have our
copper samples analyzed by a contact laboratory, Research and
Analytical Labs. Attached is quality control information from
the lab. We hope that if the past spikes in copper were caused
by contaminated samples or laboratory contamination our review
and oversite has eliminated future problems.
In the event you have questions comments, or need further
information please call me at (828) 465-2279.
Sincerely,
Michael Fox
Wastewater Treatment and
Collection Supervisor
A. (6)CO143NIPLL&NCE-215A(b)] SCHEDULE FOR TOTAL COPPER
[G,9,
1. No latcr than November 30, 201 1, the Pernilttee shall:
a. Improve and impletnent "clean" techniques, Some steps that can be invetigated:
0 Discuss procedures, wi(h Qontraaed lab to ensure eliminabon of potential
contaminationsou,rce�,
a Fxamlne basic sampling handling processes (field sampling, laboratory haiid] inn
and anal�rsis)
0 Examine sampling equipment clecmiiig procedures
reagent quality)
a Ensure that sampling persomiel are non-smokers.
b, S-Libmit to the Division of Water lke�sources a report surnm2-1-lizint
,; impmvetnnts. and stating if
the actions taken will enable the Permittee to achieve coi-ripliance with the Total Coj)per-
Limits at Oud'all 001 withi'mit ficulher actions.
CONOVER NEWWTP SAMPLING SOP 11/2017
Compliance schedule for Total Copper Sampling
The effluent sampler is set up in the lab building, and is a dipper type sampler. A line runs from the
effluent sampler pump to the lab and the effluent pump runs continuously.
The effluent sampler is paced to take samples only when water is flowing through the effluent
discharge. Once each week the operator turns the effluent pump on and off a few times to backwash
the effluent sampler line to keep solids from accumulating in the line. The sampler is cleaned daily of
any buildup of solids or organic matter.
For metals sampling, the sampler jugs are lined with new, single use disposable food grade plastic bags.
Sampling is done by lab personnel trained in SOP procedures and include using clean latex gloves.
The operators are non-smokers and wear clean, disposable latex gloves during sampling. Metal samples
are collected in clean, single use plastic bottles provided by the contract lab. The samples are preserved
to pH <2 with Nitric acid and stored in a refrigerator. They are picked up by the contract lab in a manner
to ensure all holding times are maintained. Proper documentation is maintained with Chain of Custody
documents properly filled out and stored according to state guidelines.
Evan Rubins
City of Conover Pretreatment and sample collections specialist
SAMPLING PROCEDURES AND HANDLING
Sample containers are preserved in the laboratory unless a client instructs
otherwise It is acceptable for samples to be preserved in the field at the
time of collection Additionally, some samples may be preserved in the
laboratory after collection if the samples can be kept on ice and if the
preservatives are added within 4 hours of collection
Written sample instructions are available to clients Instructions available
for clients include by are not limited to bacteriologicals, wastewater
composites and grabs, volatile and semi -volatile collection, stormwater, and
groundwater monitoring. Other sampling procedures can be developed on a
case by case basis Water Tech personnel are available to provide sampling
assistance Some Water Tech personnel have been trained in drinking water
and wastewater collection
CHAIN OF CUSTODY PROCEDURES
Chain of custody (COC) procedures are used to verify the client, project,
sampler, date and time of collection, type of sample (composite or grab),
type and number of containers, test parameters needed and preservatives
used The laboratory verifies the holding times, preservatives, pH, and total
chlorine residuals of any samples upon receipt in the laboratory If the COC
form is correct and all sample validity requirements are met, the samples are
accepted by the check-in person for check-in and identification If there are
any questions about the COC, the client is notified and the check-in person
makes a note of comments in the comment sections of the COC form
SAMPLE CHECK-IN AND HANDLING
Upon receipt in the laboratory samples are checked -in The purpose of the
check-in step is to verify that the temperature reflects a downward trend in
temperature, samples are properly preserved, and that holding times have
not been exceeded A COC document should accompany each sample A
COC document is used to provide information about the clients' name, date
and time samples were collected, description of samples collected, type of
containers used (i e glass or plastic), tests that are requested for analyses,
and what preservatives were used
The check-in person should complete the following steps to check-in
samples
1) Open the cooler and examine contents for the presence or
absence of ice Measure the temperature of the samples by
inserting a pre -calibrated thermometer into a temperature blank
Water Tech Labs bottle provided in the cooler The thermometer is allowed
PO Box 1056
Granite Falls, IVC 28630 4
I
adequate time for the temperature to stabilize, 1-2 minutes. Temperature is
recorded on the COC Temperature must be <6°C. For grab samples taken
within 30 minutes of arrival at the laboratory and received on ice, the temperature
minimum is waived but noted on the COC. If the grab sample temperature was
taken in the field, recorded on the COC and arrives on ice at the laboratory with a
temperature >6°C, the downward trend in temperature from the field to the
laboratory is noted on the COC. In lieu of temperature blank and glass
thermometer, an infrared laser thermometer may be used — carefully point laser
into sample and read
2 Check the pH of the samples by using pH paper. Check for correct sample
preservation. See attached preservative requirements in the Appendix. Note the
preservatives used by checking the appropriate preservative on the COC.
