HomeMy WebLinkAbout#559_0512_FINALINSPECTION REPORT ROUTING SHEET
To be attached to all inspection reports in-house only.
Laborator
y C ert. #: 559
Laboratory Name: K & W Laboratories
Inspection Type:
Inspector Name(s):
Inspection Date:
Date Report Completed:
Date Forwarded to Reviewer:
Reviewed by:
Date Review Completed:
Cover Letter to use:
Unit Supervisor/Chemist III:
Date Received:
Date Forwarded to Linda:
Date Mailed:
Commercial Maintenance
Beth Swanson, Gary Francies Nick Jones
Tonia Springer, Todd Crawford Dana Satterwhite
Jason Smith
May
12,
2015 and June 8 2015
July
21,
2015
July
21,
2015
Todd Crawford
July
24,
2015
❑ Insp. Initial
❑ Insp. No Finding
❑ Corrected
® Insp. Reg.
❑ Insp. CP
❑ Insp. Reg. Delay
Gary Francies
7/29/2015
8/31 /2015
8/31 /15
U(;: Wes Bell, MRO wes.bell@ncdenr.gov
Chris Goforth
e
CDENR
North Carolina Department of Environment and Natural Resources
Pat McCrary Donald R. van der Vaart
Governor Secretary
August 31, 2015
'559
Ms. Gosia Kraska
K & W Laboratories.
1121 Hwy. 24/27 W
Midland, NC 28107
Subject: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC)
Maintenance Inspection
Dear Ms. Kraska:
Enclosed is a report for the inspection performed on May 12 and June 8, 2015 by staff of the NC
WW/GW LC program. I apologize for the delay in getting this report to you. 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 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.
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 (828)
296-4677.
Attachment
cc: Beth Swanson
Chris Goforth
Wes Bell
Sincerely,
Gary Francies, Technical Assistance/Compliance Specialist
Division of Water Resources
Water Sciences 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
Phone; 919-733-3908 t FAX; 919-733-6241
Internet; www.dMIab.org
An Equal Opportunity i Affirmative Action Employer
On -Site Inspection Report
LABORATORY NAME:
ADDRESS:
CERTIFICATE #:
DATE OF INSPECTION:
TYPE OF INSPECTION:
AUDITOR(S):
LOCAL PERSON(S) CONTACTED:
I. INTRODUCTION:
K & W Laboratories
1121 Hwy. 24/27 W
Midland, NC 28107
559
May 12, 2015 and June 8, 2015
Commercial Maintenance
Beth Swanson, Gary Francies, Jason Smith, Dana Satterwhite,
Nick Jones, Tonja Springer, and Todd Crawford
Gosia Kraska and Wioleta Montgomery
This laboratory was inspected by a representative 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.
II. GENERAL COMMENTS:
This inspection spanned two separate days. During the intervening time between the two inspection days,
the lab was very proactive in initiating corrective actions for Findings noted on the first day. The laboratory
staff is commended on their efforts. Certification staff noted that the analysts were forthcoming and
competent in discussing their analyses. There appears to be a positive organizational culture with an eye
on data integrity and ethics.
The facility has all the equipment necessary to perform the analyses. Laboratory personnel communicate
well with sample collectors and coordinate sample analyses effectively to manage workload and holding
times. Records are well organized and easy to retrieve.
All the Proficiency Testing (PT) samples for the 2015 proficiency testing calendar year have been
analyzed except Cobalt (EPA 200.7, Rev 4.4, 1994). The laboratory is reminded that initial results must
be submitted to this office directly from the vendor by September 30, 2015.
The laboratory is also 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. Note that some findings attributed to one
particular parameter may also be relevant to other parameters not specifically cited in this report.
Please remember to evaluate applicability of each finding across the scope of your accreditation.
Contracted analyses are performed by Pace Analytical Services, Inc.-Huntersville (Certification #12),
Prism Laboratories, Inc. (Certification #402), and PAR Laboratories, Inc. (Certification #20).
The requirements associated with Findings M, T, and EE have been implemented by our program since
the last inspection.
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#559 K & W Laboratories
III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:
General
Recommendation: It is recommended that the sample storage temperature requirements be changed in
accordance with 40 CFR Part 136.3 Table II in all pertinent SOPs and in practice. The current practice is
to store "at 40C". 40 CFR Part 136.3 Table II allows 560C for most inorganic and metals parameters and
<10°C for bacterial tests, without evidence of freezing.
A. Finding: Preservative is not being added to reagent blanks and/or laboratory fortified blanks,
where applicable.
Requirement: A reagent blank (method blank) consists of reagent water (see section 1080) and
all reagents (including preservatives) that normally are in contact with a sample during the entire
analytical procedure. The reagent blank is used to determine whether, and how much, reagents
and the preparative analytical steps contribute to measurement uncertainty. Ref: Standard
Methods, 1020 B-2011. (5).
Requirement: A laboratory fortified blank [laboratory control standard (LCS)] is a reagent water
sample (with associated preservatives) to which a known concentration of the analyte(s) of
interest has been added. An LFB is used to evaluate laboratory performance and analyte recovery
in a blank matrix. Ref: Standard Methods, 1020 B-2011. (6).
Comment: This Finding is applicable to any Standard Methods referenced method where
chemical preservatives are used. This Finding was specifically noted for Ammonia, TKN, COD,
and TOC, but may be pertinent to other currently certified parameters.
Documentation
B. Finding: Improper error corrections were observed.
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-Outg, 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: Specific observations included error corrections made with just a line or line and
initials. The date and initials were not always documented with error corrections.
C. Finding: The infrared (IR) detection device used to measure sample temperature at receipt did
not have the temperature correction posted on the IR device.
Requirement: The correction factor must be indicated on the thermometer and applied when
recording temperature measurements. Ref: NC WW/GW LC Policy.
Comment: The correction factor must be posted, even when there is zero correction.
Comment: Laboratory personnel were mistakenly told that, in addition to the daily check, the IR
thermometer calibration must be verified quarterly using a National Institute of Standards and
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#559 K & W Laboratories
Technology (NIST) traceable thermometer at a minimum of two different temperatures over the
full temperature range that the IR thermometer will be used. It is only required every six months,
as the laboratory is doing. Following the inspection, the Infrared Thermometer Calibration
Verification Policy was revised on June 26, 2015, and is attached to the end of this report.
D. Finding: The field benchsheet does not include instrument identification for pH, temperature, and
dissolved oxygen.
Requirement: The following must be documented in indelible ink whenever sample analysis is
performed: Instrument identification. Ref: NC WW/GW LC Approved Procedure for the Analysis
of pH, NC WW/GW LC Approved Procedure for the Analysis of Dissolved Oxygen and NC
WW/GW LC Approved Procedure for the Analysis of Temperature.
E. Finding: Units of measure are missing on laboratory daily logs. This is considered to be pertinent
information.
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: Units for the oil and grease weights on the balance log and units for temperature on
the BOD incubator log were missing.
Standard Operating Procedures
Recommendation: It is recommended that SOPs include a revision and review history with relevant
dates (e.g., effective, review and revision dates) and a brief description of the change(s) made.
Recommendation: It is recommended that the Total and Fecal Coliform SOP include a definition for the
acronym "TMTC".
Recommendation: It is recommended that the Fecal Coliform SOP add a direct reference (i.e., title and
date) to the current NC WW/GW LC Fecal Reporting Guidelines document (i.e., 10/30/2014).
Recommendation: It is recommended that the Turbidity SOP identifies primary and secondary
standards.
