HomeMy WebLinkAbout#278_2016_0113_NJ_FINAL
INSPECTION REPORT ROUTING SHEET
To be attached to all inspection reports in-house only.
Laboratory Cert. #: 278
Laboratory Name: South Cary WRF
Inspection Type: Municipal Maintenance
Inspector Name(s): Nick Jones, Dana Satterwhite,
Gary Francies, Todd Crawford,
Beth Swanson and Anna Ostendorff
Inspection Date: January 13, 2016
Date Report Completed: February 11, 2016
Date Forwarded to Reviewer: February 11, 2016
Reviewed by: Beth Swanson
Date Review Completed: 2/12/2016
Cover Letter to use: Insp. Initial Insp. Reg.
Insp. No Finding Insp. CP
Corrected
Unit Supervisor/Chemist III: Todd Crawford
Date Received: February 12, 2016
Date Forwarded to Linda: February 22, 2016
Date Mailed: February 23, 2016
_____________________________________________________________________
PAT MCCRORY
Governor
DONALD R. VAN DER VAART
Secretary
S. JAY ZIMMERMAN
Director
Water Sciences Section
NC Wastewater/Groundwater Laboratory Certification Branch
1623 Mail Service Center, Raleigh, North Carolina 27699-1623
Location: 4405 Reedy Creek Road, Raleigh, North Carolina 27607
Phone: 919-733-3908 \ FAX: 919-733-6241
Internet: http://deq.nc.gov/about/divisions/water-resources/water-resources-data/water-sciences-home-page/laboratory-certification-branch
February 23, 2016
278
Ms. Kelly Spainhour
South Cary WRF
4900 West Lake Road
Apex, NC 27502
Subject: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC)
Maintenance Inspection
Dear Ms. Spainhour:
Enclosed is a report for the inspection performed on January 13, 2016 by Nick Jones, Dana Satterwhite,
Gary Francies, Todd Crawford, Beth Swanson and Anna Ostendorff. Where Finding(s) are cited in this
report, a response is required. Within thirty days of receipt, please supply this office with a written item
for item description of how these Finding(s) were corrected. Please describe the steps taken to prevent
recurrence and include an implementation date for each corrective action. If the Finding(s) cited in the
enclosed report are not corrected, enforcement actions may be recommended. For Certification
maintenance, your laboratory must continue to carry out the requirements set forth in 15A NCAC 2H
.0800.
Copies of the checklists completed during the inspection may be requested from this office. Thank you
for your cooperation during the inspection. If you wish to obtain an electronic copy of this report by email
or if you have questions or need additional information, please contact me at (919) 733-3908 ext. 251.
Sincerely,
Todd Crawford
Technical Assistance & Compliance Specialist
NC WW/GW Laboratory Certification Branch
Attachment
cc: Nick Jones; Master File
On-Site Inspection Report
LABORATORY NAME: South Cary WRF
NPDES PERMIT #: NC0065102
ADDRESS: 4900 West Lake Road
Apex, NC 27502
CERTIFICATE #: 278
DATE OF INSPECTION: January 13, 2016
TYPE OF INSPECTION: Municipal Maintenance
AUDITOR(S): Nick Jones, Dana Satterwhite, Gary
Francies, Todd Crawford, Beth Swanson and
Anna Ostendorff
LOCAL PERSON(S) CONTACTED: Kelly Spainhour and Stephen Avent
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:
Ms. Kelly Spainhour, the laboratory Supervisor, requested this inspection as part of the
laboratory’s internal quality assurance assessment.
During the year leading up to the inspection, the lab worked with the Laboratory
Certification Branch to revise its Standard Operating Procedures (SOPs). The laboratory
has responded quickly to modify and update their operations to new requirements as they
arise.
The facility has all the equipment necessary to perform the analyses. The system for
traceability of standard and reagent preparation is effective, thorough and easy to follow.
Laboratory personnel communicate well with sample collectors and coordinate sample
analyses effectively to manage workload and holding times.
We would like to thank the entire staff for their professionalism.
Proficiency Testing (PT) samples have been analyzed for all certified parameters for the
2015 proficiency testing calendar year and the graded results were 100% acceptable.
The laboratory is reminded that all changes made in response to the Findings,
Recommendations or Comments listed in this report must be incorporated in the Quality
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Assurance (QA)/SOP document(s). The laboratory must ensure the method is being
performed as stated, references to methods are accurate, and the QA and/or SOP
document(s) is/are 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 policies will be implemented.
