HomeMy WebLinkAbout#193_2019_07_23_TLH_FINALLaboratory Cert. #:
193
Laboratory Name:
Elizabeth City WWTP Lab
Inspection Type:
Municipal Maintenance
Inspector Name(s):
Tom Halvosa, Todd Crawford
Inspection Date:
July 23, 2019
Date Forwarded for Initial
August 20, 2019
Review:
Initial Review by:
Tonja Springer
Date Initial Review
August 26, 2019
Completed:
❑ Insp. Initial ® Insp. Reg
Cover Letter to use:
❑Insp. No Finding ❑Insp. CP
❑Corrected
❑Insp. Reg. Delay
(to use: rt dick, properties, check)
Unit Supervisor/Chemist III:
Todd Crawford
Date Received:
August 26, 2019
Date Forwarded to Admin.:
September 12, 2019
Date Mailed:
September 13, 2019
Special Mailing Instructions:
Include the Regional Office and inform them that fecal coliform results are
suspect due to the low incubator temperature.
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193
Ms. Rebecca Miller
Elizabeth City WWTP Lab
P.O. Box 347
Elizabeth City, NC 27907
NOR rH CAAOLitIA
triviron..Fi1eP tal Oualfty
September 12, 2019
Subject: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC)
Maintenance Inspection
Dear Ms. Miller:
Enclosed is a report for the inspection performed on July 23, 2019 by Tom Halvosa. 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.
Attachment
cc: Tom Halvosa, Dana Satterwhite
Sincerely,
Todd Crawford
Technical Assistance & Compliance Specialist
NC WW/GW Laboratory Certification Branch
North Carolina Department of Environmental Quality I Division of Water Resources
9.623 Mail Service Center i Raleigh, Noith Carolina 27699-1623
Phone 919.733.3903/Fax 919,733,6241
LABORATORY NAME: Elizabeth City WWTP Lab
NPDES PERMIT : NC0025011
ADDRESS: 450 Knobbs Creek Drive
Elizabeth City, NC 27907
CERTIFICATE #: 193
DATE OF INSPECTION: July 23, 2019
TYPE OF INSPECTION Municipal Maintenance
AUDITOR(S): Tom Halvosa and Todd Crawford
LOCAL PERSON(S) CONTACTED: Rebecca Miller, Yasheka Brothers and Andrew Edwards
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 environmental samples.
Staff were forthcoming and seemed eager to adopt necessary changes. We would like to
commend them for their willingness to make their facility more compliant.
All required Proficiency Testing (PT) Samples for the 2019 PT Calendar Year have not yet been
analyzed. The laboratory is reminded that results must be received by this office directly from the
vendor by September 30, 2019.
The laboratory submitted their Quality Assurance (QA) and/or Standard Operating Procedure
(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 July 31, 2020.
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 documents) is in agreement with each
approved practice, test, analysis, measurement, monitoring procedure or regulatory
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#193 Elizabeth City WWTP Lab
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 exacter 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".
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 Pace Analytical Services LLC - Asheville NC (Certification
#40), Pace Analytical Services LLC - Eden NC (Certification #633), Pace Analytical Services
LLC - Huntersville NC (Certification #12) and Pace Analytical Services LLC - Raleigh NC
(Certification #67)
Approved Procedure documents for the analysis of the facility's currently certified Field
Parameters were provided at the time of the inspection.
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Documentation
Recommendation: It is recommended that the laboratory separate the temperature log for the
refrigerator, oven and incubator into individual logs and attach them to the front of each device.
Recommendation: It is recommended that the results on the "River Sample Sheet" be combined
with the effluent benchsheets for each respective parameter.
A. Finding: The laboratory needs to increase the traceability documentation of purchased
materials and reagents, as well as documentation of standards and reagents prepared in
the laboratory.
Requirement: All chemicals, reagents, standards and consumables used by the
laboratory must have the following information documented: 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.
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 does not have a standard and reagent preparation log for the
preparation of Total Residual Chlorine (TRC) calibration and check standards and
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#193 Elizabeth City WWTP Lab
Suspended Resic
log template was
inspection.