Recommendation: It is recommended that the Turbidity SOP defines a batch of samples.
Recommendation: It is recommended that the Turbidity SOP includes more detail on the processes of
sample cell cleaning.
Recommendation: It is recommended that the laboratory name be identified in the Total Dissolved
Residue SOP.
Recommendation: It is recommended that the Total Organic Carbon (TOC) SOP be updated from
"plastic or glass containers", to specify which types of plastic containers (e.g., polyethylene,
fluoropolymer) are acceptable according to 40 CFR Part 136.3, Table II.
Recommendation: It is recommended that the Total and Fecal Coliform SOP include references to
Standard Methods 9020 A, B, and C-2005, and 9030 through 9060-2006, which contain QC requirements
for this method. These are only found in Standard Methods, 22"d Edition.
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#559 K & W Laboratories
Recommendation: It is recommended that the Fluoride SOP address why a distillation study is not
needed for the samples received by this laboratory (i.e., they are not subject to any of the interferences at
the levels listed in Table 4500-F-:I or SM4500-F- C (1) (b)).
Recommendation: It is recommended that the Ammonia Nitrogen SOP state that distillation is not
required for the electrode method per 40 CFR Part 136, Table IB, Footnote 6 and SM 4500 NH3 D-1997
(1) (b).
Recommendation: The laboratory SOP for Chloride analysis does not address adjusting sample pH to
approximately 8 S.U. Standard Methods 4500 Cl- C-1997. (4) (a) states: For highly alkaline or acid
waters, adjust pH to about 8 before adding indicator -acidifier reagent. Although highly alkaline or acid
waters are rarely encountered, it is recommended that the SOP be updated to include this instruction.
Comment: The SOP stated that the blank must be 1/2 the lowest standard. NC WW/GW LC policy
allows _<1/2 the reporting limit.
Comment: An inconsistency and/or omission was noted between the Standard Operating Procedure
(SOP) and laboratory practice as follows: personnel were not following procedures as stated in the
Laboratory's SOP, the method reference in the SOP is not correct, the SOP is in direct conflict with
method and/or regulatory requirements, and the SOP does not describe in detail how the method is
performed (observations are listed below). The North Carolina Administrative Code, 15A NCAC 2H .0805
(a) (7) states: 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. Demonstration of
acceptable corrective actions (i.e., revised SOPs), were provided before or during the second day of
inspection with an implementation date of June 8, 2015. No further response is necessary for these
Findings.
Nitrogen, NO3 + NO2 (SM 4500 NO3" F-2000)
o The SOP did not define the maximum number of samples in a batch.
o The SOP incorrectly stated that samples held at 40C could be preserved within 24
hours of collection. Samples must be preserved within 15 minutes of collection per
40 CFR Part 136 Table II.
o The SOP stated that samples are preserved with 2mL H2SO4, but did not specify to
pH <2 S.U.
o The SOP had incorrectly referenced Ammonia Nitrogen in sections 12.5.1.11 and
14.2.
o The acceptance criterion of the correlation coefficient for calibration curves was not
defined in the SOP.
o Quality Control (QC) standard and blank acceptance criteria (e.g., % recovery,
relative percent difference, etc.) were not defined in the SOP.
o The SOP incorrectly stated that blanks were analyzed once per batch instead of
initially (i.e., prior to sample analysis), after every tenth sample, and at the end of
each sample group.
o The SOP did not state a calibration verification standard (CVS) is analyzed initially
(i.e., prior to sample analysis), after every tenth sample, and at the end of each
sample group to check for carry over and calibration drift.
o The SOP did not state that the concentration of each calibration point was back -
calculated.
o The SOP did not contain detailed instructions for matrix spike (MS) preparation.
o The SOP did not define the relative percent difference (RPD) acceptance criterion
for the MS duplicate.
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#559 K & W Laboratories
• Nitrogen, Nitrate ((SM 4600 NOX F-2000) — (SM, 4500 NO2" B-2000))
o The SOP did not contain detailed instructions for MS preparation.
o The SOP stated that a blank was analyzed initially and at the end of analysis but
did not state that a blank was analyzed after every ten samples.
• Nitrogen, Total Kjeldahl (SM 4500 Norg B-1997 (SM 4500 NH3 D-1997))
o The SOP did not include the method reference years.
o The SOP did not contain detailed instructions for MS preparation.
• Nitrogen, Ammonia (SM 4500 NH3 D-1997)
o The SOP did not include a reference year for the distillation procedure method
(e.g., SM 4500-NH3 B-1997).
o The formula for matrix spike percent recovery calculation and detailed preparation
instructions were not included in the SOP.
• Phosphorous, Total and Phosphate, Ortho (SM 4500 P F-1999)
o The SOP combined total phosphorous and orthophosphate, but there were no
references to the different treatment of the two types of samples.
o The SOP did not define quality control acceptance criteria (e.g., % recovery,
relative percent difference, etc.).
o The SOP did not describe the source (i.e., primary vs. secondary to calibration
standards) of quality control standards.
o The SOP did not state the CVS and blank frequency.
o The SOP did not contain detailed instructions for MS preparation.
o The concentrations of calibration standards listed in the SOP did not match those
used in daily practice.
Bacteria — Coliform, Fecal (SM 9222 D-1997)
o The SOP did not describe the sample transportation and storage temperature
requirement of <10°C.
o The SOP did not state that the funnel is rinsed with three 20 mL portions of sterile
water after filtration of the blank.
o The SOP incorrectly stated that the pH of the phosphate buffer must be 7.2 + 0.5.
The pH of the phosphate buffer must be 7.2 ± 0.5.
o The SOP did not state that the phosphate buffer must be sterilized by autoclave
and stored under refrigerated conditions.
o The SOP did not describe corrective actions for duplicate precision failures.
o The SOP did not state what would be done if a client was unable to re -collect a
sample when collection or preservation issues occurred.
Metals (EPA 200.7, Rev. 4.4 (1994))
o Analysis of the calibration blank and reagent blank, including their frequency and
acceptance criteria, were not described in the SOP.
o The SOP did not include spectral interference check (SIC) solution requirements.
o The SOP did not state that 24 hours must pass between the time of preservation
and time of analysis for applicable metals (excludes boron, CrVI and mercury).
o The SOP did not state that Boron is an exception to the 24 hour interval between
preservation and analysis. Boron must be preserved at the time of collection.
o The SOP did not contain detailed instructions for MS preparation.
• Oil and Grease (EPA 1664 Rev. B)
o The SOP did not include the verification of sample preservation (i.e., pH <2) and
directions for the process.
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#559 K & W Laboratories
o The SOP did not include the matrix spike percent recovery calculation.
o The SOP did not include balance calibration requirements and acceptance criteria.
BOD (SM 6210 B-2001)
o The SOP did not describe corrective actions for failure of the drift check.
o The pH correction section of the SOP stated that if the sample pH is not 6.0 to 8.0
S.U.. "adjust to 7.1". If the sample pH is not 6.0 to 8.0 S.U., samples must be
adjusted to the range of 7.0 to 7.2 S.U.
o The SOP did not state that the volume of sample must not be changed by more
than 0.5% through pH adjustment.
o The SOP incorrectly stated that the sodium sulfite was prepared weekly versus
daily.
o The SOP did not state that seed was prepared by decanting the supernatant and
stirring while drawing seed aliquots.
o The SOP did not state that the DO of the initial blank must be between 7.5 and 9.0
mg/L.
o The SOP did not state that the sample initial DO must be between 7.0 and 9.0
mg/L.
o The SOP did not state that sample volumes less than 20 mL must be measured
using a wide -tipped pipette.
o The SOP did not state that the water seals must be maintained during incubation.