Confirm that samples are received with the required holding time Reference the
holding time list in the Appendix. If information is missing call the client and
obtain information. If you are unable to reach the client, proceed with check-in so
that the samples can be processed as quickly as possible. If samples have
exceeded their holding time, do not analyze the samples without expressed verbal
or written permission of the client. Exception: If receipt of samples is delayed
due to inclement weather, Water Tech will accept fecal coliform samples whose
holding time may have expired. Note such conditions on the chain of custody.
The final report will also reflect that the samples were analyzed out of hold time
due to inclement weather.
4 Examine COC to ensure sample test parameters are clearly recorded and that each
parameter requested on the COC has a corresponding sample container. Match
COC entries with sample bottles received. If information is missing or sample
bottles are missing, the client is notified immediately.
5. Samples are distributed to the appropriate analysts for immediate analysis or to
re$7gerated storage (<4°C) to be analyzed at the appropriate time within sample
holding time requirements.
6 The laboratory should reject any sample taken for compliance purposes which
does not meet the specifications for containers and preservatives, holding times,
proper collection and/or transport, or completion of appropriate sections of report
form.
7 Samples improperly collected, handled, preserved, documented or out of holding
time are rejected
8. For rejected samples, a resample is requested. If re -sampling is not possible and
the sample is analyzed, the sample data is clearly identified in the data packet and
on the final report as being unusable for compliance purposes.
SAMPLE DISPOSAL
The analyst will dispose of samples after all assigned tests have been completed. If
questions exist concerning proper disposal of samples, the lab supervisor will be notified
so that proper disposal techniques can be identified.
5
SAMPLE PRESERVATION
Once the sample has been collected, it should be analyzed as quickly as possible or
preserved and stored in a container in an attempt to maintain the sample integrity.
Complete preservation procedures are an attempt to modify (retard or stop) the chemical
and biological changes that can occur after the sample has been collected and placed in a
storage container. Approved methods of preservation are pH control, chemical addititon,
refrigeration, and freezing in an attempt to (1) slow biological reactions, (2) control
chemical reactions (hydrolysis, oxidation, reduction, etc.), (3) reduce volatility, and (4)
reduce adsorption of the components of interest
Recommendations for Preservation of Samples
Vol.
Recommended
Req
Holding
Measurement
ml
Container (a)
Preservative
Time (b,c,d)
Physical Properties
Conductance
100
P,G
Cool, 4°C
28 days(e)
pH
100
P,G
Determine on site
15 minutes
Residue
Filterable
500
P,G
Cool, 4°C
7 days
Non -filterable
500
P,G
Cool, 4°C
7 days
Total
500
P,G
Cool, 4°C
7 days
Volatile
100
P,G
Cool, 4°C
7 days
Settleable Matter
1000
P,G
None required
48 hours
Temperature
100
P,G
Determine on site
No holding
Turbidity
100
P,G
Cool, 4°C
48 hours
Metals
Dissolved
200
P,G
Filter on site
6 months( f)
HNO3 to pH <2
Suspended
200
Filter on site
6 months
Total
100
P,G
HNO3 to pH <2
6 months( f)
Hardness
200
P,G
Cool, 4°C
6 months( fl
HNO3 to pH <2
Mercury
Dissolved
100
P,G
Filter on site
28 days
HNO3 to pH <2
Total
100
P,G
HNO3 to pH <2
28 days
Inorganics,
Non -Metallics
Acidity
200
P,G
Cool, 4°C
14 days
Alkalinity
200
P,G
Cool, 4°C
14 days
Chloride
200
P,G
None required
28 days
Chlorine
200
P,G
Determine on site
No holding;
Analyze
immediately
Cyanides
500
P,G
Cool, 4°C
14 days
NaOH to pH 12
Fluoride
300
P
None required
28 days
Nitrogen, Ammonia
400
P,G
Cool, 4°C
28 days
H2SO4 to pH <2
Kjeldahl, Total
500
P,G
Cool, 4°C
28 days
H2SO4 to pH <2
Nitrate plus Nitrite
200
P,G
Cool, 4°C
28 days
H2SO4 to pH <2
OA
Organics
BOD
Vol.
