#5342_0825_FINAL

MCDENR
North Carolina Department of Environment and Natural Resources
Pat McCrory
Governor
September 11, 2015
5342
j,Ms. Cheryl Johnson
Pace Analytical Field Services
!9800 Kincey Avenue - Suite 100
Huntersville, NC 28078
Donald R, van der Vaart
Secretary
Subject: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC)
Maintenance Inspection
;Dear Ms. Johnson:
(Enclosed is a report for the inspection performed on August 25, 2015 by Beth Swanson and Gary
IFrancies. Where finding(s) are cited in this report, a response is required. Within thirty days of
;receipt, please supply this office with a written item for item description of how these finding(s)
,were corrected. If the finding(s) cited in the enclosed report are not corrected, enforcement actions
may be recommended. For certification maintenance, your laboratory must continue to carry out
the requirements set forth in 15A NCAC 2H .0800.
,Copies of the checklists completed during the inspection may be requested from this office. Thank
you for your cooperation during the inspection. _If you wish to obtain an electronic copy of this
',report by email or if you have questions or need additional information, please contact us at (828)
I296-4677.
Attachment
�cc: Master file
Beth Swanson
Sincerely,
Gary Francies, Technical Assistance/Compliance Specialist
Division of Water Resources
Water Sciences Section
NC Wastewater/Groundwater Laboratory Certification Branch
1623 Mail Service Center, Raleigh, North Carolina 27699-1623
Location: 4405 Reedy Creek Road, Raleigh, North Carolina 27607
Phone: [phone] FAX: [phone]
Internet: www.dwolab.oro
An Equal Opportunity': Affirmative Action Employer

INSPECTION REPORT ROUTING SHEET
To be attached to all inspection reports in-house only.
Laboratory Cert. #:
5342
Laboratory Name:
Pace Analytical Field Services
Inspection Type:
Field Maintenance Abbreviated
Inspector Name(s):
_ Beth Swanson, Gary Francies
Inspection Date:
August 25, 2015
Date Report Completed:
September 9, 2015
Date Forwarded to Reviewer:
September 9, 2015
Reviewed by:
Jason Smith
Date Review Completed:
September 9, 2015
Cover Letter to use:
❑ Insp. Initial ® Insp. Reg.
❑ Insp. No Finding ❑ Insp. CP
❑ Corrected ❑ Insp. Reg. Delay
Unit Supervisor/Chemist III: Gary Francies
Date Received: 9/11/2015
Date Forwarded to Linda: 9/11/2015
Date Mailed:

On -Site Inspection Report
LABORATORY NAME:
ADDRESS:
CERTIFICATE #:
DATE OF INSPECTION:
TYPE OF INSPECTION:
AUDITOR(S):
LOCAL PERSON(S) CONTACTED:
INTRODUCTION:
Pace Analytical Field Services
9800 Kincey Avenue - Suite 100
Huntersville, NC 28078
5342
August 25, 2015
Field Maintenance Abbreviated
Beth Swanson and Gary Francies
Barry Johnson and Michael McCrickard
This laboratory was inspected by a representative of the North Carolina Wastewater/Groundwater
Laboratory Certification (NC WW/GW LC) program to verify its compliance with the requirements of 15A
NCAC 2H .0800 for the analysis of environmental samples.
II. GENERAL COMMENTS:
This abbreviated audit was conducted at the Pace Eden facility (Certification #633) with the help of field
analyst, Michael McCrickard.
We would like to especially thank Michael for his time and cooperation despite the inconvenience it caused to
leave his post in the field. Michael was very forthcoming and seemed eager to adopt necessary changes.
The Approved Procedures for applicable field analyses are included with this report.
Proficiency Testing (PT) samples have been analyzed for all certified parameters for the 2015 proficiency
testing calendar year and the graded results were 100% acceptable.
III. FINDINGS REQUIREMENTS COMMENTS AND RECOMMENDATIONS:
Chlorine, Total Residual — Standard Methods, 4500 Cl G-2000
Comment: During the audit, it was noticed that the DPD powder packets were for use with 25 mL of sample
even though the sample cell size was for 10 mL. Upon further investigation, Hach's product description states
that these pillows can be used for mid -range samples (i.e., 0.05-4.00 mg/L) with a sample volume of 10 mL. As
such, this was not a Finding but we recommended that the packets for 10 mL samples be used once the
current powder packs are used. Notification was received by email on September 8, 2015, that 10 mL packets
were put into use as of that date.
Comment: The field analyst uses a Hach Pocket Colorimeter II for analyses. The data reviewed only
contained one TRC analysis and it was a regular -level sample. The laboratory is reminded that if any client has
a permit limit below 100 ug/L, an instrument capable of detecting concentrations at that level must be used.
This would require the use of a spectrophotometer or filter photometer.
Comment: The laboratory is reminded that a post -analysis check is required if analyses are conducted at
multiple sites during the day.

