HomeMy WebLinkAbout#57 - 10 - 2011 - FINALTo be attached to all inspection reports in-house only.
Laboratory Cert. #.
57
Laboratory Name:
Environmental Inc.
Inspection Type:
Commercial Maintenance
Inspector Name(s):
Jason Smith
Inspection Date:
November 18, 2011
Date Report Completed:
December 20, 2011
Date Forwarded to Reviewer: December 20, 2011
Reviewed by:
Chet Whiting
Date Review Completed:
January 18, 2012
Cover Letter to use: _
Insp. Initial X Insp. Reg. _ Insp. No Finding _ Insp. CP _Corrected
Unit Supervisor:
Gary Francies
Date Received:
1/20/2012
Date Forwarded to Linda:
1/27/2012
Date Mailed:
I
4-NCDENR
NAA
Ir
North Carolina Department of Environment and Natural Resources
Division of Water Quality
Beverly Eaves Perdue
Governor
57
Mr. Anthony Tirona
Environmental, Inc.
P.O. Box 954
Cullowhee, NC 28723
Charles Wakild, P. E.
Director
January 27, 2012
Dee Freeman
Secretary
Subject: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW
LC) Maintenance Inspection
Dear Mr. Tirona:
Enclosed is a report for the inspection performed on November 18, 2011 by Jason Smith. I
apologize for the delay in getting this report to you. Where finding(s) are cited in this report, a
response is required. Within thirty days of receipt, please supply this office with a written item for
item description of how these finding(s) were corrected. If the finding(s) cited in the enclosed
report are not corrected, enforcement actions may be recommended. For certification
maintenance, your laboratory must continue to carry out the requirements set forth in 15A
NCAC 2H .0800.
Copies of the checklists completed during the inspection may be requested from this office.
Thank you for your cooperation during the inspection. If you wish to obtain an electronic copy of
this report by email or if you have questions or need additional information, please contact us at
828-296-4677.
Sincerely,
G c?�
Gary Francies
Certification Unit Supervisor
Laboratory Section
Enclosure
cc: master file
DENR DWQ Laboratory Section NC Wastewater/Groundwater Laboratory Certification Branch
1623 Mail Service Center, Raleigh, North Carolina 27699-1623
Location: 4405 Reedy Creek Road. Raleigh, North Carolina 27607-6445
Phone: 919-733-3908 \ FAX: 919-733-6241
Internet: www.dwglab.org
One
N6fthCarohna
Naturally
An Equal opportunity \ Affirmative Action Employer
LABORATORY NAME:
F_10101
CERTIFICATE #:
TYPE OF INSPECTION:
AUDITOR(S):
I. INTRODUCTION:
I -6•
Environmental, Inc.
P.O. Box 954
Cullowhee, NC 28723
57
November 18, 2011
Commercial Maintenance
Jason Smith
Anthony Tirona and Steve Graham
This laboratory was inspected to verify its compliance with the requirements of 15A NCAC 2H .0800 for
the analysis of environmental samples.
II. GENERAL COMMENTS:
The facility is neat and well organized and has all the equipment necessary to perform the analyses.
Laboratory personnel communicate well with sample collectors and coordinate sample analyses
effectively to manage workload and holding times. Findings A, B, C, D, E, H, I, K, L, M, N, O, P, Q, R, and
S are new policies that have been implemented by our program since the last inspection.
A. Finding: The laboratory is not calibrating the mechanical volumetric liquid -dispensing devices.
Requirement: Mechanical volumetric liquid -dispensing devices (e.g., fixed and adjustable auto-
pipettors, bottle -top dispensers, etc.) must be calibrated at least twice per year, approximately
six months apart. Each liquid -dispensing device must meet the manufacturer's statement of
accuracy. For variable volume devices used at more than one setting, check the accuracy at
the maximum, middle and minimum values. Testing at more than three volumes is optional.
