HomeMy WebLinkAboutNC0005762_Lab Inspection_20091027Beverly Eaves Perdue
Governor
NCDENR
North Carolina Department of Environment and Natural Resources
Division of Water Quality
Coleen H. Sullins Dee Freeman
Director Secretary
156
Mr. Fred Locklear
WestPoint Home Incorporated
P.O. Box 388
Wagram, NC 28396
October 27, 2009
Nov 0 2
Subject: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC)
Maintenance Inspection
Dear Mr. Locklear :
-Enclosed is a report for the inspection performed on August 4, 2009 by Ms. Tonja Springer. 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. 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.
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 us at 919-733-3908.
incerely,
Dana Sdtterwhite
Certification Unit Supervisor
Laboratory Section
Enclosure
cc: Tonja Springer
Raleigh Regional Office
DENR
DENR DWQ Laboratory Section NC Wastewater/Groundwater Laboratory Certification Branch
1623 Mail Service Center, Raleigh, North Carolina 27699-1623
Location: 4405 Reedy Creek Road. Raleigh, North Carolina 27607-6445
Phone: 919-733-39081 FAX: 919-733-6241
Internet: www.dwglab.org
An Equal Opportunity 1 Affirmative Action Employer Customer Service: 1-877-623-6748 www.ncwaterquality.org
NorthCarolina
Naturally
On -Site Inspection Report
LABORATORY NAME: WestPoint Home, Incorporated
NPDES PERMIT #: NC0005762
MAILING ADDRESS: P.O. Box 388
Wagram, NC 28396
CERTIFICATE #: 156
DATE OF INSPECTION: August 4, 2009
TYPE OF INSPECTION: Municipal Maintenance
AUDITOR(S): Tonja Springer
LOCAL PERSON(S) CONTACTED: Ronald Locklear and Fred Locklear
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 facility has all the equipment necessary to perform the analyses; however, improvements in quality
control and documentation must be made. Several guidance documents are attached to this report.
Findings D, G, J, M, and V are new policies that have been implemented by our program since the last
inspection.
III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:
General Laboratory
A. Finding: The laboratory has Standard Operating Procedures (SOPs) but they do not contain all
the pertinent information.
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. A
standard operating procedure describes the method in such detail that an experienced analyst
unfamiliar with the method can obtain acceptable results. Standard operating procedures must
be developed which describe in detail how a method is performed in that particular laboratory.
Ref: 15A NCAC 2H .0805 (a) (7). (See attached guidance on preparing Standard Operating
Procedures.)
Recommendation: It is recommended that the SOPs be reviewed at least every one to three
years. It is also recommended that a revision and/or review history with pertinent dates be
documented so that it is clear what changes were madein each revision.
B. Finding: Duplicate analyses are not evaluated for acceptability.
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#156 WestPoint Home Incorporated
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: North Carolina Wastewater/Groundwater Laboratory Certification Policy requires,
when Quality Control (QC) failures occur, the laboratory must attempt to determine the source
of the problem and must apply corrective action. Control limits for duplicate sample analysis
must be established. Acceptance values must be established, documented, and evaluated
against results obtained on analyses. The results obtained must be documented on the
benchsheet and evaluated against the acceptance criteria to demonstrate that the analyst was
aware of any out -of -control situation and the corrective action that was taken. Any samples not
meeting the criteria must be reanalyzed if possible. Where applicable, a notation must be
made on the Discharge Monitoring Report (DMR) form, in the comment section, when any
required sample quality control does not meet specified criteria, and another sample cannot be
obtained.
C. Finding: No acceptance criteria have been established to evaluate the precision . of sample
duplicate analyses.
Requirement: Any time quality control results indicate an analytical problem, the problem must
be resolved and any samples involved must be rerun if the holding time has not expired. 'Ref:
15A NCAC 2H .0805 (a) (7) (F).
D. Finding: Auto-pipettors are not calibrated twice a year.
Requirement: Mechanical volumetric liquid -dispensing devices (e.g., fixed and adjustable auto-
pipettors, bottle -top dispensers, etc.) must be calibrated at least twice per year, approximately
six months apart. 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: North Carolina Wastewater/Groundwater
Laboratory Certification Policy. (See attached procedure.)
E. Finding: The laboratory does not have a system for the traceability of chemicals, reagents, and
standards to source material. A log of prepared reagents and standards is not maintained.
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, 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. (See attached
examples and guidance information.)