P,G
Cool, 4°C
Recommended
COD
Req.
P,G
H2SO4 to pH <2
Holding
Measurement
ml
Container (a)
Preservative
Time (b,c,d)
Nitrate
200
P,G
Cool, 4°C or
48 hours
Organic carbon
200
S
Chloroform, 4°C
28 days
Nitrite
100
P,G
Cool, 4°C or
48 hours
MBAS
250
P,G
Chloroform, 4°C
48 hours
Dissolved Oxygen
Probe
300
G only
Determine on site
No holding;
BOD bottle
analyze
immediately
Winkler
300
G only
Fix on site
4 — 8 hours,
BOD bottle
after acidified
Phosphorus
Orthophosphorus
Dissolved
100
P,G
Filter on site
48 hours
Cool, 4°C
Hydrolyzable
100
P,G
Cool, 4°C
48 hours
H2SO4 to pH <2
r
� Total Phosphorus
Total
100
P,G
Cool, 4°C
24 hours
H2SO4 to pH <2
Dissolved
100
P,G
Filter on site
24 hours
Cool, 4°C
H2SO4 to pH <2
Silica
100
P only
Cool, 4°C
28 days
Sulfate
100
P,G
Cool, 4°C
28 days
Sulfite
100
P,G
Determine on site
No holding;
analyze
immediately
Organics
BOD
1000
P,G
Cool, 4°C
48 hours
COD
100
P,G
H2SO4 to pH <2
28 days
Oil and Grease
1000
G only
Cool, 4°C
28 days
MSOatopH<2
Organic carbon
200
S
Cool, 4°C
28 days
H2SO4 to pH <2
MBAS
250
P,G
Cool, 4°C
48 hours
�-qj
(a) Plastic (P) or Glass (G). For most metal, polyethylene with a polypropylene cap (no liner) is
preferred.
(b) It should be pointed out that holding times listed are recommended for properly preserved
samples based on currently available data. It is recognized that for some sample types,
extension of these times may be possible while for other types, these times may be too long
Where shipping regulations prevent the use of the proper preservation technique or the
holding time is exceeded, such as the case of a 24-hour composite, the final reported data for
these samples should indicate the specific variance.
(c) Standard Methods for the Examination of Water and Wastewater, American Public Health
Association, Washington DC.
(d) EPA. Methods for Chemical Analysis of Water and Wastes. U.S. Environmental Protection
Agency, EPA -690/4-79-020, Cincinnati, OR
(e) If the sample is stabilized by cooling, it should be warmed to 25°C for reading, or
temperature correction made and results reported at 25°C.