When a device capable of variable settings is dedicated to dispense a single specific volume,
calibration is required at that setting only. Ref: North Carolina Wastewater/Groundwater
Laboratory Certification Policy.
Recommendation: It is recommended that the laboratory document the date that the Standard
Operating Procedures (SOPs) are reviewed.
Recommendation: Most benchsheets include a place for the analyst to circle yes or no for all quality
control criteria being met. This section is rarely completed. It is recommended that the laboratory
consistently complete this section of the benchsheets.
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#57 Environmental, Inc.
B. Finding: The laboratory needs to increase the documentation of purchased materials and
reagents.
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.
Comment: The laboratory has a good system of traceability in place; however, the date put in use
needs to be documented when it is not the same as the date opened. For example, fecal coliform
consumables are opened in order to perform comparison tests, but not put into use for sample
analysis until a later date.
C. Finding: The laboratory needs to increase the documentation of standards and reagents
prepared 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.
D. Finding: Error corrections are not dated.
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: North Carolina Wastewater/
Groundwater Laboratory Certification Policy.
Settleable Solids — Standard Methods, 18tn Edition, 2540 F
E. Finding: The laboratory is not documenting the agitation of the sample after 45 minutes.
Requirement: Settle for 45 min, gently agitate sample near the sides of the cone with a rod or by
spinning, settle for 15 min longer. Ref: Standard Methods, 18th Edition, 2540 F. (3) (a).
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#57 Environmental, Inc.
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).
Fecal Coliform — Standard Methods, 18th Edition, 9222 D
Comment: The laboratory has not been checking the operating temperature weekly with a maximum
holding thermometer in the autoclave. Standard Methods, 18th Edition, 9020 B. (2) (i) states: Autoclave:
Check operating temperature weekly with a minimum/maximum thermometer. This procedure was
implemented on November 17, 2011, prior to the inspection. No further response is necessary for
this finding.
F. Finding: The laboratory has not established acceptance criteria for duplicates and consumable
comparison testing.
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).
Requirement: When samples have measurable levels of the constituent being determined,
analyses of duplicate samples is effective for assessing precision. See table 1020 1: for
acceptable limits for duplicate analysis. Ref: Standard Methods, 18th Edition, 1020 B (6).
Comment: Other sound acceptable procedures for establishing duplicate acceptance criteria may
be used.
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• • - • •II-Em . • I M - • • a 11 • 1 k
Requirement: Excluding Oil and Grease, all residue parameters, leachate extractions, residual
chlorine, and coliform, analyze one known standard in addition to calibration standards each
day samples are analyzed to document accuracy. Analyze one suspended residue, one
dissolved residue, one residual chlorine and one oil and grease standard quarterly. For residual
chlorine, all calibration standards required by the approved procedure in use and by EPA must
be analyzed. Ref: 15A NCAC 2H .0805 (a) (7) (B).
Comment: Only one standard (the Proficiency Testing sample) was analyzed in the last year.
IF
.. • - : •1 r
H. 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
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#57 Environmental, Inc.
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).
I. 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).
Comment: 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.
StandardAmmonia Nitrogen — ..
J. Finding: Samples are not being distilled prior to analysis and no distillation study is on file.
Requirement: The titration method requires all samples to be distilled. For all other methods,
manual distillation is not required if comparability data on representative effluent samples are
on file to show that this preliminary distillation step is not necessary; however, manual
distillation will be required to resolve any controversies. In the case of low concentration
effluents, the samples must be spiked to allow for a meaningful statistical comparison. It is
recommended that samples with a concentration < 1.0 mg/L be spiked to yield a value in the 1 -
5 mg/L range. Comparisons performed in this concentration range should check within 20%
RPD. Additional samples must be analyzed comparatively if the results do not indicate
approximately the same values for distilled and undistilled samples. It is recommended that
both the distilled and undistilled portions of the sample be analyzed by the same laboratory
using the same methodology. The following frequencies are required:
Commercial Laboratories shall analyze initially at least six samples distilled and undistilled, but
at least two samples from all waste types. Analyze one sample distilled and undistilled yearly
from all wastes types. Ref: North Carolina Wastewater/Groundwater Laboratory Certification
(NC WW/GW LC) Policy, 01/15/2009; based upon Code of Federal Regulations, Title 40, Part
136; Federal Register Vol. 72, No. 47, March 12, 2007: Table 1 B Footnote 6.
