HomeMy WebLinkAbout#143_2017_1207_JS_FINALTo be attached to all inspection reports in-house only.
Laboratory Cert. #:
143
Laboratory Name:
City of Newton Clark Creek WW Facility
Inspection Type:
Municipal Maintenance
Inspector Name(s):
Jason Smith and Todd Crawford
Inspection Date:
December 7, 2017
Date Forwarded for Initial
Review:
January 3, 2018
Initial Review by:
Anna Ostendorff
Date Initial Review
Completed:
January 5, 2018
Cover Letter to use:
❑ Insp. Initial
❑Insp. No Finding
❑Corrected
❑ Insp. Reg
❑Insp. CP
®Insp. Reg. Delay
Unit Supervisor/Chemist III:
Todd Crawford
Date Received:
January 9, 2018
Date Forwarded to Admin.:
February 14, 2018
Date Mailed:
February 15, 2018
Special Mailing Instructions:
Email to wes.bell@ncdenr.gov
(/Vats=r Resour ces
f N V I R G N M F N 1 A L Q U A, L'Ty
February 15, 2018
143
Mr. Eric Jones
City of Newton Clark Creek WW Facility
P.O. Box 550
Newton, NC 28658
ROY COOPER
MICHEAL S. REGAN
LINDA CULPEPPER
Subject: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC)
Maintenance Inspection
Dear Mr. Jones:
Enclosed is a report for the inspection performed on December 7, 2017 by Jason Smith. I apologize for
the delay in getting this report to you. 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. Please describe the steps taken to prevent recurrence and include an
implementation date for each corrective action. 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.
A copy of the laboratory's Certified Parameter List at the time of the audit is attached. This list will reflect
any changes made during the audit. 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 me at (919) 733-3908 ext. 251.
Sincerely,
Todd Crawford
Technical Assistance & Compliance Specialist
NC WW/GW Laboratory Certification Branch
Attachment
cc: Dana Satterwhite, Jason Smith, Master File #143
Water Sciences Section
NC Wastewater/Groundwater Laboratory Certification Branch
1623 Mail Service Center, Raleigh, North'Carohna 27699-1623
Location: 4405 Reedy Creek Road, Raleigh, North Carolina 27607
Phone: 919-733-39081 FAX: 919-733-6241
Internet: http://deg.nc,goviaboutldivisions/water-resources/water-resources-data/water-sciences-home-pagetlaboratory-certification branch
On -Site Inspection Report
LABORATORY NAME:
NPDES PERMIT #:
ADDRESS:
CERTIFICATE #:
DATE OF INSPECTION:
TYPE OF INSPECTION:
AUDITOR(S):
LOCAL PERSON(S) CONTACTED
INTRODUCTION:
City of Newton Clark Creek WW Facility
NC0036196
1407 McKay Farm Road
Newton, NC 28658
143
December 7, 2017
Municipal Maintenance
Jason Smith and Todd Crawford
Eric Jones, Stacy Rowe, Scott Bryan, Carmella Tucker and
Matt Herman
This laboratory was inspected by representatives 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 compliance monitoring samples.
II. GENERAL COMMENTS:
The laboratory is clean, spacious and contains all equipment necessary to perform the analyses.
The analysts were forthcoming and expressed interest in the inspection process.
All required Proficiency Testing (PT) Samples have been analyzed and the laboratory has fulfilled
its PT requirements for the 2017 PT Calendar Year.
The laboratory submitted their Quality Assurance (QA) and/or Standard Operating Procedures
(SOP) document(s) in advance of the inspection. These documents were reviewed and editorial
and substantive revision requirements and recommendations were made by this program
outside of this formal report process. Although subsequent revisions were not requested to be
submitted, they must be completed by December 31, 2018.
The laboratory is reminded that any time changes are made to laboratory procedures, the
laboratory must update the QA/SOP document(s) and inform relevant staff. Any changes made
in response to the pre -audit review or to Findings, Recommendations or Comments listed in this
report must be incorporated to insure the method is being performed as stated, references to
methods are accurate, and the QA and/or SOP document(s) is in agreement with each
approved practice, test, analysis, measurement, monitoring procedure or regulatory
requirement being used in the laboratory. In some instances, the laboratory may need to create
an SOP to document how new functions or policies will be implemented.
The laboratory is also reminded that SOPs are intended to describe procedures exactly as they
are to be performed. Use of the word "should" is not appropriate when describing requirements
(e.g., Quality Control (QC) frequency, acceptance criteria, etc.). Evaluate all SOPs for the proper
use of the word "should".
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#143 City of Newton Clark Creek WW Facility
Laboratory Fortified Matrix (LFM) and Laboratory Fortified Matrix Duplicate (LFMD) are also
known as Matrix Spike (MS) and Matrix Spike Duplicate (MSD) and may be used
interchangeably in this report.
Requirements that reference 15A NCAC 2H .0805 (a) (7) (A), stating "All analytical data pertinent
to each certified analysis must be filed in an orderly manner so as to be readily available for
inspection upon request", are intended to be a requirement to document information pertinent to
reconstructing final results and demonstrating method compliance. Use of this requirement is not
intended to imply that existing records are not adequately maintained unless the Finding speaks
directly to that.
