#87 12-Final

INSPECTION REPORT ROUTING SHEET

To be attached to all inspection reports in-house only.

Laboratory Cert. #: #87

Laboratory Name: Anson County WWTP Laboratory

Inspection Type: Municipal Maintenance

Inspector Name(s): Jeffrey R. Adams

Inspection Date: July 12, 2012

Date Report Completed: July 23, 2012

Date Forwarded to Reviewer: July 23, 2012

Reviewed by: Jason Smith

Date Review Completed: July 27, 2012

Cover Letter to use: Insp. Initial X Insp. Reg. Insp. No Finding Insp. CP ___ Corrected

Unit Supervisor: Dana Satterwhite

Date Received: August 3, 2012

Date Forwarded to Linda Chavis August 20, 2012

Date Mailed: August 20, 2012

_____________________________________________________________________

On-Site Inspection Report

LABORATORY NAME: Anson County WWTP Laboratory

NPDES PERMIT #: NC0041408

ADDRESS: P.O. Box 553
Wadesboro, NC 28170

CERTIFICATE #: 87

DATE OF INSPECTION: July 12, 2012

TYPE OF INSPECTION: Municipal Maintenance

AUDITOR(S): Jeffrey R. Adams

LOCAL PERSON(S) CONTACTED: Silvia Jeter and Leon Gatewood

I. INTRODUCTION:

This laboratory was inspected to verify its compliance with the requirements of 15A NCAC 2H .0800 for
the analysis of environmental samples.

II. GENERAL COMMENTS:

The laboratory was clean and well organized. The facility has all the equipment necessary to perform the
analyses, however, some quality control procedures need to be implemented.

The laboratory is reminded that any time changes are made to laboratory operations; the laboratory
must update the Quality Assurance (QA)/Standard Operating Procedures (SOP) document(s). Any
changes made in response to the 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 approved practice and regulatory
requirements. In some instances, the laboratory may need to create a SOP to document how new
functions or policy will be implemented.

On May 18, 2012, EPA promulgated changes to the list of Clean Water Act (CWA) methods at 40 CFR
Part 136.3. This action, referred to as the Methods Update Rule (MUR) approves new methods, or
changes to existing methods, that affects over 100 EPA methods, Standard Methods, ASTM methods,
and other test procedures in Part 136 of Title 40 of the Code of Federal Regulations (CFR). The rule
also contains a number of clarifications relating to approved methods, sample preservation and holding
times, and method modifications. The final rule may be found at:
http://water.epa.gov/scitech/methods/cwa/update_index.cfm. The North Carolina
Wastewater/Groundwater Laboratory Certification (NC WW/GW LC) program will be asking certified
laboratories to move toward implementation of the new rule with changes fully implemented by the end
of 2012. Each laboratory will need to review the MUR and evaluate its effect on current laboratory
practices. These changes must be made in the laboratory’s Standard Operating Procedures and in
Quality Manuals, as well as any other place where the method is cited, e.g., reports, benchsheets,
logs, etc. During this transition period, inspection reports will refer to the methods employed at the
laboratory at the time of the inspection, but will reference the requirements in the most recently
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approved version of the method. Any difficulties encountered with meeting the requirements of these
references by the date due may be addressed in the written corrective action response.

The laboratory has volunteered to assist the Town of Ansonville with its Total Residual Chlorine annual
verification curve. The inspector would like to thank the laboratory for its willingness to assist smaller
field laboratories in meeting their certification requirements.

The laboratorys contract laboratory is Meritech, Inc. of Reidsville, NC #165

The laboratory was given a packet containing North Carolina Laboratory Certification quality control
requirements and policies during the inspection.

The requirements associated with Findings B and H are new policies that have been implemented by our
program since the last inspection.

III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:

General

Recommendation: In order to improve the quality of the data being reported, it is recommended that
the laboratory expand their data verification system to include a technical peer review process to check
for accuracy and completeness of data on laboratory benchsheets and DMR forms. Steps must be
taken to minimize and correct errors in calculations and may include checks for the following:
transcription errors, errors of omission, calculation errors, correct application of dilution factors, etc.
The review should include, at a minimum, a percentage of “raw data calculation verifications.” The
transcription errors noted in the Paper Trail Investigation section of this report, underscore the
importance of this type of technical peer review process.

Documentation

A. Finding: Standard Operating Procedures (SOPs) have not been updated for all of the
parameters included on the laboratory’s certificate attachment.