Recommendation: SOP revisions implementing the following recommendations were provided before
or during the second day of inspection with an implementation date of June 8, 2015. Thank you for
implementing these recommendations.
• Nitrogen, NO3 + NO2 (SM 4500 NOX F-2000)
• Nitrogen, Nitrate ((SM 4500 NOX F-2000) — (SM, 4500 NOZ B-2000))
• Nitrogen, Ammonia (SM 4500 NH3 D-1997)
o The SOP stated that the blank must be 1/2 the lowest standard. NC WW/GW LC
policy allows 51/2 the reporting limit (which must be equal to the concentration of
the lowest calibration standard). The SOPs were revised to the :51/2 the reporting
limit blank acceptance criterion.
• Nitrogen, Ammonia (SM 4500 NH3 D-1997)
o Part D 25 and 26 in the SOP were repetitive and one section was eliminated.
o Recommended language (i.e., "with pH meter") was added after "adjust to pH 9.5"
in part C. 1. of the SOP.
• BOD (SM 5210 B-2001)
o The SOP had a tighter acceptance criterion than the required ±0.2 mg/L for the
drift check. The SOP was revised to reflect the ±0.2 mg/L drift check acceptance
criterion.
F. Finding: An inconsistency and/or omission was noted between the Standard Operating
Procedure (SOP) and laboratory practice as follows (observations are listed for each):
• The SOP does not describe in detail how the method is performed.
o COD (SM 5220 D-1997) —The SOP does not contain detailed instructions for MS
preparation.
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*559 K & W Laboratories
o COD (SM 5220 D-1997) and Turbidity (SM 2130 B-2001) — The SOP does not
include quality control acceptance criteria.
o COD (SM 5220 D-1997) and Turbidity (SM 2130 B-2001) — The SOP does not
include corrective actions for quality control failures.
o Residue, Dissolved (SM 2540 C-1997) — The SOP does not list the routine
reporting limit.
o Residue, Dissolved (SM 2540 C-1997) — Directions for the annual drying study
are not clear. The directions for the annual drying study lacks sufficient detail such
that an experienced analyst unfamiliar with the method can obtain acceptable
results by following it. In addition, NC WW/GW LC policy requires: 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.
o Bacteria — Coliform Total (SM 9222 B-1997) — The SOP did not state that the
funnel is rinsed with three 20 mL portions of sterile buffered dilution water after
filtration of the blank.
o Bacteria — Coliform Total (SM 9222 B-1997) — The SOP lacks sufficient detail
such that an experienced analyst unfamiliar with the method can obtain acceptable
results by following it.
o Bacteria — Coliform Fecal (SM 9222 D-1997) — The SOP does not state that the
plates are completely submerged in the waterbath while being incubated.
o Chloride (SM 4500 Cl' C-1997) — The SOP does not include acceptance criteria
for QC (i.e., blanks, duplicates, LCS and titrant standardization).
o Chloride (SM 4500 Cl" C-1997) — The SOP lists the wrong value for the
conversion factor in the results calculation (i.e., it lists 3545 instead of 35450).
Reported sample results were calculated correctly.
o Fluoride (SM 4500 F' C-1997) — The SOP does not include the formula for
percent recovery calculation.
o Fluoride (SM 4500 F" C-1997) — The SOP does not include detailed preparation
instructions and true values for the Instrument Calibration Verification (ICV)
standard, Continuing Calibration Verification (CCV) standard and Laboratory
Fortified Matrix (LFM).
o Organic Carbon Total (TOC) (SM 5310 B-2000) — The SOP does not state the
volume injected during analysis.
• Personnel were not following procedures as stated in the laboratory's SOP.
o Residue, Suspended (SM 2540 D-1997) — The SOP states the acceptance
criterion for duplicates is within ±5% of the average, but the benchsheets show
calculation of RPD. Calculation of RPD is acceptable; however, the SOP must
accurately reflect laboratory practice.
o Bacteria — Coliform Total (SM 9222 B-1997) and Bacteria — Coliform Fecal
(SM 9222 D-1997) — The SOP states that the microscope magnification is between
15 and 20x power but it is being used on 10X power which meets the method
requirement of 10 to 15 magnifications.
• The SOP is in direct conflict with the method and/or a regulatory requirement.
o Residue, Dissolved (SM 2540 C-1997) — The SOP lists the minimum weight gain
requirement as selecting a sample volume to yield between 10 to 200 mg. The
method specifies 2.5 to 200 mg.
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#559 K & W Laboratories
o Organic Carbon Total (TOC) (SM 5310 B-2000) — The SOP states that the
requirement for thermal preservation is ± 6°C instead of <_ 6°C per 40 CFR Part
136 Table II.
o Bacteria — Coliform Total (SM 9222 B-1997) — The SOP references an older
method, which is no longer approved.
• The SOP does not contain the method approval year.
o Residue, Dissolved (SM 2540 C-1997)
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). Please submit updated SOPs with the items listed above addressed by December 1, 2015.
Metals — EPA 200.7, Rev. 4.4 (1994)
Comment: The laboratory was not analyzing an Instrument Performance Check (IPC) solution
immediately following calibration. EPA Method 200.7, Rev. 4.4 (1994), Section 9.3.4 states: For all
determinations the laboratory must analyze the IPC solution (Section 7.11) and a calibration blank
immediately following daily calibration.... Analysis of the IPC solution immediately following calibration
must verify that the instrument is within ±5% of calibration with a relative standard deviation <3% from
replicate integrations z4. Demonstration of acceptable corrective action (i.e., a revised SOP documenting
the analysis of an IPC with an implementation date of June 8, 2015) was provided during the second day
of the inspection. No further response is necessary for this finding.
Comment: The laboratory was using ±10% as the acceptance criterion for their ICV, which corresponds
to the Quality Control Sample (QCS) in the method. EPA Method 200.7, Rev. 4.4 (1994), Section 9.2.3
states: To verify the calibration standards the determined mean concentrations from three analyses of the
QCS must be within ±5% of the stated values. Demonstration of acceptable corrective action (i.e., a
revised SOP documenting the use of ±5% as acceptance criterion for the mean concentration of triplicate
measurements of the QCS, with an implementation date of June 8, 2015) was provided during the
second day of the inspection. No further response is necessary for this finding.
Comment: The temperature of samples inside the digestion vessel was not being documented. This is
considered pertinent information. EPA Method 200.7 Rev. 4.4 (1994), Section 11.2.3 states: Note: For
proper heating adjust the temperature control of the hot plate such that an uncovered Griffin beaker
containing 50 mL of water placed in the center of the hot plate can be maintained at a temperature
approximately but no higher than 85°C. (Once the beaker is covered with a watch glass the
temperature of the water will rise to approximately 950C.) The North Carolina Administrative Code, 15
NCAC 2H .0805 (a) (7) (A) states: 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. Demonstration of acceptable
corrective action (i.e., a revised SOP stating the water sample digestion temperature must be
documented and a revised benchsheet dated 5/28/2015 with the water sample digestion temperature
documented at 95.6°C) was provided during the second day of the inspection and by email on August 20,
2015. No further response is necessary for this finding.
Nitrogen, NO3 + NO2 — Standard Methods, 4500-NO3' F-2000
Comment: The laboratory was not analyzing a Matrix Spike Duplicate (MSD) at any time and did not
analyze a MS on a consistent basis. These are called a Laboratory Fortified Matrix and Laboratory
Fortified Matrix Duplicate (LFM/LFMD) in Standard Methods. Standard Methods, 4020 B-2009, Rev.