Contracted analyses are performed by Meritech (Certification # 165).
Approved Procedure documents for the analysis of the facility's currently certified Field
Parameters were provided at the time of the inspection.
III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:
General Laboratory
A. Finding: The analytical balance weights have not been verified against ASTM standard
weights in the past 5 years.
Requirement: ASTM Class 1 and 2 weights must be verified at least every 5 years. ASTM
Class 1 weights (20 g to 25 kg) and ASTM Class 2 weights (10 g to 1 mg) are equivalent
to the NBS Class S weights specified in 15A NCAC 2H .0805 (a) (7) (K). Ref: NC
WW/GW LC Policy. See the attached Weight Verification policy for additional
guidance.
B. Finding: The National Institute of Standards and Technology (NIST) traceable
thermometer used to check laboratory thermometers is not documented to be accurate to
0.1 °C.
Requirement: Temperature measuring devices used in fecal coliform incubators, or NIST
traceable temperature measuring devices used to calibrate fecal coliform incubator
temperature measuring devices, must have a stated accuracy of at least ± 0.1 °C. Ref: NC
WW/GW LC Policy.
Comment: The policy referenced above was based on consultation with NIST and was
implemented after the inspection took place.
Comment: The NIST traceable thermometer had a stated accuracy of ± 0.4 °C and was
0.2 °C away from the manufacturer tested temperatures. The thermometer must be
accurate to at least ± 0.1 °C due to the acceptable incubation temperature being 44.5 ±
0.2 °C.
C. Finding: The laboratory is not checking all thermometers with a NIST certified or
traceable thermometer annually.
Requirement: All thermometers must meet NIST specifications for accuracy or be
checked, at a minimum annually, against a NIST traceable thermometer and proper
corrections made. Ref: 15 NCAC 2H .0805 (a) (7) (0).
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#143 City of Newton Clark Creek WW Facility
Requirement: All thermometers and temperature measuring devices must be checked
every 12 months against a NIST certified or NIST traceable thermometer and the process
documented. Ref: NC WW/GW LC Policy.
Comment: The thermometer for the drying oven has not been checked since 2015
because the NIST traceable thermometer the laboratory purchased would not fit in the
drying oven. All other thermometers and meters have been checked annually.
Comment: If unable to find a thermometer that fits in the drying oven, the laboratory may
put both thermometers in sand and heat it on a hot plate to the appropriate temperature if
both are partial immersion thermometers.
Proficiency Testing
D. Finding: The laboratory does not have a documented plan for PT procedures.
Requirement: Each laboratory shall develop and maintain a document outlining the
analytical quality control practices used for the parameters included in their certification.
Supporting records shall be maintained as evidence that these practices are being
effectively carried out. Ref: 15A NCAC 2H .0805 (a) (7).
Requirement: Laboratories must have a documented plan (this is usually detailed in the
laboratory's Quality Assurance Manual or may be a separate Standard Operating
Procedure (SOP) of how they intend to cover the applicable program requirements for
Proficiency Testing per their scope of accreditation. This plan shall cover any commercially
available PT Samples and any inter -laboratory organized studies, as applicable. The
laboratory must also be able to explain when PT Sample analysis is not possible for
certain methods and provide a description of what the laboratory is doing in lieu of
Proficiency Testing. This shall be detailed in the plan. The plan must also address the
laboratory's process for submission of PT results and related Corrective Action Reports
(CARs). Ref: Proficiency Testing Requirements, May 31, 2017, Revision 2.0.
Requirement: SOPs must address situations where the instructions from the Accredited
PT Provider for the preparation, analysis or result calculations would constitute a deviation
from the laboratory's routine procedure. Examples of this may include how low-level
samples will be analyzed, including concentration of the sample or adjustment of the
normality of a titrant. These instructions shall be followed when the concentration of a PT
sample falls below the range of their routine analytical method. Instructions shall also be
included in the laboratory's SOP for how high-level samples will be analyzed, including
preparation of multiple dilutions of the sample. These instructions will be followed when the
concentration of a PT falls above the range of their routine analytical method. Ref:
Proficiency Testing Requirements, May 31, 2017, Revision 2.0.
E. Finding: The laboratory is not documenting the preparation of PT Samples,
Requirement: PT Samples received as ampules are diluted according to the Accredited
PT Sample Provider's instructions. It is important to remember to document the
preparation of PT Samples in a traceable log or other traceable format. The diluted PT
Sample then becomes a routine Compliance Sample and is added to a routine sample
batch for analysis. No documentation is needed for whole volume PT Samples which
require no preparation (e.g., pH), but it is recommended that the instructions be
maintained. Ref: Proficiency Testing Requirements, May 31, 2017, Revision 2.0.
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#143 City of Newton Clark Creek WW Facility
Comment: Dating and initialing the instruction sheet for each prepared PT Sample would
satisfy the documentation requirement.