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#5342 Pace Analytical Field Services
Comment: The Gel® standards used for the daily check were not within the verified portion of the curve. The
assigned true values for the set of Gel@ standards purchased in 2014 were 2.1, 3.7, and 6.8 mg/L. The curve
was verified to 2.0 mg/L. The previous Gel® standards had been within the range of the calibration verification.
The NC WW/GW LC Approved Procedure for the Analysis of Total Residual Chlorine document states: When
a five -standard annual standard curve verification is used, the laboratory must check the calibration curve each
analysis day. Notification of acceptable corrective action (i.e. check standards within the verified portion of the
curve were obtained and their true values determined in order to be put into immediate use) was received by
email on September 8, 2015. No further response is necessary for this Finding.
pH — Standard Methods, 4600 H+ B- 2000
A. Finding: The analysis of the calibration check standard was not consistently documented.
Requirement: The following must be documented in indelible ink whenever sample analysis is
performed: Value obtained for the check standard buffer (verification of ± 0.1 S.U.). Ref: NC WW/GW
LC Approved Procedure for the Analysis of pH.
Comment: This was specifically noted for the time period of 6/9/2015 through 7/11/2015. The field
analyst stated that he was performing the check but not documenting it due to work load. The most
recent analyses include documentation of the calibration check standard.
B. Finding: The meter is not recalibrated when the calibration verification check buffer is outside ±0.1
S.U. of the true value.
Requirement: The check standard buffer must read within ±0.1 S.U. to be acceptable. If the meter
verification does not read within ±0.1 S.U., the meter must be recalibrated before any samples are
analyzed. Ref: NC WW/GW LC Approved Procedure for the Analysis of pH.
C. Finding: A post -analysis calibration verification check buffer is not being analyzed.
Requirement: When performing analyses away from the certified laboratory's primary location, a post
analysis calibration verification using the check standard buffer must be analyzed at the end of the run.
It is recommended that a mid -day check standard buffer be analyzed when samples are analyzed over
an extended period of time. The post analysis check standard buffer(s) must read within ±0.1 S.0 or
corrective actions must be taken. Ref: NC WW/GW LC Approved Procedure for the Analysis of pH.
Requirement: The following must be documented in indelible ink whenever sample analysis is
performed: True value and value obtained for the post analysis calibration verification(s), where
applicable. Ref: NC WW/GW LC Approved Procedure for the Analysis of pH.
Temperature — Standard Methods, 2560 B- 2000
Comment: It could not be verified that the probe used for the analysis of temperature had been checked
against an NIST thermometer. The documentation was not readily available at the laboratory where the
instrument is based. The Approved Procedure for the Analysis of Temperature document states: The following
must be documented in indelible ink whenever sample analysis is performed: Annual calibration verification
against an NIST traceable thermometer. Demonstration of corrective action (i.e., documentation of the
calibration verification that had been performed on March 20, 2015) was received by email on September 8,
2015. No further response is necessary for this Finding.
D. Finding: The temperature correction is not posted on the meter used for temperature analysis.
Requirement: The following must be documented in indelible ink whenever sample analysis is
performed: The temperature correction (even if it is zero) must be posted on the meter as well as in

Page 3
#5342 Pace Analytical Field Services
hard copy format (to be retained for 5 years). Ref: NC WW/GW LC Approved Procedure for the
Analysis of Temperature.
Recommendation: The current temperature correction is 0 °C. The field analyst stated that he
believes the temperature correction was originally applied with a sticker that had fallen off the meter. It
is recommended that a different method of posting the temperature correction be utilized that accounts
for the heavy use of the instrument and the environmental conditions it is used in.
Dissolved Oxygen — Standard Methods, 4500 O G-2001
E. Finding: The post -analysis calibration verification is not being documented.
Requirement: When performing analyses away from the certified laboratory's primary location, a post -
analysis calibration verification must be analyzed at the end of the run. It is recommended that a mid-
day calibration verification be performed when samples are analyzed over an extended period of time.
The calculated DO value must verify the meter reading within ±0.5 mg/L. If the meter verification does
not read within ±0.5 mg/L of the theoretical DO, corrective action must be taken. Ref: NC WW/GW LC
Approved Procedure for the Analysis of Dissolved Oxygen.
Requirement: The following must be documented in indelible ink whenever sample analysis is
performed: True value and value obtained for the post analysis calibration verification(s), where
applicable. Ref: NC WW/GW LC Approved Procedure for the Analysis of Dissolved Oxygen.
Comment: The field analyst stated that he was performing the post -analysis calibration verification but
was not documenting it.
Conductivity —Standard Methods, 2510 B-1997
F. Finding: A post -analysis calibration verification check standard is not being analyzed.
Requirement: When performing analyses away from the certified laboratory's primary location, a post
analysis calibration verification must be analyzed at the end of the run. It is recommended that a mid-
day calibration verification be performed when samples are analyzed over an extended period of time.
The value obtained for the post analysis calibration verification check standard must read within 10%
of the true value of the post analysis calibration verification check standard. If the obtained value is
outside of the ±10% range, corrective action must be taken. Ref: NC WW/GW LC Approved
Procedure for the Analysis of Conductivity.
Requirement: The following must be documented in indelible ink whenever sample analysis is
performed: True value and value obtained for the post analysis calibration verification(s), where
applicable. Ref: NC WW/GW LC Approved Procedure for the Analysis of Conductivity.
IV. PAPER TRAIL INVESTIGATION:
A paper trail was not performed due to the abbreviated audit.
V. CONCLUSIONS:
Correcting the above -cited Findings and implementing the recommendation will help this lab to produce quality
data and meet certification requirements. The inspector would like to thank the staff for its assistance during
the inspection and data review process. Please respond to all Findings and include an implementation
date for each corrective action.
Report prepared by: Beth Swanson Date: September 9, 2015
Report reviewed by: Jason Smith Date: September 9, 2015

