HomeMy WebLinkAbout#604_2012
INSPECTION REPORT ROUTING SHEET
To be attached to all inspection reports in-house only.
Laboratory Cert. #: 604
Laboratory Name: Element One, Inc.
Inspection Type: Commercial Maintenance
Inspector Name(s): Todd Crawford
Inspection Date: September 12, 2012
Date Report Completed: October 15, 2012
Date Forwarded to Reviewer: October 15, 2012
Reviewed by: Nick Jones
Date Review Completed: October 22, 2012
Cover Letter to use: Insp. Initial Insp. Reg.
Insp. No Finding Insp. CP
Corrected
Unit Supervisor: Dana Satterwhite
Date Received: October 22, 2012
Date Forwarded to Linda: November 8, 2012
Date Mailed: November 8, 2012
_____________________________________________________________________
On-Site Inspection Report
LABORATORY NAME: Element One, Inc
ADDRESS: 5022-C Wrightsville Ave.
Wilmington, NC 28403
CERTIFICATE #: 604
DATE OF INSPECTION: September 12, 2012
TYPE OF INSPECTION: Commercial Maintenance
AUDITOR(S): Todd Crawford, Gary Francies, Nick Jones, Dana Satterwhite and
Tonja Springer
LOCAL PERSON(S) CONTACTED: Nick Figueroa, Amber Jennings, Ken Smith, Daphne Woodman,
I. INTRODUCTION:
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:
The laboratory was clean and well organized. The facility has all the equipment necessary to perform the
analyses. A system for traceability of standard and reagent preparation is in place but needs to include
some additional information. Proficiency Testing (PT) samples have been analyzed for all certified
parameters for the 2012 proficiency testing calendar year and the graded results were 100% acceptable.
The laboratory is reminded that any time changes are made to laboratory operations, the laboratory
must update the Quality Assurance (QA)/Standard Operating Procedure (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.
On May 18, 2012, EPA promulgated changes to the list of Clean Water Act (CWA) methods at 40 CFR
Part 136.3. This action, referred to as the Methods Update Rule (MUR) approves new methods, or
changes to existing methods, that affects over 100 EPA methods, Standard Methods, ASTM methods,
and other test procedures in Part 136 of Title 40 of the Code of Federal Regulations (CFR). The rule also
contains a number of clarifications relating to approved methods, sample preservation and holding times,
and method modifications. The final rule may be found at:
http://water.epa.gov/scitech/methods/cwa/update_index.cfm. The North Carolina Wastewater/
Groundwater Laboratory Certification (NC WW/GW LC) program will be asking certified laboratories to
move toward implementation of the new rule with changes fully implemented by the end of 2012. Each
laboratory will need to review the MUR and evaluate its effect on current laboratory practices. These
changes must be made in the laboratory’s Standard Operating Procedures and in Quality Manuals, as
well as any other place where the method is cited, e.g., reports, benchsheets, logs, etc. During this
transition period, inspection reports will refer to the methods employed at the laboratory at the time of the
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inspection, but will reference the requirements in the most recently approved version of the method. Any
difficulties encountered with meeting the requirements of these references by the date due may be
addressed in the written corrective action response.
Contracted analyses are performed by Environmental Chemists, Inc. (Certification #94).
The requirements associated with Findings B, C, D, P, S and T are new policies that have been
implemented by our program since the last inspection.
III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:
Documentation
Comment: The preparation of standards and reagents are documented in a logbook and traceable
identifiers (IDs) are assigned; however, traceable IDs are not used in the raw data to unequivocally link
calibration standards, quality control (QC) standards, spikes, etc. to preparation and analytical batches.
The link is currently being inferred by date.
Recommendation: It is recommended that traceable identifiers (IDs) be used in the raw data to
unequivocally link calibration standards, QC standards, spikes, etc. to the preparation and receipt logs.
Recommendation: Analytical and/or preparation batches sometimes continue onto a second worksheet.
It is recommended that space to document, “page of “, be added to worksheets in order to signal
additional data is associated with the batch and to help link pages together if they were to get separated.
A. Finding: The State Laboratory is not notified when samples are received out of compliance.
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).
