HomeMy WebLinkAbout#67 12-Final
INSPECTION REPORT ROUTING SHEET
To be attached to all inspection reports in-house only.
Laboratory Cert. #: #67
Inspection Type: Commercial Maintenance
Inspector Name(s): Jeffrey R. Adams
Inspection Date: April 17 & 18, 2012
Date Report Completed: June 5, 2012
Date Forwarded to Reviewer: June 5, 2012
Reviewed by: Jason Smith
Date Review Completed: June 8, 2012
Cover Letter to use: Insp. Initial X Insp. Reg. Insp. No Finding Insp. CP ___ Corrected
Unit Supervisor: Dana Satterwhite
Date Received: June 14, 2012
Date Forwarded to Linda Chavis July 3, 2012
Date Mailed: July 3, 2012
_____________________________________________________________________
On-Site Inspection Report
LABORATORY NAME: Tritest, Inc.
ADDRESS: P.O. Box 33190
Raleigh, NC 27636-3190
CERTIFICATE #: 67
DATE OF INSPECTION: April 17 & 18, 2012
TYPE OF INSPECTION: Commercial Maintenance
AUDITOR(S): Jeffrey Adams, Gary Francies, Dana Satterwhite, Todd Crawford,
Chet Whiting and Nick Jones
LOCAL PERSON(S) CONTACTED: William Sherman, Sarah Caldwell, Gary Folk, Ashley Taylor, and
Matt Loftis
I. INTRODUCTION:
This laboratory was inspected to verify its compliance with the requirements of 15A NCAC 2H .0800 for
the analysis of environmental samples.
II. GENERAL COMMENTS:
The laboratory was clean and well organized. The facility has all the equipment necessary to perform the
analyses. After a review of the laboratory’s Standard Operating Procedures (SOPs), it appears they do
not always accurately reflect the analytical procedures and/or the reference methods that are being
employed in the laboratory. The development and use of SOPs are an integral part of a successful
quality system as they provide individuals with the information to perform a job properly, minimize
variation and promote quality through consistent implementation of a process or procedure within the
organization. SOPs can indicate compliance with organizational and governmental requirements and
can be used as a part of a personnel training program. It minimizes opportunities for
miscommunication and can address safety concerns. When historical data are being evaluated for
current use, SOPs can also be valuable for reconstructing analytical activities when no other
references are available. SOPs are needed even when published methods are being utilized.
The laboratory is 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.
The requirements associated with Findings B and C are new policies that have been implemented by our
program since the last inspection.
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III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:
General
A. Finding: Laboratory benchsheets lacked critical and/or accurate information. Observations are
listed below.
The Color benchsheet lists EPA Method 110.2. This method is no longer an EPA
approved method for Clean Water Act (CWA) compliance monitoring. The laboratory is
currently certified for Standard Methods, 20th Edition, 2120 B.
The Total Solids and Total Dissolved Solids benchsheets list the residue weight gain
criteria as “10 – 200 mg”. The reference methods specify 2.5 – 200 mg.
The Total Solids benchsheet references Standard Methods, 2540 B and 2540 G, 18th
Edition. The laboratory indicated that the 20th Edition of Standard Methods is referenced
for all residue methods.
The pH benchsheet lists SW -846 Method 9045 C as the reference method. The
laboratory is certified for SW -846 Method 9045 D.
The laboratory is not documenting the initial and final volumes used for Fluoride
distillation. (This information may be recorded on a separate distillation log as long as
traceability is maintained and the five-year record retention schedule is observed.)
The Enterococci benchsheet had no volume, units, or MPN value units.
The Settleable Solids benchsheet lists EPA Method 160.5. This method is no longer an
EPA approved method for NPDES compliance monitoring. The laboratory is currently
certified for Standard Methods, 20th Edition, 2540 F.
The Fecal Coliform benchsheet did not reference the correct methods being used in the
analyses. It referenced Standard Methods 9223.
The Fecal Coliform benchsheet has no units of measure.
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).
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.
The quality control document shall be available for inspection by the State Laboratory. Ref: 15A
NCAC 2H .0805 (a) (7).
Recommendation: It is recommended that the laboratory review all laboratory benchsheets to
ensure they contain accurate and required information.
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Proficiency Testing
B. Finding: The laboratory does not have an Analytical Quality Control Document or Standard
Operating Procedure (SOP) for proficiency testing procedures.
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).
