HomeMy WebLinkAbout#402_2016_0510_BS_FINALTo be attached to all inspection reports in-house only.
Laboratory Cert. #:
Laboratory Name:
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 Admin:
Date Mailed:
402
Prism Laboratories, Inc.
Commercial Maintenance
Beth Swanson, Gary Francies, Anna
Ostendorff, Dana Satterwhite, Todd
Crawford, Tonia Springer, Nick Jones
Jason Smith
May 10-11, 2016
June 1, 2016
June 2. 2016
Jason Smith
June 9, 2016
❑ Insp. Initial ® Insp. Reg.
❑ Insp. No Finding ❑ Insp. CP
❑ Corrected ❑ Insp. Reg. Delay
Gary Francies
e 13. 2016
7/21 /2016
7/22/201
Special Mailing Instructions: Wes Bell - MRO
Water Resources
ENVIRONMENTAL allAU! Y
July 21, 2016
402
Mr. Helmuth M.B. Janssen
Prism Laboratories, Inc.
P.O. Box 240543
Charlotte, NC 28224-0543
PAT MCCRORY
DONALD R. VAN DER VAART
S. JAY ZIMMERMAN
Subject: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC)
Maintenance Inspection
Dear Mr. Janssen:
Enclosed is a report for the inspection performed on May, 11, 2016 by Beth Swanson Gary Francies,
Dana Satterwhite, Todd Crawford, Tonja Springer, Jason Smith, Nick Jones, and Anna Ostendorff
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. Please describe the steps taken to prevent recurrence 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 me at (828) 296-4677.
Sincerely,
Gary Francies, Technical Assistance/Compliance Specialist
Division of Water Resources
Attachment
cc: Beth Swanson
Master file
LABORATORY NAME:
CERTIFICATE :
DATE OF INSPECTION:
F&79Ar6Tx1H3 114WIXIF
AUDITOR(S):
LOCAL PERSON(S) CONTACTED:
I. INTRODUCTION:
Prism Laboratories, Inc.
449 Springbrook Road
Charlotte, NC 28217
402
May 10 and 11, 2016
Commercial Maintenance
Beth Swanson, Gary Francies, Anna Ostendorff, Dana
Satterwhite, Todd Crawford, Tonja Springer, Nick Jones and
Jason Smith
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:
Overall, the laboratory's system of traceability is thorough, well thought out and easy to follow.
Interaction with laboratory staff showed analysts who are knowledgeable and forthcoming and
management that is quality control oriented. The laboratory has instituted many quality control
practices throughout their systems that are beyond our program requirements.
All required Proficiency Testing (PT) samples for the 2016 PT calendar year have not yet been
analyzed. The laboratory is reminded that results must be received by this office directly from the
vendor by September 30, 2016.
The laboratory submitted their Quality Assurance (QA) and/or Standard Operating Procedures
(SOP) document(s) in advance of the inspection. These documents were reviewed and editorial
and substantive revision requirements and recommendations were made by this program
outside of this formal report process. Although subsequent revisions were not requested to be
submitted, they must be completed by May 10, 2017.
The laboratory is reminded that any time changes are made to laboratory procedures; the
laboratory must update the QA/SOP document(s) and inform relevant staff. Any changes made
in response to the pre -audit review or to 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 each
approved practice, test, analysis, measurement, monitoring procedure or regulatory requirement
being used in the laboratory. In some instances, the laboratory may need to create an SOP to
document how new functions or policies will be implemented.
The laboratory is also reminded that SOPs are intended to describe procedures exactly as they
are to be performed. Use of the word "should" is not appropriate when describing requirements
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#402 Prism Laboratories, Inc.
(e.g. Quality Control (QC) frequency, acceptance criteria, etc.). Evaluate all SOPS for the proper
use of the word "should".
Requirements that reference 15A NCAC 2H .0805 (a) (7) (A), stating "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", are intended to be a requirement to document information pertinent to
reconstructing final results and demonstrating method compliance. Use of this requirement is not
intended to imply that existing records are not adequately maintained unless the Finding speaks
directly to that.
Contracted analyses are performed by Gulf Coast Analytical Laboratories (Certification #618).
III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:
Documentation
Recommendation: It is recommended that an indication such as "out of service" be included on
the thermometer calibration records when that thermometer is no longer being used. The
calibration records could be misconstrued, indicating that calibrations were not being performed at
the required frequency.
Recommendation: It is recommended that a diagram be made of the metals digestion block so
that it is possible to tell which digestion well is used for the daily temperature check.
A. Finding: Error corrections are not always properly performed.
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-Out®, 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.
Recommendation: It is recommended that when any documentation correction that
affects the final reported sample result is made, the lab also note the reason the change
was made. For example, changing an original sample absorbance or weight observation
due to further stabilization of the spectrophotometer or balance, the lid to the
spectrophotometer was left open in error during sample measurement, etc. Also be
aware that improper error corrections that result in QC evaluations going from outside
the acceptance range to within the acceptance range, could give the perception of
falsification. Some instances of this were noted on the Hexavalent Chromium data from
2/12/2016.
B. Finding: All traceability information is not documented or is documented incorrectly.
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
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#402 Prism Laboratories, Inc.
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: INC WW/GW
LC Policy.
Comment: While the laboratory has a good system of traceability, there were instances
noted where the proper traceability information was not transferred to the applicable
benchsheet or the volumes/concentrations of stock standards were either not documented
or were incorrect. Much of this information can be found in the laboratory's information
management system (LIMS), but when spaces for this information are left blank or the
information is incorrect, it appears there is a lack of traceability. The following examples
were noted during data review, but this list is not all inclusive. Please review all
benchsheets and supporting records for adherence to the Requirement. If a specific
method reference is not listed, the Finding is referring to all methods on the laboratory's
Certified Parameter Listing at the time of the inspection:
® Hexavalent Chromium (Standard Methods (SM) 3500-Cr B-2009)
benchsheet — The Continuing Calibration Verification (CCV) ID is not
documented.
® Hexavalent Chromium (SW-846 7196 A (Non -Aqueous)) digestion log —
Traceability information for the insoluble spike (PbCr04) is not
documented.
® Oil & Grease (EPA 1664 Rev. B) — The Laboratory Control Sample
(LCS) true value was not documented on any of the three data sets
reviewed.