Lie check standards. An example standard and reagent preparation
provided to the laboratory with instructions on use at the time of the
Comment: Dates received and opened were written on the Enterolert reagent boxes,
Sodium Permanganate Total Residual Chlorine (TRC) standard stock solution bottle,
conductivity standard bottles and pH buffer bottles. While this can provide a traceability
link to analyses by looking at the dates that the chemicals were in use, that link is lost
once the bottles are discarded. An example receipt log template was provided to the
laboratory with instructions on use at the time of the inspection.
B. 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: NC WW/GW LC Policy.
Comment: Error corrections on the July 2019 Vector Attraction Reduction (VAR):
Option 6 — Addition of Alkali benchsheet were not initialed or dated.
C. Finding: The laboratory benchsheets for Conductivity, TRC, Dissolved Oxygen (DO),
pH, Temperature and VAR: Option 6 are lacking pertinent data: Permit number,
instrument identification, and method reference.
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).
Requirement: The following must be documented in indelible ink whenever sample
analysis is performed: Permit number, instrument identification (serial number preferred)
and method reference. Ref: NC WW/GW LC Approved Procedure for the Analysis of Total
Residual Chlorine (DPD Colorimetric), 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 Specific Conductance
(Conductivity), NC WW/GW LC Approved Procedure for the Analysis of Temperature and
NC WW/GW LC Approved Procedure for the Analysis of Vector Attraction Reduction
(VAR): Option 6 — Addition of Alkali.
Comment: Both the "River Sample Sheet" and the benchsheet for the effluent were
lacking this information.
D. Finding: The Suspended Residue, Enterococci and VAR: Option 6 benchsheets do not
reference the approved methods.
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).
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#193 Elizabeth City WWTP Lab
Requirement: The following must be documented in indelible ink whenever sample
analysis is performed: Method reference. Ref: NC WW/GW LC Approved Procedure for
the Analysis of Vector Attraction Reduction (VAR): Option 6 — Addition of Alkali.
Comment: The laboratory needs to list the associated method with each parameter.
Example, Enterococci - IDEXX EnterolertO, Suspended Residue - SM 2540 D-2011 and
Vector Attraction Reduction - Option 6: Addition of Alkali.
Comment: Our revised Rule number 15A NCAC 2H .0805 (a) (7) (F) (i) states that
certified data shall be traceable to the associated sample analyses and consist of the
method or standard operating procedure.
E. Finding: The laboratory benchsheets for Conductivity and pH are lacking pertinent data:
Meter calibration times.
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).
Requirement: The following must be documented in indelible ink whenever sample
analysis is performed: Meter calibration and meter calibration time(s). Ref: NC WW/GW
LC Approved Procedure for the Analysis of pH.
F. Finding: The laboratory benchsheet for TRC is lacking pertinent data: Daily Check
Standard analysis date and time(s).
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).
Requirement: The following must be documented in indelible ink whenever sample
analysis is performed: Daily Check Standard analysis date and time(s). Ref: NC WW/GW
LC Approved Procedure for the Analysis of Total Residual Chlorine (DPD Colorimetric).
Comment: The TRC benchsheet was lacking Daily Check Standard times.
G. Finding: The laboratory benchsheets for Temperature are lacking pertinent data:
Parameter analyzed.
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).
Requirement: The following must be documented in indelible ink whenever sample
analysis is performed: Parameter analyzed. Ref: NC WW/GW LC Approved Procedure for
the Analysis of Temperature.
Comment: The laboratory was recording Temperature on the same benchsheet as DO
and did not include the parameter on the benchsheet.
H. Finding: The laboratory benchsheets for pH, Temperature and VAR: Option 6 are lacking
pertinent data: Units of measure.
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#193 Elizabeth City WWTP Lab
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).
Requirement: The following must be documented in indelible ink whenever sample
analysis is performed: Units of measure. Ref: NC WW/GW LC Approved Procedure for
the Analysis of pH, NC WW/GW LC Approved Procedure for the Analysis of Temperature
and NC WW/GW LC Approved Procedure for the Analysis of Vector Attraction Reduction
(VAR): Option 6 —Addition of Alkali.
Comment: The pH benchsheet lacked S.U. and the Temperature benchsheet lacked 'C.
The VAR: Option 6 benchsheet lacked both units of measure.
Finding: Sample collection date is not documented for Suspended Residue.