Requirement: Laboratory Standard Operating Procedures (SOPs) must address how low level
samples will be analyzed, including concentration of the sample or adjustment of the normality of
a titrant. These instructions shall be followed when the concentration of a PT sample falls below
the range of their routine analytical method. Instructions shall also be included in the laboratory’s
SOP for how high level samples will be analyzed, including preparation of multiple dilutions of the
sample. These instructions will be followed when the concentration of a PT falls above the range
of their routine analytical method. Ref: Proficiency Testing Requirements, February 20, 2012,
Revision 1.2.
C. 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.
Traceability
D. Finding: The laboratory needs to increase the documentation of materials and reagents used
or purchased for use in the laboratory.
Requirement: All chemicals, reagents, standards and consumables used by the laboratory
must have the following information documented: Date received, Date Opened (in use), Vendor,
Lot Number, and Expiration Date (where specified). A system (e.g., traceable identifiers) must
be in place that links standard/reagent preparation information to analytical batches in which the
solutions are used. Documentation of solution preparation must include the analyst’s initials,
date of preparation, the volume or weight of standard(s) used, the solvent and final volume of
the solution. This information as well as the vendor and/or manufacturer, lot number, and
expiration date must be retained for primary standards, chemicals, reagents, and materials
used for a period of five years. Consumable materials such as pH buffers, lots of pre-made
standards and/or media, solids and bacteria filters, etc. are included in this requirement. Ref:
North Carolina Wastewater/Groundwater Laboratory Certification Policy.
Documentation
Recommendation: It is recommended that all records of preventative maintenance performed on
analytical instrumentation be documented in an individual equipment maintenance log book maintained
by the laboratory. All records of corrective action taken or minor troubleshooting and repair performed
should also be documented in the equipment maintenance log. The records may include the following,
as appropriate:
a. The identity of the item of equipment and its software;
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b. The manufacturer’s name, type identification, and serial number or other unique
identifier;
c. The current location;
d. The dates, results and copies of reports and certificates or all calibrations,
adjustments, acceptance criteria, and the due date of the next calibration.
e The maintenance plan, where appropriate, and maintenance completed date.
f. Documentation of any damage, malfunction, modification, or repair to the equipment.
g. Signature or initials of the person performing the maintenance or troubleshooting.
These records provide an historical reconstruction of the maintenance performed, a reference for
effective troubleshooting in the future, and can also serve as a valuable training tool for new analysts.
Currently, equipment maintenance logs are employed in the organics lab only.
Recommendation: The laboratory is documenting the preservation of samples by noting pH
verifications (e.g., pH<2); however, it is recommended that the laboratory also document the chemical
preservative used (e.g., HCl, conc.) to produce the change in pH. This is recommended for any
chemical preservative or preliminary treatment used (e.g., 0.008% sodium thiosulfate for
dechlorination). For samples collected from sites known to be free of total residual chlorine, the lab
may simply document a statement to that effect.
E. Finding: The laboratory is not notifying the State Lab when samples, which do not meet
sample collection, holding time, or preservation requirements, are received.
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).
Comment: For Total Residual Chlorine, the laboratory is not qualifying data on the client report
or notifying the State Laboratory when sample hold times are exceeded.
F. Finding: Proper preservation (i.e., neutralization of Total Residual Chlorine) of VOC samples
is not verified and documented.
Requirement: Dechlorinating agents used at the time of sampling must be documented to
have been effective upon receipt in the laboratory. A variety of field testing kits are co nsidered
to be adequate for most chlorine checks and a maximum detection limit of 0.5 mg/L is allowed.
Ref: “Required Documentation for Sampling Preservation and Hold Time”, North Carolina
Wastewater/Groundwater Laboratory Certification memorandum dated June 20, 2007.
Requirement: A record of date collected, time collected, sample collector, and use of proper
preservatives must be maintained. Each sample must clearly indicate the State of North
Carolina collection site on all record transcriptions. Ref: 15A NCAC 2H .0805 (a) (7) (M).
Comment: Since samples collected for VOC analysis must be handled in a manner that will
minimize losses due to volatilization, sample preservation cannot be verified upon receipt in the
laboratory. Sample preservation must be verified after analysis or on a separate subsample used
only for the preservation verification.
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G. Finding: The sample temperature at the time of collection is not documented for short
transportation time samples.