® Oil & Grease (EPA 1664 Rev. B) — The Matrix Spike (MS) true value
was not documented on 9/8/2015 or 3/9/2016.
® Nitrogen, Ammonia (SM 4500 NH3 C-1997) — The stock concentration
was incorrectly documented as 100 mg/L for the MS/Matrix Spike
Duplicate (MSD) and LCS instead of 1000 mg/L on the 3/6/2015 titration
log.
® Nitrogen, Ammonia (SM 4500 NH3 C-1997) — The stock concentration
was incorrectly documented as 100 mg/L for the LCS instead of 1000
mg/L on the 8/13/2015 and 11 /6/2015 titration logs.
® Total Kjeldahl Nitrogen (TKN) (EPA 351.2, Rev, 2.0, 1993) — The
MS/MSD stock solution was not identified on the 8/31/2015 digestion
log.
® Anions IC — The Nitrite CCV is consistently not documented in the
Source Standard column of the "IC Standards and Reagents
Documentation Sheet".
® MBAS — The stock concentration for the LCS was incorrectly
documented as 10 mg/L instead of 100 mg/L on the two benchsheets
reviewed.
C. Finding: Method references are incomplete or incorrect on some benchsheets and/or
supporting documentation. 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).
Requirement: Analytical methods, sample preservation, sample containers and sample
holding times shall conform to those requirements found in 40 CFR-136.3. Ref: 15A NCAC
2H .0805 (a) (1).
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#402 Prism Laboratories, Inc.
Comment: Data is reported on client reports with the correct methods/revisions. The
following examples were noted during data review, but this list is not all inclusive. Please
review all benchsheets and supporting records for adherence to the Requirement:
e Most benchsheets and supporting records for Standard Methods methods did
not include the approval year as stated in 40 CFR Part 136.3 Table IB (i.e., the
Turbidity reference would be SM 2130B-2001 rather than SM 2130B).
• The Mercury Analysis Review Checklist and Instrument printouts reference
7471 A rather than 7471 B.
e The TKN digestion log references Nor9 B instead of No,9 C.
D. Finding: The units of measure are not consistently documented on the benchsheets.
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 units of measure are not documented and/or incorrect in the following
locations. If a specific method reference is not listed, the Finding is referring to all
methods on the laboratory's Certified Parameter Listing at the time of the inspection:
e MBAS benchsheet — Reporting Limit column.
• Acidity benchsheet — pH.
• Alkalinity benchsheet — pH and Total Volume column of the standard
preparation section.
e Coliform- Fecal (MF) benchsheet — Waterbath Temperatures
e COD benchsheet — wavelength and Quality Control (QC) true value.
• Color, PC benchsheet — Instrument Reading column, LCS calculation and LCS
obtained value.
e Oil & Grease (EPA 1664 Rev. B) — the units for the 2 mg weight column are
listed as mg but analysts occasionally document in grams.
• Oil & Grease (SW-846 9071 B) — the units for the spike concentration are mg/kg
instead of mg/L.
e Total, Dissolved and Suspended Residue benchsheets — QC True Value
• Turbidity benchsheet — Initial Calibration Verification (ICV), True Value, pH,
Meter Reading, Reporting Limit (RL) and duplicate results.
• Settleable Residue benchsheet — Reported Result column.
• Hexavalent Chromium benchsheet (SM 3500 Cr-B-2009) — cell path length,
Absorbance column, Minimum Reporting Limit (MRL) column, and wavelength.
E. Finding: Precision (e.g., Relative Percent Difference (RPD)) and/or accuracy (e.g., percent
recovery) of quality control results are not consistently evaluated and/or documented to
demonstrate the analytical process is in control and the established acceptance criteria are
met.
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: The precision and accuracy of QC results must be documented and
evaluated against the prescribed acceptance criteria to demonstrate that the analytical
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#402 Prism Laboratories, Inc.
process is in control. Any samples associated with QC not meeting the criteria must be
reanalyzed if possible. If this is not possible, the data must be flagged on the laboratory
reports as all quality control requirements not met and giving a brief description of the
QC exceedance that occurred. The laboratory indicated that all QC calculations are
entered into the LIMS system and evaluated at a later time, however there are some
instances where the analyst needs to know immediately if the QC results are within
acceptance criteria. Also, for instances where there is a space to enter QC results on the
benchsheet and that space is left blank, it appears that the evaluation did not occur,
even if it was later executed in LIMS. The following examples were noted during data
review, but this list is not all inclusive. Please review all benchsheets and supporting
records for adherence to the Requirement. If a specific method reference is not listed,
the Finding is referring to all methods on the laboratory's Certified Parameter Listing at
the time of the inspection:
® Suspended Residue benchsheet — The RPD for duplicates was not
documented for two benchsheets reviewed. The third benchsheet did
not include analysis of a duplicate.
® Dissolved Residue benchsheet — The RPD for duplicates was not
documented for all three benchsheets reviewed and LCS recovery was
not documented for two out of three benchsheets reviewed.
® Total Residue benchsheets — The RPD for duplicates was not
documented on all three benchsheets reviewed.
® Oil & Grease (EPA 1664 Rev. B) — The standard concentration and the
volume used to prepare the LCS were not documented on the 3/9/2016
benchsheet.
® Oil & Grease (EPA 1664 Rev. B) — The concentration of the standard
used for the LCS and spike preparation were incorrectly documented as
40 mg/L instead of 4000 mg/L on the 1/4/2016 benchsheet.
® Oil & Grease (SW-846 7071 B) — The LCS for both Oil & Grease and Oil
& Grease (SGT) are not always calculated. Occasionally, the SGT
recovery is calculated.
® Oil & Grease (SW-846 7071 B) — The MS/MSD recoveries and RPD
were not documented on the 1/27/2016 benchsheet, which has spaces
to enter all values. One recovery and the RPD failed, and the sample
was qualified on the client report since the results were entered into the
LIMS system and calculated there.
® Oil & Grease (EPA 1664 Rev. B) — The LCS result and evaluation were
not documented on any of the three data sets reviewed.
® Oil & Grease (EPA 1664 Rev. B) — The matrix spike evaluation was not
documented on 9/8/2015 or 3/9/2016.
® Oil & Grease (EPA 1664 Rev. B) — The duplicate was not evaluated on
any of the three data sets reviewed.
® Anions IC — The evaluation of all QC standard percent recoveries is not
documented, however, it appears they are calculated at some point
based on the "Analysis Review Checklist".