NORTH CAROLINA WASTEWATER/GROUNDWATER LABORATORY CERTIFICATION APPROVED PROCEDURE FOR
THE ANALYSIS
OF DISSOLVED OXYGEN (DO)
This document provides an approved procedure for the analysis of DO per 15A NCAC 2H .0805 (a) (6) (F) and (g) (3). The
procedures in this document, in addition to all requirements of the EPA approved method found in 40 CFR Part 136.3, must
be met.
HOLDING TIME:
• Samples must be analyzed within 15 minutes of collection (40 CFR Part 136 Table II); however, in situ or immediate
analysis is recommended due to the unstable nature of dissolved oxygen in samples.
GENERAL INFORMATION:
• Types of probes:
a. Dissolved Oxygen Membrane Electrode
b. Luminescence Dissolved Oxygen (LDO) Sensor
• Movement of water across the membrane (for membrane electrode technologies) is important to good readings. Some
probes come with stirrers for this purpose. Measurements should be taken while the stirrer is in use or by swirling the DO
probe in the sample flow.
• Follow the manufacturer's instructions for probe storage.
METER CALIBRATION:
• Instruments are to be calibrated according to the manufacturer's calibration procedure prior to analysis of samples each
day compliance monitoring is performed.
• The laboratory must use moist air for the air calibration. This is accomplished by calibrating the electrode in an
environment with a high relative humidity. Using dry air for the calibration can result in errant readings.
• The laboratory must document each time that a calibration is performed. Calibration documentation must include the
following, where applicable to the instrument used and the type of calibration performed: elevation, temperature,
barometric pressure (in mmHg), salinity, slope, or %efficiency. Simply recording a final reading (in mg/L) for instruments
that auto calibrate (e.g., LDO sensors and Membrane Electrodes that AUTOCAL) is also acceptable.
• For LDO sensors that cannot be calibrated, the calibration must be verified each day of use. This can be performed by
back calculating the theoretical DO for the current air calibration conditions (e.g., temperature, elevation, barometric
pressure, etc.). The calculated DO value must verify the meter reading within ±0.5 mg/L. Refer to the Dissolved Oxygen
Meter Calibration Verification handout at the end of this document. If the meter verification does not read within ±0.5 mg/L
of the theoretical DO, corrective action must be taken.
When performing analyses away from the certified laboratory's primary location, a post analysis calibration verification must
be analyzed at the end of the run. It is recommended that a mid -day calibration verification be performed when samples are
analyzed over an extended period of time. The calculated DO value must verify the meter reading within ±0.5 mg/L. If the
meter verification does not read within ±0.5 mg/L of the theoretical DO, corrective action must be taken.

DOCUMENTATION:
The following must be documented in indelible ink whenever sample analysis is performed.
1. Date and time of sample collection.
2. Date and time of sample analysis to verify the 15 minute holding time is met. Alternatively, one time
may be documented for collection and analysis with the notation that samples are measured in situ
or immediately at the sample site.
3. Sample site including facility name and location, ID, etc.
4. Collector's/analyst's name or initials.
5. Meter calibration and meter calibration time(s).
6. True value and value obtained for the post analysis calibration verification(s), where applicable.
7. All data must be reported in mg/L.
8. Instrument identification.
9. Parameter analyzed.
10. Data qualifier(s), when applicable.
11. Equipment maintenance (recommended).
Refer to Quality Assurance Policies for Field Laboratories (at htfiaWportal,ncdenr.ora/web/wg/lab/cert/field/policy) for additional
quality assurance and quality control requirements. Note: Sample duplicates are not a required quality control element for field
parameters.
Ref: Standard Methods 4500-0 G - 2001
Hach Method 10360
In Situ Method 1002-8-2009
ASTM Method D888-09 (B)
ASTM Method D888-09 (C)

Dissolved Oxygen Meter Calibration Verification
D.O. meters/probes must be calibrated each day of use prior to sample analysis. If the meter cannot be calibrated, the
calibration must be verified each day of use, Additionally, when performing D.O. analyses away from the certified laboratory's
primary location, a post analysis calibration verification must be analyzed at the end of the run for all types of D.O. probes
(LDO Sensor and membrane electrode). Below is a procedure for verifying the calibration of a D.O. probe.
1)li Follow the manufacturer's instructions for meter operation.
2)1 Place probe in a plastic bag, the probe storage cup, the storage well of the meter (each containing a wet sponge), or
a BOD bottle partially filled with water. Allow appropriate instrument warm up time.
3) Read D.O. and temperature.
4): Check the reading vs. the solubility table below and apply appropriate atmospheric (barometric) pressure or altitude
correction factor.
5)1 Calculated D.O. value must verify meter reading within ± 0.5 mg/L (do NOT calculate and apply a correction factor to
calculated D.O.).
Temp.:,
°C
D.O. m /L
Temp. °C
D.O. m /L
Atmospheric
Pressure mm
H
Equivalent
Altitude Ft.
Correctio
n Factor
4
1
13.11
19.5
9.18 `'
4.5
12.94
20
9.09
5
i
12.77
20.5
9.00 ''
760 `
0
1.00
5.5
12.61
21
8.92
752
278
.99
6
12.45
21.5
8.83
745
558
.98
6.5
12.30
22
8.74
737
841
.97
7 1
12.14
22.5
8.66
730
1126
.96
7.5
11.99
23
8.58
722
1413
95
8
11.84
23.5
8.50
714
1703
.94
8.5
11.70
24
8.42
707
1995
.93
9
11.56
24.5
8.34 '
699
2290
.92
9.5
11.42
25
8.26
692
2587
.91
10
11.29
25.5
8.18 =
684
2887
.90
10.5
11.16
26
8.11
676
3190
.89
11
11.03
26.5
8.04
669 :
3496
.88
11.5
10.90
27
7.97
661 '
3804
.87
12
10.78
27.5
7.90
654
4115
.86
12.5
10.66
28
7.83
646
4430
.85
13
10.54
28.5
7.76
638 '
4747
.84
13.5
10.42
29
7.69
631
5067
83
14
10.31
29.5
7.62 :'
623
5391
.82
14.5
10.20
30
7.56
616
5717
.81
15
10.08
30.5
7.50
608 ;'
6047
.80
15.5
9.98
31
7.43
600
6381
.79
16
9.87
31.5
7.37
593
6717
.78
16.5
9.77
32
7.31
ely 1126 ft, the theoretical D.O. would be:
8.92 X 0.96 = 8.56 mg/L
or, If ambient temperature is 21 °C and the at
(barometric) pressure is 745 mm Hg, the thei
17
9.67
32.5
7.24
17.5
9.57
33
7.18
18
9.47 <
33.5
7.12
18.5
!
9.38
34
7.07
19
9.28
34.5
7.01
would be:
8.92 X 0.98 = 8.74 mg/L
Ref: YSI
Model
5000/5100 DO
Meter Manual.
Slight
variations in
D.O.,
pressure,
and/or altitude
may be found
in other
manuals.
Example: If
ambient
temperatur
e is 21 °C
and
elevation is
approximat
mospheric
Dretical D.O.