Requirement: Since it has been more than a year since the last distillation study was performed,
the laboratory is required to perform a distillation study on six samples. Please submit the
distillation studies by June 1, 2012.
K. Finding: The volume of 10N NaOH added is not documented.
Requirement: Record volume of 10N NaOH added in excess of 1 mL. The volume of 10N
NaOH used is a part of the calculation to determine the concentration of NH3-N. Ref: Standard
Methods, 18th Edition, 4500 NH3 F. (4) (e) and (5).
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#57 Environmental, Inc.
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 laboratory is currently adding 2 mL of color indicating Ammonia pH Adjusting
ISA, per manufacturer's instructions, to all samples standards and blanks. Therefore, the
calculation of the final result has been correct for samples. This documentation requirement can
be fulfilled by adding the following statement to the benchsheet: "Unless otherwise noted, 2 mL
of Ammonia pH Adjusting ISA added to all samples, standards, and blanks".
L. Finding: After the addition of the 10 N NaOH, the pH is verified to be greater than 11 with
Ammonia pH Adjusting ISA; however, the elevated pH is not documented.
Requirement: Supporting records shall be maintained as evidence that these practices are being
effectively carried out. Ref: 15A NCAC 2H .0805 (a) (7).
M. Finding: The laboratory is not analyzing matrix spikes.
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. Prepare the matrix spike from a
reference source different from that used for calibration unless otherwise stated in the method.
If matrix spike results are out of control, the results must be qualified or the laboratory must
take corrective action to rectify the effect, use another method, or employ the method of
standard additions. When the method of choice specifies matrix spike performance acceptance
criteria for accuracy, and the laboratory chooses to develop statistically valid, laboratory -specific
limits, the laboratory -generated limits cannot be less stringent than the criteria stated in the
approved method. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy.
Recommendation: If the duplicate sample value is near or below the reporting limit, it is
recommended that a Matrix Spike Duplicate (MSD) be analyzed. The MSD fulfills the duplicate
required by 15A NCAC 2H .0805 (a) (7) (C). This would result in better statistical results to
monitor method and analyst precision.
N. Finding: A calibration verification standard (mid -range) is not analyzed.
Requirement: The calibration blank and calibration verification standard (mid -range) must be
analyzed initially (i.e., prior to sample analysis), after everyy 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, 20`h 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. The laboratory was analyzing a mid -range second source standard at the frequency
required for the calibration verification standard. The second source standard does not have to
be at mid -range and is only required to be analyzed once each day samples are analyzed.
O. Finding: A calibration blank is not analyzed after every tenth sample.
Requirement: See Finding M.
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#57 Environmental, Inc.
Biochemical Oxygen Demand — Standard Methods, 18th Edition, 5210 B
P. Finding: The final Dissolved Oxygen (DO) is not always analyzed after 5 days ± 6 hours.
Requirement: After 5 d ± 6 h of incubation, determine DO in all sample dilutions, and in all blanks
and checks. North Carolina Wastewater/Groundwater Laboratory Certification Policy based upon
Standard Methods, 21 st Edition, 5210 B. (5) (h) and (i).
Comment: Samples are always read out after five days, but occasionally the ± 6 hour portion of
the requirement is not met.
Q. Finding: The laboratory is not documenting that the blank meets the required acceptance
criterion.
