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INSPECTION REPORT ROUTING SHEET
To be attached to all inspection reports in-house only.
Laboratory Cert. #: #5454
Laboratory Name: Southern Nash Sr. High & Middle Schools
Inspection Type: Field Municipal Maintenance
Inspector Name(s): Jeffrey R. Adams
Inspection Date: July 21, 2011
Date Report Completed: August 03, 2011
Date Forwarded to Reviewer: August 03, 2011
Reviewed by: Chet Whiting
Date Review Completed: August 17, 2011
Cover Letter to use: Insp. Initial Insp. Reg. Insp. No Finding X Insp. CP __ Corrected
Unit Supervisor: Dana Satterwhite
Date Received: August 24, 2011
Date Forwarded to Linda: August 25, 2011
Date Mailed: August 25, 2011
_____________________________________________________________________
On-Site Inspection Report
LABORATORY NAME: Southern Nash Senior High & Middle Schools
NPDES PERMIT #: NC0037915; NC0037885
ADDRESS: 930 Eastern Ave.
Nashville, NC 27807
CERTIFICATE #: 5454
DATE OF INSPECTION: July 21, 2011
TYPE OF INSPECTION: Field Municipal Maintenance
AUDITOR(S): Jeffrey R. Adams
LOCAL PERSON(S) CONTACTED: Donna Ritterpusch and Dan Hackney
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. Laboratory documentation, however, was incomplete, inaccurate and additional quality control
procedures need to be implemented. The inspector is concerned about the number of transcription errors and
record omissions detected during the data review process. Many of the data points recorded on the
benchsheet did not compare to the values reported on the Discharge Monitoring Reports (DMRs) or there was
no reported value and/or supporting data. These observations are documented in the Paper Trail Investigation
section of this report.
The laboratory was given a packet containing North Carolina Laboratory Certification quality control
requirements and policies during the inspection.
III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:
Documentation
A. Finding: The laboratory needs to increase the 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: 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
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standards and/or media, solids and bacteria filters, etc. are included in this requirement. Ref:
Quality Assurance Policies for Field Laboratories.
General Laboratory
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. Steps must be taken to minimize and correct errors in
calculations and may include checks for the following: transcription errors, calculation errors, correct
application of dilution factors, completeness of data, etc. The transcription errors and data omissions,
noted during the paper trail investigation and cited in Finding H, underscore the importance of this type
of technical peer review process.
B. Finding: The laboratory is not calibrating the Tensette® Pipet annually.
Requirement: Mechanical volumetric liquid-dispensing devices (e.g., fixed and adjustable
auto-pipettors, bottle-top dispensers, etc.) must be calibrated at least every twelve months and
documented. Each liquid-dispensing device must meet the manufacturer’s statement of
accuracy. For variable volume devices used at more than one setting, check the accuracy at
the maximum, middle and minimum values. Testing at more than three volumes is optional.
When a device capable of variable settings is dedicated to dispense a single specific volume,
calibration is required at that setting only. Ref: Quality Assurance Policies for Field
Laboratories. (See the attached Calibration of Mechanical Volumetric Liquid-
Dispensing Devices Procedure for an example procedure for pipet calibration.) The
calibration must be performed and a copy submitted with the response to this report.
Dissolved Oxygen – Standard Methods, 18th Edition, 4500 O G
pH – Standard Methods, 18th Edition, 4500 H+ B
C. Finding: The laboratory is not documenting the instrument calibrations and the time
calibrations are performed on laboratory benchsheets.
Requirement: A record of instrument calibration where applicable must be filed in an orderly
manner so as to be readily available for inspection upon request. Ref: 15A NCAC 02H .0805 (g)
(2). Please submit an updated benchsheet with the response to this report.
Requirement: The following must be documented whenever sample analysis is performed.
Time of calibration. Ref: Technical Assistance for Field Analysis of Dissolved Oxygen and
Technical Assistance for Field Analysis of pH.
D. Finding: The laboratory is not documenting sample collection and analysis times on the
benchsheet.
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 02H .0805 (g) (1).
Please submit an updated benchsheet with the response to this report.