2011, Table 4020:1 and (2) (g) states: When appropriate for the analyte (Table 4020:1), include at least
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#559 K & W Laboratories
one LFM/LFMD daily or with each batch of 20 or fewer samples. This is a new method requirement since
the last inspection. The laboratory was analyzing a duplicate sample and was told that the analysis of the
LFMD is acceptable to satisfy the sample duplicate requirement in North Carolina Administrative Code,
15A NCAC 2H .0805 (a) (7) (C). Demonstration of acceptable corrective action (i.e., a revised SOP
describing the required frequency of the LFM/LFMD, with an implementation date of June 8, 2015) was
provided during the second day of the inspection. No further response is necessary for this finding.
Nitrogen, Nitrate — (Standard Methods, 4500-NO3" F-2000) — (Standard Methods, 4500 NOZ- B-2000)
Comment: The benchsheet did not include the reference methods approval years. This is considered
pertinent information. The North Carolina Administrative Code, 15 NCAC 2H .0805 (a) (7) (A) states: 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. Demonstration of acceptable corrective action (i.e., an updated
benchsheet with the reference methods approval years was generated and put into place June 8, 2015)
was provided during the second day of the inspection. No further response is necessary for this
finding.
Comment: Standard Methods, 4500-NO2- B-2000, is used to determine nitrite for the calculation of
nitrate. For this analysis, an LFM, also known as the MS, is not analyzed each analysis day. This was
specifically noted on 5/14/2015 and 5/22/2015. Standard Methods, 4020 B-2009, Rev. 2011 Table 4020:1
and (2) (g) state: When appropriate for the analyte (Table 4020:1), include at least one LFM/LFMD daily
or with each batch of 20 or fewer samples. Demonstration of acceptable corrective action (i.e., a revised
SOP describing the required frequency of the LFM, with an implementation date of the SOP and practice
June 8, 2015) was provided during the second day of the inspection. No further response is necessary
for this finding.
Nitrogen, Total Kieldahl — Standard Methods, 4500 N org B-1997 (Standard Methods 4600 NH3 D-
1997)
Comment: The laboratory was not analyzing a LFMD. Standard Methods, 4020 B-2009, Rev. 2011,
Table 4020:1 and (2) (g) states: When appropriate for the analyte (Table 4020:1), include at least one
LFM/LFMD daily or with each batch of 20 or fewer samples. The laboratory was analyzing a duplicate
sample and was told that the analysis of the LFMD is acceptable to satisfy the sample duplicate
requirement in North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (C). Demonstration of
acceptable corrective action (i.e., a revised SOP describing the required frequency of the LFMD, with an
implementation date of June 8, 2015) was provided during the second day of the inspection. No further
response is necessary for this finding.
Comment: The benchsheet did not reference the preparation procedure method and the analytical
method reference was missing the approval year. This is considered pertinent information. The North
Carolina Administrative Code, 15 NCAC 2H .0805 (a) (7) (A) states: 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. Demonstration of acceptable corrective action (i.e., an updated benchsheet that included the
analytical method approval year and preparation procedure method was generated and put into place
June 8, 2015) was provided during the second day of the inspection. No further response is necessary
for this finding.
Bacteria — Coliform Fecal — Standard Methods, 9222 D-1997 (MF)
Recommendation: When performing comparisons of old and new lots of consumables, sample results
are not consistently within the acceptable range of 20-60 colonies. In order to more consistently meet this
criterion, it is recommended that the sample be analyzed at multiple dilutions in order to establish the best
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volume to use, and then analyzed for comparison testing at that volume the next day. See attached
Testing of Consumable Materials for Fecal Coliform MF Method document for further guidance.
j Comment: The SOP notebook contained a copy of an older version of the reference method. This must
be replaced with the currently approved reference method (i.e., SM 9222 D-1997), which can be found in
the 201h and 21 st Editions of Standard Methods.
Comment: The laboratory was using a total immersion thermometer in the fecal water bath improperly.
The Environmental Protection Agency's (EPA) guidance website titled "Selecting Alternatives to Mercury -
Filled Thermometers" (btpL//www.epa.gov/mercury/alternafiveshtm) states: Thermometers with no
indicated depth are the total immersion type. When a partial -immersion thermometer is used, the bottom
of the thermometer up to the immersion line should be exposed to the temperature being measured, with
the remainder of the thermometer exposed to ambient conditions. When a total immersion thermometer
is used, the bulb and the entire portion of the stem containing liquid, except for the last 1 cm, are exposed
to the temperature being measured. If the thermometer is not used in this manner, the thermometer
immersion is incorrect. Demonstration of acceptable corrective action (i.e., the total immersion
thermometer was replaced with a partial immersion thermometer immersed to the specified immersion
line) was observed by certification staff on June 8, 2015. No further response is necessary for this
finding.
Comment: Sample dilutions were not consistently set to yield counts between 20 and 60 fecal coliform
colonies per membrane. Many samples were set up with dilutions of 10 mL and 50 mL, with counts of 0
and/or <20. The SOP had prescribed the following sample dilution scheme: Effluent - 10 mL and 50 mL;
Upstream/Downstream - 1 mL, 10 mL, and 50 mL; Groundwater - 10 mL and 100 mL. In addition, section
CA.d. of the SOP instructs analysts to pour 100 mL of sample and section C.S. instructs analysts to set
additional dilutions as appropriate. Standard Methods, 9222 D-1997. (2) (a). states: Use sample volumes
that will yield counts between 20 and 60 fecal coliform colonies per membrane. Demonstration of
acceptable corrective action (i.e., several weeks of completed benchsheets with 100 mL dilutions,
representing a whole volume sample with counts of 0 and/or <20 fecal coliform colonies per membrane)
was observed by certification staff on June 8, 2015. No further response is necessary for this finding.
Comment: The full method reference including approved year, was not listed on the benchsheets. This is
considered pertinent information. The North Carolina Administrative Code, 15 NCAC 2H .0805 (a) (7) (A)
states: 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. Demonstration of acceptable corrective action (i.e., an
updated benchsheet with the complete method reference including approved year) was observed by
certification staff on June 8, 2015 with implementation effective upon next analysis. No further response
is necessary for this finding.
Comment: The laboratory was not documenting time of sample filtration to demonstrate that the time
from sample filtration until incubation was 5 30 minutes, as required by the method. The North Carolina
Administrative Code, 15 NCAC 2H .0805 (a) (7) (A) states: 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.
Demonstration of acceptable corrective action (i.e., completed benchsheets starting May 19, 2015,
showing handwritten filtration start times and an updated benchsheet with start and end filtration times)
was observed by certification staff on June 8, 2015 with implementation of the benchsheet effective upon
next analysis. No further response is necessary for this finding.
Comment: The incubator log did not contain units of measurement for temperature. This is considered
pertinent information. The North Carolina Administrative Code, 15 NCAC 2H .0805 (a) (7) (A) states: 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. Demonstration of acceptable corrective action (i.e., "°C" was added
by hand to the temperature column on the incubator log currently in use, and an updated log sheet with
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"°C" was developed) was observed by certification staff on June 8, 2015 with implementation of the log
sheet upon completion of the current log sheet. No further response is necessary for this finding.