NORTH CAROLINA WASTEWATER/GROUNDWATER LABORATORY CERTIFICATION APPROVED
PROCEDURE FOR THE ANALYSIS OF pH
This document provides an approved procedure for the analysis of pH per 15A NCAC 2H .0805 (a) (6) (F) and (g) (3).The
procedures in this document, in addition to all requirements of the EPA approved method found in 40 CFR Part 136.3, must be met.
HOLDING TIME:
• Samples must be analyzed within 15 minutes of collection (40 CFR Part 136 Table ll).
METER CALIBRATION:
• Instruments are to be calibrated according to the manufacturer's calibration procedure prior to analysis of samples each day
compliance monitoring is performed.
• U$e a pH meter accurate and reproducible to 0.1 pH unit (as demonstrated daily by acceptable performance of a check
standard buffer) with a range of 0 to 14 and equipped with temperature -compensation adjustment. The meter must be
calibrated with at least two buffers. In addition to the calibration buffers, the meter calibration must be verified with a third
standard buffer solution. The calibration and check standard buffers must bracket the range of the samples being analyzed. A
portion of the buffer solutions should not be used for more than one calibration. Discard any used buffer portions.
• Tlje check standard buffer must read within t0.1 S.U. to be acceptable. If the meter verification does not read within t0.1 S.U.,
the meter must be recalibrated before any samples are analyzed.
• When performing analyses away from the certified laboratory's primary location, a post analysis calibration verification using the
check standard buffer must be analyzed at the end of the run. It is recommended that a mid -day check standard buffer be
analyzed when samples are analyzed over an extended period of time. The post analysis check standard buffer(s) must read
within t0.1 S.0 or corrective actions must be taken.
General Information:
• Samples shall be gently stirred during measurement. Steps must be taken to eliminate cross contamination between
measurements (e.g., rinsing and blotting the electrode dry, dipping the electrode in stream multiple times, etc.).
• The units of measure for pH analyses are Standard Units (S.U.). It is recommended that pH be read in one -hundredths (0.01).
Values must be reported in tenths (0.1). It should be noted that many proficiency testing (PT) providers require samples be
reported to one -hundredths.
DOCUMENTATION:
The following must be documented in indelible ink whenever sample analysis is performed
1. Date and time of sample collection.
2. Date and time of sample analysis to verify the 15 minute holding time is met. Alternatively, one time may be
documented for collection and analysis with the notation that samples are measured in situ or immediately at the
sample site.
3. Sample site including facility name and location, ID, etc.
4. Collector's/analyst's name or initials.
5. Meter calibration and meter calibration time(s).
6. True values of buffers used for calibration.
7. True value for the check standard buffer.
8. Value obtained for the check standard buffer (verification of t 0.1 S.U.).
9. True value and value obtained for the post analysis calibration verification(s), where applicable.
10. Report all data values to the nearest 0.1 pH unit.
11. Traceability for chemicals, reagents, standards and consumables.
12. Instrument identification.
13. Parameter analyzed.
14. Data qualifier(s), when applicable.
15. Equipment maintenance (recommended).
Refer to Quality Assurance Policies for Field Laboratories (at bttp://portal.ncdenr.org/web/wq/lab/cert/field/policy) for additional quality
assurance and quality control requirements.. Note: Sample duplicates are not a required quality control element for field parameters.
Ref: Standard Methods 4500-H+ B — 2000