Comment: A blanket statement may be added to laboratory benchsheets to indicate that
readings are taken “in-situ”, in which case only an analysis time need be documented.
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#5454 Southern Nash Senior & Middle Schools
pH – Standard Methods, 18th Edition, 4500 H+ B
E. Finding: The laboratory is not performing a calibration check after each calibration.
Requirement: In addition to the calibration standards, the meter must be verified with a third
calibration standard (e.g., pH 7 buffer). If compliance samples are analyzed throughout the day, a
post calibration check (e.g., pH 7 buffer) must be analyzed mid-day and at the end of the run (i.e.,
roughly every 4 hours based on an eight hour day). Ref: Technical Assistance for Field Analysis of
pH. Cited previously on 7/16/2008. Submit copies of all pH benchsheets, generated since
the inspection, with the response to this report.
Settleable Residue – Standard Methods, 18th Edition, 2540 F
Comment: Settleable Residue is no longer required on this facility’s permit, so it was recommended
that the lab drop this parameter from the certificate attachment. An Amendment to Laboratory
Certification form was completed and given to the inspector during the audit and an updated certificate
attachment was sent to the laboratory on 7/21/11.
Total Residual Chlorine – Standard Methods, 18th Edition, 4500 Cl G
F. Finding: The laboratory is not analyzing a check standard each day that samples are analyzed.
Requirement: When a factory-set calibration is used, the laboratory must check the calibration
curve each analysis day. To do this, the laboratory must analyze a blank to zero the instrument
and analyze a check standard each day that samples are analyzed. If compliance samples are
analyzed throughout the day, a post calibration check (mid-range) must be analyzed mid-day
and at the end of the run (i.e., roughly every 4 hours based on an eight hour day). The check
standard concentration must be at mid range and recovery must be within 10% of the known
value. Ref: Technical Assistance for Field Analysis of Total Residual Chlorine.
Recommendation: It is recommended that the laboratory use a 20 mg/L (i.e., 200 µg/L) gel-
type standard for the daily calibration verification check.
Comment: The instructions for using a gel standard are included in the Technical Assistance
for Field Analysis of Total Residual Chlorine document left for the analyst during the inspection.
Before use, determine the actual value of the gel standard against a properly verified
instrument calibration and assign that value to the standard. The assigned values will be used
for the next twelve months, or until a new curve verification is performed. The gel/liquid
standard verification must be performed for each instrument on which they are to be used. If
multiple instruments and/or standard sets are used, each must have assigned values specific
for the instrument and standard set.
H. Finding: Data and supporting information are not always documented.
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. Ref: 15A NCAC 2H .0805 (g) (1).
Comment: It is of concern that there was no Total Residual Chlorine compliance data for the
week of April 09, through April 13, 2011 and no supporting benchsheet records for data entered
on the DMR for April 16 and April 26, 2011. (Refer to the Paper Trail Investigation in Section IV
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of this report.) The absence of supporting data may be considered falsification. A laboratory
that submits falsified data or other information may be decertified for all parameters for up to
two years in accordance with 15A NCAC 2H .0807 (c).
IV. PAPER TRAIL INVESTIGATION:
The paper trail consisted of comparing field testing records and contract lab reports to Discharge
Monitoring Reports (DMRs) submitted to the North Carolina Division of Water Quality. Data were
reviewed for Southern Nash Senior High School (NPDES permit #NC0037915), and Southern Nash
Middle School (NPDES permit #NC0037885), for March, April and May, 2011. The following errors
were noted.
(Southern Nash Senior High School)
Date Parameter Location Value on Benchsheet Value on DMR
04/06/11 Temperature Effluent 18.2 °C 18.1 °C
(Southern Nash Middle School)
Date Parameter Location Value on Benchsheet
*Contract Data
Value on DMR
03/23/11 Total Residual
Chlorine
Effluent 22 µg/L 24 µg/L
04/06/11 Total Nitrogen Effluent TKN + (NO3 + NO2) = TN
*8.62+69.2 = *77.82 mg/L
75.82 mg/L
04/09/11 -
04/13/11
Total Residual
Chlorine
Effluent No Values Recorded No Values Reported
04/16/11 Total Residual
Chlorine
Effluent No Value Recorded 25 µg/L
04/26/11 Total Residual
Chlorine
Effluent No Value Recorded 42 µg/L
In order to avoid questions of legality and possible monitoring frequency violations, 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 forwarded to the Regional Office.