Requirement: Samples received for analysis must be verified and documented to have been
properly preserved. The temperature of a temperature blank, or of a representative sample, if
the second choice does not compromise the integrity of the samples, from each cooler must be
recorded upon receipt in the laboratory. Samples are transported from the main lab and
transport is less than two hours from the time of collection. For these samples, temperature at
the time of collection must be compared to temperature upon receipt to document a downward
trend in temperature. When samples are received out of compliance, the lab must inform the
State Lab in writing. Ref: 15A NCAC 2H .0805 (a) (1) and (7) (M) and (N), EPA 40 CFR,
Chapter 1, Part 136, Table II, Required Containers, Preservation Techniques, and Holding Times.
Comment: If the temperature of the sample is documented at collection and the sample arrives
at the lab with a temperature > than 6 degrees C, as long as a downward trend in temperature is
documented the sample is considered in compliance for thermal preservation. No notification of
the State laboratory is required in these situations.
H. Finding: An inconsistency was noted between the Standard Operating Procedure (SOP) and
laboratory practice as follows (observations are listed for each):
The method reference in the SOP is not correct (except where noted in this report,
samples were analyzed and reported by the proper method).
o The BOD SOP references EPA Method 405.1. This method is no longer EPA-
approved for CWA compliance monitoring. The laboratory is certified for
Standard Methods, 20th Edition, 5210 B.
o The Color SOP references EPA Method 110.2. This method is no longer EPA-
approved for CWA compliance monitoring. The laboratory is certified for
Standard Methods, 20th Edition, 2120 B.
o The pH SOP references EPA Method 150.1. This method is no longer EPA-
approved for CWA compliance monitoring. The laboratory is certified for
Standard Methods, 20th Edition, 4500 H+ B.
o The Total Solids SOP references EPA Method 160.3. This method is no longer
EPA-approved for CWA compliance monitoring. The SOP also references
Standard Methods 2540 B, 18th Edition. The laboratory indicated the 20th Edition
of Standard Methods is referenced for all Standard Methods methods.
o The Total Suspended Solids SOP references EPA Method 160.2. This method is
no longer EPA-approved for CWA compliance monitoring. The SOP also
references Standard Methods 2540 D, 18th Edition. The laboratory indicated the
20th Edition of Standard Methods is referenced for all Standard Methods
methods.
o The Total Dissolved Solids SOP references EPA Method 160.1. This method is
no longer EPA-approved for CWA compliance monitoring. The laboratory is
certified for Standard Methods, 20th Edition, 2540 B.
o The Settleable Solids SOP references EPA Method 160.5. This method is no
longer EPA-approved for CWA compliance monitoring. The SOP also references
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SM 2540F, 18th Edition. The laboratory indicated the 20th Edition of Standard
Methods is referenced for all Standard Methods methods.
o The Temperature SOP references EPA Method 170.1. This method is no longer
EPA-approved for CWA compliance monitoring. The laboratory is certified for
Standard Methods, 20th Edition, 2550 B.
o The Total Residual Chlorine SOP references EPA Method 330.5 on their
benchsheets and client reports. This method is no longer EPA-approved for
CWA compliance monitoring. The laboratory is certified for Standard Methods,
20th Edition, 4500 Cl G.
o The Fluoride SOP references EPA Method 340.2. This method is no longer EPA-
approved for CWA compliance monitoring. The SOP also references Standard
Methods, 4500 F- C, 18th Edition. The laboratory indicated the 20th Edition of
Standard Methods is referenced for all Standard Methods methods.
.
The SOP does not describe in detail how the method is performed.
o The Total Dissolved Solids and Total Suspended Solids SOPs do not describe
the total maximum filtration time allowed for samples (i.e., 10 min).
o The Total Dissolved Solids SOP cites incorrect column number references (when
compared to the current laboratory benchsheet) for the weight of dried residue
plus dish (in grams), and the weight of dish (in grams), in the TDS calculation.
o The laboratory was using a BOD blank acceptance criterion of 0.20 mg/L, but the
laboratory’s SOP states 0.2 mg/L.
o The COD SOP does not describe procedures for soluble COD analysis of
process water samples. These samples are filtered at the lab within 48 hours of
collection through a 0.45 micron filter.
o The Total Solids SOP has a typographical error in section 114.6.2.1 which
states, “if the maximum sample volume is used and the minimum residue
requirement hasn’t been achieved, report as >2.5 mg/L”. The method states to
report as <2.5 mg/L based on a 1000 ml sample volume.
o For organic analyses, the SOPs have not been developed and/or updated for all
of the parameters included on the laboratory’s certificate attachment (e.g.,
Organochlorine Pesticides and Purgeable Organics).
o The SOPs for Organochlorine Pesticides and Purgeable Organics do not include
the laboratory’s established control limits for percent recoveries of quality control
standards and surrogates.