Comment: The analyst was not conducting a monthly self -recount of one plate or a side -by -side count of
one plate with another analyst. Standard Methods, 9020 B-2005. (9) (a) states: For routine performance
evaluation, repeat counts on one or more positive samples at least monthly, record results, and compare
the counts with those of other analysts testing the same samples. Replicate counts for the same analyst
should agree within 5% (within analyst repeatability of counting) and those between analysts should
agree within 10% (between analysts reproducibility of counting). If they do not agree, initiate investigation
and any necessary corrective action. Demonstration of acceptable corrective action (i.e., the procedure
was added to section D.5.k. of the SOP and three benchsheets showing the monthly comparison counts)
were observed on June 8, 2015 and submitted by email on August 20, 2015. No further response is
necessary for this finding.
Comment: The laboratory is not starting a new filtration series (i.e., using newly sterilized filtration units
and analyzing a blank) when 30 minutes or more elapse between sample filtrations. The benchsheet from
April 24, 2015 showed approximately 4 % hours between filtration of samples that were treated as one
filtration series. Standard Methods, 9222 D-1997. (2) (b) states: Follow the same procedure and
precautions as prescribed under 9222B.4c.Use sterile filtration units at the beginning of each filtration
series as a minimum precaution to avoid accidental contamination. A filtration series is considered to be
interrupted when an interval of 30 minutes or longer elapses between sample filtrations. After such
interruption, treat any further sample filtration as a new filtration series and sterilize all membrane filter
holders in use. Demonstration of acceptable corrective action (i.e., a revised SOP stating that a new
filtration series would be initiated when greater than 30 minutes elapsed between sample filtration, with an
implementation date of June 8, 2015) was provided during the second day of the inspection. No further
response is necessary for this finding.
G. Finding: The pH of the phosphate buffer is not being documented. This is considered pertinent
information.
Requirement: Stock phosphate buffer solution - Dissolve 34.0 g potassium dihydrogen
phosphate (KH2PO4) in 500 mL reagent grade water, adjust to pH 7.2 ± 0.5 with 1 N NaOH and
dilute to 1 L with reagent grade water. Ref: Standard Methods, 9050 C-2006. (1) (a) (1).
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).
H. Finding: The laboratory is analyzing compliance samples without having determined that the
consumables are acceptable.
Requirement: Once you determine that the new material is acceptable to use; you may begin to
do so. Document the date the new lot # is put into use. Ref: NC WW/GW LC Policy.
Comment: Since the test is performed on a compliance sample, if it is determined that the
consumables are not acceptable, the compliance sample results would not be valid.
COD — Standard Methods, 5220 D-1997
Recommendation: It is recommended that the benchsheet be revised to contain a space for both the
standard curve date and the date of analysis to provide unequivocal traceability to the curve used with
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each set of data. Currently, the space for the standard curve date is where the analyst records the date of
analysis.
I. Finding: The manufacturer -prepared digestion test tube lot number is neither documented nor
traceable to the specific analytical batches where it was used.
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:
NC WW/GW LC Policy.
J. Finding: The times that samples are placed into and removed from the digester are not
documented. This is considered pertinent information.
Requirement: Prepare, digest, and cool samples, blank, and one or more standards as directed
in 5220C.4. Place tubes or ampules in block digester preheated to 150 °C and reflux for 2 h
behind a protective shield. Ref: Standard Methods, 5220 D-1997. (4) (a).
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).
Residue. Dissolved — Standard Methods, 2540 C-1997
Comment: The LCS is being analyzed daily. The North Carolina Administrative Code, 15A NCAC 2H
.0805 (a) (7) (B) states the requirement is quarterly.
Recommendation: It is recommended that the LCS quality control acceptance criterion be listed on the
benchsheet.
K. Finding: A drying study was not performed within the previous 12 months.
Requirement: 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. Ref: NC WW/GW LC Policy.
Comment: NC WW/GW LC interprets the meaning of the term "annual" as every 12 months. The
last drying study was performed on 2/19/14.
L. Finding: The benchsheet does not contain units of measure (i.e., mg/L) for the quality control
standard true value.
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Requirement: All laboratories must use printed laboratory bench worksheets that include a space
to enter the signature or initials of the analyst, date of analyses, sample identification, volume of
sample analyzed, value from the measurement system, factor and final value to be reported and
each item must be recorded each time samples are analyzed. Ref: 15A NCAC 2H .0805 (a) (7)
(H).
Organic Carbon, Total — Standard Methods, 5310 B-2000
Recommendation: It is recommended that "SPL#" on the instrument printout be added to corresponding
samples on the benchsheet to provide unequivocal traceability.
M. Finding: The laboratory is not analyzing a LFM and LFMD at the proper frequency.
Requirement: When appropriate for the analyte (Table 5020:1), include at least one LFM/LFMD
daily or with each batch of 20 or fewer samples. Ref: Standard Methods, 5020 B-2010. Table
5020:1 and (2) (g).
Comment: The laboratory was analyzing LFMs on an inconsistent basis. LFMs were not always
included daily and the LFMD was not analyzed at all. Analysis of the LFM/LFMD at the required
frequency will also satisfy the duplicate quality control requirement.
N. Finding: The spiking procedure is not being documented.
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. Ref: NC WW/GW LC Policy.
O. Finding: Client reports do not always include qualification for QC failures.
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. Ref: NC WW/GW LC Policy.
Comment: The client report for sample 1050307 did not contain qualifiers for failed acceptance
criterion on the LFM and sample duplicate.
Comment: Data qualification is added after the client report is printed and a copy of the report
with data qualification is not kept on file. In order to meet this requirement a copy of the final client
report including data qualifications must be kept on file at the laboratory.
P. Finding: The software output does not show whether dilution factors are entered, and therefore
applied, for a sample.
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Requirement: All laboratories must use printed laboratory bench worksheets that include a
space to enter the signature or initials of the analyst, date of analyses, sample identification,
volume of sample analyzed, value from the measurement system, factor and final value to be
reported and each item must be recorded each time samples are analyzed. Ref: 15A NCAC 2H
.0805 (a) (7) (H).
Comment: The benchsheet contained a space for the dilution factor but the final result did not
always reflect that the dilution factor was applied. The analyst stated that the instrument allowed
the input of a dilution factor but the instrument printout did not reflect whether or not a dilution
factor was entered and therefore applied to the result. The instrument does not have the ability to
recall that information. Of the data reviewed (see Section IV: Paper Trail Investigation), only one
sample is in question.
Comment: Since it is impossible to recall whether a dilution factor was entered into the system, all
dilution factors must be documented and applied on the benchsheet instead of through
instrumentation.
Residue, Suspended — Standard Methods, 2540 D-1997
Recommendation: It is recommended that the drying times be added to the drying study sheet so that all
pertinent information is in one place and the original benchsheet does not have to be retrieved to verify
the drying times.
Recommendation: It is recommended that the acceptance range of the quarterly check standards be
added to the quarterly check log.
Recommendation: The current drying time verified by a study is overnight. In case samples are received
which require a shorter turn -around time; in order to avoid having to weigh those samples to constant
weight, it is recommended that the study time be decreased.
Recommendation: The drying study needs to be representative of samples received. It is recommended
that the laboratory include a large enough sample set to insure all sample types encountered are
represented.
Comment: The laboratory analyzes a reagent water blank, which is not required.
Bacteria — Coliform, Total — Standard Methods, 9222 B-1997 (MF)
Q. Finding: Adequate dilutions to produce the method required colony counts are not consistently
made.
