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INSPECTION REPORT ROUTING SHEET
To be attached to all inspection reports in-house only.
Laboratory Cert. #: 348
Laboratory Name: Little Creek Water Reclamation Facility
Inspection Type: Municipal Maintenance
Inspector Name(s): Jeffrey R. Adams
Inspection Date: July 13, 2010
Date Report Completed: July 16, 2010
Date Forwarded to Reviewer: July 16, 2010
Reviewed by: Chet Whiting
Date Review Completed: August 4, 2010
Cover Letter to use: Insp. Initial X Insp. Reg. Insp. No Finding Insp. CP
Unit Supervisor: Dana Satterwhite
Date Received: August 13, 2010
Date Forwarded to Alberta: August 31, 2010
Date Mailed: August 31, 2010
_____________________________________________________________________
On-Site Inspection Report
LABORATORY NAME: Little Creek Water Reclamation Facility
NPDES PERMIT #: NC0025453
ADDRESS: P.O. Box 879
Clayton, NC 27520
CERTIFICATE #: 348
DATE OF INSPECTION: July 13, 2010
TYPE OF INSPECTION: Municipal Maintenance
AUDITOR(S): Jeffrey R. Adams
LOCAL PERSON(S) CONTACTED: James Warren and Leigh Honeycutt
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 neat and equipment was well maintained. Records were maintained and well
organized, however, some quality control procedures need to be implemented.
The laboratory was given a packet containing North Carolina Laboratory Certification quality control
requirements and policy changes during the inspection.
Findings A, C, D, G and H are new policies that have been implemented by our program since the last
inspection.
III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:
Chemicals and Reagents
A. 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
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.
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Comment: The laboratory is maintaining a logbook, documenting most pertinent information.
However, it is not documenting when reagents or chemicals are opened and put into use.
Fecal Coliform – Standard Methods, 18th Edition, 9222 D
B. Finding: The mercury was separated in the maximum holding thermometer in the autoclave
yielding erroneous temperature measurements.
Requirement: Record items sterilized temperature, pressure and time for each run. Optimally
use a recording thermometer. Check operating temperature weekly with a minimum/maximum
thermometer. Ref: Standard Methods, 18th Edition, 9020 B. (2) (i).
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: If the separation in mercury cannot be rejoined, the thermometer must be replaced
with a new maximum holding thermometer in order to meet these requirements.
Ammonia – Standard Methods, 18th Edition, 4500 NH3 F
Total Phosphorous – Standard Methods, 18th Edition, 4500 P F
C. Finding: The laboratory is not analyzing matrix spikes.
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 each month samples are analyzed. Prepare the matrix spike from a
reference source different from that used for calibration unless otherwise stated in the method.
If matrix spike 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 matrix spike 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: North Carolina Wastewater/Groundwater Laboratory Certification Policy.
BOD – Standard Methods, 18th Edition, 5210 B
D. Finding: Extra nutrient, mineral, and buffer solutions are not added to the sample bottles
containing more than 67% sample.
Requirement: When a bottle contains more than 67% of the sample after dilution, nutrients
may be limited in the diluted sample and, subsequently, reduce biological activity. In such
samples, add the nutrient, mineral, and buffer solutions (3a through e) directly to individual BOD
bottles at a rate of 1 mL/L (0.33 mL/300-mL bottle) or use commercially-prepared solutions
designed to dose the appropriate bottle size. Ref: North Carolina Wastewater/Groundwater
Laboratory Certification Policy based upon Standard Methods, 20th Edition, 5210 B. (4) (f) and
Standard Methods, 21st Edition, 5210 B. (5) (c) (2).
Comment: Dilution water prepared as normal with nutrient, mineral, and buffer solutions would
still be used in the BOD bottles. For the bottles containing more than 67% sample, extra
nutrient, mineral, and buffer solutions would be added in addition to the dilution water.
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Recommendation: Rather than pipetting 0.33 mL of each reagent into the BOD bottle, it is
recommended that commercially prepared nutrient buffer pillows for 300 mL bottles be used.
E. Finding: The DO meter is not always checked and documented for drift during, and at the end of
the analytical series,
Requirement: If the membrane electrode method is used, take care to eliminate drift in
calibration between initial and final DO readings. Ref: North Carolina Wastewater/Groundwater
Laboratory Certification Policy based upon Standard Methods, 21st Edition, 5210 B. (5) (g) and
15A NCAC 2H .0805 (a) (7).
Comment: Immediately after calibration, measure the DO of a BOD bottle of dilution water.
Stopper the bottle. Document the concentration on the bench sheet = Day one initial meter
check. The laboratory should verify the DO Meter calibration every 10 readings (to include
dilutions), and at the end of the sample set = Day one final. Repeat process on Day 5. If the
meter drifts more than 0.20 mg/L then recalibrate meter and reanalyze all samples since the
last drift check.