NORTH CAROLINA WASTEWATER/GROUNDWATER LABORATORY CERTIFICATION
APPROVED PROCEDURE FOR THE ANALYSIS OF SPECIFIC CONDUCTANCE (CONDUCTIVITY)
This document provides an approved procedure for the analysis of Specific Conductance per 15A NCAC 2H .0805 (a) (6)
(F) and (g) (3). The procedures in this document, in addition to all requirements of the EPA approved method found in 40
CFR Fart 136.3, must be met.
Holding Time:
• Samples must be analyzed within 28 days of collection (40 CFR Part 136 Table II).
• Samples must be stored above freezing and <_6°C, if not analyzed immediately.
General Information:
• In water analysis, the measurement is expressed in pmhos/cm. Some meters display units in µS/cm. (Ipmho/cm
= 1 µS/cm)
• Conductivity samples must not be diluted.
• When performing analyses away from the certified laboratory's primary location, a post analysis calibration
verification must be analyzed at the end of the run. It is recommended that a mid -day calibration verification be
performed when samples are analyzed over an extended period of time. The value obtained for the post analysis
calibration verification check standard must read within 10% of the true value of the post analysis calibration
verification check standard. If the obtained value is outside of the ±10% range, corrective action must be taken.
• The Automatic Temperature Compensator (ATC) must be verified annually (i.e., 12 months) at two temperatures
by analyzing a standard or sample at 250C (the temperature that conductivity values are compensated to) and a
temperature(s) that brackets the temperature ranges of the environmental samples routinely analyzed. This may
require the analysis of a third temperature reading that is > 250C (see #3 below). The manner in which the ATC is
verified may depend upon the meter's capabilities and the manufacturer's instructions. The following is one option.
1. Pour an adequate amount of conductivity standard or sample into a beaker or other container and analyze at
25°C. Document the temperature and conductivity value.
2. Lower the temperature of the standard or sample (e.g., by placing the container in a refrigerator or ice chest)
to less than the lowest anticipated sample temperature and analyze. Document the temperature and
conductivity value.
3. If samples greater than 25°C are to be analyzed, perform the following additional
step: Raise the temperature above 25°C to greater than the highest anticipated sample
temperature (e.g., by placing the container in a hot water bath) and analyze. Document the
temperature and conductivity value.
As the temperature increases or decreases, the value of the conductivity standard or sample must be within ±10%
of the true value of the standard or ±10% of the value of the sample at 25°C. If not, corrective action must be taken.
Anticipated temperatures can be obtained from a review of the Discharge Monitoring Reports (DMRs) from the peak
summer and winter months. Historical data should provide a reasonably accurate estimation of ranges that will bracket the
expected sample temperatures.
Other certified laboratories may provide assistance in meeting this ATC verification requirement.

Standards:
Potassium Chloride (KCI) Conductivity standards may be purchased in the ranges desired, or they may be prepared
according to Table 2510:1 of Standard Methods, 2510 A - 1997. A portion of the standard should not be used for more than
one calibration. Discard any used standard portions.
Calibration:
1. Instruments are to be calibrated according to the manufacturer's calibration procedure prior to analysis of
samples each day compliance monitoring is performed. For most meters, this is a one- point calibration.
2. Thoroughly rinse cell with one or more portions of sample.
3. Analyze and document a calibration verification check standard prior to environmental sample analysis. It is
recommended that this standard value bracket (may be higher or lower than the calibration standard, as
applicable) the expected range of sample values measured.
4. The value obtained for the calibration verification check standard must read within 10% of the true value of
the calibration verification check standard. If the obtained value is outside of the ±10% range, corrective action must be
taken.,
Documentation:
The following must be documented in indelible ink whenever sample analysis is performed.
1. I Date and time of sample collection.
2. 1 Date and time of sample analysis to verify the 28 day holding time is met. Alternatively, one time may
be documented for collection and analysis with the notation that samples are measured in situ or
immediately at the sample site.
3. Sample site including facility name and location, ID, etc.
4. Collector's/analyst's name or initials.
5. Meter calibration and meter calibration time(s).
6. True value of the standard used for calibration.
7. ! True value of the calibration verification check standard.
8. Value obtained and time analyzed for the check standard (verification of ± 10% recovery).
9. True value and value obtained for the post analysis calibration verification(s), where applicable.
10. All data must be reported in pmhos/cm at 25°C or corrected to 25°C.
11. Traceability for chemicals, reagents, standards and consumables.
12. Instrument identification.
13. Parameter analyzed.
14. Data qualifiers, when necessary.
15. Equipment maintenance (recommended).
Refer to Quality Assurance Policies for Field Laboratories (at http:Hportal.ncdenr.org/web/wg/lab/cert/fieldfpolicy) for additional
quality', assurance and quality control requirements. Note: Sample duplicates are not a required quality control element for field
parameters.
Ref: Standard Methods 2510 B —1997
EPA Method 120.1

NORTH CAROLINA WASTEWATER/GROUNDWATER LABORATORY CERTIFICATION APPROVED
PROCEDURE FOR THE ANALYSIS
OF TEMPERATURE
This document provides an approved procedure for the analysis of Temperature per 15A NCAC 2H .0805 (a) (6) (F) and (g)
(3). The procedures in this document, in addition to all requirements of the EPA approved method found in 40 CFR Part
136.3,1i must be met.
HOLDING TIME:
• Immediate (i.e., in situ) analysis is required (40 CFR Part 136 Table II).
• When analyzing samples at a site where in situ analysis will interfere with obtaining an accurate reading due to conditions
present (e.g., low flow, etc.), it is acceptable to collect the sample in a container and analyze on site.
e
When analyzing samples in a hazardous area (such as some highway bridges, etc.), the samples should be transported
and analyzed at a safe location near the collection point.
GENERAL INFORMATION:
• Temperature measurements must be made with a Celsius thermometer or other acceptable temperature -measuring
device. Infrared (IR) devices are not acceptable for compliance monitoring. It is recommended that all liquid -in -glass
thermometers have a metal case to prevent breakage.
• A IlConductivity, Dissolved Oxygen, pH or multi -parameter meter with a temperature sensing device may be used to
measure and document temperature for compliance monitoring. Any temperature sensing device, used to measure
temperature for compliance monitoring, must be verified prior to initial use and re -verified any time an instrument is
serviced.
• The number of decimal places that the measurement is reported to will determine the degree increments required for the
temperature measuring device. Standard Methods 2550 B — 2000 states that the thermometer should have a scale
indicated for every 0.1°C. This is required for all measurements performed to tenth degree increments. (e.g., 24.70C). If
measurements are reported in whole numbers, a temperature measuring device having a scale indicated for every 10C is
adequate (e.g., 221C),
• Unless greater precision is required by the permit or data receiving agency, it is recommended that all temperatures
reported for compliance monitoring, be reported in whole numbers. It should be noted that many vendors require
proficiency testing (PT) samples be reported to two decimal places.
• Al� thermometers and temperature measuring devices must be checked every 12 months against a National Institute of
Standards and Technology (NIST) traceable thermometer. The process must be documented and proper corrections
made to all compliance data. To check a thermometer or the temperature sensor of a meter, read the temperature of the
thermometer/meter against a NIST traceable thermometer and record the two temperatures. The verification must be
performed in the approximate range of the sample temperatures measured. The thermometer/meter readings must be
s than or equal to 10C from the NIST traceable thermometer reading. The documentation must include the serial
le
of the NIST traceable thermometer that was used in the comparison. Also document any correction that applies
on both the thermometer/meter and on a separate sheet to be filed. (NOTE: Other certified laboratories may provide
assistance in meeting this requirement.)
o NIST traceable thermometers used for temperature measurement must be recalibrated in
accordance with the manufacturer's recalibration date. If no recalibration date is given, the NIST
traceable thermometer must be recalibrated annually.
NIST raceable thermometers used to verify the calibration of other thermometers or temperature sensors (i.e., limited use
only) must be recalibrated in accordance with the manufacturer's recalibration date and the process documented. If no
recalibration date is given, the NIST traceable thermometer must be recalibrated every 5 years.
MENT,
The foi lowing must be documented in indelible ink whenever sample analysis is performed.