Requirement: Sample identification must be associated with the date and time of sample
collection and analysis. The time elapsed between sampling and analysis must be
documented to determine if hold times are met. Ref: North Carolina
Wastewater/Groundwater Laboratory Certification Policy.
J. Finding: The analyst is not signing or initialing the DO, Temperature and VAR: Option 6
laboratory benchsheets.
Requirement: Data pertinent to each analysis must be maintained for five years. Certified
Data must consist of date collected, time collected, sample site, sample collector, and
sample analysis time. The field benchsheets must provide a space for the signature or
initials of the analyst, and proper units of measure for all analyses. Ref: 15A NCAC 2H
.0805 (g) (1).
Requirement: The following must be documented in indelible ink whenever sample
analysis is performed: Collector's/analyst's name or initials. Ref: NC WW/GW LC
Approved Procedure for the Analysis of Dissolved Oxygen, NC WW/GW LC Approved
Procedure for the Analysis of Temperature and NC WW/GW LC Approved Procedure for
the Analysis of Vector Attraction Reduction (VAR): Option 6 — Addition of Alkali.
K. Finding: Sample collection and/or analysis time is not always documented for pH.
Requirement: Sample identification must be associated with the date and time of
sample collection and analysis. The time elapsed between sampling and analysis must
be documented to determine if hold times are met. Ref: NC WW/GW LC Policy.
Requirement: The following must be documented in indelible ink whenever sample
analysis is performed: Date and time of sample collection, 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.]. Ref: NC WW/GW LC Approved Procedure for
the Analysis of pH.
Comment: The pH benchsheet for April 18, 2019 was missing sample collection and
analysis times.
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#193 Elizabeth City WWTP Lab
L. Finding: Data qualifiers from the contract laboratory reports are not being transferred to
the Discharge Monitoring Report (DMR).
Requirement: When quality control (QC) failures occur, the laboratory must attempt to
determine the source of the problem and must apply corrective action. Part of the
corrective action is notification to the end user. If data qualifiers are used to qualify
samples not meeting QC requirements, the data may not be useable for the intended
purposes. It is the responsibility of the laboratory to provide the client or end -user of the
data with sufficient information to determine the usability of the qualified data. Where
applicable, a notation must be made on the Discharge Monitoring Report (DMR) form, in
the comment section or on a separate sheet attached to the DMR form, when any
required sample quality control does not meet specified criteria and another sample
cannot be obtained. Ref: NC WW/GW LC Policy.
Analytical Balance
M. Finding: The analytical balance weights have not been verified against ASTM standard
weights in the past 5 years.
Requirement: The analytical balance shall be checked with one ASTM Type 1, Class 1 or
2, or equivalent standard weight each day used. These weights shall be verified every five
years. Ref: 15A NCAC 2H .0805 (a) (7) (J).
Comment: The laboratory last verified the analytical balance weights on October 18,
2008.
N. Finding: The analytical balance is not being checked with three weights at the required
frequency.
Requirement: The analytical balance must be checked with one class S, or equivalent,
standard weight each day used and at least three standard weights quarterly. The
values obtained must be recorded in a log and initialed by the analyst. Ref: 15A NCAC
2H .0805 (a) (7) (K).
Requirement: 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.
Comment: The Rule [15A NCAC 2H .0805 (a) (7) (J)J revised in July 1, 2019, which must
be implemented by December 31, 2019, requires a monthly verification with three weights
and does not reference Class S weights.
Recommendation: It is recommended that the monthly checks be implemented with the
report reply so that the laboratory will be in compliance with the revised Rule before the
implementation date.
0. Finding: The weights used to check the balance are not documented to be the
appropriate class. This is considered pertinent data.
Requirement: The analytical balance shall be checked with one ASTM Type 1, Class 1 or
2, or equivalent standard weight each day used. Ref: 15A NCAC 2H .0805 (a) (7) (J).
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#193 Elizabeth City WWTP Lab
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).
Comment: The analytical balance weights have no documented classification.
P. Finding: Thermometers in the ovens and refrigerators are not being checked against a
National Institute of Standards and Technology (NIST) 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).
Requirement: Excluding digital, incubator and infrared temperature -measuring devices,
all non -Reference Temperature -Measuring Devices must be verified at least every 12
months (or sooner if the temperature -measuring device has been exposed to temperature
extremes or other stresses) against a Reference Temperature -Measuring Device and the
process documented. Ref: NC WW/GW LC Policy.