(fl Where HNO3 cannot be used because of shipping restrictions, the sample may be initially
preserved by icing and immediately shipped to the laboratory. Upon receipt in the
laboratory, the sample must be acidified to a pH < 2 with HNO3 (normally 3 ml 1 + 1
HNO3/L is sufficient). At the time of analysis, the sample container should be thoroughly
rinsed with 1 + 1 HNO3 and the washings added to the sample (volume correction may be
required)
HOLDING TIMES & PRESERVATIVES--NPDES PARAMETERS
PARAMETER
PRESERVATIVE
CONTAINER
HOLDING TIME
Ammonia
H2SO4
PL
28 days
COD
H2SO4
PL
28 days
NC2+NO3
H2SO4
PL
28 days
Phenol
H2SO4
GL- Amber
28 days
Phosphorus, Total
H2SO4
PL
28 days
TKN
H2SO4
PL
28 days
TOC
H2SO4
GL
28 days
TOX
H2SO4
GL
28 days
Cyanide
NaOH/ AA
PL
14 days
Sulfide
NaOH/ Zn Acetate
GL
7 days
Fecal Coliform Bacteria
Na Thiosulfate
PL- Sterile
8 hours
Total Coliform Bacteria
Na Thiosulfate
PL- Sterile
8 hours
Hardness
HNO3
PL
28 days
Metals (except Mercury)
HNO3
PL
6 months
Mercury
HNO3
PL
28 days
Metals for DWQ GW
HNO3
PL
Special 3030C Digestion
within 72 hours
Oil & Grease
H2SO4
GL
28 days
VOCs: 524.2/ 624/ 8240/
8260/ 601/ 602/ 8010/ 8020/
BTEX
HCL
GL- VOA vial
14 days
Alkalinity
NP
PL
14 days
BOD & CBOD
NP
PL
48 hours
Chloride
NP
PL
28 days
Chlorine Residual, Total
NP
PL
Immediate- Field
Chlorophyll a
NP
PL- Amber
Filter within 24 hours
Color
NP
PL
48 hours
Conductivity
NP
PL
28 days
Dissolved Oxygen
Immediate- Field
Fluoride
NP
PL
28 days
Herbicides: 615/ 8150/ 8151
NP
GL- Amber
7 days
MBAS
NP
PL
48 hours
NO2
NP
PL
48 hours
pH - Field
NP
PL
Immediate- Field
pH - Lab
NP
PL
Immediate
Orthophosphate
NP
PL
48 hours
Pesticides/PCBs- 608/ 8140/
8141/8080/8081
NP
GL- Amber
7 days
Semivolatiles- 625/ 8270
NP
GL- Amber
7 days
Solids- Dissolved (TDS)
NP
PL
7 days
Solids- Settable
NP
PL
48 hours
Solids- Suspended (TSS)
NP
PL
7 days
Solids- Total (TS)
NP
PL
7 days
Solids- Volatile Suspended
NP
PL
7 days
Solids- Volatile Total
NP
PL
7 days
Sulfate
NP
PL
28 days
Temperature
Immediate- Field
TPH 8015- 3550/ 5030
NP
GL
7 days
Turbidity
NP
PL
48 hours
Water Level
Field
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QC Excerpt of doe L.) lrleA-"
SOP for Metals Analyses by ICP -MS Doc#MA00101.ra
Date: Feb 2017
9.2 Initial Calibration Curve
9.2.1 A blank and at least three calibration standards must be prepared and
analyzed daily. These standards will include the highest and lowest
concentrations of the calibration curve for each analyte. The Standards
Formulation Chart for all analytes can be found in Appendix I of this SOP.
The correlation coefficient of the curve must be 0.995 or greater.
9.2.2 The instrument performance check (IPC) is used to determine
the instrument performance and verify that the instrument is properly
calibrated. The IPC is a mid-range standard analyzed immediately after
calibration. The analysis of all analytes within the standard solution must be
within ±10% of calibration. If not, the instrument must be recalibrated.
9.2.3 After the analysis of the IPC, a Quality Control Standard (QCS) sample is
analyzed daily. The recovery of the sample must fall within +/- 10% of the
true value in the check sample. If this criteria is not met, corrective action
must be taken. If corrective action does not solve the problem, the
calibration curve and the QCS must be reanalyzed.
9.2.4 After the analysis of the QCS, an Initial Calibration Blank (ICB)
must be analyzed. The concentration of the ICB must be less than or equal
to one half of the low standard. If this criteria is not met, corrective action
must be taken.
*When analyzing samples using SW -846 Method 6020B, the following criteria must be
added:
9.2.5 After the initial calibration curve is completed the Spectral
Interference Check (SIC) is analyzed. The concentration of all elements
NOT included in the SIC solution must be no more than two (2) times the
LLOQ value of each element. If this criteria is not met, corrective action
must be taken.