® Conductivity (SM 251013-1997) — The RPD for duplicates were not
calculated and documented.
General
F. Finding: The State Laboratory is not notified when samples are received out of
compliance and analyzed at the client's request.
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#402 Prism Laboratories, Inc.
Requirement: At any time a laboratory receives samples which do not meet sample
collection, holding time, or preservation requirements, the laboratory must notify the
sample collector or client and secure another sample if possible. If another sample
cannot be secured the original sample may be analyzed but the results reported must
be qualified with the nature of the infraction(s) and the laboratory must notify the State
Laboratory about the infraction(s). The notification must include a statement indicating
corrective actions taken to prevent the problem for future samples. Ref: 15A NCAC 2H
.0805 (a) (7) (N).
Proficiency Testing
G. Finding: The preparation of Proficiency Testing (PT) samples is not documented.
Requirement: PT samples received as ampules must be diluted according to the PT
provider's instructions. The preparation of PT samples must be documented in a
traceable log or other traceable format. The diluted PT sample becomes a routine
environmental sample and is added to a routine sample batch for analysis. Ref:
Proficiency Testing Requirements, February 20, 2012, Revision 1.2.
Comment: Dating and initialing the instruction sheet for the preparation of applicable PTs
would satisfy the documentation requirement.
H. Finding: The laboratory is not always analyzing PT samples in the same manner as
routine compliance samples.
Requirement: All PT samples are to be analyzed and the results reported in a manner
consistent with the routine analysis and reporting requirements of compliance samples and
any other samples analyzed according to the requirements of 15A NCAC 2H .0800. Ref:
Proficiency Testing Requirements, February 20, 2012, Revision 1.2.
Comment: The Nitrogen, Nitrite PT sample was analyzed with three additional QC
standards which are not routinely analyzed with compliance samples. Other PT analyses
observed did not include extra QC.
Quality Control
I. Finding: Data that does not meet all quality control requirements is not always qualified on
the client report.
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: Two instances were noted during data review where the relative percent
difference (RPD) for the duplicates was not acceptable and it was flagged in LIMS but not
carried through to the client report. These were for Settleable Residue sample # 6010269
and Dissolved Residue sample #601-103. Duplicates are not required for Settleable
Residue, but if analyzed, the QC criterion must be evaluated and corrective action and/or
qualifying the results must be performed when necessary.
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#402 Prism Laboratories, Inc.
Acidi —Standard Methods, 2310 B-1997, Rev. 2011 (Aqueous)
J. Finding: The laboratory is correcting the sample result for the method blank.
Requirement: The calculation does not include blank correction:
Acidity, as mg CaCO3/L = [(A a)—(CxA)]x5D000
mL saniple
Where:
A = mL NaOH titrant used,
B = normality of NaOH,
C = mL H2SO4 used (2310B.4a), and
D = normality of H2SO4
Ref: Standard Methods, 2310 B-1997. (5).
K. Finding: The laboratory is not documenting all sample volumes.
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 did not include the volume analyzed for the blank, LCS, or RL
standard. The volume is needed to calculate the Acidity result for these samples.
Bacteria — Coliform Fecal — Standard Methods, 9222 D-1997 (MF) (Aqueous)
Bacteria — Coliform Fecal — Standard Methods, 9222 D-1997 (MF) 24hr 503 (Non -Aqueous)
L. Finding: Consumable materials used for the Fecal and Total Coliform Membrane Filtration
(MF) methods are not properly tested.
Requirement: When a new lot of culture medium, pads, or membrane filters is to be used,
a comparison of the current lot in use (reference lot) against the new lot (test lot), be made.
As a minimum, make single analyses on five positive samples. Ref: NC WW/GW LC Policy.
Comment: The laboratory is analyzing a culture positive with each new lot of filters and
media. The old and new lots are not compared, and new lots of pads are not being tested
at all. A copy of the Testing of Consumable Materials for Fecal Coliform MF Method policy
is attached to the end of this report.
M. Finding: Plate comparison counts are not performed and documented monthly.
Requirement: 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. Ref: Standard Methods, 9020 13-
2005. (9) (a).
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#402 Prism Laboratories, Inc.
Comment: The analyst stated that positive plate count comparisons among analysts were
occasionally performed, but not on a monthly basis and the process was not documented.
N. Finding: Filtration start time is not documented to show that plates are placed into the
incubator within 30 minutes.
Requirement: Place all prepared cultures in the water bath within 30 min after filtration.
Ref: Standard Methods, 9222 D-1997. (2) (d).
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).
O. Finding: Culture positive plates are not countable.
Requirement: A culture positive must be analyzed with each batch of prepared media and
once per week for purchased ready -to -use media. A sample volume that yields a countable
plate must be analyzed so that individual colonies may be verified to have proper
morphology (i.e. color, shape, size, surface appearance). Ref: NC WW/GW LC Policy.
P. Finding: The UV lamp bulbs are not cleaned monthly.
Requirement: When used, disconnect lamps monthly and clean blubs with a soft cloth
moistened with ethanol, 70% methanol/30% reagent -grade water, or use spectroscopic
grade 2-propanol where baked on material may be collecting. Ref: Standard Methods,
9020 B-2005. (4) (1).
Q. Finding: The laboratory is using a partial immersion thermometer in the fecal water bath
improperly.
Requirement: 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. Ref: "Selecting Alternatives to Mercury -
Filled Thermometers", http:l/tLy\iv v.e a.goy/mercury/alternatives.htrn.
Comment: The thermometers in the #1 and #3 fecal water baths were not immersed to the
proper depth. The water was a few inches above the immersion line on each thermometer.
Bacteria — Coliform Total — Standard Methods, 9222 B-1997 (MF) (Aqueous)
Recommendation: It is recommended that the shelf on which the incubator temperature is
obtained be documented on the benchsheet. The laboratory currently has an incubator with three
shelves and a thermometer on each one.
Bacteria — Coliform Fecal — Standard Methods, 9221C E-2006 (MPN) 24hr 503 (Non -
Aqueous)
Bacteria — Coliform Fecal — Standard Methods, 9221C E-2006 (MPN) (Aqueous)
R. Finding: The laboratory is not analyzing duplicates.
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#402 Prism Laboratories, Inc.
Requirement: Analyze five percent of all samples in duplicate to document precision.