1. Date and time of sample collection.
2. Date and time of sample analysis. Alternatively, one time may be documented for collection and analysis with the
notation that samples are measured in situ or immediately at the sample site.
3. Sample site including facility name and location, ID, etc.
4. Collector's/analyst's name or initials.
5. Document sample temperature measurements with any applicable temperature corrections applied.
6. All data must be reported in °C.
7. li The temperature correction (even if it is zero) must be posted on the meter as well as in hard copy format (to be
retained for 5 years).
8. i Annual calibration verification against an NIST traceable thermometer.
9. Thermometer/instrument identification.
10. Parameter analyzed.
11. Data qualifiers, when necessary.
12. Equipment maintenance (recommended).
Refer to Quality Assurance Policies for Field Laboratories (at http:/iportal.ncdenr.orglweb/wg/lab/certlfield/poiioy) for additional
quality assurance and quality control requirements. Note: Sample duplicates are not a required quality control element for field
parameters.
Ref: Standard Methods 2550 B - 2000.

NORTH CAROLINA WASTEWATER/GROUNDWATER LABORATORY CERTIFICATION APPROVED PROCEDURE FOR
THE ANALYSIS OF
TOTAL RESIDUAL CHLORINE
This document provides an approved procedure for the colorimetric analysis of Total Residual Chlorine (TRC) per 15A NCAC
2H .0805 (a) (6) (F) and (g) (3). The procedures in this document, in addition to all requirements of the EPA approved method
found in 40 CFR Part 136.3, must be met.
Holding Time:
Samples must be analyzed within 15 minutes of collection (40 CFR Part 136 Table ll).
General Information:
If there is a limit required by the facility permit, you must have an instrument capable of detecting concentrations at
that level, such as a spectrophotometer or filter photometer.
If a facility has no effluent limit for TRC Oust a monitoring requirement), then use of a hand-held meter, sometimes
described as a pocket colorimeter, is acceptable. For facilities using these hand-held meters, the North Carolina
Division of Water Quality has established the minimum reporting level at 100 lag/L. Any values obtained less than that
concentration must be reported as "<100 lag/L". Ref: Division of Water Quality, Point Source
Compliance/Enforcement Unit letter dated August 14, 2001.
Since Hach Method ULR 10014 is approved by EPA as an alternate test procedure, all steps in the method must be
followed. This means that the sample must be filtered, liquid reagents must be used and the flow-thru cell must be
used.
Instrument Calibration or Standard Curve Verification:
Instruments are to be calibrated according to the manufacturer's calibration procedure or a standard curve verification must
be performed prior to analysis of samples each day compliance monitoring is performed. The instrument calibration must be
re -constructed or re -verified any time the instrument is serviced. Standard curve verification checks must be performed for the
standard curve and/or program used for sample analysis.
Depending upon the meter, you may either construct a laboratory -generated calibration curve or verify the factory -set
calibration. Most field photometric instruments have factory -set calibration programs, which when selected in combination with
the optimum wavelength for a particular analysis, give a direct readout in concentration. These factory -set calibration
programs are acceptable for quantitation, but due to possible analyst error, variation in sample or standard preparation,
variation in reagents or malfunction of the instrument, the factory -set calibration must be verified at least every 12 months.
The definition of a laboratory -generated calibration; as opposed to a factory -set calibration verification is as follows:
Laboratory -generated Calibration means: A series of standards are analyzed by the permitted facility and the obtained
values are programmed into the instrument, computer spreadsheet, scientific calculator, or plotted manually. Sample
results are obtained by comparison to the linear regression of those values. The standard materials used must be of
an acceptable purity. Each analyst performing the test must generate an individual calibration curve.
Factory -set Calibration Verification means: An internal standard curve, generated by the instrument manufacturer, is
checked (i.e., verified) using a series of known standards. The standard materials used to verify the factory -set
calibration must be of an acceptable purity. This procedure may be performed by the permitted facility or may be
contracted to a vendor or another laboratory. Since a single curve is always used for sample measurement and is
verified for accuracy, each analyst does not have to perform factory -set calibration verifications, this may be done per
instrument.
The concentrations of the calibration standards must bracket the concentrations of the samples analyzed. One of the
standards must have a concentration equal to or below the lower reporting concentration for Total Residual Chlorine. The
lower reporting limit must be less than or equal to the permit limit.
Example:
If the laboratory chooses to have a lower reporting limit of 20 tag/L for residual chlorine, you must analyze at least a 20 ❑g/L or
lower standard and report lower concentrations as <20 tag/L or < the concentration of the chosen standard.