Personnel were not following procedures as stated in the Laboratory’s SOP.
o For organic analyses, the analyst is not following the SOP for manual integration.
The laboratory’s SOPs state that a “before” integration and “after” integration
chromatogram must retained for future reference. The before and after
chromatograms are not being retained as required in the laboratory’s SOPs.
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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).
Requirement: The laboratory must have an updated Quality Control/Standard Operating
Procedures document for the parameters included on the certificate attachment by December
31, 2012. A written response is required.
Recommendation: It is recommended that during the SOP review process, all current methods
are compared to the new 40 CFR Methods Update Rule (MUR) published on May 18, 2012 to
make sure the most recently approved method is being used and that all benchsheets are
updated to reflect those changes. It is also recommended that SOPs include a revision history
with relevant dates and a brief description of the change(s) made.
Fluoride – Standard Methods, 20th Edition, 4500 F- C
Recommendation: It is recommended that the laboratory document the slope per mV decade change
for each calibration to demonstrate it meets the manufacturer’s suggested criterion. The laboratory
currently expresses this as a percent. The manufacturer’s optimum operating range is defined in terms
of slope per mV decade.
Acidity – Standard Methods, 20th Edition, 2310 B (4a)
I. Finding: The laboratory is not standardizing the titrants once a month.
Requirement: All certified titrants which are purchased, may be used initially without
standardization. They must be standardized monthly, thereafter, for as long as they are used. If
the normality changes, a new titrant must be purchased or the results must be calculated by a
factor derived from the new adjusted normality. Each titrant must be standardized monthly. Ref:
“Titrant Standardization”, North Carolina Wastewater/Groundwater Laboratory Certification
memorandum dated August 6, 1999.
BOD – Standard Methods, 20th Edition, 5210 B
J. Finding: The meter calibration is not being documented.
Requirement: All analytical data pertinent to each certified analysis must be filed in an orderly
manner so as to be readily available for inspection upon request. Ref: 15A NCAC 2H .0805 (a)
(7) (A).
K. Finding; The meter is not checked for drift during, and at the end of the analytical series.
Requirement: If the membrane electrode method is used, take care to eliminate drift in
calibration between initial and final DO readings. Ref: North Carolina Wastewater/Groundwater
Laboratory Certification Policy based upon Standard Methods, 21st Edition, 5210 B. (5) (g) and
15A NCAC 2H .0805 (a) (7).
L. Finding: The laboratory is not following the method when preparing the Glucose-Glutamic Acid
(GGA) standard.
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Requirement: Dry reagent – grade glucose and reagent-grade glutamic acid at 103 ºC for 1 hr.
Add 150 mg glucose and 150 mg glutamic acid to distilled water and dilute to 1 L. Ref: Standard
Methods, 20th Edition, 5210 (B) 3. h.
Comment: The laboratory is buying a double strength solution of Glucose-Glutamic Acid, i.e. 300
mg glucose and 300 mg Glutamic acid per liter. It is acceptable to use this material, but in order to
meet the requirements of the method, the dosage must be adjusted accordingly. That means 3
mL must be added to the 300 mL bottle. Currently, different dilutions of the GGA are analyzed, 2
mL and 2.5 mL. If the laboratory chooses to analyze a duplicate GGA it must be the same dilution
and the average of the results must meet the method acceptance criteria (198 ± 30.5 mg/L) or the
data must be qualified.
E. Coli – Colilert Method
M. Finding: Process control data is not labeled as such.
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 benchsheet for E. Coli also contains process control data for Total Coliform
analyses. Process control data must either be put on a separate appropriately labeled
benchsheet or clearly identified. Regulatory and process control data must be distinguishable
from each other.
Cyanide – Lachat Method 10-204-00-1-X (Total)
Ammonia Nitrogen – Standard Methods, 20th Edition, 4500 NH3 G
Ammonia Nitrogen – EPA Method 350.1
Total Kjeldahl Nitrogen – EPA Method 351.2
N. Finding: Raw data entries and documentation of quality control sample analyses (i.e.,
calibration verification standards and blanks) are not recorded in chronological order and
maintained so as to enable reconstruction of the analytical sequence.