Recommendation: The requirement above applies only to regulatory samples. It is
recommended that a space be added to the Chain of Custody (COC) form to document the
applicable regulatory program (e.g., NC Aquifer Protection Section) so that it can be easily
determined whether State notification is required.
B. Finding: The vendor and/or manufacturer is not documented in the chemical/material receipt
logbook.
Requirement: All chemicals, reagents, standards and consumables used by the laboratory
must have the following information documented: Date received, Date Opened (in use), Vendor,
Lot Number, and Expiration Date (where specified). A system (e.g., traceable identifiers) must
be in place that links standard/reagent preparation information to analytical batches in which the
solutions are used. Documentation of solution preparation must include the analyst’s initials,
date of preparation, the volume or weight of standard(s) used, the solvent and final volume of
the solution. This information as well as the vendor and/or manufacturer, lot number, and
expiration date must be retained for primary standards, chemicals, reagents, and materials
used for a period of five years. Consumable materials such as pH buffers, lots of pre-made
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standards and/or media, solids and bacteria filters, etc. are included in this requirement. Ref:
North Carolina Wastewater/Groundwater Laboratory Certification Policy.
C. Finding: There is no language in applicable SOPs that states that laboratory reagent blanks
must not exceed 50% of the reporting limit.
Requirement: For analyses requiring a calibration curve, the concentration of method and
reagent blanks must not exceed 50% of the reporting limit, unless otherwise specified by the
reference method. Ref: North Carolina Wastewater/Groundwater Laboratory Certification
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).
Quality Control
D. Finding: Data that does not meet all quality control requirements is not 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: North Carolina Wastewater/Groundwater
Laboratory Certification Policy based upon Standard Methods, 20th Edition, 1020 B. (14).
Comment: Specific examples include:
TOC blanks exceeding 50% of the reporting limit.
The recovery of the QC standard analyzed on 5/16/12 was outside the stated recovery
acceptance range of ± 10%.
E. Finding: The laboratory does not have an Analytical Quality Control Document or Standard
Operating Procedure (SOP) for the calibration of temperature sensing devices.
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 Analytical Quality Control document must include standard operating procedures.
A standard operating procedure describes the method in such detail that an experienced analyst
unfamiliar with the method can obtain acceptable results and meet documentation requirements.
Standard operating procedures must be developed which describe in detail how a method is
performed in that particular laboratory.
F. Finding: Temperature sensing thermocouple calibrations are not adequately documented.
Requirement: All thermometers and temperature measuring devices must be checked every 12
months against a NIST certified or NIST traceable thermometer and the process documented. To
check a thermometer or the temperature sensor of a meter, read the temperature of the
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thermometer/meter against a NIST certified or NIST traceable thermometer and record the two
temperatures. The calibration must be performed at a temperature that corresponds to the
temperature used by the incubator, refrigerator, freezer, etc. In the case of temperature
measuring devices used to perform variable temperature readings the calibration must be
performed at a temperature range that approximates the range of the samples. The
thermometer/meter readings must be less than or equal to 1ºC from the NIST certified or NIST
traceable thermometer reading. The documentation must include the serial number of the NIST
certified thermometer or NIST traceable thermometer that was used in the comparison. Also
make any corrections to the data and document any correction that applies (even if zero) on both
the thermometer/meter and on a separate sheet to be filed. Ref: NC WW/GW LC Policy.
Requirement: All thermometers must meet National Institute of Standards and Technology
(NIST) specifications for accuracy or be checked, at a minimum annually, against a NIST
traceable thermometer and proper corrections made. Ref: 15A NCAC 02H .0805 (a) (7) (O).
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 02H .0805 (a)
(7) (A).
Requirement: All analytical records must be available for a period of five years. Records, which
are stored only on electronic media, must be maintained and supported in the laboratory by all
hardware and software necessary for immediate data retrieval and review. Ref: 15A NCAC 02H
.0805 (a) (7) (G).
Comment: Nearly all laboratory equipment temperatures are monitored using thermocouples
controlled with a computer. The data, however, is not being consistently stored. No calibration
data could be produced for any of 2010 or 2011. Prior to that, there was data from January, 2008
but then not again until September, 2009. The most recent data was from February, 2012.