Requirement: An ideal sample volume will yield 20 to 80 coliform colonies and not more than 200
colonies of all types on a membrane -filter surface.... Analyze other waters [other than drinking
water] by filtering three different volumes (diluted or undiluted), depending on the expected
bacterial density. Ref: Standard Methods, 9222 B-1997. (5) (a).
Recommendation: The data showed that dilutions of 5 mL, 10 mL or 50 mL were generally set,
which most often resulted in counts of TMTC [i.e., Too Many to Count]. It is recommended
samples be analyzed at a higher dilution. See Standard Methods, 9222 B-1997, Table 9222:1 for
suggested sample volumes and Standard Methods, 9215 B-2000 (2) (a), for guidance on
preparing serial dilutions.
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R. Finding: The benchsheet does not include the correct method reference. This is considered
pertinent information.
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).
Recommendation: The laboratory does not have a separate total coliform benchsheet. The
analyst marks out "fecal' and writes "total', but does not change the method reference. It is
recommended that a separate benchsheet solely for the use of total coliform be created and used.
Chloride — Standard Methods 4500 CI" C-1997
S. Finding: The laboratory is not using the method required normality of sodium chloride and
mercuric nitrate.
Requirement: Standard sodium chloride, 0.0141 M (0.0141 N). Ref: Standard Methods 4500 CI-
C-1997. (3) (a).
Requirement: Reagents for chloride concentrations below 100 mg/L: Standard mercuric nitrate
titrant, 0.00705 M (0,0141 N). Ref: Standard Methods 4500 Cl- C-1997. (3) (d) (2).
Requirement: Reagents for chloride concentrations greater than 100 mg/L: Strong standard
mercuric nitrate titrant, 0.0705 M (0.141 N). Ref: Standard Methods 4500 Cl- C-1997. (3) (e) (2).
Comment: The laboratory is using 0.025 N for sodium chloride and mercuric nitrate.
Comment: The laboratory is reminded that the QC (i.e., blank and LCS) need to be treated to the
same procedure as the samples require. If an analysis includes samples both greater and less
than 100 mg/L Cl-, QC would need to be analyzed by both procedures.
T. Finding: The laboratory is not analyzing a Laboratory Fortified Matrix (LFM) and/or Laboratory
Fortified Matrix Duplicate (LFMD) at the required frequency.
Requirement: Include at least one LFM/LFMD daily or with each batch of 20 or fewer samples.
Ref: SM 4020 B-2009, Rev. 2011, Table 4020:1 and (2) (g).
Comment: LFM and LFMD are also known a Matrix Spike (MS) and Matrix Spike Duplicate
(MSD).
Comment: Analysis of the LFMD (or MSD) is acceptable to satisfy the sample duplicate
requirement listed in the North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (C).
U. Finding: The calculated percent recovery of the LCS and RPD of duplicates are not documented
on a consistent basis.
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 21-1.0805 (a) (7).
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Comment: The percent recovery of LCS and RPD of duplicates are not always documented on
the chloride benchsheet. The laboratory is reminded to include documentation of the recovery and
RPD of LFM/LFMD when those begin to be analyzed per Finding T
V. Finding: The calculated normality of the mercuric nitrate titrant is not being used in the result
calculation.
Requirement: Calculation:
mg C17L = (A-B) x N x 35450
mL sample
where:
A = mL titration for sample,
B = mL titration for blank, and
N = normality of Hg(NO3)2•
Ref: Standard Methods, 4500 Cl- C-1997. (5).
Comment: The laboratory is using 0.025 for N in all calculations, so the result is not being
adjusted for the individual sample batch calculated normality of Hg(NO3)2•
Oil and Grease — EPA 1664 Rev. B
Comment: The laboratory was determining the volume of the sample incorrectly. Section 11.1.4 of EPA
1664, Rev. B states: Either mark the sample bottle at the water meniscus or weigh the bottle for later
determination of sample volume. Weighing will be more accurate. Demonstration of acceptable
corrective action (i.e., an updated SOP stating that the level of sample will be marked on the sample
bottle) was observed by certification staff on June 8, 2015 with implementation effective upon next
analysis. No further response is necessary for this finding.
Comment: When the total sample volume was less than 900 mL, the laboratory was not using the actual
volume of the sample to calculate the elevated reporting limit. Section 12.1 of EPA Method 1664, Rev. B
states: Calculate the concentration of HEM ('oil and grease") in the sample per the following equation:
HEM (mg/L) = Wh (mg)/ VS (L); where: Wh = Weight of extractable material from Section 11.4.4.1 (mg)
and VS = Sample volume from Section 11.4.5 (Q. Cited previously on February 16, 2012.
Demonstration of acceptable corrective action (i.e., an updated SOP stating that different volumes of
sample will be taken into account in determining the concentration of the reporting limit) was observed by
certification staff on June 8, 2015 with implementation effective upon next analysis. Please send copies
of completed benchsheets showing properly calculated sample results for five sets of sample
analyses with the response to this report.
Comment: The spike volume was greater than 10% of the total volume and the final result was not
corrected for dilution by the spike volume through calculation. The NC WW/GW LC Matrix Spiking Policy
states: The volume of spike solution used in MS preparation must in all cases be <_ 10% of the total MS
volume. It is preferable that the spike solution constitutes _< 1 % of the total MS volume so that the MS
can be considered a whole volume sample with no adjustment (i.e., volume correction) by calculation
necessary. If the spike solution volume constitutes >1% of the total sample volume, the sample
concentration or spike concentration must be adjusted by calculation. Demonstration of acceptable
corrective action (i.e., an updated SOP stating the total volume of sample used would be increased such
that the volume of spike solution is 5 1 % of the total MS volume) was observed by certification staff on
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June 8, 2015 with implementation effective upon next analysis. No further response is necessary for
this finding.
Comment: The benchsheet did not include units of measure in columns 3, 8, 10 and 11. The North
Carolina Administrative Code, 15 NCAC 2H .0805 (a) (7) (H) states: All laboratories must use printed
laboratory bench worksheets that include a space to enter the signature or initials of the analyst, date of
analyses, sample identification, volume of sample analyzed, value from the measurement system, factor
and final value to be reported and each item must be recorded each time samples are analyzed.
Demonstration of acceptable corrective action (i.e., an updated benchsheet including all the proper units
of measure) was observed by certification staff on June 8, 2015 with implementation effective upon next
analysis. No further response is necessary for this finding.
W. Finding: Lot numbers for all standards, reagents and consumables was neither documented nor
traceable.
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:
NC WW/GW LC Policy.
Comment: The lot number for hexane was added to the benchsheet before the second day of
inspection, June 8, 2015, but it still lacked information for the OPR, spike solution and solid phase
extraction disks.
Conductivity — Standard Methods, 2510 B-1997
Residue. Settleable — Standard Methods, 2540 F-1997
Comment: Duplicate analyses are not required for field parameters.
Conductivity — Standard Methods, 2510 B-1997
Comment: The conductivity benchsheet did not include units of measure. The North Carolina
Administrative Code, 15 NCAC 2H .0805 (a) (7) (H) states: All laboratories must use printed laboratory
bench worksheets that include a space to enter the signature or initials of the analyst, date of analyses,
sample identification, volume of sample analyzed, value from the measurement system, factor and final
value to be reported and each item must be recorded each time samples are analyzed. Ref: 15A NCAC
2H .0805 (a) (7) (H). Demonstration of acceptable corrective action (i.e., an updated benchsheet including
all the proper units of measure) was observed by certification staff on June 8, 2015 with implementation
effective upon next analysis No further response is necessary for this finding.