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. The quality
control document shall be available for inspection by the State Laboratory. Ref: 15A NCAC 2H
.0805 (a) (7). Please submit copies of the revised and updated SOPs no later than
December 31, 2012. A written response to this finding is required with the response to this
report.

Recommendation: It is recommended that SOPs include a revision history with relevant dates
(e.g., effective, review and revision dates) and a brief description of the change(s) made. It is
recommended that SOPs be reviewed annually.

Comment: The last time the SOPs were reviewed and revised was in 1999.

B. Finding: The laboratory needs to increase the documentation of materials and reagents used
or made in the laboratory.

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
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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 media, solids and bacteria filters, etc. are included in this requirement. Ref:
North Carolina Wastewater/Groundwater Laboratory Certification Policy.

General Laboratory

Recommendation: It was observed during the inspection that the analytical weights exhibited
scratches. After further inspection, it was discovered that the analyst was using metal tweezers to
retrieve the weights when weighing. It is recommended that the laboratory use plastic or plastic coated
blunt-tipped forceps when handling the analytical weights used for daily verification of the analytical
balance calibration since scratching can change their weight. The weights were checked on 7/28/2011
by Mettler Toledo and found to be within tolerance.

C. Finding: The alcohol in the thermometer used for monitoring the refrigerator temperature was
separated and was not measuring accurately.

Requirement: Each laboratory requesting certification must contain or be equipped with the
glassware, chemicals, supplies and equipment required to perform all analytical procedures
included in their certification. Ref: 15A NCAC 02H .0805 (a) (6) (H).

Comment: During the inspection the analyst checked the refrigerator temperature with another
thermometer and found the temperature to be acceptable at 4ºC.

Dissolved Oxygen – Standard Methods, 18th Edition, 4500 O G

D. Finding: The Dissolved Oxygen (DO) probe gold cathode was tarnished and was not bright,
indicating it to be oxidized and needing maintenance or replacing.

Requirement: For correct operation of the probe, the gold cathode must always be bright. If it
is tarnished (which can result from contact with certain gases), or plated with silver (which can
result from extended use with a loose membrane), the gold surface must be restored. To
restore the cathode, you may either return the instrument to the factory or clean it using the YSI
Model 5680 Probe Reconditioning Kit. Never use chemicals or abrasives not supplied with this
kit. Ref: YSI Model 55 Handheld Dissolved Oxygen and Temperature Operators Manual, YSI
Incorporated, January 2007, Section 4.5.5.

Fecal Coliform – Standard Methods, 18th Edition, 9222 D (MF)

Recommendation: The laboratory is using an alcohol thermometer in the Fecal Coliform waterbath.
When compared to a National Institute of Standards and Technology (NIST) traceable thermometer, it
had a 0.4ºC correction. Due to the strict temperature tolerance requirement for fecal coliform colony
development (i.e., ± 0.2ºC), it is recommended that the laboratory use another thermometer for the
Fecal Coliform waterbath.

E. Finding: The laboratory is not checking for Total Residual Chlorine.

Requirement: Dechlorinating agents used at the time of sampling must be documented to
have been effective upon the receipt into the laboratory. A variety of field testing kits are
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considered to be adequate for most residual chlorine checks and a maximum detection limit of
0.5 mg/L is allowed. Ref: Memorandum: Required Documentation for Sample Preservation and
Hold Time, Pat Donnelly, June 20, 2007.

Comment: If Fecal Coliform sampling occurs at the same time as Total Residual Chlorine
(TRC) sampling, the TRC sample analysis could document the absence of Total Residual
Chlorine.

F. Finding: Consumable materials used for the Fecal Coliform MF method are not tested prior to
use to ensure that they are reliable.

Requirement: When a new lot of culture medium, pads, or membrane filters is to be used, a
comparison of the current lot in use (reference lot) against the new lot (test lot), be made. As a
minimum, make single analyses on five positive samples. Ref: Standard Methods, 9020 B-1997.
(4) (e). Include all supporting documentation with your response to this report.

Recommendation: It is recommended that the comparison tests be performed with a culture
positive sample that will yield the desired 20 to 60 colonies. The culture positive sample should
be analyzed the day prior to the comparison testing to determine the appropriate dilution to
yield 20 – 60 colonies.