G. Finding: The temperatures reported by many of the temperature sensing thermocouples
differed from the National Institute of Standards and Technology (NIST) traceable thermocouple
by more than 1ºC.
Requirement: All thermometers and temperature measuring devices must be checked every 12
months against a NIST certified or NIST traceable thermometer and the process documented. To
check a thermometer or the temperature sensor of a meter, read the temperature of the
thermometer/meter against a NIST certified or NIST traceable thermometer and record the two
temperatures. The calibration must be performed at a temperature that corresponds to the
temperature used by the incubator, refrigerator, freezer, etc. In the case of temperature
measuring devices used to perform variable temperature readings the calibration must be
performed at a temperature range that approximates the range of the samples. The
thermometer/meter readings must be less than or equal to 1ºC from the NIST certified or NIST
traceable thermometer reading. The documentation must include the serial number of the NIST
certified thermometer or NIST traceable thermometer that was used in the comparison. Also
make any corrections to the data and document any correction that applies (even if zero) on both
the thermometer/meter and on a separate sheet to be filed. Ref: NC WW/GW LC Policy.
Comment: Specific examples of thermocouples with correction factors that exceeded 1ºC are:
Water Bath (laude), Water Bath, Oven 2, Oven 3, Furnace, Fluoride 1, Fluoride 2, and COD.
Comment: Special attention must be paid to the manufacturer’s instructions about the placement
and depth to which thermocouple probes are inserted in order to obtain reliable readings. Total
immersion thermometers are designed with scales which indicate the actual temperature when
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the bulb and the entire liquid column are exposed to the temperature being measured. The total
immersion thermometer must be immersed into the medium being measured to within
approximately one-half inch of where the top of the liquid column (the meniscus) resides (ASTM
E-77). Partial immersion thermometers are designed to indicate the actual temperature when a
specified portion of its stem is exposed to the temperature being measured. Partial immersion
thermometers must be immersed to the inscribed immersion line or the prescribed depth (e.g., 76
mm) for correct temperature indication.
Requirement: Send documentation of all thermocouple calibrations. Documentation should
include the serial numbers of both the laboratory thermocouples and the NIST traceable
thermocouple used in the calibration. Also document the placement, the submersion depth of the
thermocouples and the temperature of interest that each thermocouple is monitoring.
H. Finding: The laboratory does not have an Analytical Quality Control Document or Standard
Operating Procedure (SOP) for the calibration of mechanical volumetric liquid-dispensing devices
(e.g., fixed and adjustable auto-pipettors, bottle-top dispensers, etc.).
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: Mechanical pipettes are being calibrated on a quarterly basis. The calibration process
assumes a 1 gram per milliliter water density. The actual water temperature, barometric pressure
and related Z factor are not taken into consideration. A percent difference in the average weight
of five aliquots and the volume setting is calculated. The Quality Assurance officer stated that a ±
3% relative percent difference (RPD) was the acceptance criterion, however, several RPDs of
greater than ± 3% were marked “pass” in the calibration logbook.
Recommendation: It is recommended that the calibration take into account the temperature of
the water and the pressure in the room. The average weight of at least five aliquots should then
be compared to the theoretical weight, determined by use of the Z factor, and have a maximum
percent difference of 2%.
I. Finding: The laboratory does not have an Analytical Quality Control Document or Standard
Operating Procedure (SOP) for manual integration for EPA Method 300.0.
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. 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: North Carolina Wastewater/Groundwater Laboratory Certification Policy.
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Temperature – Standard Methods, 2550 B - 2000
J. Finding: The analyst that performs field testing for temperature stated that the temperature
correction factor, posted on the meter used to measure regulatory temperatures, was not being
applied.
Requirement: All thermometers must meet National Institute of Standards and Technology
(NIST) specifications for accuracy or be checked, at a minimum annually, against a NIST
traceable thermometer and proper corrections made. Ref: 15A NCAC 2H .0805 (a) (7) (O).
Ammonia Nitrogen – Standard Methods, 4500 NH3 D - 1997
Comment: Distillation of samples is no longer required for the electrode method.