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#156 WestPoint Home Incorporated
iH — Standard Methods, 18th Edition, 4500 H+ B
Comment: Samples were not stirred gently and at a constant rate during measurement. The method
states, "Establish equilibrium between electrodes and sample by stirring sample to insure homogeneity;
stir gently to minimize carbon dioxide entrainment". Ref: Standard Methods, 18th Edition, 4500 H+ B. (4)
(b). At the time of the inspection, the laboratory indicated they will begin to use the stir plate when reading
the samples. No further response is necessary for this finding.
F. Finding: The calibration buffers used to calibrate the meter do not bracket the pH range of the
environmental samples encountered.
Requirement: Choose buffers to bracket the samples. Ref: Standard Methods, 18th Edition,
4500 H+ B. (1) (a).
Comment: Calibrations were being performed using the pH 4, 7 and 10 S.U. pH buffers. The 7
S.U. buffer is also used as the check buffer. Typical effluent samples were in the range of 7-8
pH units but the influent samples are sometimes in the range of 11-12 pH units.
Recommendation: It is recommended that the laboratory purchase a 12 S.U. buffer and
calibrate with the 7 and 12 S.U. buffers and check the calibration with the 10 S.U. buffer.
G. Finding: Calibration timesare not being documented.
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).
H. Finding: Data values are reported on the Discharge Monitoring Report to 0.01 S.U. not 0.1 S.U.
as required by the method.
Requirement: A variance of ± 0.1 pH unit represents the limit of accuracy under normal
conditions, especially for measurement of water and poorly buffered solutions. For this reason,
report pH values to the nearest 0.1 pH unit. Ref: Standard Methods, 18th Edition, 4500 H+ B. (6).
I, Finding: The temperature sensor verification has been performed, but it was not documented.
Requirement: All thermometers and temperature measuring devices must be checked every
twelve months against a NIST certified or NIST traceable thermometer and the process
documented. The documentation must include the serial number of the NIST certified
thermometer or NIST traceable thermometer that was used in the comparison. The meter
temperature reading must be less than 1°C from the NIST certified or NIST traceable
thermometer reading. Ref: North Carolina Wastewater/Groundwater Laboratory Certification
Policy.
J. Finding: Temperature corrections are not posted on the meters.
Requirement: Document any correction that applies (even if zero) on both the
thermometer/meter and on a separate sheet to be filed. Ref: North Carolina
Wastewater/Groundwater Laboratory Certification Policy.
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#156 WestPoint Home Incorporated
Comment: When determining the temperature correction, the temperature of the NIST certified
or NIST traceable thermometer compared against the thermometer in the meter will either be no
correction or (+) or (-). For example, if the reading on the NIST certified or NIST traceable
thermometer is 25.0 °C and the meter thermometer is 24.6 °C, the correction would be +0.4 °C.
Total Residual Chlorine — Standard Methods, 18th Edition, 4500 CI G
K. Finding: The internal curve has "not been verified annually (i.e. 12 months).
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. The curve must be
updated as set forth in the standard procedures, each time the slope changes by more than 10
percent at mid -range, each time a new stock standard is prepared, or at least every twelve
months. Ref: 15A NCAC 2H .0805 (a) (7) (I).
Recommendation: It is recommended that the lab analyze a curve in the range of 25 µg/L, 35
µg/L, 50 µg/L, 250 µg/L and 350 µg/L. There are several advantages of analyzing a curve at
these concentrations: (1) this curve verifies a standard which is less than the permitted limit of
28 µg/L and a standard at the compliance enforcement limit (50 µg/L) and (2) Low-level
Proficiency Testing standards supplied by vendors are within this concentration range.
L. Finding: The laboratory is reporting values below the verified calibration range of the
instrument on the Discharge Monitoring Report (DMR).
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. Ref: 15A NCAC 2H .0805 (a) (7) (I).
Comment: Once an annual verification curve is analyzed, the lower reporting limit will be
equivalent to the lowest calibration verification standard. For example, if the lowest standard is
25 µg/L, the lab will report any numbers lower than 25 as <25 µg/L on the DMR.
Total Residual Chlorine — Standard Methods, 18th Edition, 4500 CI G
Color — Standard Methods, 18th Edition, 2120 E
Conductivity — Standard Methods, 18th Edition, 2510 B
M. Finding: A calibration blank and calibration verification standard is not analyzed initially, after
every tenth sample and at the end of the sample group.
Requirement: The calibration blank and mid -range standard must be analyzed initially (i.e.,
prior tosample 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: North
Carolina Wastewater/Groundwater Laboratory Certification Policy based upon Standard
Methods, 20th Edition, 1020 B. (10) (c), 3020 B. (2) (b), and.4020 B. (2).