Laboratories analyzing less than 20 samples per month must analyze at least one
duplicate each month samples are analyzed. Ref: 15A NCAC 2H .0805 (a) (7) (C).
Comment: A duplicate is only required on one dilution per sample for Fecal Coliform.
Bacteria — Coliform Fecal — Standard Methods, 9221C E-2006 (MPN) 24hr 503 (Non -
Aqueous)
Bacteria — Coliform Fecal — Standard Methods, 9221 C E-2006 (MPN) (Aqueous)
S. Finding: The A-1 media is not properly stored and is used beyond the method stated shelf
life.
Requirement: Store in the dark at room temperature for not longer than 7 days. Ref:
Standard Methods, 9221 E-2006. (2) (a).
Comment: The A-1 media is currently stored in the refrigerator for 2 weeks.
BOD —Standard Methods, 5210 B-2001 (Aqueous)
CBOD — Standard Methods, 5210 B-2001, Rev. 2011 (Aqueous)
Recommendation: It is recommended that the spaces for the drift check and calibration check be
labeled accordingly. The current system causes confusion, as the calibration check is labeled "drift
±0.1 mg/L" and the drift check is labeled "calibration blank".
T. Finding: Seed controls with less than 2.0 mg/L Dissolved Oxygen (DO) depletion are used
for seed correction calculation.
Requirement: For the ratio method, divide the DO depletion by the volume of seed in
milliliters for each seed control bottle having a 2.0 mg/L depletion and greater than 1.0 mg/L
minimum residual DO and average the results. Ref: Standard Methods, 5210 B-2001. (6)
(d) .
Comment: This was noted on BOD data from 3/3/2016 and the analyst indicated that a
minimum depletion is not considered when evaluating the individual seed controls.
U. Finding: The laboratory is incorrectly reporting results for samples that do not meet the
minimum depletion.
Requirement: The reporting limit for BOD5/CBOD5 is 2 mg/L. Only bottles giving a
minimum DO depletion of 2.0 mg/L and a residual DO of 1.0 mg/L after 5 days of
incubation are considered to produce valid data. It is not acceptable to elevate the reporting
limit and report as less than the value that would have been obtained if the dilution had
depleted the required 2.0 mg/L. It is required that the data be flagged as a quality control
failure if it does not deplete the 2.0 mg/L. The only exception to this is when a 100% sample
does not deplete 2.0 mg/L. In this case, report the value as <2.0 mg/L without qualification.
Ref: NC WW/GW LC Policy.
Comment: The laboratory does not analyze 100% samples and when there are no
dilutions that meet the minimum DO depletion, the reporting limit is elevated and it is
reported as less than the elevated reporting limit without qualification. This is automatically
performed in LIMS. The BOD/CBOD value must be calculated using the smallest dilution
(i.e., most sample) and reported with a qualifier and not reported as a less than value.
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#402 Prism Laboratories, Inc.
V. Finding: The barometric pressure at the time of meter calibration is not documented. This
is considered pertinent data.
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).
W. Finding: Initial DO concentrations of all bottles other than the blank are not always brought
to the required range of 7 and 9 mg/L.
Requirement: The working range is equal to the difference between the maximum initial
DO (7 to 9 mg/L) and minimum DO residual of 1 mg/L corrected for seed, and multiplied by
the dilution factor. Ref: Standard Methods, 5210 B-2001. (8) (b).
Requirement: Samples supersaturated with DO — Samples containing DO concentrations
above saturation at 20 °C may be encountered in cold waters or in water where
photosynthesis occurs. To prevent loss of oxygen during incubation of such samples,
reduce DO to saturation by bringing sample to about 20 ± 3 °C in partially filled bottle while
agitating by vigorous shaking or by aerating with clean, filtered compressed air. Ref:
Standard Methods, 5210 B-2001. (4) (b) (4).
Comment: The laboratory is using an initial DO maximum of 9.2 mg/L. The DO saturation
table used as part of the DO meter calibration verification procedure lists the saturation of
DO at 20 ° C as 9.08 mg/L.
X. Finding: The benchsheet does not document that initial DO is read within 30 minutes of
dilution preparation.
Requirement: After preparing dilution, measure initial DO within 30 minutes. Ref: Standard
Methods, 5210 B-2001. (5) (g).
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).
Y. Finding: The position of the drift check during the analytical batch is not indicated on the
benchsheet.
Requirement: If the membrane electrode method is used, take care to eliminate drift in
calibration between initial and final DO readings. Ref: Standard Methods, 5210 B-2001. (5)
(g)
Requirement: Immediately after calibration, measure the DO of a BOD bottle of dilution
water. Stopper the bottle. Document the concentration on the benchsheet (day one initial
drift check). At the end of the sample set reanalyze the drift check bottle and document the
concentration (day one final drift check). The laboratory should verify the DO Meter
calibration throughout the sample set if needed. Repeat process on Day 5. If the meter
drifts more than 0.20 mg/L, recalibrate meter and reanalyze all samples since the last drift
check. Ref: NC WW/GW LC Policy.
Comment: There is one spot for a drift check on each page of the BOD/CBOD
benchsheet, but it is not clear at what point during analysis these drift checks are read.
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Anions (Cl-, F-, SO4, NO2, NO3, NO3+NO2) — EPA 300.0, Rev. 2.1, 1993 (Aqueous & Non -
Aqueous)
Anions (Cl-, F-, SO4, NO2, NO3, NO3+NO2) — SW-846 9056 A (Aqueous & Non -Aqueous)
Comment: An acceptance criterion for method/reagent blanks of <_ 1/2 RL may be used in place of
the EPA 300.0 requirement of <MDL.
Recommendation: It is recommended that the Analysis Review Checklist be edited to remove the
phrase "percent recoveries and" in item #4, which only concerns RPD acceptance.
Z. Finding: The initial and continuing calibration blank acceptance criterion exceeds 50% of
the reporting limit.
Requirement: For analyses requiring a calibration curve, the concentration of reagent,
method and calibration blanks must not exceed 50% of the reporting limit or as otherwise
specified by the reference method. Ref: NC WW/GW LC Policy.
Comment: The laboratory's initial and continuing calibration blank acceptance criterion is
<RL. The reviewed data often showed calibration blanks that were >'/2 RL for Nitrate, so the
RL for this analyte may need to be elevated.