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).
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., repeating sample
determinations since the last acceptable calibration verification, repeating the initial calibration,
etc.). Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy based upon
Standard Methods, 20th Edition, 1020 B. (10) (c), 3020 B. (2) (b), and 4020 B. (2).
Comment: The calibration verification standards and blanks are recorded on separate
benchsheets. This does not allow for reconstruction of the analytical sequence or
representation of the chronological order or frequency of quality control samples.
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Chloride – Standard Methods, 20th Edition, 4500 Cl E
O. Finding: The laboratory does not have a Standard Operating Procedure (SOP) for manual
integration.
Requirement: Each laboratory must develop a Standard Operating Procedure (SOP),
describing manual integration procedures. Alternatively, the laboratory may include manual
integration procedures in all applicable method SOPs. Ref: North Carolina Wastewater/
Groundwater Laboratory Certification Policy.
Comment: It was observed during the chloride data review, that the analyst was manually
integrating some peaks.
Chemical Oxygen Demand – EPA Method 410.4
P. Finding: Process control data is not labeled as such.
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: Process water samples for soluble COD analysis are not clearly labeled. These
samples are filtered at the lab within 48 hours of collection through a 0.45 micron filter. Process
control data must either be put on a separate sheet or clearly identified. Regulatory and process
control data must be distinguishable from each other.
Nitrate – Nitrite Nitrogen – Standard Methods, 20th Edition, 4500 NO3 F
Nitrate – Nitrite Nitrogen – EPA Method 353.2
Q. Finding: The column efficiency is not documented.
Requirement: Each laboratory shall develop and maintain a document outlining the analytical
quality control practices used for the parameters included in their certification. Supporting records
shall be maintained as evidence that these practices are being effectively carried out. Ref: 15A
NCAC 2H .0805 (a) (7).
Total Solids – Standard Methods, 20th Edition, 2540 B
Total Dissolved Solids – Standard Methods, 20th Edition, 2540 C
Total Suspended Solids – Standard Methods, 20th Edition, 2540 D
R. Finding: The annual drying time study did not adequately verify the minimum daily drying time.
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
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cycles must be a minimum 1 hour for verification. Ref: North Carolina Wastewater/Groundwater
Laboratory Certification Policy based on Standard Methods 20th Edition, 2540 D. (3) (c), 2540 B.
(3) (b), and 2540 C. (3) (d). Repeat the drying time verification studies and submit them
with the response to this report.
Comment: Total Suspended Solids samples were dried for 1.5 hours during the drying time
study performed on 3/6/2012. Total Dissolved Solids samples were dried for 1.5 hours during
the drying time study performed on 4/4/2012. Total Solids samples were dried for 24 hours
during the drying time study performed on 4/4/2012. Laboratory analysts indicated that some
samples are dried for a minimum of 1 hour and the SOPs state 1 hour is the minimum drying
time.
Comment: North Carolina allows for an annual drying study in lieu of the requirement above to
repeat the drying cycle for every sample. A random full set of sam ples should be used for the
drying study. The repeated drying time in the oven should be at least 1 hour long. The time
used for the annual drying study is the minimum time that samples are to be dried until a new
drying study is performed.
S. Finding: The laboratory is not basing the reporting limit on the minimum weight gain required
by the method.
Requirement: The minimum weight gain allowed by any approved method is 2.5 mg. Choose
sample volume to yield between 2.5 and 200 mg dried residue. This establishes a minimum
reporting value of 2.5 mg/L when 1000 mL of sample is analyzed. If complete filtration takes
more than 10 minutes increase filter diameter or decrease sample volume. In instances where
the weight gain is less than the required 2.5 mg, the value must be reported as less than the
appropriate value based upon the volume used. Ref: North Carolina Wastewater/Groundwater
Laboratory Certification Policy based upon Standard Methods, 20th and 21st Editions, 2540 D.
(3) (b) and North Carolina Wastewater/Groundwater Laboratory Certification Policy based upon
Standard Methods, 20th and 21st Editions, 2540 C. (3) (d) and 2540 B. (3) (b).