F. Finding: PT Samples are not logged in using the sample tracking (sample receipt) system
that is used for Compliance Samples.
Requirement: Laboratories shall conduct the analyses in accordance with their routine
testing, calibration and reporting procedures, unless otherwise specified in the instructions
supplied by the Accredited PT Sample Provider. This means that they are to be logged in
and analyzed using the same staff, sample tracking systems, standard operating
procedures including the same equipment, reagents, calibration techniques, analytical
methods, preparatory techniques (e.g., digestions, distillations and extractions) and the
same quality control acceptance criteria. Ref: Proficiency Testing Requirements, May 31,
2017, Revision 2.0.
Documentation
Comment: A method reference was not documented on the benchsheets for Dissolved Oxygen
(DO), pH, Temperature, Total Residual Chlorine (TRC) and Conductivity. Although not required at
the time of the inspection, this is now required. Please review all benchsheets to ensure that this
requirement is met.
Recommendation: The laboratory documents the manufacturer and model of the meters in use
on the benchsheet. It is recommended that the serial number also be documented in order to
more specifically identify the meter in use.
G. Finding: Error corrections are not always properly performed.
Requirement: All documentation errors must be corrected by drawing a single line
through the error so that the original entry remains legible. Entries shall not be obliterated
by erasures or markings. Wite-Out®, correction tape or similar products designed to
obliterate documentation are not to be used. Write the correction adjacent to the error.
The correction must be initialed by the responsible individual and the date of change
documented. All data and log entries must be written in indelible ink. Pencil entries are not
acceptable. Ref: INC WW/GW LC Policy.
Comment: Some instances of overwriting and omitting the date of the correction were
noted.
H. Finding: The date opened (in use) of purchased reagents is not consistently
documented.
Requirement: All chemicals, reagents, standards and consumables used by the
laboratory. must have the following information documented: Date received, Date
Opened (in use), Vendor, Lot Number, and Expiration Date (where specified). A system
(e.g., traceable identifiers) must be in place that links standard/reagent preparation
information to analytical batches in which the solutions are used. Documentation of
solution preparation must include the analyst's initials, date of preparation, the volume or
weight of standard(s) used, the solvent and final volume of the solution. This information
as well as the vendor and/or manufacturer, lot number, and expiration date must be
retained for primary standards, chemicals, reagents, and materials used for a period of
five years. Consumable materials such as pH buffers, lots of pre -made standards and/or
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#143 City of Newton Clark Creek WW Facility
media, solids and bacteria filters, etc. are included in this requirement. Ref: NC
WW/GW LC Policy.
Requirement: Supporting records shall be maintained as evidence that these practices
are being effectively carried out. All analytical records must be available for a period of
five years. Ref: 15A NCAC 2H .0805 (a) (7) and (a) (7) (G).
Comment: The laboratory has an adequate reagent preparation log; however, one
instance of a new lot being put into use without updating the log was noted. The
laboratory began using a new lot of Dextrose on September 14, 2017 as indicated on
the container, but the reagent preparation log indicated that the old lot was still in use at
the time of the inspection.
I. Finding: The laboratory benchsheets for DO, pH, TRC, Temperature and Conductivity
were lacking pertinent data: facility name.
Requirement: The following must be documented in indelible ink whenever sample
analysis is performed: Sample site including facility name and location, ID, etc. Ref: NC
WW/GW LC Approved Procedure for the Analysis of Dissolved Oxygen, NC WW/GW LC
Approved Procedure for the Analysis of pH, NC WW/GW LC Approved Procedure for the
Analysis of Total Residual Chlorine, NC WW/GW LC Approved Procedure for the Analysis
of Temperature and NC WW/GW LC Approved Procedure for the Analysis of Specific
Conductance (Conductivity).
J. Finding: The DO meter calibration documentation does not include all applicable
information.
Requirement: 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. Ref: NC WW/GW LC Approved Procedure for the
Analysis of Dissolved Oxygen,
K. Finding: The time of analysis is not documented when pH is analyzed for Vector
Attraction Reduction, Option 6: Addition of Alkali. This is considered pertinent data.
Requirement: Sewage sludge is considered to have undergone adequate vector
attraction reduction if sufficient alkali is added to:
• Raise the pH to at least 12
• Maintain a pH of at least 12 without addition of more alkali for 2 hours
• Maintain a pH of at least 11.5 without addition of more alkali for an additional 22
hours
Ref: Control of Pathogens and Vector Attraction in Sewage Sludge, EPA/625/R-92/013,
July 2003, Section 8.7.
Requirement: All analytical data pertinent to each certified analysis must be filed in an
orderly manner so as to be readily available for inspection upon request. Ref: 15 NCAC
2H .0805 (a) (7) (A).
L. Finding: The BOD documentation does not demonstrate that the initial DO is measured
within 30 minutes of sample preparation. This is considered pertinent data.
Requirement: After preparing dilution, measure initial DO within 30 min. Ref: Standard
Methods, 5210 B-2001. (5) (g).