Chlorine, Total Residual — Standard Methods, 4500 Cl G- 2000, Rev. 2011 (Aqueous)
AA. Finding: A reagent blank is not analyzed each day standards are prepared.
Requirement: Each day that prepared standards are analyzed, a reagent blank must be
analyzed to determine if method analytes or other interferences are present in the
laboratory environment, the reagents or the apparatus. 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 currently prepares and analyzes three standards daily.
COD — Standard Methods, 5220 D-1997, Rev. 2011 (Aqueous)
COD — Hach 8000 (Aqueous)
Inorganic Phenols — EPA 420.1 Rev. 1978 (Aqueous)
Inorganic Phenols — SW-846 9065 (Aqueous)
MBAS — Standard Methods, 5540 C-2000, Rev. 2011 (Aqueous)
Phosphate, Ortho — Standard Methods, 4500 P E-1999, Rev. 2011 (Aqueous)
Phosphorus, Total — Standard Methods, 4500 P E-1999, Rev. 2011 (Aqueous)
Phosphorus, Total — EPA 365.1, Rev. 2.0, 1993 (Aqueous)
Chromium Hexavalent— Standard Methods, 3500 Cr-B-2009 (Aqueous)
BB. Finding: A blank is not analyzed after every ten samples and/or at the end of the sample
group.
Requirement: The calibration blank and calibration verification standard (mid -range) must
be 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. If either fall outside
established quality control acceptance criteria, corrective action must be taken (e.g.,
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repeating sample determinations since the last acceptable calibration verification, repeating
the initial calibration, etc.). Ref: NC WW/GW Policy.
Comment: Most of the data reviewed had fewer than 10 samples, so only the blank at the
end of the group would apply.
COD —Standard Methods, 5220 D-1997, Rev. 2011 (Aqueous)
CC. Finding: The CCV acceptance criterion is ±10% recovery.
Requirement: Prepare calibration curve for each new lot of tubes or ampules or when
standards prepared in ¶a above differ by >_5% from calibration curve. Ref: Standard
Methods, 5220 D-1997. (4) (c).
Comment: The three benchsheets reviewed included CCV values that did not differ by
more than >_5% from the calibration curve.
Cyanide — Standard Methods, 4500 CN- E-1999, Rev. 2011 (Total) (Aqueous)
DD. Finding: The laboratory is not always documenting the sample volume and/or final
distillation volume.
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. The date
and time BOD and coliform samples are removed from the incubator must be included on
the laboratory worksheet. Ref: 15A NCAC 2H .0805 (a) (7) (H).
Comment: The sample volume and final distillation volumes were documented as a check
mark on the 9/1/2015 distillation sheet.
EE. Finding: The laboratory is not back calculating the calibration standards.
Requirement: Back calculate the concentration of each calibration point. The back -
calculated and true concentrations should agree within ± 10%. Ref: Standard Methods,
4020 B-2009. (2) (a).
Cyanide — Standard Methods, 4500 CN- E-1999, Rev. 2011 (Total) (Aqueous)
Cyanide — SW-846 9014 (Total) (Colorimetric) (Aqueous & Non -Aqueous)
Comment: Samples analyzed by SW-846 9014 are distilled according to SW-846 9010C, which is
a Method Defined Parameter. SW-846 9010C must be followed exactly as written, or the resulting
data cannot be used to ensure regulatory compliance.
FF. Finding: Ethylenediamine solution is being added to all samples.
Requirement: There is no mention of this compound in either SW-846 9010C or SW-846
9014 Ref: EPA SW-846 Test Methods for Evaluating Solid Waste, Physical/Chemical
Methods; 3rd Edition, Method 9010 C. Rev. 3, November 2004 and EPA SW-846 Test
Methods for Evaluating Solid Waste, Physical/Chemical Methods; 3rd Edition, Method 9014.
Rev. 1, July 2014.
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#402 Prism Laboratories, Inc.
Requirement: If formaldehyde, acetaldehyde, or other water-soluble aldehydes are known
or suspected to be present, treat the sample with 2 mL 3.5 % ethylenediamine (Section
6.10) per 100 mL of sample to avoid the formation of cyanohydrins. It has been found that
this quantity of ethylenediamine addition is suitable to overcome the interference caused by
up to 50 mg/L CH2O present. Samples can be screened for the presence of formaldehyde
and other watersoluble aldehydes using test strips for formaldehyde or aldehydes. Ref:
Code of Federal Regulations, Title 40, Part 136; Federal Register Vol. 77, No. 97, May
18, 2012; Table II, #23 Footnote 6 and ASTM Method D7365-09a, Section 8.3.8.
Recommendation: It is recommended that Ethylenediamine solution only be added to
samples that have tested positive for aldehydes.
Cyanide — SW-846 9014 (Total) (Colorimetric) (Aqueous & Non -Aqueous)
Comment: Samples analyzed by SW-846 9014 are distilled according to SW-846 9010C, which is
a Method Defined Parameter. SW-846 9010C must be followed exactly as written, or the resulting
data cannot be used to ensure regulatory compliance.
GG. Finding: A 0.25 N sodium hydroxide solution is being used in the gas scrubber.
Requirement: Pipet 50 mL of 1.25 N sodium hydroxide into the gas scrubber. Ref: EPA
SW-846 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods; 3rd Edition,
Method 9010 C. Rev. 3, November 2004, Section 7.2.1.
MBAS — Standard Methods, 5540 C-2000, Rev. 2011 (Aqueous)
HH. Finding: The linear alkylbenzene sulfonate (LAS) molecular weight is not documented on
the calibration curve.
Requirement: From the calibration curve (5540C.4a) read micrograms of apparent LAS
(mol wt ___) corresponding to the measured absorbance. Ref: Standard Methods, 5540
C-2000. (5).
Nitrogen, Ammonia — Standard Methods, 4500 NH3 C-1997, Rev. 2011 (Aqueous)
II. Finding: Sample pH adjustment to 9.5 s.u. is not checked with a pH meter.
Requirement: Add 25 mL borate buffer solution and adjust to pH 9.5 with 6N NaOH using
a pH meter.
JJ. Finding: Borate buffer is not being used to steam out the distillation apparatus.
Requirement: Equipment preparation: Add 500 mL water and 20 mL borate buffer, adjust
pH to 9.5 with 6N NaOH solution, and add to a distillation flask. Add a few glass beads or
boiling chips and use this mixture to steam out the distillation apparatus until distillate
shows no traces of ammonia. Ref: Standard Methods, 4500 NH3 B- 1997, Rev. 2011. (4)
(a).