Comment: The laboratory did not have an NIST traceable thermometer. A list of
examples of NIST traceable thermometers was provided to the laboratory after the
inspection.
Q. Finding: The laboratory is not verifying the thermometer in the incubator quarterly.
Requirement: Digital temperature -measuring devices and temperature -measuring
devices used in incubators must be verified at least quarterly (i.e., every 3 months) (or
sooner if the temperature -measuring device has been exposed to temperatures beyond
the manufacturer's recommended range of use or other stresses) against a Reference
Temperature -Measuring Device with the appropriate accuracy and the process
documented. Ref: NC WW/GW LC Policy.
Comment: The requirement to check temperature -measuring devices used in incubators
quarterly was added to the revised Rule, 15 NCAC 2H .0805 (a) (7) (N).
R. Finding: SOPs have not been developed and/or updated for all of the methods included
on the laboratory's Certified Parameters Listing (CPL).
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).
Comment: The laboratory did not have SOPs for PT, Temperature and Vector Attraction
Reduction: Option 6.
Proficiency 12stinq
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#193 Elizabeth City WWTP Lab
S. Finding: Additional QC beyond what is routine for Compliance Samples is being analyzed
with PT Samples.
Requirement: Laboratories are required to analyze an appropriate PT Sample by each
parameter method on the laboratory's CPL. The same PT Sample may be analyzed by
one or more methods. 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. PT Samples shall not be
analyzed with additional quality control. They are not to be replicated beyond what is
routine for Compliance Sample analysis. Although, it may be routine to spike
Compliance Samples, it is neither required, nor recommended, for PT Samples. PT
sample results from multiple analyses (when this is the routine procedure) must be
calculated in the same manner as routine Compliance Samples. Ref: Proficiency
Testing Requirements, October 29, 2018, Revision 3.
T. Finding: PT Samples are not distributed among all analysts from year to year.
Requirement: Laboratories shall also ensure that, from year to year, PT Samples are
equally distributed among personnel trained and qualified for the relevant tests and
instrumentation (when more than one instrument is used for routine Compliance Sample
analyses), that represents the routine operation of the work group at the time the PT
Sample analysis is conducted. Ref: Proficiency Testing Requirements, October 29,
2018, Revision 3.
U. Finding: The laboratory is analyzing samples and reporting data for Salinity without North
Carolina Wastewater/Groundwater Laboratory Certification.
Requirement: Municipal and Industrial Laboratories are required to obtain certification for
parameters which will be reported to the State to comply with State surface water
monitoring, groundwater, and pretreatment Rules. Ref: 15A NCAC 2H .0804 (a).
Comment: The laboratory is analyzing Salinity for upstream and downstream samples on
their "River Sample Sheet" but they are not currently certified for that parameter.
Comment: The Salinity data needs to be documented as uncertified on both the "River
Sample Sheet" and the DMR until the laboratory obtains certification for that parameter.
V. Finding: The laboratory does not report results of all tests on the characteristics of the
effluent when duplicate sample analyses are performed.
Requirement: The results of all tests on the characteristics of the effluent, including but
not limited to NPDES permit monitoring requirements, shall be reported on the monthly
report forms. Ref: 15A NCAC 213 .0506 (b) (3) (J).
Comments: If more than one pH concentration has been measured on a particular day,
these values cannot be averaged due to the logarithmic nature of pH concentrations. All
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#193 Elizabeth City WWTP Lab
values must be reported on the DMR, either in the daily cell or the comments section. The
following convention must be followed when deciding which value to report in the daily cell:
® Any value in violation of permit limits must be reported in the daily cell. If multiple
samples yielded noncompliant results, the most extreme noncompliant value must
be reported in the daily cell. The additional values must be reported in the DMR
comment section.
® If all values taken during the day were compliant with the permit limits, the value
closest to the bounds of the limit range (high or low) must be reported in the daily
cell. The additional values must be reported in the DMR comment section.
Comment: The laboratory is analyzing duplicates for pH and reporting the average on the
DMR.
Recommendation: It is recommended that the laboratory not analyze duplicates for pH.
Recommendation: It is recommended that the laboratory include the acceptance criteria for the
daily check standard on the benchsheet.