V. CONCLUSIONS:
We are concerned with the finding that was cited previously and not corrected.
Laboratory Decertification Ref: 15A NCAC 2H .0807 (a) (1), (13) and (14):
A laboratory may be decertified for any or all parameters for up to one year for any or all of the
following infractions:
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(1) Failing to maintain the facilities, or records, or personnel, or equipment, or quality control
program as set forth in the application, and these Rules; or
(13) Failing to respond to requests for information by the date due; or
(14) Failing to comply with any other terms, conditions, or requirements of this Section or of a
Laboratory certification.
Correcting the above-cited findings and implementing the recommendations will help this lab to
produce quality data and meet certification requirements. Please respond to all findings.
Report prepared by: Jeffrey R. Adams Date: August 03, 2011
Report reviewed by: Chet Whiting Date: August 17, 2011
Calibration of Mechanical Volumetric Liquid-Dispensing Devices Procedure
A laboratory may use the following method for the gravimetric determination of measurement error of
mechanical volumetric liquid-dispensing devices (e.g., fixed and adjustable auto-pipettors, bottle-top
dispensers, etc.) used to dispense volumes greater than or equal to 100 μl.
Apparatus and Equipment
Weighing vessel (of sufficient capacity to hold all volumes dispensed for the test and a 3:1 height-to-
diameter ratio is recommended to minimize evaporation)
Reagent water (e.g., distilled or deionized water)
Analytical balance (accurate to 0.0001 g for 100 μl to 10 ml, and accurate to 1 mg for 10 ml to 200 ml
dispensed volumes)
Calibrated thermometer (graduated, at a minimum, in 0.5 ºC increments)
Documentation Requirements
Date
Analyst's signature or initials
Device identification (if there is no unique identification such as serial number, assign a laboratory
identification)
Temperature of the reagent water
Nominal or test volume
Weights of dispensed volumes
Procedure
1. Allow apparatus and reagent water to equilibrate to room temperature.
2. Check the calibration of the balance.
3. Wet the liquid-dispensing device and lubricate the piston insuring smooth operation by pipetting
several volumes to waste.
4. Weigh the vessel and tare the balance.
5. Dispense a minimum of five aliquots of water into the vessel, weighing and recording the mass
for each replicate.
6. Calculate the following:
m = mean mass = total of individual weight measurements ÷
total number of measurements
Z = Z correction factor obtained from Table 1 using the temperature of the test liquid and
current barometric pressure.
V = volume equivalent (or corrected volume) of mass measured = m x Z
RE = relative error (%) = [Vm - Vo] x 100
Vo
where:
Vm = corrected mean volume = total of corrected volumes ÷
total number of dispensed volumes
Vo = nominal or test volume
S = standard deviation = For each replicate, subtract the mean volume from the corrected
volume, then square the value. Sum the squared values of all replicates, and then divide the
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sum by n-1 (the number of measurements minus 1). Take the square root of this value to get
the standard deviation.
CV = coefficient of variation (%) = s x 100
Vm
To simplify this process, spreadsheets for calculating and documenting the relative error and
coefficient of variation can be found on the NC Wastewater/Groundwater Laboratory Certification (NC
WW/GW LC) website at http://h2o.enr.state.nc.us/lab/download.htm.
The Relative Error (a measure of accuracy) and Coefficient of Variation (a measure of precision) must
not be greater than the manufacturer's specifications. If the results are greater than the manufacturer's
specification, repeat the procedure. If the results remain greater, follow the manufacturer's instructions
for maintenance and adjustment and repeat the procedure. If repeated calibration attempts do not yield
results within the manufacturer's specifications, the liquid-dispensing device must be repaired or
replaced.