K. Finding: The benchsheet had no indication that the pH of the samples was adjusted to above
11 S.U.
Requirement: Add a sufficient volume of 10N NaOH solution to raise the pH above 11. Ref:
Standard Methods, 4500 NH3 D–1997. (4) (b).
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: Since a color indicating Ionic Strength Adjuster (ISA) solution is used, a check box to
indicate that the sample turned blue would be sufficient documentation.
Ammonia Nitrogen – Standard Methods, 4500 NH3 D - 1997
Total Kjeldahl Nitrogen – Standard Methods, 4500 NH3 D - 1997
L. Finding: The volume of 10N NaOH (or ISA solution) is not documented.
Requirement: Record volume of 10N NaOH added. Ref: Standard Methods, 4500 NH3 D-1997.
(4) (e).
Comment: The following formula must be used in the calculation:
mg NH3 – N/L = A x B x (100 + D)
(100 + C)
A= Dilution Factor
B= Concentration of NH3-N/L, mg/L, from calibration curve
C= Volume of 10N NaOH added to the calibration standards, mL
D= Volume of 10N NaOH added to sample, mL
Comment: If the same volume of ISA is added to both standards and samples, then the
volume need not be taken into account in the calculation.
Total Kjeldahl Nitrogen – Standard Methods, 4500 NH3 D - 1997
M. Finding: The laboratory is not documenting the digestion process.
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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).
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 documentation of the digestion process must include all information necessary to
provide adequate traceability of standards and reagents and to provide historical reconstruction of
final calculated sample results, Examples of pertinent information include, initial and final
digestion volumes, reagent lot numbers, traceable identifiers for quality control samples, etc.
Conductivity – Standard Methods, 2510 B - 1997
N. Finding: The meter is not being calibrated each day of analysis.
Requirement: Calibrate instruments and ensure that measurements do not drift. Ref: Standard
Methods, 20th Edition, 2020.
Comment: The meter was not being calibrated because the manufacturer suggested that it was
not necessary. Three check standards were being analyzed each time sample analyses were
performed.
Recommendation: It is recommended that the meter be calibrated each day that analyses are
performed with a standard in the range of 1413 µmhos/cm. The calibration should then checked
by analyzing a second standard at a concentration nearer to that of the samples.
O. Finding: The Automatic Temperature Compensator (ATC) has not been verified.
Requirement: The ATC must be verified annually (i.e., every twelve months) and the process
documented. The ATC must be verified by analyzing a standard at 25 °C (the temperature that
conductivity values are compensated to) and a temperature(s) that brackets the temperature
ranges of the samples to be analyzed. This may require the analysis of a third temperature
reading that is > 25 °C. Ref: North Carolina Wastewater/Groundwater Laboratory Certification
Policy.
Total Phosphorus – Standard Methods, 4500 P E – 1999
MBAS - Standard Methods, 5540 C – 2000
Cyanide – Standard Methods, 4500 CN E – 1999
Ammonia Nitrogen – Standard Methods, 4500 NH3 D - 1997
Total Kjeldahl Nitrogen – Standard Methods, 4500 NH3 D - 1997
COD – HACH Method 8000
P. Finding: A calibration blank and calibration verification standard (mid-range) are not analyzed
at the end of the sample group and/or after every tenth sample.
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
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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 standard is prepared from the calibration stock standard
solution.
Cyanide – Standard Methods, 4500 CN E – 1999
Q. Finding: An inconsistency was noted between the Standard Operating Procedure (SOP) and
laboratory practice as follows:
Personnel were not following procedures as stated in the Laboratory’s SOP.
The SOP is in direct conflict with method and/or regulatory requirements.
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 SOP stated that a calibration blank and calibration verification standard (mid-
range) must be analyzed initially, after every twentieth sample and at the end of each sample
group, however blanks and mid-range standards were only analyzed at the beginning of the
run.
Requirement: Refer to the requirement in Finding O.
R. Finding: The SOP does not include any acceptance criteria for duplicates or spikes or
explanation as to how those criteria are to be derived.
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: Acceptance criteria were stated on the benchsheet.