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#156 WestPoint Home Incorporated
Conductivity — Standard Methods, 18th Edition, 2510B
N. Finding: The Automatic Temperature Compensator (ATC) has not been verified.
Requirement: The internal Automatic Temperature Compensator (ATC) must be verified every
12 months and the process documented. Other certified laboratories may provide assistance in
meeting this requirement. 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. (See Attachment for Procedure) Please send a copy of the verification to
our office with your reply.
Color — Standard Methods, 18th Edition, 2120 E
O. Finding: The laboratory is analyzing samples by an unapproved method.
Requirement: Analytical methods, sample preservation, sample containers and sample holding
times shall conform to those requirements found in 40 CFR-136.3; Standard Methods for the
Examination of Water and Wastewater, 18th Edition; or Test Methods for Evaluating Solid Waste,
SW 846, Third Edition. Ref: 15A NCAC 2H .0805 (a) (1).
Comment: The laboratory has been using the Hach program 10048 on a DR4000 instrument,
which is not an approved method.
P. Finding: The correlation coefficient of the daily factory -set curve verification is not calculated to
show that it is >_ 0.995.
Requirement: When linear regression is used, use the minimum correlation coefficient specified
in the method. If the minimum correlation coefficient is not specified, then a minimum value of
0.995 (or a coefficient of determination, r2, of 0.99) is required. Ref: North Carolina
Wastewater/Groundwater Laboratory Certification Policy based upon Standard Methods, 20th
Edition 1020 B. (10) (b).
Comment: Once the laboratory implements the approved method, a calibration curve will have to
be manually constructed which meets the correlation coefficient requirements above.
Recommendation: It is recommended the laboratory analyze a 5-point laboratory -generated
curve annually and verify the calibration by analyzing a mid -range standard each analysis day. It is
recommended a curve in the range of 50, 100, 150, 200 and 250 ADMI color units be constructed.
Since this is an annual laboratory -generated curve each analyst performing the test must have an
individual calibration curve. This type of curve must be constructed at least annually (i.e., at least
every 12 months), or any time a new stock standard is prepared or quality control indicates a
problem.
Q. Finding: Samples are not filtered or centrifuged prior to analysis.
Requirement: Turbidity must be removed. Centrifugation is acceptable only if turbidity removal
equivalent to filtration is achieved. Ref: Standard Methods, 18th Edition, 2120 E. (1) (c) and (3)
(b).
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#156 WestPoint Home Incorporated
R. Finding: Samples are not prepared with two 100 mL sample portions, one at the original pH
and one at pH 7.6.
Requirement: Prepare two 100 mL sample portions (one at the original pH, one at pH 7.6) as
described in Section 2120 C. '(3) (a), or by centrifugation. Ref: Standard Methods, 18th Edition,
2120 E. (3) (b).
S. Finding: The pHs of the original and the adjusted (pH 7.6) samples are not documented.
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: Document the pH of the original sample and the adjusted pH, as well as the
number of drops of the sulfuric acid (H2SO4) and/or sodium hydroxide (NaOH) used to adjust
the pH..
T. Finding: The ADMI color values at pH 7.6 and at the original pH are not reported.
Requirement: Report ADMI color values at pH 7.6 and at the original pH. Ref: Standard
Methods, 18th Edition, 2120 E. (3) (d).
Comment: The .two portions of samples are to be treated separately for analysis. Report both
(i.e., adjusted and unadjusted) values.
U. Finding: ADMI values are not calculated properly.
Requirement: Determine sample light transmittance with the three filters to obtain the
transmittance values: T, from Filter 1, T2 from Filter 2, and T3 from Filter 3. Standardize the
instrument with each filter at 100% transmittance with distilled water. Ref: Standard Methods,
18th Edition, 2120 E. (3) (c). (A step-by-step procedure of how to analyze samples to properly
calculate results is attached.)
Comment: The attached step-by-step procedure will read the absorbances at three different
wavelengths in a single measurement. You will need to manually transfer the data to the
spreadsheet. (The spreadsheet will be emailed.)
Comment: The data being reported is actually Platinum Cobalt since results are not calculated
correctly reading the 3 transmittance values.
V. Finding: Matrix spike analyses are not performed.
Requirement: Unless the referenced method states a greater frequency, include one Matrix
Spike (MS) with each sample set (batch — 20 or fewer samples) or on a 5% basis. Prepare the
MS from a reference source different from that used for calibration unless otherwise stated in
the method. Laboratories analyzing less than 20 samples per month must analyze at least one
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. Refer to the method of choice for specific
acceptance criteria for the MS until the laboratory develops or adopts statistically valid,
laboratory -specific performance criteria for accuracy. Ref: North Carolina Wastewater/
Groundwater Laboratory Certification Policy.