Nitrogen, Nitrite — Standard Methods, NOz" B-2000, Rev. 2011 (Aqueous)
KK. Finding: The blank acceptance criterion is not properly evaluated.
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Requirement: For analyses requiring a calibration curve, the concentration of reagent,
method and calibration blanks must not exceed 50% of the reporting limit or as otherwise
specified by the reference method. Ref: NC WW/GW LC Policy.
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: The precision and accuracy of QC results must be documented and evaluated
against the prescribed acceptance criteria to demonstrate that the analytical process is in
control. Any samples associated with QC not meeting the criteria must be reanalyzed if
possible. If this is not possible, the data must be flagged on the laboratory reports and
Discharge Monitoring Reports (DMR) as all quality control requirements not met and giving
a brief description of the QC exceedance that occurred.
Comment: Blank values were being documented on benchsheets as < 0.01 mg/L, which is
the reporting level. This does not allow for proper evaluation against the required
acceptance criterion.
Nitrogen, Total Kieldahl — Standard Methods, Nog C-1997 (Standard Methods 4500 NH3 C-
1997, Rev. 2011) (Aqueous)
Comment: No results are reported by this method, only EPA 351.2, Rev. 2.0, 1993.
Nitrogen, Total Kieldahl — EPA 351.2, Rev. 2.0, 1993
LL. Finding: The incorrect volume of mercury -free digestion solution is being added to the
samples.
Requirement: Note 1: An alternate mercury -free digestion solution can be prepared by
dissolving 134 g K2SO4 and 7.3 g CUSO4 in 800 mL reagent water and then adding 134 mL
conc. H2SO4 and diluting to 1 L. Use 10 mL solution per 25 mL of sample.
Comment: The laboratory is adding 5 mL of mercury -free digestion solution per 25 mL of
sample, which is the volume used for digestion solutions that contain mercury.
MM. Finding: Each calibration standard is not being digested independently.
Requirement: Prepare a series of at least three standards, covering the desired range,
and a blank by diluting suitable volumes of standard solution (Section 7.11) with reagent
water. Ref: EPA 351.2, Rev. 2.0, 1993, Section 10.1.
Requirement: Process standards and blanks as described in Section 11.0, Procedure.
Ref: EPA 351.2, Rev. 2.0, 1993, Section 10.2.
Comment: The laboratory is digesting a 10 mg/L intermediate standard and then making
dilutions of that to prepare the curve.
Oil & Grease — EPA 1664 Rev. B (Aqueous)
NN. Finding: The acceptance criterion for the 2 mg weight is not within the method specified
limit and the balance is not always recalibrated if outside the laboratory's acceptance limit.
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Requirement: Calibration shall be within ± 10% (i.e. ± 0.2 mg) at 2 mg, ± 0.5% (i.e., ± 5
mg) at 1000 mg, and if applicable, at the appropriate user -specified tolerance for Class 1
weights greater than 1000 mg. If values are not within these limits, recalibrate the balance.
Ref: EPA Method 1664 Rev. B, Section 10.2.
Comment: The laboratory uses an acceptance criterion of ± 0.5 mg for the 2 mg weight.
On 9/8/2015, the weight check was recorded as 0.0026 (which is in grams instead of the
column heading of mg), which would have failed the laboratory's elevated acceptance
criterion. The balance was not recalibrated at this time.
Oil & Grease — SW-846 9071 B (Non -Aqueous)
Recommendation: It is recommended that the blank on the benchsheet be identified as the
method blank.
Paint Filter Liquids — SW-846 9095B
Recommendation: It is recommended that the LCS and Blank, which are pre-printed onto the
benchsheet, be removed since they are not analyzed.
Residue, Settleable — Standard Methods, 2540 F-1997 (Aqueous)
00. Finding: The 45-minute sample stir time is not documented.
Requirement: The following must be documented in indelible ink whenever sample
analysis is performed: 45-minute stir time (use of a check box is acceptable). Ref: NC
WW/GW LC Approved Procedure for the Analysis of Settleable Solids.
Residue, Dissolved 180 C — Standard Methods, 2540 C-1997, Rev. 2011 (Aqueous)
Residue, Suspended —Standard Methods, 2540 D-1997, Rev. 2011 (Aqueous)
Residue, Total — Standard Methods, 2540 B-1997, Rev. 2011 (Aqueous)
PP. Finding: The oven temperature and the amount of time in the oven are not documented for
the second drying cycle. This is considered pertinent information.
Requirement: Dry evaporated sample for at least 1 h in an oven at 180 ± 2°C, cool in a
desiccator to balance temperature, and weigh. Repeat drying cycle of drying, cooling,
desiccating, and weighing until a constant weight is obtained or until weight change is less
than 4% of previous weight or 0.5 mg, whichever is less. Ref: Standard Methods, 2540 C-
1997. (3) (d).
Requirement: Dry for at least 1 h at 103 to 105°C in an oven, cool in a desiccator to
balance temperature, and weigh. Repeat drying cycle of drying, cooling, desiccating, and
weighing until a constant weight is obtained or until weight change is less than 4% of
previous weight or 0.5 mg, whichever is less. Ref: Standard Methods, 2540 D-1997. (3) (c).
Requirement: Dry evaporated sample for at least 1 h in an oven at 103 to 105°C, cool in a
desiccator to balance temperature, and weigh. Repeat drying cycle of drying, cooling,
desiccating, and weighing until a constant weight is obtained or until weight change is less
than 4% of previous weight or 0.5 mg, whichever is less. Ref: Standard Methods, 2540 B-
1997. (3) (b).
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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).
Comment: In lieu of drying to a constant weight daily, the laboratory may choose to
perform a drying study at least every 12 months. The drying study policy is attached to the
end of this report.
Residue, Dissolved 180 C — Standard Methods, 2540 C-1997, Rev. 2011 (Aqueous)
Residue, Suspended —Standard Methods, 2540 D-1997, Rev. 2011 (Aqueous)
QQ. Finding: The sample is occasionally allowed to filter for more than 10 minutes.
Requirement: If more than 10 min are required to complete filtration, increase filter size or
decrease sample volume. Ref: Standard Methods, 2540 C-1997. (3) (c).