Comment: The laboratory had not been conducting the annual automatic temperature compensator
(ATC) check. The NC WW/GW LC Approved Procedure for the Analysis of Specific Conductance
document states: The Automatic Temperature Compensator (ATC) must be verified annually (i.e., 12
months) at two temperatures by analyzing a standard or sample at 25°C (the temperature that
conductivity values are compensated to) and a temperature(s) that brackets the temperature ranges of
the environmental samples routinely analyzed. This may require the analysis of a third temperature
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reading that is >25°C.The manner in which the ATC is verified may depend upon the meter's capabilities
and the manufacturer's instructions. Demonstration of acceptable corrective action (i.e., an acceptable
ATC check was performed and the results documented) was witnessed during the second day of
inspection, June 8, 2015. The laboratory is reminded to include this requirement in the SOP to
prevent recurrence of this Finding.
X. Finding: The date standard bottles are opened is missing from standard traceability
documentation.
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). 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.
Comment: The date opened was only written on the standard bottles. The traceability link is lost
once the bottles are discarded since there is no standard lot number on the benchsheet.
PH — Standard Methods, 4500 H+ B-2000
Y. Finding: Values were reported that exceed the method specified accuracy of 0.1 units.
Requirement: By careful use of a laboratory pH meter with good electrodes, a precision of ±0.02
unit and an accuracy of ±0.05 unit can be achieved. However, ± 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,
4500 H+ B-2000. (6).
Comment: As an example, the result from Pilgrim's Pride sample on March 11, 2015 was
reported as 7.46 S.U.
Z. Finding: Traceability information for the pH buffers is not documented.
Requirement: The following must be documented in indelible ink whenever sample analysis is
performed: Traceability for chemicals, reagents, standards and consumables. Ref: NC WW/GW
LC Approved Procedure for the Analysis of pH.
Chlorine, Total Residual — Standard Methods, 4500 Cl G-2000
AA. Finding: The current gel standard assigned value is recorded incorrectly on the benchsheets.
Requirement: The following must be documented in indelible ink whenever sample analysis is
performed: True value of the check standard. Ref: NC WW/GW LC Approved Procedure for the
Analysis of Total Residual Chlorine.
Comment: The currently assigned true value is 210 tag/L, but it is recorded on the benchsheets
as 196 lag/L. There were no instances noted where the observed value of the check standard was
not within ± 10% of the correct true value.
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BB. Finding: The meter calibration time is not recorded on the benchsheet.
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 Total Residual Chlorine.
CC. Finding: The laboratory is not analyzing a reagent blank with the annual curve verification.
Requirement: Each day that prepared standards are analyzed a reagent blank must be
analyzed. A reagent blank is made from the same laboratory water source used to make quality
control and/or calibration standards with DPD. The concentration of reagent blanks must not
exceed 50% of the reporting limit (i.e., the lowest calibration or calibration verification standard
concentration), unless otherwise specified by the reference method, or corrective action must be
taken. Ref: NC WW/GW LC Approved Procedure for the Analysis of Total Residual Chlorine.
Comment: The laboratory was not analyzing the reagent blank. They were zeroing the instrument
with it before the curve verification. The instrument must be zeroed using either the sealed blank
that is provided in the Gel standard kit or laboratory water without DPD added.
Phosphorous, Total — Standard Methods, 4500 P F-1999
Phosphate, Ortho — Standard Methods, 4500 P F-1999
Comment: The MS contained greater than 1 % of spiking solution and the result was not corrected for
the sample volume adjustment through calculation. NC WW/GW LC Policy states: If the spike solution
volume constitutes >1% of the total sample volume, the sample concentration or spike concentration
must be adjusted by calculation. Demonstration of acceptable corrective action (i.e., a revised SOP
stating the spike volume would be 1 % or less of the total volume, with an implementation date of June 8,
2015) was provided during the second day of the inspection. No further response is necessary for this
finding.
DD. Finding: The start and end times of digestion are not being documented. This is considered
pertinent information.
Requirement: Alternately, heat for 30 min in an autoclave or pressure cooker at 98 to 137 kPa.
Ref: Standard Methods, 4500 P B-1999. (5) (c).
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).
Fluoride — Standard Methods, 4500 F- C-1997
EE. Finding: The laboratory is not analyzing a Laboratory Fortified Matrix (LFM) and Laboratory
Fortified Matrix Duplicate (LFMD) at the required frequency.
Requirement: Include at least one LFM/LFMD daily or with each batch of 20 or fewer samples.
Ref: SM 4020 B-2009, Rev. 2011, Table 4020:1 and (2) (g).
Comment: LFM and LFMD are also known a Matrix Spike (MS) and Matrix Spike Duplicate
(MSD).
Comment: This was noted on the analytical batch from February 2, 2015.
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Comment: The laboratory is analyzing sample duplicates at 10% frequency. The analysis of a
LFMD (or MSD) is acceptable to satisfy the sample duplicate requirement in North Carolina
Administrative Code, 15A NCAC 2H .0805 (a) (7) (C).
Nitrogen, Ammonia — Standard Methods, 4500 NH3 D-1997
Comment: The daily minimum detection limit (MDL) standard that the laboratory analyzed was changed
to a PQL standard. This was implemented on June 8, 2015.
Comment: MDL studies are not required for this method. The SOP was edited on June 8, 2015 to
remove the MDL study procedure.
Comment: There was no documentation of the CCV preparation or true value in the SOP or on
benchsheets. The North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) states: 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. Demonstration of acceptable corrective action (i.e., an
updated benchsheet with the true value and preparation of the CCV) was observed by certification staff
on June 8, 2015 with implementation effective upon next analysis. No further response is necessary
for this finding.
BOD — Standard Methods, 5210 B-2001
Comment: It was recommended on the first day of inspection that 3 seed controls be set up for each
batch. The direction to analyze three seed controls was added to the SOP and laboratory personnel
stated on June 8, 2015 that the recommendation would be implemented effective immediately.
Comment: It was recommended on the first day of inspection that the analyst screen samples for Total
Residual Chlorine with DPD powder to determine if the titration needed to be performed. The SOP was
updated and laboratory personnel stated on June 8, 2015 that the practice would be implemented
effective immediately.
Comment: The laboratory is reminded that it may not be necessary to flag data when the Seed Control
Factor (SCF) is not between 0.6-1.0 mg/L. A SCF greater than 1.0 mg/L is allowed, but only if the
laboratory has data on file to show this is the only way to obtain acceptable results for the GGA. The SCF
in this case should not exceed 1.4 mg/L.
Comment: The BOD benchsheet did not include units of measure on the pH calibration or for column
numbers 5, 6, 7, 8, 9, 13, 14 and 16. The North Carolina Administrative Code, 15 NCAC 2H .0805 (a) (7)
(H) states: All laboratories must use printed laboratory bench worksheets that include a space to enter the
signature or initials of the analyst, date of analyses, sample identification, volume of sample analyzed,
value from the measurement system, factor and final value to be reported and each item must be
recorded each time samples are analyzed. Demonstration of acceptable corrective action (i.e., a revised
benchsheet including all applicable units of measure) was observed by certification staff on June 8, 2015
with implementation effective upon next analysis. No further response is necessary for this finding.
Comment: Extra nutrients were not being added to all samples containing more than 67% of the sample
(i.e. 201 ml) after dilution. Extra nutrients were only being added to full volume (i.e. 300 mL) samples.