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#156 WestPoint Home Incorporated
W. Finding: A second source standard is not analyzed.
Requirement: When a standard curve is manually prepared (as opposed to a factory -set
calibration), it is required to analyze one known standard in addition to calibration standards
each day samples are analyzed to document accuracy. This standard must be prepared from
materials obtained from a source independent from the one used for preparing the calibration
standards (often referred to as a second source standard or external reference standard). Ref:
Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy. (Additional
guidance information is attached.)
Comment: Acceptance criteria will need to be established for the second source standard.
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 NPDES permit NC0005762 for January and April, 2009. No transcription errors were
detected; however; the color data must be qualified.
X. Finding: Color data is not being qualified on the DMR.
Requirement: When quality control (QC) failures occur, the laboratory must attempt to
determine the source of the problem and must apply corrective action. If data qualifiers are
used to qualify samples not meeting QC requirements, the data may not be useable for the
intended purposes. A notation must be made on the Discharge Monitoring Report (DMR) form, in
the comment section, when any required sample quality control does not meet specified criteria,
and another sample cannot be obtained. Ref: North Carolina Wastewater/Groundwater.
Laboratory Certification Policy based upon Standard Methods, 20th Edition, 1020 B. (14).
Comment: See Finding O. The data must be qualified since an unapproved method is used and
since the constituent results are not ADMI color as is required by the facility permit. The reported
values are actually platinum cobalt color.
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: Tonja Springer Date: September 16, 2009
Report reviewed by: Jason Smith Date: September 28, 2009
Tracing Reagents and Standards
There are of course many ways to track reagent and standard preparation however, one of the most
effective ways is through the use of unique identification. An example chemical receipt log and reagent
preparation log are below in Tables 1 and 2.
Table-1 Chemical Receipt Lo
Date .
Rec'd
Vendor and lot #
Lab I.D
Date
Opened
Comment
analyst
6/13/03
ChemCo. Potassium Permanganate lot#
12345-b 1000mg/L
TRC stock703
7/3/03
JD
6/25/03
ChemCo. Potassium Permanganate lot#
12543-h 100mg/L
TRCLCS
Stock703
7/3/03
Second
source
JD
7/1/03
Nitric Acid ChemCo. Lot 3321456
Nitric7103
7/10/03
RS
7/5/03
BioCo. MFC Media lot #234-453
7/11/03
Exp. Date
6/5/05
CR
7/11/03
ChemCo. Sodium Chloride lot # RS-234-E34
NACL71103
7/18/03
Chloride
standard
AW
Log in new chemicals and reagents. Assign a short unique I.D. that can be referenced in the reagent
prep. log. Using a receipt date is a good idea.
Table-2 Regent Preparation Lo
Date
Standard or reagent
Standard I.D
Conc.
calculation
analyst
JD
7/703.
TRC working std
TRC7703
10 mg/L
10 mis TRC Stock703/1L lab water
7/703
Mid -range TRC7703
MRTRC7703
0.1 mg/L
1 ml TRC7730/ 100ml lab water
JD
7/7/03
Working TRC Q.C.
TRCLCS7703
10mg/L
10 ml TRCLCS stcok703/1 L lab water
JD
7/7/03
Daily LCS
TRCLCS7703
0.1 mg/L
1 ml TRCLCS7703/ 100m1 lab water
JD
7/15/03
TRC Working std
TRC71503
10 mg/L
10 mis TRC Stock/1 L lab water
JD
7/1503
Mid -range TRC71503
MRTRC71503
0.1 mg/L
1 ml TRC71503/ 100m1 lab water
JD
7/15/03
Daily LCS
TRCLCS71503
0.1 mg/L
1 ml TRCLCS7703/ 100m1 lab water
JD
The example above shows how the lab I.D of a primary standard is used to create working standard.
The advantage: 4 years and nine months later analytical data is officially questioned. Was the instrument
calibrated properly? How? How were the reagents made? Answer: The calibration standard for July 15,
2003 was made using a 1/100 dilution of a 10mg/L working standard made on July 15, 2003 using a 10m1
to 1 liter dilution of ChemCo. Lot 12345-b 1000mg/L.
How you decide to track reagent and standard preparation will need to be suited to your particular facility
and situation. For a small facility with relatively few standards and reagents a simple logbook may be
adequate. Whatever the method it is important to be able to trace standard and reagent preparation.