W. Finding: The laboratory is applying a blank correction for the chlorine contribution from
the reagents on all results.
Requirement: The use of a blank correction for the chlorine contribution from the
reagents is not allowed by the method. Ref: Standard Methods, 4500 Cl G-2011.
Comment: The laboratory is analyzing TRC using the Hach 10014 ULR method which
requires the use of a blank correction for the contribution of chlorine from the reagents.
The laboratory is currently certified for Standard Methods, 4500 Cl G-20'11.
Conductivity — Standard Methods, 2510 5-2011 (Aqueous)
Recommendation: It is recommended, based off historical compliance data results, that the
laboratory calibrate with the 447 pmhos/cm standard and measure the 1413 pmhos/cm
standard
as the calibration verification check.
X. Finding: The Automatic Temperature Compensator (ATC) check is not being performed.
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.
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#193 Elizabeth City WWTP Lab
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 250C 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).
Comment: The laboratory is not performing an ATC check.
Y. Finding: The laboratory is not analyzing a second -source calibration verification check
standard prior to analyzing compliance samples.
Requirement: Analyze and document a second -source calibration verification check
standard prior to compliance sample analysis. It is recommended that this standard
value approximate (may be higher or lower than the calibration standard, as applicable)
the expected range of sample values measured. Ref: NC WW/GW LC Approved
Procedure for the Analysis of Specific Conductance (Conductivity).
Comment: The laboratory is calibrating with three standards (i.e. 447 pmhos/cm, 2070
pmhos/cm and 1413 pmhos/cm).
Dissolved Oxygen — Hach 10360-2011, Rev. 1.2 (LDO) (Aqueous)
Z. Finding: The laboratory is not applying the barometric pressure correction factor to
determine the theoretical DO value.
Requirement: 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.).
Ref: NC WW/GW LC Approved Procedure for the Analysis of Dissolved Oxygen (DO).
Comment: The laboratory is determining a barometric pressure correction factor but not
applying it to the theoretical DO value associated with the sample temperature .
Recommendation: It is recommended that the laboratory update the benchsheet to state
that the observed DO reading during calibration must be within ± 0.5 mg/L of the
determined theoretical DO.
Dissolved Oxygen — Hach 10360-2011, Rev. 1.2 (LDO) (Aqueous)
pH — Standard Methods, 4500 H+B-2011 (Aqueous)
AA. Finding: The laboratory is not performing a post -analysis calibration verification when
analyses are performed at multiple sample sites.
Requirement: When performing analyses at multiple sample sites, a post -analysis
calibration verification must be performed at the end of the run, regardless of meter
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#193 Elizabeth City WWTP Lab
type. 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. Alternatively, if the
meter is calibrated at each sample site prior to analysis, a post -analysis calibration
verification is not required. Ref: NC WW/GW LC Approved Procedure for the Analysis of
Dissolved Oxygen.
Requirement: When performing analyses at multiple sample sites, a post -analysis
calibration verification using the check standard buffer must be analyzed at the end of
the run. The post -analysis check standard buffer(s) must read within ±0.1 S.U. or
corrective actions must be taken. If recalibration is necessary, all samples analyzed
since the last acceptable calibration verification must be reanalyzed, if possible. If
samples cannot be reanalyzed, the data must be qualified. Ref: NC WW/GW LC
Approved Procedure for the Analysis of pH.
Comment: The laboratory is not performing a post -analysis calibration verification after
analyzing upstream and downstream samples. The laboratory has the option to calibrate
before sample analysis at each site instead.
Temperature — Standard Methods, 2550 D-2010 (Aqueous)
D13. Finding: The temperature sensor on the DO meter used to obtain reported temperature
values has not been checked against an NISI traceable thermometer.
Requirement: All compliance temperature -measuring devices without a valid NISI
certificate must be checked initially and every 12 months against an NIST traceable
temperature -measuring device and the process documented. Documentation must
include the serial number of the device being checked. The serial number, stated
accuracy and expiration date of the NIST traceable temperature -measuring device used
in the comparison must also be documented. Verification data must be kept on file and
be available for inspection for 5 years. (NOTE: Vendors or other Certified laboratories
may provide assistance in meeting this requirement. When a vendor or other Certified
laboratory provides this assistance, they must provide a copy of their NIST Certificate or
the serial number, accuracy and calibration expiration date.) Ref: NC WW/GW LC
Approved Procedure for the Analysis of Temperature.