If you choose 400 pg/L for the top of your standard curve, all samples above this limit must be diluted and reanalyzed to fall
within the range of the chosen lower standard and 400 ❑g/L.
Reaaent Blanks and Calibration Blanks:
Zeroing the Instrument: For colorimetric analyses, a calibration blank must be analyzed each day to zero the instrument prior
to analyzing any standards, samples or the reagent blank. A calibration blank is a volume of reagent water of the same matrix
as the calibration standards, but without the target analyte and without DPD. A sealed standard (e,g., gel) blank may also be
used for this purpose.
Reagent Blank: A reagent blank (sometimes also referred to as a method blank) is only required when laboratory water is
used to make quality control and/or calibration standards. If you are using a sealed standard (e.g., gel) for your daily check
standard, a reagent blank would only be analyzed when preparing the annual 5-point calibration curve or 5 annual calibration
curve verification standards.
A reagent blank is made from the same laboratory water source used to make quality control and/or calibration standards with
DPD. The concentration of reagent blanks must not exceed 50% of the reporting limit (i.e., the lowest calibration or calibration
verification standard concentration), unless otherwise specified by the reference method, or corrective action must be taken.
Calibration and Standard Curve Verification Options:
Option 1 — Annual Factory -set Standard Curve Verification: Analyze a calibration blank to zero the instrument and then
analyze a series of five standards (do not use gel or sealed liquid standards for this purpose). The curve verification must
check 5 concentrations (not counting the blank) that bracket the range of the sample concentrations to be analyzed. This type
of standard curve verification must be performed at least every 12 months. The values obtained must not vary by more than
10% of the known value for standard concentrations greater than or equal to 50 ❑g/L and must not vary by more than 25% of
the known value for standard concentrations less than 50 ❑g/L. The overall correlation coefficient of the curve must be
4.995.
If the stored program readings vary by more than the above acceptance criteria, the stored calibration program must not be
used for quantitation until troubleshooting is carried out to determine and correct the source of error.
Each day that prepared standards are analyzed, a reagent blank must be analyzed.
• When a five -standard annual standard curve verification is used, the laboratory must check the calibration curve each
analysis day. To do this, the laboratory must analyze a calibration blank to zero the instrument and analyze a check
standard each day that samples are analyzed. The value obtained for the check standard must read within 10%
of the true value of the check standard. If the obtained value is outside of the ±10% range, corrective action must be
taken.
• When performing analyses away from the certified laboratory's primary location, a post analysis calibration verification
must be analyzed at the end of the run. The post analysis calibration verification standard concentration must be at
mid range. It is recommended that a mid -day calibration verification be performed when samples are analyzed over
an extended period of time. The value obtained for the post analysis calibration verification check standard must read
within 10% of the true value of the post analysis calibration verification check standard. If the obtained value is outside
of the ±10% range, corrective action must be taken.
NOTE: General absorbance standards (i.e., DR/check) supplied by some manufacturers cannot be used for the check
standard. Gel -type standards may be used for this purpose.
Option 2 — Daily Factory -set Standard Curve Verification: Analyze a calibration blank to zero the instrument and then
analyze a series of three standard concentrations (not counting the blank) that bracket the range of the sample
concentrations to be analyzed (do not use gel or sealed liquid standards for this purpose). The values obtained must not vary
by more than 10% of the known value for standard concentrations greater than or equal to 50 ❑g/L and must not vary by more
than 25% of the known value for standard concentrations less than 50 ❑g/L. The overall correlation coefficient of the curve
must be >_0.995. Each day that prepared standards are analyzed, a reagent blank must be analyzed.
Option 3 — Annual Laboratory -generated Calibration Curve: Analyze a calibration blank to zero the instrument and then
analyze a series of five standard concentrations (not counting the blank) that bracket the range of the sample concentrations
to be analyzed. The obtained values are programmed into the instrument, computer spreadsheet, scientific calculator, or
plotted manually. Sample results are obtained by comparison to the linear regression of those values. The standard materials