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#143 City of Newton Clark Creek WW Facility
Requirement: All analytical data pertinent to each certified analysis must be filed in an
orderly manner so as to be readily available for inspection upon request. Ref: 15 NCAC
2H .0805 (a) (7) (A).
M. Finding: The laboratory benchsheet for the analysis of the quarterly Suspended Residue
standard was lacking pertinent data: value from the measurement system (i.e., units of
measure).
Requirement: All laboratories must use printed laboratory bench worksheets that include
a space to enter the signature or initials of the analyst, date of analyses, sample
identification, volume of sample analyzed, value from the measurement system, factor and
final value to be reported and each item must be recorded each time samples are
analyzed. The date and time BOD and coliform samples are removed from the incubator
must be included on the laboratory worksheet. Ref: 15A NCAC 2H .0805 (a) (7) (H).
Requirement: All analytical data pertinent to each certified analysis must be filed in an
orderly manner so as to be readily available for inspection upon request. Ref: 15A NCAC
21-1.0805 (a) (7) (A).
N. Finding: The time coliform samples are removed from the incubator is not consistently
documented.
Requirement: The date and time BOD and coliform samples are removed from the
incubator must be included on the laboratory worksheet. Ref: 15A NCAC 2H .0805 (a) (7)
(H)
Comment: This was noted for samples removed from the incubator on June 19, 2017.
O. Finding: The time sample filtration begins for Fecal Coliform is not recorded on the
benchsheet to show that no more than 30 minutes has passed before filters are placed
into the incubator. This is considered pertinent data.
Requirement: Place all prepared cultures in the water bath within 30 min after filtration.
Ref: Standard Methods, 9222 D-1997. (2) (d).
Requirement: All analytical data pertinent to each certified analysis must be filed in an
orderly manner so as to be readily available for inspection upon request. Ref: 15 NCAC
2H .0805 (a) (7) (A).
Bacteria — Coliform Fecal — Standard Methods, 9222 D-1997 (MF) (Aqueous)
Recommendation: The acceptance criteria for duplicates is set at ± 3 for 0-5 colonies, ± 10 for 6-
19 colonies and ± 15 for 20 or more colonies. It is recommended that the acceptance criteria be
made more stringent. For example, ± 5 for 0-20 colonies and ± 15% Relative Percent Difference
(RPD) for 20 or more colonies could be established or the acceptance could be based on the
standard deviation for the different count ranges of actual duplicate sample results over time.
Recommendation: It is recommended that the laboratory refer to the "spike" as a "positive
control sample" in order to avoid confusion with Matrix Spike analyses used for other parameters.
P. Finding: The laboratory is not monitoring the quality of the reagent water used in fecal
coliform analysis.
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#143 City of Newton Clark Creek WVV Facility
Requirement: At a minimum, reagent water used to prepare buffered dilution/rinse water
or media must be analyzed at least every twelve months for the following parameters:
Specific Conductance, Total Organic Carbon, Cadmium, Chromium, Copper, Nickel, Lead,
and Zinc.
Maximum Acceptable Limits are:
Total Organic Carbon < 1.0 mg/L
Specific Conductance < 2 pmhos/cm
Heavy Metals, single element < 0.05 mg/L
Heavy Metals, Total of cited elements < 0.10 mg/L
If the facility is using vendor purchased dilution/rinse water this testing is not required as
long as the Certificate of Analysis from the manufacturer meets these requirements and is
kept on file. Ref: NC WW/GW LC Policy.
Q. Finding: The Fecal Coliform incubator temperature is not being monitored and recorded
twice daily.
Requirement: When incubator is in use, monitor and record calibration -corrected
temperature twice daily. Ref: Standard Methods, 9020 B- 2005 (4) (n).
Comment: The incubator temperature is checked and recorded once per day.
R. Finding: Heat -indicating tape is not used each sterilizing cycle.
Requirement: Use heat -indicating tape to identify supplies and materials that have been
sterilized. Ref: Standard Methods 9020 B-2005. (4) (h).
Requirement: All analytical data pertinent to each certified analysis must be filed in an
orderly manner so as to be readily available for inspection upon request. Ref: 15A NCAC
2H .0805 (a) (7) (A).
Comment: This is considered pertinent data and documentation must be maintained.
S. Finding: Plate comparison counts are not being performed.
Requirement: For routine performance evaluation, repeat counts on one or more positive
samples at least monthly, record results, and compare the counts with those of other
analysts testing the same samples. Replicate counts for the same analyst should agree
within 5% (within analyst repeatability of counting) and those between analysts should
agree within 10% (between analysts reproducibility of counting). If they do not agree,
initiate investigation and any necessary corrective action. Ref: Standard Methods, 9020 13-
2005. (9) (a).
Comment: The primary analyst must recount one plate monthly and compare the two
values and any auxiliary analysts will count the same plate twice comparing the two values
and compare the values with the main analyst. If any comparisons do not agree with the
established criteria, retraining may be necessary. All counts must be documented.