Requirement: Data pertinent to each analysis must be maintained for five years. Ref:
15A NCAC 2H .0805 (g) (1).
Comment: The temperature sensor on the DO meter used to obtain reported
Temperature values has only been checked against a thermometer that is not NISI
traceable. Once verification against an NISI traceable temperature -measuring device is
implemented, the documentation of that verification must include the items indicated in the
Approved Procedure Requirement above.
Enterococci — IDEXX Enterolert® (MPN) (Aqueous)
Comment: The laboratory is retaining an autoclave run log printout that does not include items
autoclaved and is not initialed. The revised Rule (15A NCAC 2H .0805 (a) (7) (1)] states: During
each use of an autoclave, the temperature, pressure, cycle time, and items autoclaved shall be
checked, recorded, dated, and initialed. This must be implemented by December 31, 2019.
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#193 Elizabeth City WWTP Lab
Recommendation: It is recommended that the laboratory use 95 % confidence limits when
determining acceptance criteria for duplicates. The 95% Confidence Limits table can be found
here:
httisv//files.nc.c�ov/r7cde�/Water%20Cuality/Chcmistry°1o20LabPCertification/Technicai%a20Ass_i
stance%20Documents/Quanti-Trav 2000 MPN Table.odf
CC. Finding: The temperature of the incubator is not recorded to the tenths of a degree.
Requirement: Incubate at 41 ± 0.5°C for 24 hours. Ref: IDEXX Enterolert® instructions.
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 .0505 (a) (7).
Comment: The incubator temperature must be documented to the tenth of a degree to
demonstrate compliance with the ± 0.5°C tolerance required by the method.
DD. Finding: The incubator temperature is not consistently checked and recorded daily.
A4
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Requirement: Each day an incubator, oven, waterbath or refrigerator is used, the
temperature must be checked, recorded, and initialed. During each use, the autoclave
maximum temperature and pressure must be checked, recorded, and initialed. Ref: 15A
NCAC 2H .0805 (a) (7) (J).
Comment: From July 1, 2019 to July 23, 2019 the incubator temperature was only
recorded twice.
Comment: The temperature requirement in the incubator temperature log was
erroneously listed as 40.0 ± 0.5°C whereas the actual requirement is 41.0 ± 0.5°C.
Finding: The incubator temperature was not within the acceptable range.
Requirement: Incubate at 41 ± 0.5°C for 24 hours. Ref: IDEXX Enterolert® instructions.
Comment: During the inspection it was noted that the air incubator temperature -
measuring device was indicating 39.0°C. Upward adjustments were made to the air
incubator during the inspection and the temperature -measuring device eventually
indicated the correct temperature of 41.0°C.
Finding: Samples are not consistently checked and documented for the presence of
residual chlorine.
Requirement: Dechlorinating agents used at the time of sampling must be documented
to have been effective upon receipt in the laboratory. A variety of field testing kits are
considered to be adequate for most chlorine interference checks and a maximum
detection limit of 0.5 mg/L is allowed. Ref: NC WW/GW LC Policy.
GG. Finding: The Quanti-Tray® sealer is not checked monthly for leaks.
Requirement: If the Quanti-Tray® or Quanti-Tray®/2000 test is used, the sealer must
be checked monthly by adding a dye (e.g., bromcresol purple) to a water blank. If dye is
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#193 Elizabeth City WWTP Lab
observed outside the wells, either perform maintenance or use another sealer. Ref: NC
WW/GW LC Policy.
Comment: Effective January 1, 2021, NC WW/GW LC will no longer allow drying studies or dry
filter blanks to substitute for drying and weighing to a constant weight. Prior to filtering samples,
all filters will have to be washed and dried to a constant weight (within 0.5 mg of the prior weight).
All filters after filtering samples will also have to be dried and weighed to a constant weight (within
0.5 mg of the prior weight).
Comment: The Suspended Residue benchsheet had a column listed as "Dilution Factor
1,000,000/2" which they used to calculate the final result.
Recommendation: It is recommended that the laboratory name this column "Conversion Factor"
and include the following conversion factor: 1,000,000/ mL of sample.
HH. Finding: Filters are not weighed to constant weight prior to sample analysis, nor is a dry
filter blank analyzed with each set of samples.