Residue Suspended – Standard Methods, 2540 D - 1997
S. Finding: Filters are not weighed to constant weight prior to sample analysis, nor is a dry filter
blank analyzed with each set of samples.
Requirement: If pre-prepared filters are not used, the method requires that filters must be
weighed to a constant weight after washing. Repeat cycle of drying, cooling, desiccating, and
weighing until a constant weight is obtained or until weight change is less than 4% of the previous
weighing or 0.5 mg, whichever is less. In lieu of this process, it is acceptable to analyze a single
daily dry filter blank to fulfill the method requirement of drying all filters to a constant weight prior to
analysis. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy based
upon Standard Methods 20th Edition 2540 D. (3) (a).
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Residue Suspended – Standard Methods, 2540 D – 1997
Residue Dissolved – Standard Methods, 2540 C - 1997
Residue Total – Standard Methods, 2540 B - 1997
Comment: Drying cycles are routinely repeated to insure constant dried weight. 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 samples 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.
Residue Total – Standard Methods, 2540 B - 1997
Comment: On 04/16/12, sample #18494 was chosen to be analyzed in duplicate. However, the
sample volumes analyzed were not the same. A true duplicate requires that all the subsampling and
analytical parameters be the same.
Total Organic Carbon – Standard Method, 5310 B – 2000
T. Finding: Laboratory reagent blanks often exceed 50% of the reporting limit.
Requirement: For analyses requiring a calibration curve, the concentration of method and
reagent blanks must not exceed 50% of the reporting limit, unless otherwise specified by the
reference method. Ref: North Carolina Wastewater/Groundwater Laboratory Certification
Policy.
Total Organic Carbon – Standard Method, 5310 B – 2000
COD – HACH Method 8000
U. Finding: The calibration verification standard concentration is not at the mid-range of the
calibration curve.
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 standard is prepared from the calibration stock standard
solution.
Sulfide – Standard Method, 4500 S2- D – 2000
Comment: Samples were being analyzed according to HACH Method 8131, but reported as Standard
Method 4500 S2- D. Hach Method 8131 is an EPA-accepted method; however, the chemistry in this
method is not the same. North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (1) states, in
part, that analytical methods, sample preservation, sample containers and sample holding times shall
conform to those requirements found in 40 CFR-136.3. Demonstration of acceptable corrective action
(i.e., an amendment form requesting to drop Standard Method 4500 S2- D from its Certification and add
HACH Method 8131.) was received on 11/2/12. All results must now be reported as being analyzed by
Hach Method 8131. No further response is necessary for this finding.
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Fecal Coliform – Standard Method, 9222 D – 1997
V. Finding: Bacteria filters not being documented in the receipt log.
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.
W. Finding: Consumable materials used for the Fecal Coliform MF method are not 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), must be made. As
a minimum, make single analyses on five positive samples. Ref: Policy based on Procedure for
Testing Consumable Materials for Biological Testing.
X. Finding: Preparation of bacteria media is not being documented.
Requirement: All chemicals, reagents, standards and consumables used by the laboratory
must have the following information documented: Date received, Date Opened (in use), Vendor,
Lot Number, and Expiration Date (where specified). A system (e.g., traceable identifiers) must
be in place that links standard/reagent preparation information to analytical batches in which the
solutions are used. Documentation of solution preparation must include the analyst’s initials,
date of preparation, the volume or weight of standard(s) used, the solvent and final volume of
the solution. This information as well as the vendor and/or manufacturer, lot number, and
expiration date must be retained for primary standards, chemicals, reagents, and materials
used for a period of five years. 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.
Y. Finding: The buffer pillows used to prepare dilution water do not contain Magnesium Chloride.
Requirement: Add 1.25 ml stock phosphate buffer and 5.0 ml magnesium chloride solution
(81.1 g MgCl2
-6H2O/L reagent-grade water) to 1 L reagent-grade water. Dispense in amounts
that will provide 99 ± 2.0 ml or 9 ± 0.2 ml after autoclaving for 15 minutes. Ref: Standard
Methods, 9050 C-2000. (1) (a).
Comment: Buffer pillows may be purchased but they must contain Magnesium Chloride.
Z. Finding: The time that filtering of samples begins is not documented to demonstrate that
samples are placed in the water bath within 30 minutes.