Contracted analyses are performed by Environment 1, Inc. (Certification #10) and
Environmental Testing Solutions, Inc. (Certification #600).
Approved Procedures for the analysis of the facility’s currently certified Field parameters
were provided to the laboratory before the inspection.
Laboratory Fortified Matrix (LFM) and Laboratory Fortified Matrix Duplicate (LFMD) are
also known a Matrix Spike (MS) and Matrix Spike Duplicate (MSD) and may be used
interchangeably in this report.
III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:
General Laboratory
Recommendation: It is recommended that the laboratory implement a temperature grid
check of all block digesters by alternating the well location of the thermometer each time
samples are digested. This will document heating uniformity and consistency of all
sample wells in the block.
Comment: The sample preservation and storage temperature requirements may be
changed in accordance with 40 CFR Part 136.3 Table II in all pertinent SOPs and in
practice. The current practice is to store “at 4°C”. 40 CFR Part 136.3 Table II allows ≤6°C
for most inorganic parameters and <10°C for bacterial tests, without evidence of freezing.
Quality Control
A. Finding: The laboratory only duplicates effluent samples.
Requirement: Duplicate samples are analyzed randomly to assess precision on an
ongoing basis. Ref: Standard Methods, 1020 B-2011. (8).
B. Finding: The laboratory only spikes effluent samples.
Requirement: To prepare an LFM, add a known concentration of analytes (ideally
from a second source) to a randomly selected routine sample without increasing its
volume by more than 5%. Ref: Standard Methods, 4020 B-2011. (2) (g).
Recommendation: It is recommended that random selection of samples for spiking
be implemented for metals analysis as well.
C. Finding: Improper error correction was observed.
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Requirement: All documentation errors must be corrected by drawing a single
line through the error so that the original entry remains legible. Entries shall not
be obliterated by erasures or markings. Wite-Out®, correction tape or similar
products designed to obliterate documentation are not to be used. Write the
correction adjacent to the error. The correction must be initialed by the
responsible individual and the date of change documented. All data and log
entries must be written in indelible ink. Pencil entries are not acceptable. Ref: NC
WW/GW LC Policy.
Comment: Writing over a number as a means of error correction was observed
on the Biochemical Oxygen Demand (BOD) and Total Suspended Residue
benchsheets.
D. Finding: The laboratory is utilizing a thermometer with a correction factor of >1ºC
from the NIST traceable thermometer.
Requirement: The thermometer/meter readings must be less than or equal to
1ºC from the NIST certified or NIST traceable thermometer reading. Ref: NC
WW/GW LC Policy.
Comment: The thermometer in the Total Suspended Residue oven had a
correction factor of -4°C posted on the thermometer. However, it was actually
+4°C. So, when the oven temperature was adjusted by +4°C, it was adjusted the
wrong direction. This caused the oven to be off by +8°C.
Comment: The +4°C correction factor is most likely due to opening the door
when taking the verification reading. The thermometer was immersed in
vermiculite, not sand or oil, inside the oven, so the temperature fluctuates rapidly
when the door opens.
Recommendation: It is recommended that the laboratory use sand or oil to
immerse the thermometer.
Proficiency Testing
E. Finding: The preparation of Proficiency Testing (PT) samples is not documented.
Requirement: PT samples received as ampules must be diluted according to the
PT provider’s instructions. The preparation of PT samples must be documented in
a traceable log or other traceable format. The diluted PT sample becomes a
routine environmental sample and is added to a routine sample batch for analysis.
Ref: Proficiency Testing Requirements, February 20, 2012, Revision 1.2.
Comment: Dating and initialing the instruction sheet for the preparation of the PT
sample would satisfy the documentation requirement.
F. Finding: The laboratory is not always analyzing Proficiency Testing (PT) samples
in the same manner as environmental samples.
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Requirement: All PT samples are to be analyzed and the results reported in a
manner consistent with the routine analysis and reporting requirements of
compliance samples and any other samples analyzed according to the
requirements of 15A NCAC 2H .0800. Ref: Proficiency Testing Requirements,
February 20, 2012, Revision 1.2.
Comment: The laboratory occasionally analyzed PT samples in duplicate. The
thought was that they would just use the PT sample as the duplicate for the
analytical batch. However, duplicates are to be chosen randomly.
Standard Operating Procedures
Recommendation: It is recommended that the laboratory document the kPa to psi
conversion factor in the Total Phosphorus SOP.