Standard Methods 5210 B-2001, Section 5. b. 2 states: 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 (¶s 3a-e) directly to diluted sample
at a rate of 1 mUL (0.30 mU300mL) or use commercially prepared solutions designed to dose the
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appropriate bottle size. Demonstration of acceptable corrective action (i.e., an updated SOP stating extra
nutrients must be added to samples containing more than 67% of sample) was observed by certification
staff on June 8, 2015 with implementation effective upon next analysis. No further response is
necessary for this finding.
Comment: The SOP did not instruct, and the benchsheet did not document, that the initial DOs are
measured within 30 minutes of preparation. Standard Methods 5210 B-2001, Section 5. g. states: After
preparing dilution, measure initial DO within 30 minutes. Demonstration of acceptable corrective action
(i.e., an updated SOP stating that initial DOs are measured within 30 minutes of preparation and a
benchsheet with a space to document this) was observed by certification staff on June 8, 2015 with
implementation effective upon next analysis. No further response is necessary for this finding.
CBOD - Standard Methods, 5210 B-2001
Comment: On the first day of the inspection, certification staff stated that CBOD GGA recovery could be
164 ± 30.7 mg/L. On the second day of the inspection, June 8, 2015, an updated SOP was reviewed and
laboratory personnel stated that the criteria would be implemented immediately. Review of benchsheets
showed that they were not having issues meeting the 198 ± 30.5 mg/L criterion.
Comment: The laboratory did not have separate benchsheets for BOD and CBOD or any place to
indicate which analysis was being conducted. Demonstration of acceptable corrective action (i.e., a
separate benchsheet for CBOD analysis was generated) was observed by certification staff on June 8,
2015 with implementation effective upon next analysis. No further response is necessary for this
finding.
IV. PAPER TRAIL INVESTIGATION:
The paper trail consisted of comparing original records (e.g., laboratory benchsheets, logbooks, etc.) and
client reports. BOD data were reviewed for West Stanley WWTP NPDES permit number NCO043532 and
Carolina Village WWTP NPDES permit number NCO063762 from May 5, 2015. Field parameter data
were reviewed for Pilgrim Pride from January, 28 2015, March 11, 2015 and April 1, 2015. Fecal coliform
data were reviewed from January, 2015 through May, 2015. TSS data were reviewed for April 17, 20, and
24, 2015, and May 4, 11, 15, 18, 22, and 26, 2015. TOC data were reviewed for August 4, 2014, October
20, 2014, November 24, 2014, December 29, 2014, March 9, 2015 and March 10, 2015. TDS data were
reviewed for March 5, 6, and 11, 2015, April 15, 2015, March 21, 2015, and June 1, 2015. The following
errors were noted: The pH result from Pilgrim's Pride from March 11, 2015 reported a result to 0.01 pH
units (See Finding Y).
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 and include
an implementation date for each corrective action.
Report prepared by: Beth Swanson Date: July 21, 2015
Report reviewed by: Todd Crawford Date: July 24, 2015
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Testing of Consumable Materials for Fecal Coliform MF Method (NC WW/GW LC Policy 08/07/2015)
Standard Methods requires that before a new lot of consumable materials are used for the Fecal Coliform MF
method, those materials be tested to ensure they are reliable. North Carolina policy requires the testing of the
following consumable materials before they can be used for sample analyses: membrane filters and/or pads
(often packaged together) and media. It is recommended that only one consumable be tested at a time.
The following is provided as guidance in performing the required testing. Let's say you got a new batch of
membrane filters in. We will call the currently used filters lot #1 and the new filters lot #2.
I. Select a culture positive sample.
What you want is something that will yield 20-60 colonies when a reasonable sample volume is filtered. This may
be a stream sample or a sample taken somewhere within the waste treatment plant. If the concentration is high
enough that greater than 60 colonies are obtained when 1 mL is filtered then the solution is too strong and must
be diluted. Any time a sample is diluted be sure it is done with the BUFFERED dilution water used for rinsing the
funnels.
2. Test the culture positive to determine the appropriate volume to use.
When collecting the culture positive sample do not think about it as a sample. You do not have to be concerned
with a sterile sample bottle or 6 hour hold time. Collect enough sample so that you have plenty to work with,
probably more than your normal fecal bottle holds. Set a series of dilutions using the currently used materials, in
this example filter lot #1. Do not use the materials you want to prove are OK at this point. All you are trying to do
is to determine the volume of sample that will yield 20-60 colonies. Put the rest of the sample in the refrigerator.
For example:
Volume used Colonies obtained on lot #1 filters
50 ml TNTC
25 ml 138
10 ml 50
5 ml 22
1 ml 4
Based on this preliminary testing it appears that a 10 ml volume would probably be appropriate to use and will
yield the desired 20-60 colonies. Remember when you do the actual consumable test, the culture positive sample
will be 24 hours old and the results you obtain may be lower than the initial results yielded, but not so significantly
lower as to change your dilution choice. It is better to have your initial results on the high side of the 20-60 range
for this reason. In this example the 5 ml volume would probably be too low and would likely yield less than 20
colonies the next day.
3. Perform the consumable test
Once you determine the appropriate volume, in this case 10 mis, take the remaining culture positive sample from
the refrigerator, bring to room temperature and set five 10 ml plates with the currently used filters, lot #1, and five
10 ml plates with the new filters, lot #2.
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4. Determine acceptability of new material
For example:
Lot #1-current filters Colonies obtained on lot #1 filters
10 ml 48
10ml 45
10 ml 50
10 ml 44
10 ml 43
Average: 46
Lot #2-new filters Colonies obtained on lot #2 filters
10 ml 40
10ml 45
10 ml 38
10 ml 46
10 ml 37
Average: 41
When determining the acceptability of the new material, compare the average of the five replicates for lot #1 to
the average of the five replicates for lot #2; that is 46 vs. 41 colonies. The recommended acceptance criteria
would be your current acceptance criteria used for your Fecal Coliform duplicates. If the test and reference
materials check within what you have determined is acceptable for duplicates of samples, the test material would
be considered acceptable to use. This may be a calculated acceptance criteria based on 3 times the standard
deviation of the mean or a set value like 20% RPD. No matter how you determine your duplicate acceptance
criteria make sure you use colony counts not final calculated values in doing this. Other factors to consider when
determining if a new material is suitable include:
Are the colonies obtained typical, that is normal looking blue colonies?
Are the colonies evenly distributed across the membrane surface?
Are there an unusual number of non -typical colonies present?
Is there a pattern to the colony recoveries? For example are all the plates for the test materials significantly lower
in counts than the reference lot?
It is recommended that new consumables be tested as soon as possible after receipt to avoid problems if the
materials are not acceptable. Once you determine that the new material is acceptable to use; you may begin to
do so. Document the date the new lot # is put into use.
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Infrared Thermometer Calibration Verification Policy (NC WW/GW LC 06/26/2015)
When an infrared (IR) detection device is used to measure the temperature of samples, the device must be
verified at least every six months using a National Institute of Standards and Technology (NIST) traceable
thermometer at a minimum of two different temperatures over the full temperature range that the IR thermometer
will be used (e.g., 0°C to 10°C for a sample receipt thermometer). Each day of use, perform a single check of the
IR thermometer by checking the temperature of a bottle of water at the temperature of interest that contains a
calibrated thermometer. Agreement between the two must be within 0.5°C, or the device must be rechecked. If
the second calibration verification fails, the device must be repaired and/or replaced. Document the semi-annual
and daily calibration checks. The correction factor must be indicated on the thermometer and applied when
recording temperature measurements.