Comment: Since the publication of the Code of Federal Regulations, Title 40, Part 136; Federal
Register Vol. 72, No. 47, March 12, 2007, there is no longer an approved method that allows for
a 1 mg weight gain. Currently, the minimum weight gain allowed is 2.5 mg. In instances where
the weight gain is less than the required 2.5 mg, the value must be reported as less than the
appropriate value based upon the volume used. For example, if 500 mL of sample is analyzed
and < 2.5 mg of dried residue is obtained, the value reported would be < 5 mg/L. If 100 mL of
sample is analyzed and < 2.5 mg of dried residue is obtained, the value reported would be < 25
mg/L. The laboratory was using reporting all samples as <2.5 mg/L, regardless of volume
analyzed. The laboratory routinely filters 500 mL of sample.
TCLP Organics – SW-846 Method 1311
TCLP Metals – SW-846 Method 1311
Recommendation: In completing the TCLP checklist provided by our program, the laboratory
indicated that the volume of filtrate is not documented. To date, the laboratory has been able to
combine phases so the volume has not been necessary to calculate the final result. The only reference
in the Standard Operating Procedure is the citation from SW -846 Method 1311, 7.2.14. It is
recommended that the laboratory clarify the SOP so that the analyst understands that if the phases are
to be analyzed separately that the volume of the filtrate must be documented in order to complete the
calculation.
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Organochlorine Pesticides & PCBs – EPA Method 608, SW-846 Method 8081 B
Purgeable Organics – EPA Method 624, SW-846 Method 8260 B
Base Neutral/Acid Organics – EPA Method 625, SW-846 8270 D
T. Finding: The analyst is not clearly calculating and documenting the percent recoveries of the
quality control samples, sample duplicates, matrix spikes and matrix spike duplicates on the
laboratory benchsheets and data summaries.
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).
U. Finding: The laboratory is performing manual integration in an inappropriate manner.
Requirement: Under no circumstances will manual integration be performed solely for the
purpose of meeting quality control criteria, nor is it to be used as a substitute for proper sample
preparation (e.g., cleanup), proper instrument optimization or maintenance on the
chromatographic system. Corrective actions, with regard to the instrumentation for computer
software, must be taken if manual integrations become common for an analysis or an
instrument that normally uses automated peak integration. Ref: North Carolina Wastewater/
Groundwater Laboratory Certification Policy.
Comment: The laboratory appears to be manually integrating far too many analytes in the initial
calibration of the instrument. On the purgeable organics data set of 12-5-2011, 22 analytes were
manually integrated in the initial calibration of the instrument. Manual integration should rarely be
used when analyzing an initial calibration standard. This can indicate a shift in analyte retention
times that may indicate column degradation or poor maintenance of the system, i.e., dirty or leaky
injection septum, etc.
Recommendation: It is recommended that the analyst troubleshoot and determine the need
and cause of the large number of manual integrations and re-establish new analyte retention
times and integration settings so as to properly automatically integrate the peaks of interest.
Purgeable Aromatics – EPA Method 602
Organochlorine Pesticides & PCBs – EPA Method 608, SW-846 Method 8081 B
V. Finding: The instrument printout narrative indicates the wrong detector.
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).
Recommendation: The instrument printout indicates an FID detector is being used when in
actuality the PID detector is being used. It is recommended that the analyst review and update all
instrument software narratives to show the correct detector.
pH – Standard Methods, 20th Edition, 4500 H+ B (field testing)
W. Finding: The laboratory is not analyzing a check buffer after initial calibration.
Requirement: Immerse in a third buffer below pH 10, approximately 3 pH units different from
the second; the reading should be within 0.1 unit for the pH of the third buffer. If meter
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response shows a difference greater than 0.1 pH unit from expected value, look for trouble with
the electrodes or potentiometer. Ref: Standard Methods, 20th Edition, 4500 H+ B. (4) (a).
Comment: The laboratory appears to be analyzing the check buffer throughout the day and at
the end of the analysis day, but not after the initial calibration.
IV. PAPER TRAIL INVESTIGATION:
The paper trail consisted of comparing laboratory benchsheets and client reports. Data were reviewed
for November and December, 2011 and January, 2012. The following error was noted.
On Work Order #1112-00192, for Total Organic Carbon analyses, the client report
stated samples were analyzed on 12/08/11, but the benchsheets stated samples to be
analyzed on 12/07/11.
V. CONCLUSIONS:
Correcting the above-cited findings and implementing the recommendations will help this lab to
produce quality data and meet certification requirements. The inspector would like to thank the staff for
its assistance during the inspection and data review process. Please respond to all findings.
Report prepared by: Jeffrey R. Adams Date: June 5, 2012
Report reviewed by: Jason Smith Date: June 8, 2012