Requirement: Place all prepared culture in the water bath within 30 min after filtration. Ref:
Standard Methods, 9222 D-1997. (2) (d).
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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).
AA. Finding: There is an inconsistency between the laboratory’s stated policy for total residual
chorine checks and the documented acceptance criterion.
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: 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 considered 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”, Pat Donnelly memorandum
dated June 20, 2007.
Comment: The blanket statement at the bottom of the benchsheet concerning the total residual
chlorine check requirement states that if the chlorine concentration is > 0.2 mg/L, then the
sample is invalid. The column heading for the total residual chlorine check in the body of the
benchsheet says “<0.5”. There were no units associated with the number.
COD – HACH Method 8000
Recommendation: It is recommended that the cell location in which the thermometer is placed be
rotated and documented to demonstrate uniform heating across that block.
AB. Finding: Process control data is not clearly identified when documented together with regulatory
compliance data 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. 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).
AC. Finding: The units of measure for the temperature of the hot-block are not 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. 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).
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Metals – EPA Method 200.8, Rev. 5.4 (1994)
Recommendation: Neither the Dataset Report, nor Sample/Batch Report nor Batch Digestion
Worksheet indicates what method is being followed. It is recommended that all reports and worksheets
reference the method that was followed.
Recommendation: Blank concentrations are documented as being less than the reporting limit,
requiring a review of the raw data to verify that concentrations are less than 50% of the reporting limit
as required by North Carolina Wastewater/Groundwater Laboratory Certification Policy. It is
recommended that actual blank concentrations be documented so that it can be easily seen that the
requirement is being met or that they be documented as less than half the reporting limit (<½RL).
BOD – Standard Method, 5210 B – 2001
AD. Finding: The same sample bottles are dedicated to the same QC in each analytical batch.
Requirement: This dilution water blank serves as a check on quality of unseeded dilution water
and cleanliness of incubation bottles. Ref: Standard Methods, 5210 B-2001. (6) (c).
Requirement: Any time quality control results indicate an analytical problem, the problem must be
resolved and any samples involved must be rerun if the holding time has not expired. Ref: 15A
NCAC 2H .0805 (A) (7) (F).
Comment: There are three “A” labeled bottles that are only used for blanks. Bottles used for
quality control samples (including blanks) must be selected at random.
CBOD – Standard Method, 5210 B – 2001
AE. Finding: A nitrification inhibitor is not being added to the seed control, seeded blank, or GGA.
Requirement: Determine BOD of the seed suspension as for any other sample. For the 300
mg/L mixed primary standard, the average 5-d BOD would be 198 mg/L with a standard deviation
of 30.5 mg/L. Ref: Standard Methods, 5210 B-2001. (6) (d) and (8).
Sulfate – EPA Method 300.0
Fluoride – EPA Method 300.0
Chloride – EPA Method 300.0
Nitrite Nitrogen – EPA Method 300.0
Nitrate Nitrogen – EPA Method 300.0
Recommendation: The digestion log is also used as the IC sample worksheet by recording instrument
values with no units in the column labeled “weight, g”. This is misleading and makes assessing the
data difficult. It is recommended that separate sheets be devised or another column is added to record
instrument values.
Recommendation: Determine Method Detection Limits (MDLs) every 6 months, when a new operator
begins work or whenever there is a significant change in the background or instrument response. Ref:
EPA Method 300.0. Rev. 2.1, (1993), Section 9.2.4.
Sulfate – EPA Method 300.0
AF. Finding: Data was reported by an inaccurate method code.
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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: The client report to TBL indicated that samples were analyzed according to Standard
Method 4500 SO4 D instead of EPA Method 300.0 for the following sample IDs: 201109026CPR,
201109026SSB, 201109019CPR, 201109019SSB, 201109005CPR, and 201109005SSB.
IV. PAPER TRAIL INVESTIGATION:
The paper trail involved a spot check of client reports that should have had qualifiers due to QC failures
that are cited in the body of this report. No other comprehensive paper trail was performed.
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: Todd Crawford Date: October 15, 2012
Report reviewed by: Nick Jones Date: October 19, 2012