Note: Microliter pipettors may need to be tested under more rigorously controlled conditions or sent to
a calibration service for testing. Since most analytical balances used in environmental laboratories read
to only four decimal places, it may be necessary, when checking microliter pipettors (less tha n 1000
μl), to include the weight of the weighing vessel in each replicate and subtract it and subsequent
aliquots out manually in order to have a measurable mass for the purpose of this verification. Contact
your auditor if you have questions.
Rev. 03/2009
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Table 1. Z Correction Factor Table.
Temperat
ure C
Air pressure, kPa (mbar)
80
(800)
85 (850) 90 (900) 95 (950) 100
(1000)
101.3
(1013)
105
(1050)
15.0 1.0017 1.0018 1.0019 1.0019 1.0020 1.0020 1.0020
15.5 1.0018 1.0019 1.0019 1.0020 1.0020 1.0020 1.0021
16.0 1.0019 1.0020 1.0020 1.0021 1.0021 1.0021 1.0022
16.5 1.0020 1.0020 1.0021 1.0021 1.0022 1.0022 1.0022
17.0 1.0021 1.0021 1.0022 1.0022 1.0023 1.0023 1.0023
17.5 1.0022 1.0022 1.0023 1.0023 1.0024 1.0024 1.0024
18.0 1.0022 1.0023 1.0023 1.0024 1.0025 1.0025 1.0025
18.5 1.0023 1.0024 1.0024 1.0025 1.0025 1.0026 1.0026
19.0 1.0024 1.0025 1.0025 1.0026 1.0026 1.0027 1.0027
19.5 1.0025 1.0026 1.0026 1.0027 1.0027 1.0028 1.0028
20.0 1.0026 1.0027 1.0027 1.0028 1.0028 1.0029 1.0029
20.5 1.0027 1.0028 1.0028 1.0029 1.0029 1.0030 1.0030
21.0 1.0028 1.0029 1.0029 1.0030 1.0031 1.0031 1.0031
21.5 1.0030 1.0030 1.0031 1.0031 1.0032 1.0032 1.0032
22.0 1.0031 1.0031 1.0032 1.0032 1.0033 1.0033 1.0033
22.5 1.0032 1.0032 1.0033 1.0033 1.0034 1.0034 1.0034
23.0 1.0033 1.0033 1.0034 1.0034 1.0035 1.0035 1.0036
23.5 1.0034 1.0035 1.0035 1.0036 1.0036 1.0036 1.0037
24.0 1.0035 1.0036 1.0036 1.0037 1.0037 1.0038 1.0038
24.5 1.0037 1.0037 1.0038 1.0038 1.0039 1.0039 1.0039
25.0 1.0038 1.0038 1.0039 1.0039 1.0040 1.0040 1.0040
25.5 1.0039 1.0040 1.0040 1.0041 1.0041 1.0041 1.0042
26.0 1.0040 1.0041 1.0041 1.0042 1.0042 1.0043 1.0043
26.5 1.0042 1.0042 1.0043 1.0043 1.0044 1.0044 1.0044
27.0 1.0043 1.0044 1.0044 1.0045 1.0045 1.0045 1.0046
27.5 1.0045 1.0045 1.0046 1.0046 1.0047 1.0047 1.0047
28.0 1.0046 1.0046 1.0047 1.0047 1.0048 1.0048 1.0048
28.5 1.0047 1.0048 1.0048 1.0049 1.0049 1.0050 1.0050
29.0 1.0049 1.0049 1.0050 1.0050 1.0051 1.0051 1.0051
29.5 1.0050 1.0051 1.0051 1.0052 1.0052 1.0052 1.0053
30.0 1.0052 1.0052 1.0053 1.0053 1.0054 1.0054 1.0054
Z correction factors are for distilled water as a function of liquid test temperature and air
pressure.
Z values are in microliters per milligram.
Reprinted from ISO 8655-6:2002(E).
If your laboratory does not have a mercury barometer, the true local barometric pressure for locations throughout
North Carolina may be obtained from the North Carolina State University, State Climate Office of North Carolina
website at http://www.nc-climate.ncsu.edu/.