BOD – Hach 10360 (LDO)
Dissolved Oxygen – Hach 10360 (LDO)
Comment: The laboratory did not notify this office of the change in methodology (i.e., Luminescence
Dissolved Oxygen also referred to as LDO) for BOD and Dissolved Oxygen analyses. The North
Carolina Administrative Code, 15A NCAC 2H .0805 (c) (7) requires, A certified laboratory must submit a
written amendment to certification each time that changes occur in methodology, reporting limits, and
major equipment. The amendment must be received within 30 days of such changes. An amendment
form was completed during the inspection and the laboratory’s certificate attachment has been updated
to include the LDO methodology. No further response is necessary for this finding.
Conductivity – Standard Methods, 18th Edition, 2510 B
F. Finding: The Automatic Temperature Compensator (ATC) has not been verified.
Requirement: The ATC must be verified annually (i.e., every twelve months) and the process
documented. The ATC must be verified by analyzing a standard at 25 °C (the temperature that
conductivity values are compensated to) and a temperature(s) that brackets the temperature ranges
of the samples to be analyzed. This may require the analysis of a third temperature reading that is >
25 °C. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy.
Total Phosphorous – Standard Methods, 18th Edition, 4500 P F
Recommendation: It is recommended that the laboratory implement a temperature grid check of the
block digesters by alternating the well location of the thermometer each time samples are dige sted and
documenting the location of the thermometer (as well as all samples, blanks and standards) on a grid
template. This will document heating uniformity and consistency of all sample wells in the block.
Total Residue – Standard Methods, 18th Edition, 2540 B
G. Finding: The laboratory is using an incorrect reporting limit.
Requirement: Choose sample volume to yield between 2.5 and 200 mg dried residue. To
obtain the required residue yield, successive aliquots of samples may be added to the same
dish after evaporation or adjust reporting level based upon the weight gain and sample volume
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used. The minimum reporting value is established at 2.5 mg/L based upon a sample volume
used of 1000 mL. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy
based upon Standard Methods, 20th and 21st Editions, 2540 C. (3) (d) and 2540 B. (3) (b).
Comment: For example, if 100 mL sample is analyzed, and less than 2.5 mg of dried residue is
obtained, the value reported would be <25 mg/L.
Comment: Since the publication of the Code of Federal Regulations, Title 40, Part 136; Federal
Register Vol. 72, No. 47, March 12, 2007, there is no longer an approved method that allows for
a 1 mg weight gain. Currently, the minimum weight gain allowed is 2.5 mg. 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. For example, if 500 mL of sample is analyzed
and < 2.5 mg of dried residue is obtained, the value reported would be < 5 mg/L. The minimum
reporting value is now established at 2.5 mg/L based upon a sample volume used of 1000 mL.
Total Suspended Residue – Standard Methods, 18th Edition, 2540 D
H. Finding: The laboratory is using an incorrect reporting limit.
Requirement: The minimum reporting value is established at 2.5 mg/L when 1000 mL of
sample is analyzed. The minimum weight gain allowed by any approved method is 2.5 mg. 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. For example, if 500 mL of sample
is analyzed and < 2.5 mg of dried residue is obtained, the value reported would be < 5 mg/L.
Ref: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC) Policy
based upon Standard Methods, 20th and 21st Editions - Method 2540 D. (3) (b).
Vector Attraction Reduction – Option 10, Addition of Alkali
pH – EPA SW–846 Method 9040 C
Comment: The laboratory is analyzing sludge by SW -846 Method 9040 C but is not certified. 15A
NCAC 02H .0804 (a) states: 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: The laboratory completed an amendment to laboratory
certification application during the inspection and the certificate attachment has been updated to
include this method. No further response is necessary for this finding.
I. Finding: The pH meter was not calibrated with standards that bracketed the range of the sample
measurements encountered. The laboratory is analyzing its sludge for pH but is not calibrating
or bracketing the analyses with a pH 12.45 or higher buffer.
Requirement: Each instrument/electrode system must be calibrated at a minimum of two points
that bracket the expected pH of the samples. Ref: EPA SW -846 Test Methods for Evaluating
Solid Waste, Physical/Chemical Methods; 3rd Edition, Method 9040 C. Rev. 3, November 2004,
Section 7.1.2.
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 Little Creek Water Reclamation Facility (NPDES p ermit #NC0025453) for the following
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months: March, April and May, 2010. No transcription errors were detected. It appears the laboratory is
doing a good job of accurately transcribing data.
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 16, 2010
Report reviewed by: Chet Whiting Date: August 4, 2010