Biochemical Oxygen Demand – Standard Methods, 5210 B-2001
Recommendation: It is recommended that the lab analyze a seeded blank.
Comment: Data in the meter calibration area of the BOD benchsheet did not have units
of measure documented for all values. The time that sample dilutions were completed
was not documented. This is considered pertinent information. The North Carolina
Administrative Code, 15A NCAC 2H .0805 (a) (7) (H) states: All laboratories must use
printed laboratory bench worksheets that include a space to enter the signature or
initials of the analyst, date of analyses, sample identification, volume of sample
analyzed, value from the measurement system, factor and final value to be reported and
each item must be recorded each time samples are analyzed. The date and time BOD
and coliform samples are removed from the incubator must be included on the
laboratory worksheet. Standard Methods 5210 B-2001. (5) (g) states: After preparing
dilution, measure initial DO within 30 min. Documentation of the time that dilutions were
completed and the time sample went into the incubator will bracket the initial DO reading
show compliance with the method requirement. Notification of acceptable corrective
action (i.e., a revised benchsheet which includes: units of measure and the time of
sample dilution completion) was received by email on 2/17/2016 with an implementation
date of 2/25/2016. No further response is necessary for this Finding.
Comment: The laboratory was analyzing four glucose-glutamic acid (GGA) standards.
The laboratory was averaging all four. However, two of them contained 1% seed and
two contained 0.7%. There were not three of one kind available to average. Standard
Methods 5210 B-2001. (6) (b) states: Add sufficient amounts of standard glucose-
glutamic acid solution (¶ 3h) to give 3.0 mg glucose/L and 3.0 mg glutamic acid/L in
each of three test bottles (20 mL GGA solution/L seeded dilution water or 6.0 mL/300-
mL bottle). The resulting average BOD for the three bottles, after correction for dilution
and seeding, must fall into the range of 198 ± 30.5 mg/L. Notification of acceptable
corrective action (i.e., revised benchsheet including three GGA standards prepared the
same) was received by email on 2/17/2016 with an implementation date of 2/17/2016.
No further response is necessary for this Finding.
Comment: The laboratory was not analyzing a duplicate which contained 1.0% seed, as
the sample dilutions contained. A duplicate was analyzed, but contained only 0.7%
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seed. The North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (C) states:
Analyze five percent of all samples in duplicate to document precision. Laboratories
analyzing less than 20 samples per month must analyze at least one duplicate each
month samples are analyzed. Notification of acceptable corrective action (i.e., revised
benchsheet including a duplicate sample seeded the same was received by email on
2/17/2016 with an implementation date of 2/17/2016. No further response is necessary
for this Finding.
Fecal, Coliform – Standard Methods, 9222 D-1997
Comment: The sample filtration time was not recorded on the benchsheet to show that no
more than 30 minutes had passed before filters are placed into the incubator. This is
considered pertinent information. The North Carolina Administrative Code, 15A NCAC 2H
.0805 (a) (7) (A) states: All analytical data pertinent to each certified analysis must be filed
in an orderly manner so as to be readily available for inspection upon request. Standard
Methods, 9222 D-1997. (2) (d) states: Place all prepared cultures in the water bath within
30 min after filtration. Notification of acceptable corrective action (i.e., revised
benchsheets which include filtration time) was received by email on 1/21/2016 with an
implementation date of 2/2/2016. No further response is necessary for this Finding.
Comment: The laboratory was not monitoring the quality of the reagent water used in
fecal coliform analysis. The NC WW/GW LC Policy states: Fecal coliform reagent water
must be analyzed every twelve months to ensure suitability. At a minimum analyses must
be performed for conductivity, TOC, Cd, Cr, Cu, Pb, and Zn. Recommended limits for
reagent water quality are given in Standard Methods 9020 B-2005 Table 9020: II. If these
limits are not met, investigate and correct or change water source. Notification of
acceptable corrective action (i.e., a statement that the fecal coliform reagent water is
being analyzed for conductivity by Dracor each time filter tanks are changed and TOC is
being analyzed by Environment 1, Inc. on an annual basis) was received by email on
2/1/2016 and 2/17/2016 with implementation dates of 2/15/2016 and 2/17/2016,
respectively. No further response is necessary for this Finding.
G. Finding: Consumable materials are not properly tested.
Requirement: At a minimum, make single analyses on five different water samples
positive for the target organism or culture controls of known density. Ref: Standard
Methods, 9020 B-2005. (5) (f) (1) (k) (2) (a).