Requirement: If complete filtration takes more than 10 min, increase filter diameter or
decrease sample volume. Ref: Standard Methods, 2540 D-1997. (3) (b).
Comment: The analyst stated that samples were allowed to filter for approximately 15
minutes before re -analyzing a smaller volume.
Residue, Total — Standard Methods, 2540 B-1997, Rev. 2011 (Aqueous)
RR. Finding: Samples are being evaporated in an oven above 100°C.
Requirement: When evaporating in a drying oven, lower temperature to approximately 20C
below boiling to prevent splattering. Ref: Standard Methods, 2540 B-1997. (3) (b).
Comment: The Total Residue and Total Dissolved Solids (TDS) samples are being
evaporated in the 103 to 1050C oven. At the inspection, the laboratory was told that both
Total Residue and Dissolved Residue required the samples to be evaporated below 100°C,
however, it is only specified in the Total Residue method. Despite this, the same issue with
boiling and splatter is likely to occur with TDS samples.
Residue, Suspended —Standard Methods, 2540 D-1997, Rev. 2011 (Aqueous)
SS. Finding: Duplicates are not analyzed at the required frequency.
Requirement: Analyze at least 10% of all samples in duplicate. Ref: Standard Methods,
2540 D-1997. (3) (c).
Comment: On 9/3/2015, one duplicate was analyzed with 20 samples. On 1/5/2016, one
duplicate was analyzed with 14 samples. On 3/7/16, no duplicates were analyzed with 12
samples.
Residue, Dissolved 180 C — Standard Methods, 2540 C-1997, Rev. 2011 (Aqueous)
TT. Finding: The filters are not being washed before use.
Requirement: Preparation of glass -fiber filter disk: If pre -prepared glass fiber filter disks
are used, eliminate this step. Insert disk with wrinkled side up into filtration apparatus. Apply
vacuum and wash disk with three successive 20-mL volumes of reagent -grade water.
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Continue suction to remove all traces of water. Discard washings. Ref: Standard Methods,
2540 C-1997. (3) (a).
Sulfide — Standard Methods, 4500 S2- F-2000, Rev. 2011 (Aqueous)
Comment: The laboratory currently verifies the sample pH at receipt is above 12 Standard Units
(s.u.). 40 CFR Part 136.3 Table II states that it only needs to be preserved to pH >9 s.u., if the
laboratory wishes to change their requirement.
Recommendation: It is recommended that the pH column on the benchsheet be removed if it is
not consistently and correctly used. Since the sample pH is checked upon receipt and recorded
with the Chain of Custody (COC) on the Sample Receiving Summary, the extra documentation is
unnecessary. The benchsheet from 9/9/2015 documented the sample pH as <12 s.u., which would
not sufficiently demonstrate that the pH is >9 s.u. On the 3/22/2016 benchsheet, the pH was not
documented at all.
Temperature — Standard Methods, 2550 B-2000 (Aqueous)
UU. Finding: The laboratory benchsheet was lacking pertinent data: sample analysis time.
Requirement: The following must be documented in indelible ink whenever sample
analysis is performed: Date and time of sample analysis. Ref: NC WW/GW LC Approved
Procedure for the Analysis of Temperature.
Turbidi — Standard Methods, 2130 B-2001, Rev. 2011 (Aqueous)
Turbidi — EPA 180.1, Rev. 2.0, 1993 (Aqueous)
Comment: It is not necessary for the laboratory to check the pH of Turbidity samples.
Recommendation: It is recommended that the analysts be educated on properly filling out the
Turbidity benchsheet in regards to the use of the "meter reading", "dilution", "calculated value" and
"reported value" columns. Data reviewed showed that some analysts record the original meter
reading in the "reported value" column, which gives the impression that the incorrect value is being
reported to the client. In reality, this is the value that is entered into LIMS and it is then calculated in
the system with the dilution factor and reported correctly to the client.
W. Finding: The laboratory is diluting samples over 40 NTU.
Requirement: In order to insure consistency among laboratories, NC WW/GW LC policy is
to avoid dilutions whenever possible. Samples need only be diluted if their concentration
falls outside the allowable calibration range of the meter. Ref: NC WW/GW LC Policy.
Metals — EPA 200.7, Rev. 4.4, 1994 (Aqueous)
Metals — SW-846 6010 D (Aqueous)
Comment: The lab is utilizing Standard Methods, 3030 C for treatment of groundwater compliance
samples. This method is no longer required by any North Carolina permitting authority.
Recommendation: It is recommended that sample dilution and reanalysis be performed through
the dilution test as described in EPA 200.7, Rev. 4.4, 1994, Section 9.5.2, for samples with Matrix
Spike (MS) and Matrix Spike Duplicate (MSD) concentrations above the calibration range.
Metals — EPA 200.8, Rev. 5.4, 1994 (Aqueous)
Metals — SW-846 6020 B (Aqueous)
Mercury — SW-846 7471 B (Non -Aqueous)
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1,2 - Dibromoethane (EDB) — SW-846 8011 (Aqueous)
WW. Finding: The blank acceptance criterion exceeds 50% of the reporting limit or as otherwise
specified by the reference method.
Requirement: For analyses requiring a calibration curve, the concentration of reagent,
method and calibration blanks must not exceed 50% of the reporting limit or as otherwise
specified by the reference method. Ref: NC WW/GW LC Policy.
Requirement: When LRB values constitute 10% or more of the analyte level determined
for a sample or is 2.2 times the analyte MDL whichever is greater, fresh aliquots of the
samples must be prepared and analyzed again for the affected analytes after the source of
contamination has been corrected and acceptable LRB values have been obtained. Ref:
EPA 200.8, Rev. 5.4, 1994, Section 9.3.1.
Comment: For EPA 200.8 and SW-846 6020 B, the laboratory's current blank acceptance
criterion is "<10% of the analyte level or <RL". Our policy states that the laboratory must
either use the method criterion (i.e., <10% of the analyte level or <2.2 times MDL) or our
criterion (i.e., <1/2 RL). The laboratory does not have the option to use <RL as a blank
acceptance criterion by either our policy or the method. For SW-846 7471 B and SW-846
8011, the laboratory's blank criterion is < RL.
Chromium, Hexavalent — SW-846 7196 A (Non -Aqueous)
Recommendation: It is recommended that the analyst not attempt to weigh the sample to exactly
2.50 g. There is an allowance of ± 0.10 g and the actual amount weighed must be documented.