used must be of an acceptable purity. Each analyst performing the test must have an individual calibration curve. This type of
curve must be performed annually (i.e., at least every 12 months).
• Each day that prepared standards are analyzed, a reagent blank must be analyzed.
• When a five -standard annual curve is generated, the laboratory must check the calibration curve each analysis day.
To do this, the laboratory must analyze a calibration blank to zero the instrument and analyze a check standard each
day that samples are analyzed. The value obtained for the check standard must read within 10% of the true value
of the check standard. If the obtained value is outside of the ±10% range, corrective action must be taken.
• When performing analyses away from the certified laboratory's primary location, a post analysis calibration verification
must be analyzed at the end of the run. The post analysis calibration verification standard concentration must be at
mid range. It is recommended that a mid -day calibration verification be performed when samples are analyzed over
an extended period of time. The value obtained for the post analysis calibration verification check standard must read
within 10% of the true value of the post analysis calibration verification check standard. If the obtained value is outside
of the ±10% range, corrective action must be taken.
NOTE: General absorbance standards (i.e., DR/check) supplied by some manufacturers cannot be used for the check
standard. Gel -type standards may be used for this purpose.
Option 4 — Daily Laboratory -generated Calibration Curve: Analyze a calibration blank to zero the instrument and then
analyze a series of three standard concentrations (not counting the blank) that bracket the range of the sample concentrations
to be analyzed. The obtained values are programmed into the instrument, computer spreadsheet, scientific calculator, or
plotted manually. Sample results are obtained by comparison to the linear regression of those values. The standard materials
used must be of an acceptable purity. Each analyst performing the test must have an individual calibration curve. This type of
curve must be performed each day compliance samples are analyzed.
Each day that prepared standards are analyzed, a reagent blank must be analyzed
When a three -standard daily curve is generated, the laboratory must check the instrument calibration each analysis
day. To do this, the laboratory must analyze a calibration blank to zero the instrument and analyze a check standard
each day that samples are analyzed. The calibration check is performed immediately after calibration. The value
obtained for the check standard must read within 10% of the true value of the check standard. If the obtained value is
outside of the ±10% range, corrective action must be taken.
When performing analyses away from the certified laboratory's primary location, a post analysis calibration verification
must be analyzed at the end of the run. The post analysis calibration verification standard concentration must be at
mid range. It is recommended that a mid -day calibration verification be performed when samples are analyzed over
an extended period of time. The value obtained for the post analysis calibration verification check standard must read
within 10% of the true value of the post analysis calibration verification check standard. If the obtained value is
outside of the ±10% range, corrective action must be taken.
NOTE: General absorbance standard (i.e., DR/check) supplied by some manufacturers cannot be used for the check
standard. Gel -type standards may be used for this purpose.
Standard Solutions:
You may prepare a stock standard solution of potassium permanganate or chlorine and subsequent standard solutions as
described in Standard Methods 4500-CI G — 2000, DPD Colorimetric Method, Section 4 (a) (2), page 4-69.
If purchased standard solutions in sealed ampules with a stated range and average value are used, the average value must
be used for the true value of the standard.
Purchased "Gel -type" or sealed liquid ampoule standards may be used for daily standard curve verification only. These
standards must be verified initially and every 12 months thereafter, with the standard curve. When this is done, these
standards may be used after the manufacturer's expiration date. It is only necessary to verify the gel or sealed liquid standard
which falls within the concentration range of the curve used to measure sample concentrations. For example, if you are
measuring samples against a low range curve, a 200 ❑g/L standard would be verified, and not the 800 ❑g/L standard since
the 800 ❑g/L standard would be measured using a high range curve.
Immediately following curve verification:
1. Zero the instrument with the gel blank.
2. Read and record gel standard values.
3. Assign the obtained values as the true value.

The assigned values will be used for the next twelve months, or until a new curve verification is performed. The gel/liquid
standard verification must be performed for each instrument on which they are to be used. If multiple instruments and/or
standard sets are used, each must have assigned values specific for the instrument and standard set. Documentation must
link the gel standard identification to the meter with which the assigned value was determined. Some commercial laboratory
facilities may be able to provide assistance with the field photometric meter curve verifications.
Equipment Maintenance:
As cited in the laboratory certification rules, "Each facility must have glassware, chemicals, supplies, equipment, and a source
of distilled or deionized water that will meet the minimum criteria of the approved methodologies." Ref: 15A NCAC 2H .0805
(g) (4). Meeting the minimum criteria means the equipment must also be properly maintained. Clean and maintain equipment
as indicated by the manufacturer's instructions. Sample lines and the pour-thru cell can become discolored and clogged due
to a build up of colored reaction products.
Hach Method 10014 offers the following instructions for cleaning the pour-thru cell:
Cleaning the Pour-Thru Cell
The Pour-Thru Cell may accumulate a buildup of colored reaction products, especially if the reacted solutions are allowed to
remain in the cell for long periods after measurement. Remove the buildup by rinsing the cell with 5.25 N sulfuric acid followed
by rinsing with deionized water.
If your facility does not have access to or is not comfortable using sulfuric acid cleaning solution, a contract laboratory or
vendor may perform this service. Please exercise proper safety precautions when handling acid solutions.
Documentation:
The following must be documented in indelible ink whenever sample analysis is performed.
1. Date and time of sample collection.
2. Date and time of sample analysis to verify the 15 minute holding time is met. Alternatively, one time
may be documented for collection and analysis with the notation that samples are measured in situ or immediately at
the sample site.
3. Sample site including facility name and location, ID, etc.
4. Collector's/analyst's name or initials.
5. Meter calibration and meter calibration time(s).
6. True values of the standards used for calibration or standard curve verification.
7. True value of the check standard.
8. Value obtained for the check standard (verification of ± 10% recovery).
9. Value obtained for the reagent blank, when prepared standards are used (verification of <'/2 the concentration of
the lowest calibration standard).
10. All data must be reported in mg/L or lag/L (i.e., as specified in the permit).
11. True value and value obtained for the post analysis calibration verification(s), where applicable.
12. Traceability for chemicals, reagents, standards and consumables.
13. Instrument identification.
14. Parameter analyzed.
15. Data qualifier(s), when applicable.
16. Equipment maintenance (recommended).
Refer to Quality Assurance Policies for Field Laboratories (at http://portal.ncdenr.org/web/wq/lab/cerUfield/policy) for additional
quality assurance and quality control requirements. Note: Sample duplicates are not a required quality control element for field
parameters.
Ref: Standard Methods 4500-CI G - 2000
Hach Method 10014