Requirement: If pre -prepared filters are not used, the method requires that filters must be
weighed to a constant weight after washing. Repeat cycle of drying, cooling, desiccating,
and weighing until a constant weight is obtained or until weight change is less than 4% of
the previous weighing or 0.5 mg, whichever is less. In lieu of this process, it is acceptable
to analyze a single daily dry filter blank to fulfill the method requirement of drying all filters
to a constant weight prior to analysis. Ref: NC WW/GW LC Policy.
Comment: The laboratory is using pre -prepared filters but they are not twice -weighed
filters.
II. Finding: The samples are not weighed to constant weight, nor is an annual drying study
to verify the adequacy of the drying time, performed.
Requirement: The minimum weight gain allowed by any approved method is 2.5 mg.
Choose sample volume to yield between 2.5 and 200 mg dried residue. This establishes
a minimum reporting value of 2.5 mg/L when 1000 mL of sample is analyzed. If
complete filtration takes more than 10 minutes increase filter diameter or decrease
sample volume. In instances where the weight gain is less than the required 2.5 mg, the
value must be reported as less than the appropriate value based upon the volume used.
Ref: NC WW/GW LC Policy.
JJ. Finding: A check standard is not being analyzed quarterly.
Requirement: Analyze one suspended residue, one dissolved residue, one residual
chlorine and one oil and grease standard quarterly. Ref: 15 NCAC 2H .0805 (a) (7) (B).
Comment: The revised Rule [15 NCAC 2H
analyze one standard monthly during each
implemented by December 31, 2019.
0805 (a) (7) (G)] requires the laboratory to
month samples are analyzed. This must be
Recommendation: It is recommended that the analysis of a monthly check standard be
implemented with the report reply so that the laboratory will be in compliance with the
revised Rule before the implementation date.
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#193 Elizabeth City WWTP Lab
1 i tv. 1 ``�: f.. •i �. t►1; b f
KK. Finding: The range of the samples being analyzed are not bracketed by the calibration
and check standard buffers.
Requirement: The pH meter must be calibrated each day of analysis. Calibration must
include at least two buffers. The meter calibration must be verified with a third standard
buffer solution (i.e., check buffer) prior to sample analysis. The calibration and check
standard buffers must bracket the range of the samples being analyzed (i.e., 12 ± 0.5
S.U.). Ref: NC WW/GW LC Approved Procedure for the Analysis of Vector Attraction
Reduction (VAR): Option 6 — Addition of Alkali.
Comment: The laboratory was using a calibration range of 4.0 — 10.0 S.U. to analyze
sewage sludge samples with pH values greater than 12 S.U.
Recommendation: It is recommended that the laboratory use a low -sodium glass
electrode designed for pH values over 10 S.U. Also, it is recommended to calibrate with
the 7, 10 and 12.45 S.U. or 13 S.U. buffer instead of a 4 S.U. buffer. Note: High pH
buffers absorb CO2 and acidic vapors from the atmosphere which alters the pH. Ensure
high pH buffers are within expiration and stored with minimal headspace.
ILL. Finding: A correction factor is not being applied to pH values when samples are analyzed
at temperatures other than 25°C.
Requirement: If samples are not analyzed at 25°C, the results must be adjusted based
on the ambient temperature where pH is measured and the following calculation:
Correction Factor = 0.03 pH units X (T,neas 25°C)
1.0°C
Actual pH = Measured pH +/- the Correction Factor
Where Tmeas is the temperature of the sludge at the same location and depth at which
the pH is measured. Ref: NC WW/GW LC Approved Procedure for the Analysis of
Vector Attraction Reduction (VAR): Option 6 — Addition of Alkali.
The paper trail consisted of comparing original records (e.g., laboratory benchsheets, logbooks,
etc.) and contract lab reports to DMRs submitted to the North Carolina Division of Water
Resources. Data were reviewed for Elizabeth City WWTP Lab (NPDES permit # NCO025011) for
July, October and November 2018. No transcription errors were observed. The facility appears to
be doing a good job of accurately transcribing data.
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.
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#193 Elizabeth City WWTP Lab
Report prepared by: Tom Halvosa Date: August 20, 2019
Report reviewed by: Tonja Springer Date: August 26, 2019
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