XX. Finding: The laboratory is not analyzing post digestion spikes.
Requirement: A post -digestion Cr(VI) matrix spike must be analyzed per batch as
discussed in Chapter One. The post -digestion matrix spike concentration should be
equivalent to 40 mg/kg or twice the sample concentration observed in the unspiked aliquot
of the test sample, whichever is greater. Ref: EPA SW-846 Test Methods for Evaluating
Solid Waste, Physical/Chemical Methods; 31 Edition, Method 3060 A. Rev. 1, December
1996, Section 8.6.
Comment: A sample that has been spiked pre -digestion is still required.
Chromium, Hexavalent — Standard Methods, 3500 Cr-B-2009 (Aqueous)
Recommendation: The column "pH Adjust" is used to check that the pH has been adjusted to 2 ±
0.5 s.u. It is recommended that the column header be updated to indicate this adjustment.
Pesticides, Organochlorine — SW-846 8081 B (Aqueous and Non -Aqueous)
Polychlorinated Biphenyls — SW-846 8082 A (Aqueous and Non -Aqueous)
YY. Finding: The laboratory is not analyzing matrix spikes or sample duplicates.
Requirement: Unless the referenced method states a greater frequency, spike 5% of
samples on a monthly basis. Laboratories analyzing less than 20 samples per month must
analyze at least one matrix spike each month samples are analyzed. Ref: NC WW/GW LC
Policy.
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Requirement: Analyze five percent of all samples in duplicate to document precision.
Laboratories analyzing less than 20 samples per month must analyze at least one duplicate
each month samples are analyzed. Ref: 15A NCAC 2H .0805 (a) (7) (C).
Comment: The laboratory is analyzing Laboratory Control Sample/Laboratory Control
Sample Duplicate (LCS/LCSD) in place of the matrix spike and matrix spike duplicate or
sample duplicate.
Recommendation: It is recommended that the laboratory supply extra sample bottles
along with instructions to samplers that would ensure enough volume is available to
perform MS and MSD or sample duplicate analyses with each batch.
Polychlorinated Biphenyls — EPA 608 (Aqueous)
Pesticides, Organochlorine — EPA 608 (Aqueous)
ZZ. Finding: The laboratory is not analyzing matrix spikes at the required frequency.
Requirement: The laboratory must, on an ongoing basis, spike and analyze a minimum of
10% of all samples to monitor and evaluate laboratory data quality. Ref: EPA Method 608,
Section 8.1.4.
Comment: Matrix spikes are being analyzed at a 5% frequency.
Purgeable, Organics — EPA 624 (Aqueous)
Purgeable, Organics — SW-846 8260 B (Aqueous)
Purgeable, Organics — Standard Methods, 6200 B-1997 (Aqueous)
Base Neutral/Acid, Organics — EPA 625 (Aqueous)
Base Neutral/Acid, Organics — SW-846 8270 D (Aqueous)
AAA. Finding: The laboratory is not always including both the original and manually integrated
chromatograms, in a similar scale, in the data package when manual integrations are
performed.
Requirement: When manual integration is employed, the laboratory must clearly identify
manually integrated compounds, document the reason the manual integration was
performed, the date performed and who completed the work. A flag or qualifier code may
suffice for simple manual integrations. In addition, a hardcopy printout of the data displaying
the manual integration shall be included in the raw data package (i.e., both the original and
manually integrated chromatograms, of similar scale, must be present in the data package).
All information necessary for the historical reconstruction of data must be maintained by the
lab. Additionally, the laboratory must employ a systematic data validation procedure to
check manual integrations to assure integrations are technically sound and representative
of the response. Ref: NC WW/GW LC Policy.
Comment: Data reviewed shows that hard copies of manually integrated chromatograms
are only printed for calibration curves and analyte hits in samples. Individual analytes in the
calibration curve are not being printed. There was also an instance where the printed
chromatogram was not at the appropriate scale to compare the manual integration with the
original.
1,2 - Dibromoethane (EDB) — EPA 504.1 (Aqueous)
1,2 - Dibromoethane (EDB) — SW-846 8011 (Aqueous)
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Comment: Due to instrument age and the sensitivity at low levels of analysis, a large number of
manual integrations are being performed. Ways in which the analyst should seek to minimize
manual integrations include properly maintaining the instrument, updating retention times, and
optimizing peak integration parameters (e.g., area reject, peak width, threshold, etc.). While the
manual integration data reviewed were consistent and well documented, the number of manual
integrations required could leave the data open to scientific and legal scrutiny.
Recommendation: The laboratory noted that clients rarely submit trip blanks for this method. It is
recommended that project management educate clients on the importance of trip blanks due to the
sensitivity of the method.
BBB. Finding: The laboratory is not following the manual integration SOP.
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: The manual integration SOP states that the supervisor must initial and date the
printout of the manual integration. In practice, the analyst does this and the supervisor
signs the Analysis Review Checklist after reviewing the manual integrations.
IV. PAPER TRAIL INVESTIGATION:
The paper trail consisted of comparing original records (e.g., laboratory benchsheets, logbooks,
etc.) and client reports. Data were reviewed for the following project/sample numbers: 5090184
(SW-846 8270), 6020247 (SM 3500 Cr-B-2009), 6030038 and 5090042 (SW-846 7071 B), 601-103
(SM 2540 C-1997) and 6020458 (SM 5220 D-1997, Hach 8000). No transcription errors were
detected. The facility appears to be doing a good job of accurately transcribing data.
V. CONCLUSIONS:
Correcting the above -cited Findings and implementing the Recommendations will help this
laboratory to produce quality data and meet Certification requirements. The inspector would like to
thank the staff for their assistance during the inspection and data review process. Please respond
to all Findings and include supporting documentation and implementation dates for each
corrective action.
Report prepared by: Beth Swanson Date: June 2, 2016
Report reviewed by: Jason Smith Date: June 9, 2016
TSS, TDS and TS Constant Weight/Drying Time Verification Policy
(NC WW/GW LC Policy 03/09/2009)
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: North Carolina Wastewater/Groundwater Laboratory Certification Policy based
on Standard Methods, 20' Edition, 2540 D. (3) (c), 2540 B. (3) (b), and 2540 C. (3) (d).
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.
1. 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.
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.