Comment: Guidance for conducting the comparison was provided during the inspection. Since
there is no baseline for determining the acceptability of materials currently in use, acceptable
consumables from another lab (either a contract lab or peer lab) must be used for the initial
testing of materials currently in use. This testing may be performed in either laboratory.

Total Residual Chlorine – Standard Methods, 18th Edition, 4500 Cl G

G. Finding: The laboratory’s calibration curve verification does not bracket Proficiency Testing
(PT) sample concentrations.

Requirement: For analytical procedures requiring analysis of a series of standards, the
concentrations of these standards must bracket the concentration of the samples analyzed. One
of the standards must have a concentration equal to the laboratory's lower reporting concentration
for the parameter involved. For colorimetric analyses, a series of five standards for a curve
prepared annually or three standards for curves established each day or standards as set forth in
the analytical procedure must be analyzed to establish a standard curve. Ref: 15A NCAC 2H
.0805 (a) (7) (I). A copy of the new annual 5-point Total Residual Chlorine curve verification
documentation must be submitted with the response to this report.

Recommendation: The laboratory’s National Pollutant Discharge Elimination System (NPDES)
Permit limit is 28 µg/L for Total Residual Chlorine. It is recommended that the laboratory verify
the internal calibration using the concentrations: 20, 30, 50, 200 and 400 µg/L. This will verify
the analytical range used to measure Proficiency Testing (PT) samples as well as
environmental samples.

Recommendation: It is recommended that the values obtained not vary by more than 10% of the
known value for standard concentrations greater than or equal to 50 g/L and 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.

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Total Suspended Residue – Standard Methods, 18th Edition, 2540 D

Comment: The drying cycle for each sample is not being repeated, nor has the alternative annual
multiple weighing study to verify the adequacy of the drying time been conducted. North Carolina
Wastewater/Groundwater Laboratory Certification Policy states: Constant weights must be documented.
The approved methods require the following: “Repeat the cycle of drying, cooling, desiccating, and
weighing until a constant weight is obtained or until the weight change is less than 4% of the previous
weight or 0.5 mg, whichever is less.” In lieu of this, an annual study documenting the time required to dry
representative samples to a constant weight may be performed. Verify minimum daily drying time is
greater than or equal to the time used for the initial verification study drying cycle. Drying cycles must be a
minimum 1 hour for verification. Demonstration of acceptable corrective action (i.e., the laboratory
submitted an acceptable drying study) was received on 7/13/12 by electronic mail. No further response
is necessary for this finding.

H. Finding: The laboratory is not basing the reporting limit on a minimum weight gain of 2.5 mg.

Requirement: Choose sample volume to yield between 2.5 and 200 mg dried residue. If
volume filtered fails to meet minimum yield, increase sample volume up to 1 L. If complete
filtration takes more than 10 min, increase filter diameter or decrease sample volume. Ref:
Standard Methods, 2540 D-1997 (3) (b).

Comment: The laboratory is using a 100 ml sample volume, and is using <10 mg/L as its
reporting limit. Based on a 100 ml sample volume, the required reporting limit is <25 mg/L. This
reporting level may not be adequate to meet permit monitoring requirements.

IV. PAPER TRAIL INVESTIGATION:

The paper trail consisted of comparing laboratory benchsheets and contract lab reports to Discharge
Monitoring Reports (DMRs) submitted to the North Carolina Division of Water Quality. Data were
reviewed for the Anson County WWTP Laboratory (NPDES permit #NC0041408) for March, April and
May, 2012. The following errors were noted:

Date Parameter Location Value on Benchsheet
*Contract Data
Value on DMR
4/04/12 Copper Effluent *9.6 µg/L No Value Reported
4/04/12 Zinc Effluent *77.2 µg/L No Value Reported
4/04/12 Total
Phosphorous
Effluent *3.31 µg/L No Value Reported
4/04/12 Total Nitrogen Effluent *14.6 mg/L No Value Reported
4/11/12 Cadmium Effluent *<2.0 µg/L <5.0 µg/L

In order to avoid a possible monitoring frequency violation, it is recommended that you contact the
appropriate Regional Office for guidance as to whether an amended Discharge Monitoring Report will
be required. A copy of this report will be made available to the Regional Office.

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V. CONCLUSIONS:

Correcting the above-cited findings and implementing the recommendations 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.

Report prepared by: Jeffrey R. Adams Date: July 23, 2012
Report reviewed by: Jason Smith Date: July 27, 2012