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BOD —Standard Methods, 5210 B-2001 (Aqueous)
T. Finding: The laboratory does not prepare Sodium Sulfite daily.
Requirement: Sodium sulfite solution: This solution is not stable; prepare daily. Ref:
Standard Methods, 5210 B-2001. (3) (f).
Comment: The laboratory prepares the Sodium Sulfite weekly.
U. Finding: Samples used for duplicate analysis are not randomly selected.
Requirement: When appropriate (Table 5020:1), randomly select routine samples to be
analyzed twice. Ref: Standard Methods, 5020 B-2010. (2) (f).
Comment: The laboratory always duplicates the influent sample based on
recommendations made by NC WW/GW LC staff in previous inspections performed prior
to this being required.
COD — Hach 8000 (Aqueous)
Recommendation: It is recommended that the column on the benchsheet labeled "Date" be
clarified to "Collection Date".
Recommendation: It is recommended that the laboratory analyze a method blank, which
includes preservatives used in samples, with each sample group.
V. Finding: The laboratory is not analyzing an LFM.
Requirement: Unless the referenced method states a greater frequency, spike 5% of
samples on a monthly basis. Laboratories analyzing less than 20 samples per month must
analyze at least one matrix spike (MS) each month samples are analyzed. If MS results
are out of control, the results must be qualified or the laboratory must take corrective
action to rectify the effect, use another method, or employ the method of standard
additions. When the method of choice specifies MS performance acceptance criteria for
accuracy, and the laboratory chooses to develop statistically valid, laboratory -specific
limits, the laboratory -generated limits cannot be less stringent than the criteria stated in the
approved method. Ref: NC WW/GW LC Policy.
Comment: See the NC WW/GW LC Matrix Spiking Policy and Technical Assistance
document at the end of this report.
Recommendation: It is recommended that the laboratory analyze a LFMD instead of a
sample duplicate to ensure measurable concentrations for assessing precision.
W. Finding: The calibration verification standard is not mid -range.
Requirement: The calibration blank and calibration verification standard (mid -range) must
be analyzed initially (i.e., prior to sample analysis), after every tenth sample and at the end
of each sample group to check for carry over and calibration drift. If either fall outside
established quality control acceptance criteria, corrective action must be taken (e.g.,
repeating sample determinations since the last acceptable calibration verification,
repeating the initial calibration, etc.). Ref: NC WW/GW LC Policy.
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Conductivity — Standard Methods, 2510 B-1997 (Aqueous)
X. Finding: The calibration verification standards are prepared by diluting the 1412 pS
standard.
Requirement: 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. Ref: NC WW/GW LC Approved Procedure for the Analysis of Specific
Conductance (Conductivity).
Comment: The preparation of the standards in Table 2510:1 indicates that the relationship
between mass of KCI used and standard concentration is not linear; therefore, standards
may not be diluted, but must be prepared individually.
Y. Finding: The Automatic Temperature Compensator (ATC) check has not been verified
every 12 months.
Requirement: The ATC must be verified prior to initial use and annually (i.e., 12 months)
thereafter at two temperatures by analyzing a standard or sample at 25°C (i.e., the
temperature to which conductivity values are reported) 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 > 25°C (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. Ref: NC WW/GW LC Approved
Procedure for the Analysis of Specific Conductance (Conductivity).
Nitrogen, Ammonia — Standard Methods, 4500 NH3 D-1997 (Aqueous)
Comment: The laboratory reanalyzes the calibration standards after calibration. This is not
required.
Z. Finding: Samples are not warmed to room temperature prior to analysis.
Requirement: Maintain the same stirring rate and a temperature of about 25 °C
throughout calibration and testing procedures. Ref: Standard Methods, 4500 NH3 D-1997.
(4) (b).
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AA. Finding: The larger volume of 10N NaOH used in the samples versus the calibration
standards was not compensated for in the calculation.
Requirement: The following formula must be used in the calculation:
mg NH3 —N/L=AxBX 100+D
(100 + C)
A = Dilution Factor
B = Concentration of NH3-N/L, mg/L, from calibration curve
C = Volume of 10N NaOH added to the calibration standards, mL
D = Volume of 10N NaOH added to sample, mL
Ref: Standard Methods, 4500 NH3 D-1997. (5).
13I3. Finding: A calibration blank is not analyzed after every ten samples.
Requirement: The calibration blank and calibration verification standard (mid -range) must
be analyzed initially (i.e., prior to sample analysis), after every tenth sample and at the end
of each sample group to check for carry over and calibration drift. If either fall outside
established quality control acceptance criteria, corrective action must be taken (e.g.,
repeating sample determinations since the last acceptable calibration verification,
repeating the initial calibration, etc.). Ref: NC WW/GW LC Policy.
CC. Finding: A calibration verification standard (mid -range) is not analyzed after every tenth
sample and at the end of each sample group.
Requirement: The calibration blank and calibration verification standard (mid -range) must
be analyzed initially (i.e., prior to sample analysis), after every tenth sample and at the end
of each sample group to check for carry over and calibration drift. If either fall outside
established quality control acceptance criteria, corrective action must be taken (e.g.,
repeating sample determinations since the last acceptable calibration verification,
repeating the initial calibration, etc.). Ref: NC WW/GW LC Policy.