9.2.6 After the initial calibration curve is completed the Lower Limit of
Quantitation (LLOQ) check sample must be analyzed on a quarterly basis, at
a minimum. The recovery of this sample must fall within ±35% of the true
value and have a RSD of <20%. If this criteria is not met, corrective action
must be taken.
9.3 Continuing Calibration Verification
9.3.1 The accuracy of the calibration curve must be verified throughout the
analysis by a Continuing Calibration Verification sample once every 10
samples and at the end of a run sequence. The percent recovery of the CCV
must fall within +/- 10% of the true value of the CCV. If this criteria is not
met, corrective action must be taken. If corrective action does not solve the
problem, the analyses must be terminated, the instrument must be
recalibrated, and the preceding samples must be reanalyzed.
9.3.2 Immediately after the analysis of the CCV, a Continuing Calibration
Blank (CCB) must be analyzed. The CCB must be less than or equal to one
half of the low standard concentration.
NOTE: All analytical sequences must end with a CCV and CCB. Samples must be
bracketed by acceptable CCV and CCB values.
11.0 QUALITY CONTROL
11.1 The instrument detection limit (IDL) is used to characterize the instrument
performance by the statistical analysis of multiple reagent blank samples. This shall
be run when there are major changes to the method or instrumentation.
11.2 The method detection limit (MDL) determination is used to establish the lowest
verifiable detection limit for each analyte for the instrument. The MDL is a
statistical analysis of multiple low standard samples. This must be run annually or
when there are major changes to the method or instrumentation. When using SW -
846 Method 6020B for analysis, this limit is described as the Lower Limit of
Quantitation (LLOQ) and is to be established initially and then verified at least
quarterly. The LLOQ verification must have a concentration recovery of ±35% and
a RSD of <20%.
11.3 The initial demonstration of capability (IDOC) is used to prove the ability of the
analyst to produce precise and accurate results. The IDOC is a statistical analysis of
four LFB standard samples. This must be run by any analyst using the instrument
before proceeding with sample analysis.
11.4 The Spectral Interference Check (SIC) is used when using SW -846 Method 6020B
to demonstrate the appropriate magnitude of interferences and provide an adequate
test of any corrections.. The concentration of all elements NOT included in the SIC
solution must be no more than two (2) tunes the LLOQ value of each element.
11.5 Laboratory Reagent Blanks or Preparation Blanks (LRB or PB)
A Laboratory Reagent Blank or Preparation Blank is reagent grade water that is
digested or prepared and analyzed with each batch of 20 or fewer samples. It is
treated exactly as a sample including exposure to all glassware, equipment, solvents,
reagents, and internal standards that are used with other samples. The LRB/PB is
used to determine if method analytes or other interferences are present in the
laboratory environment, reagents, or apparatus. The concentration of the preparation
blank must be less than or equal to one half of the low standard concentration. The
LRB/PB may be re -analyzed once. If corrective action does not solve the problem,
all corresponding samples must be redigested and reanalyzed.
11.6 Matrix Spike and Matrix Spike Duplicate Samples (MS/MSD)
A sample is spiked with a known concentration of analytes prior to digestion every
batch of 10 samples of a similar matrix and duplicated. The percent recovery of the
spike compounds must be between 70% and 130%. If the recovery of any analyte
falls outside the designated range and laboratory performance for that analyte is
shown to be in control, the recovery problem is judged to be matrix related. The
data user should be informed that the result for that analyte in the sample is suspect
due to the nature of the sample or an uncorrected matrix effect. The relative percent
difference between the MS and MSD must be ±10%.
11.7 Laboratory Fortified Blank (LFB)
A LFB is a mid-range standard that is digested with each batch of samples. The
percent recovery of the compounds present in the LFB must be within 85% and
115% recovery. If not corrective action must betaken. If corrective action does not
solve the problem, all corresponding samples must be redigested and reanalyzed.
11.8 Internal Standard: The internal standard is added to all samples, extracts and
standard solutions via peristaltic pump during analysis. It is used to measure the
relative responses of analytes in a multi -analyte method that are components of the
same sample or solution. The percent recovery of the internal standard must be
between 60% and 125%. When EPA SW -846 Method 6020B is being used, the
internal standard recovery must be no less than 70%. If not, corrective action must
be taken. If corrective action does not solve the problem, then the sample must be
redigested or diluted.