Requirement: With each batch of samples incubate one or more bottles of dilution water that
contains nutrient, mineral, and buffer solutions but no seed or nitrification inhibitor. This dilution
water blank serves as a check on quality of unseeded dilution water and cleanliness of incubation
bottles. The DO uptake in 5 d must not be more than 0.20 mg/L and preferably not more than
0.10 mg/L, before making seed corrections. Ref: North Carolina Wastewater/Groundwater
Laboratory Certification Policy based upon Standard Methods, 21st Edition, 5210 B. (6) (c).
Requirement: Identify results in the test reports when any of the following quality control
parameters are not met: The dilution water blank is greater than 0.20 mg/L. Ref: North Carolina
Wastewater/Groundwater Laboratory Certification policy based upon Standard Methods, 21st
Edition, 5210 B. (7) (b).
Comment: In order to show that the blank is :50.20 mg/L the results must be read to two decimal
places.
R. Finding: The laboratory is not averaging the Glucose — Glutamic Acid (GGA) standard results in
order to determine if the required quality control criterion is met.
Requirement: Identify results in the test reports when any of the following quality control
parameters are not met: The GGA check falls outside the acceptance limits [i.e., 198 g/L ± 30.5
mg/L (167.5 — 228.5 mg/L) or 164 ± 30.7 mg/L (133.3 — 194.7 mg/L) for CBOD]. When multiple
GGA standards are analyzed, the average of those results must be within the acceptable limits.
Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy based upon
Standard Methods, 21st Edition, 5210 B. (7) (b).
S. Finding: Extra nutrient, mineral, and buffer solutions are not added to the Biochemical Oxygen
Demand (BOD) bottles containing more than 67% (i.e., > 201 ml-) sample.
Requirement: When a bottle contains more than 67% of the sample after dilution, nutrients
may be limited in the diluted sample and, subsequently, reduce biological activity. In such
samples, add the nutrient, mineral, and buffer solutions (3a through e) directly to individual
BOD bottles at a rate of 1 mL/L (0.33 mU300-mL bottle) or use commercially -prepared
solutions designed to dose the appropriate bottle size. Ref: North Carolina
Wastewater/Groundwater Laboratory Certification Policy based upon Standard Methods, 20th
Edition, 5210 B. (4) (f) and Standard Methods, 21st Edition, 5210 B. (5) (c) (2).
Comment: Dilution water prepared as normal with nutrient, mineral, and buffer solutions would
still be used in the BOD bottles. For the bottles containing more than 67% sample, extra
nutrient, mineral, and buffer solutions would be added in addition to the dilution water.
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#57 Environmental, Inc.
Recommendation: Rather than pipetting 0.33 mL of each reagent into the BOD bottle, it is
recommended that commercially prepared nutrient buffer pillows for 300 mL bottles be used.
T. Finding: The laboratory only considers the DO depletion of the sample, rather than sample and
seed correction, to determine if it meets the minimum depletion of 2.0 mg/L.
Requirement: Only bottles, including seed controls, giving a minimum DO depletion of 2.0 mg/L
and a residual DO of at least 1.0 mg/L after 5 d of incubation are considered to produce valid
data. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy based upon
Standard Methods, 21st Edition, 5210 B. (6) (a).
U. Finding: The laboratory elevates the reporting limit when samples do not meet the 2.0 mg/L DO
depletion requirement.
Requirement: North Carolina Wastewater/Groundwater Laboratory Certification Policy prohibits
raising the (PQL) reporting limit because the "use 2 rule" was not met. Instead the value
obtained is reported and flagged. This policy is designed to prevent labs from artificially raising
the PQL by setting "too low" dilutions and not demonstrating permit compliance. Ref: BOD
Sample Calculations and Reporting document.
The paper trail consisted of comparing laboratory benchsheets to client reports. Data were reviewed
for Sapphire Valley WWTP (NPDES permit #NC0022985) for October, 2011. No transcription errors
were detected. The facility appears to be doing a good job of accurately transcribing data.
VANNNROUTOTs�
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: Jason Smith
Report reviewed by: Chet Whiting
Date: December 20, 2011
Date: January 18, 2012