DD. Finding: The laboratory is not analyzing a Method Blank.
Requirement: Method blank (MB): Include at least one MB daily or with each batch of 20
or fewer samples, whichever is more frequent. Ref: Standard Methods, 4020 B-2011. (2)
(d).
Requirement: A reagent blank (method blank) consists of reagent water (see section
1080) and all reagents (including preservatives) that normally are in contact with a sample
during the entire analytical procedure. The reagent blank is used to determine whether,
and how much, reagents and the preparative analytical steps contribute to measurement
uncertainty. Ref: Standard Methods, 1020 B-2011. (5).
Recommendation: It is recommended that the acceptance criterion (s'/z the reporting
limit) be added to the benchsheet.
EE. Finding: A laboratory -fortified blank (LFB) is not analyzed.
Requirement: Include at least one LFB daily or per each batch of 20 or fewer samples.
Ref: Standard Methods, 4020 B-2011. (2) (e).
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Requirement: A laboratory -fortified blank [laboratory control standard (LCS)] is a reagent
water sample (with associated preservatives) to which a known concentration of the
analyte(s) of interest has been added. An LFB is used to evaluate laboratory performance
and analyte recovery in a blank matrix. Ref: Standard Methods, 1020 B-2011. (6).
FF. Finding: The laboratory is not analyzing an LFM/LFMD.
Requirement: When appropriate for the analyte (Table 4020:1), include at least one
LFM/LFMD daily or with each batch of 20 or fewer samples. To prepare an LFM, add a
known concentration of analytes (ideally from a second source) to a randomly selected
routine sample without increasing its volume by more than 5%. Ref: Standard Methods,
4020 B-2011, Table 4020:1 and (2) (g).
Residue, Suspended — Standard Methods, 2540 D-1997 (Aqueous)
Comment: The laboratory analyzes a blank using reagent water. This is not required.
Residue, Total — Standard Methods, 2540 B-1997 (Aqueous)
Comment: The laboratory does not analyze compliance samples using this method, but
maintains certification voluntarily.
Chlorine, Total Residual — Standard Methods, 4500 Cl G-2000 (Aqueous)
GG. Finding: The laboratory is not verifying the instrument's factory -set curve every 12
months.
Requirement: Zero the instrument with chlorine -free water and then analyze a reagent
blank (i.e., reagent water plus buffer and DPD) and a series of five standards. The curve
verification must bracket the range of the samples to be analyzed. This type of 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 pg/L and must not vary by more than 25% of the known value for standard
concentrations less than 50 pg/L. The reagent blank concentration must not exceed half
the concentration of the lowest standard. The overall correlation coefficient of the curve
must be >_0.995. Ref: NC WW/GW LC Approved Procedure for the Analysis of Total
Residual Chlorine. Please submit a curve verification with the report reply.
Comment: The last curve verification available during the inspection was performed on
January 8, 2016. The laboratory supervisor thought that a previous analyst performed the
curve verification in 2017 prior to his retirement, but could not find documentation of this.
Recommendation: The previous curves have been prepared by plotting the absorbance
and true values and evaluated based upon the correlation coefficient. It is recommended
that the laboratory follow the verification procedure in the Approved Procedure (Option 1),
which evaluates the curve based on the true and observed values in pg/L.
Recommendation: It is recommended that the laboratory verify the curve at the following
concentrations: 25, a concentration between 25 and 50, 50, 200 and 400 pg/L in order to
ensure PT and Compliance Sample values are bracketed by calibration standards.
Page 12
#143 City of Newton Clark Creek WW Facility
HH. Finding: The laboratory is not analyzing a reagent blank.
Requirement: 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. Ref: NC WW/GW LC Approved
Procedure for the Analysis of Total Residual Chlorine.
Comment: A reagent blank is made from the same laboratory water source used to make
QC 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.
Comment: Analysis of a reagent blank is only required when standards are prepared
(e.g., when performing the calibration curve verification and when PT Samples are
analyzed).
Comment: A reagent blank is made from the same laboratory water source used to make
QC 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.
Dissolved Oxygen — Standard Methods, 4500 O G-2001 (Aqueous)
Dissolved Oxygen — Hach 10360-2011, Rev. 1.2 (LDO) (Aqueous)
pH — Standard Methods, 4500 H+ B-2001 (Aqueous)
II. Finding: The laboratory is not performing a post -analysis calibration verification when
analyses are performed away from the certified laboratory's primary location.
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: 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.
Comment: Alternatively, the meters may be recalibrated at each sample site prior to
analysis.
Page 13
#143 City of Newton Clark Creek WW Facility
IV. PAPER TRAIL INVESTIGATION:
The paper trail consisted of comparing original records (e.g., laboratory benchsheets, logbooks,
etc.) and contract lab reports to eDMRs submitted to the North Carolina Division of Water
Resources. Data were reviewed for the City of Newton Clark Creek WW Facility (NPDES permit
# NC0036196) for January, March, May and June 2017. The following error was noted:
Date
Parameter
Location
Value on
Value on DMR
Benchsheet
3/27/2017
BOD
Effluent
6.6 mg/L
<2 mg/L
To avoid questions of legality, it is recommended that you contact the appropriate Regional Office
for guidance as to whether an amended eDMR will be required. A copy of this report will be made
available to the Regional Office.
V. CONCLUSIONS:
Correcting the above -cited Findings and implementing the Recommendations will help this
laboratory to produce quality data and meet Certification requirements. The inspector would like to
thank the staff for their assistance during the inspection and data review process. Please
respond to all Findings and include supporting documentation, implementation dates and
steps taken to prevent recurrence for each corrective action.
Report prepared by: Jason Smith Date: January 3, 2018
Report reviewed by: Anna Ostendorff Date: January 5, 2018
Weight Verification (NC WW/GW LC Policy 05/23/2008)
ASTM Class 1 and 2 weights must be verified at least every 5 years. ASTM Class 1
weights (20 g to 25 kg) and ASTM Class 2 weights (10 g to 1 mg) are equivalent to the
NBS Class S weights specified in 15A NCAC 2H .0805 (a) (7) (K). Verification may be
accomplished by:
Sending laboratory weights back to the manufacturer for recertification -
reference weights shall be calibrated by a body that can provide traceability to
ASTM specifications, or
2. Checking laboratory weights against certified reference weights (i.e., weights
that have been recertified as above) and found to be within ASTM Class 1 or
Class 2 tolerances (see table below) - often the balance service technician may
provide this service.
Note: Although some manufacturers will assign a one-year calibration due date, 5 years
is considered an acceptable calibration interval due to the limited use of the reference
weight set.
Documentation of weight verifications or recertification must be maintained for 5 years.
If the condition of a weight(s) is in question at any time due to damage (e.g., corrosion,
nicks, scratching, etc.), the laboratory must have that weight(s) re -verified as described
above.
Maximum tolerances (Ref. ASTM E 617-97, 2003)
Denomination
Maximum tolerance for
ASTM Class 1 and 2
weights, (± mg)
500 g
1.2
300 g
0.75
200 g
0.50
100 g
0.25
50 g
0.12
30 g
0.074
20 g
0.074
10 g
0.074
5 g
0.054
3 g
0.054
2 g
0.054
1 g
0.054
500 mg
0.025
300 mg
0.025
200 mg
0.025
100 mg
0.025
50 mg
0.014
30 mg
0.014
20 mg
0.014
10 mg
0.014
5 mg
0.014
3 mg
0.014
2 mg
0.014
1 mg
0.014
North Carolina Wastewater/Groundwater Laboratory Certification
Matrix Spiking Policy and Technical Assistance (05/1112012)
Policy Statement
Unless the referenced method states a greater frequency, spike 5% of samples on a monthly
basis. Laboratories analyzing less than 20 samples per month must analyze at least one matrix
spike (MS) each month samples are analyzed. If MS results are out of control, the results must be
qualified or the laboratory must take corrective action to rectify the effect, use another method, or
employ the method of standard additions. When the method of choice specifies MS performance
acceptance criteria for accuracy, and the laboratory chooses to develop statistically valid,
laboratory -specific limits, the laboratory -generated limits cannot be less stringent than the criteria
stated in the approved method.
When spiking with multi -component standards, if the method does not specify the spiking
components, the Laboratory Control Spike (LCS) and MS must contain all analytes that are
reported.
If the unspiked sample result is in the top 40% of the calibration range, the sample should be
diluted and the MS prepared using the diluted sample. The recovery of the MS samples must be
bracketed by the calibration range.
The volume of spike solution used in MS preparation must in all cases be <_ 10% of the total MS
volume. It is preferable that the spike solution constitutes s 1 % of the total MS volume so that the
MS can be considered a whole volume sample with no adjustment (i.e., volume correction) by
calculation necessary. If the spike solution volume constitutes >1% of the total sample volume,
the sample concentration or spike concentration must be adjusted by calculation.
Technical Assistance
Spike Preparation
The spike concentration may be set at either 5 to 50 times the Method Detection Limit (as
determined by the Method Detection Limit or MDL study) for the analyte, or at 1 to 10 times the
ambient level (average concentration) of the analyte in samples. There are several options for
preparing spikes, for example:
Option 1 (Recommended - easiest) - If the spike solution volume is equal to 1 % or less of
the total sample volume, direct subtraction of the unspiked sample is allowed. When the
volume of the standard solution spiked into a sample or a sample extract is less than 1 %
of the total volume then the final concentration need not be adjusted (e.g., 10 pL of spike
solution added to a 1 mL final extract results in only a negligible 1 % change in the final
extract volume).
Option 2 - Adjust spike solution to a known volume with sample. In this case the sample
concentration must be adjusted. When the volume of spike solution exceeds 1 % of the
total MS volume the sample concentration must be adjusted prior to determining spike
recovery.
The general equation for spike recovery is as follows:
% R = amt. of target in spiked sample — amt. of target in unspiked sample
(conc. or mass) (conc. or mass) x 100
amt. of target spiked into the sample
(conc. or mass)
To apply this to the sample preparation schemes described above, refer to the following
examples.
Spike Preparation Examples
Option 1 - If the spike solution volume is equal to 1 % or less of the total sample volume, direct
subtraction of the unspiked sample is allowed.
Option 1 Example:
0.5 mis of a 1000 mg/L standard spike added to 100 mis of sample has a theoretical
value of 5 mg/L.
(A) The spiked sample recovery is 5.1 mg/L
(B) If the unspiked sample result is 0.5 mg/L
(C) Theoretical value is 5.0 mg/L
The Percent Recovery = spiked sample recovery (A) — unspiked sample result (B) divided
by theoretical value (C) X 100 or
5.1 — 0.5 X 100 = 92% recovery
5.0
A — B X 100 = Percent recovery
C
Option 2 - Adjust spike solution to a known volume with sample. In this case the sample
concentration must be adjusted.
Option 2 Example 1:
10 mis of spike (concentration 50 mg/L) brought to 100 mis with sample the theoretical MS
value is 5 mg/L.
(A) The spiked sample recovery is 5.1
(B) If the unspiked sample result is 0.5 mg/L
(C) % sample is 0.90 (sample volume used (90) divided by final volume (100))
(D) Theoretical value is 5.0 mg/L
The Percent Recovery = spiked sample recovery (A) — (unspiked sample result (B) x %
sample (C)) divided by theoretical value (D) X 100 or
5.1 — (0.5 x 0.9) X 100 = 93% recovery A— (B x C) X 100 = Percent
recovery
5.0 D
Option 2 Example 2: Larger spike volume
25 mis of spike (concentration 50 mg/L) brought to 250 mis with sample the theoretical
MS value is 5 mg/L.
(A) The spiked sample recovery is 5.6
(B) If the unspiked sample result is 0.5 mg/L
(C) % sample is 0.90 (sample volume used (225) divided by final volume (250))
(D) Theoretical value is 5.0 mg/L
The Percent Recovery = spiked sample recovery (A) — (unspiked sample result (B) x %
sample (C)) divided by theoretical value (D) X 100 or
5.6 — (0.5 x 0.9) X 100 = 103% recovery A— (B x C) X 100 = Percent
recovery
5.0 D
Corrective Action/Qualifications for MS
Spike accuracy is usually based on a range of percent recovery (e.g., 80-120%). Refer to the
method of choice for specific acceptance criteria for the matrix spikes until the laboratory
develops or adopts statistically valid, laboratory -specific performance criteria for accuracy. If a MS
fails, and the LCS is acceptable, qualify the data for the MS sample. Repeated failures for a
specific matrix may require use of an alternate method or method of standard addition. Base the
sample batch acceptance on the results of the LCS analyses (and other quality control results)
rather than the MS alone, because the matrix of the spiked sample may interfere with the method
performance. If a MS and the associated LCS fail, re -prepare and reanalyze affected samples.
Post Digestion Spikes (PDS)
Post Digestion Spikes (PDS) are used for some analyses (e.g., metals) to assess the ability of a
method to successfully recover target analytes from an actual sample matrix after the digestion
process has been performed. The PDS results are used with MS results to evaluate matrix
interferences. The MS and PDS should be prepared from the same environmental sample. A PDS
is not to be analyzed in place of a MS. Post Digestion Spikes must be reported as post -digested
and must not be misrepresented as pre-digested spikes. (Exception: TCLP and SPLP samples
are always spiked post digestion.)
Corrective Action/Qualifications for Post Digestion Spikes
In general, if the MS recovery for an analyte does not fall within the quality control acceptance
range but the PDS recovery is acceptable, then a matrix affect (associated with the preparatory
process) should be suspected and the unspiked sample results must be qualified on the basis of
the matrix spike recovery. However, when historical data for the effect does not exist, the
laboratory would normally be expected to perform a second digestion and reanalysis of the MS to
confirm the result. The result would be confirmed if the MS recoveries and PDS recoveries for
both sets of analyses were similar in magnitude and bias. When both the MS recovery and PDS
recovery for a particular analyte falls outside of quality control acceptance range in the same
manner (i.e., the PDS and MS failures are of similar magnitude and the direction of bias is the
same), confirmatory analyses are unnecessary but the data must be qualified.
Parameters Excluded from MS Requirements
Acidity
BOD/CBOD
Chlorophyll
Color — ADM
Conductivity
Ignitability
Paint Filter Test
pH
Salinity
Total Residual Chlorine
Alkalinity
Aquatic Humic Substances
All Bacteriological Parameters
Color - PtCo
Dissolved Oxygen
All Residues
Turbidity
Temperature
Sulfite
Vector Attraction Reduction (All Options)
(Field Laboratories and Field Setting analyses are exempt.)
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