Requirement: NC WW/GW LC policy requires the testing of the following
consumable materials before they can be used for sample analyses: membrane
filters and/or pads (often packaged together) and media. Ref: NC WW/GW LC
Policy. Please obtain a new lot (or preferably a proven lot from another
laboratory) of media and perform the consumable testing on your current
media and submit the results of this study with your response to this report.
Recommendation: When performing comparisons of old and new lots of
consumables, sample results are not consistently within the acceptable range of 20-
60 colonies. In order to more consistently meet this criterion, it is recommended that
the sample be analyzed at multiple dilutions in order to establish the best volume to
use, and then analyzed for comparison testing at that volume the next day.
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Comment: Consumable testing was being conducted using only 3 positive
samples.
H. Finding: Plate comparison counts are not being conducted.
Requirement: For routine performance evaluation, repeat counts on one or more
positive samples at least monthly, record results, and compare the counts with
those of other analysts testing the same samples. Replicate counts for the same
analyst should agree within 5% (within analyst repeatability of counting) and those
between analysts should agree within 10% (between analysts reproducibility of
counting). If they do not agree, initiate investigation and any necessary corrective
action. Ref: Standard Methods, 9020 B-2005. (9) (a).
I. Finding: The laboratory does not have duplicate acceptance criteria for colony
counts of <20 CFU/100 mL.
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).
Comment: A tiered scale for acceptance criteria is usually required. Low count
acceptance criterion may be established using a colony count difference.
J. Finding: The laboratory is using a partial immersion thermometer in the fecal water
bath improperly.
Requirement: Thermometers with no indicated depth are the total immersion type.
When a partial-immersion thermometer is used, the bottom of the thermometer up
to the immersion line should be exposed to the temperature being measured, with
the remainder of the thermometer exposed to ambient conditions. When a total
immersion thermometer is used, the bulb and the entire portion of the stem
containing liquid, except for the last 1 cm, are exposed to the temperature being
measured. If the thermometer is not used in this manner, the thermometer
immersion is incorrect. Ref: “Selecting Alternatives to Mercury-Filled
Thermometers”, http://www.epa.gov/mercury/alternatives.htm.
Comment: The thermometer was touching the bottom of the bath and not
immersed to the partial immersion line.
Hardness, Total – Standard Methods, 2340 B-1997
K. Finding: The laboratory is referencing an unapproved method on the benchsheets.
Requirement: Laboratory Procedures. Analytical methods, sample preservation,
sample containers and sample holding times shall conform to those requirements
found in 40 CFR-136.3. Ref: 15A NCAC 2H .0805 (a) (1).
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Comment: The benchsheets references SM 18th ed 2340B.
Dissolved, Oxygen – Standard Methods, 4500 O G-2001
L. Finding: The calibration cup has copious biological growth.
Requirement: If the membrane is coated with oxygen consuming (e.g. bacteria) or
oxygen producing organisms (e.g. algae), erroneous readings may occur. Ref: YSI
556 MPS Instrument Manual, Section 11.1.1.3.
Chlorine, Total Residual – Standard Methods, 4500-Cl G-2000
Recommendation: It is recommended that the Total Residual Chlorine annual
calibration sheet be clarified with regard to the blank type. The sheet lists only “blank”,
when it is actually a reagent blank. The laboratory analysis is performed correctly.
Residue, Suspended – Standard Methods, 2540 D-1997
Recommendation: It is recommended that an acceptance criterion for duplicates be split
into two tiers. The method recommends that duplicates agree within 5% of their average
weight. However, low concentration samples may need a separate low-level acceptance
criterion which could be based upon calculated recoveries or a ± mg/L criterion.
M. Finding: The daily drying time is not consistently greater than or equal to the time
used for the initial verification study drying cycle.
Requirement: Constant weights must be documented. The approved methods
require the following: “Repeat the cycle of drying, cooling, desiccating, and
weighing until a constant weight is obtained or until the weight change is less than
4% of the previous weight or 0.5 mg, whichever is less.” In lieu of this, an annual
study documenting the time required to dry representative samples to a constant
weight may be performed. Verify minimum daily drying time is greater than or
equal to the time used for the initial verification study drying cycle. Drying cycles
must be a minimum 1 hour for verification. Ref: NC WW/GW LC Policy.
Comment: 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.
Comment: The initial verification study was for 73 minutes. The daily drying time
is typically 60 minutes.
N. Finding: The benchsheet states the incorrect minimum residue yield.
Requirement: Choose sample volume to yield between 2.5 and 200 mg dried
residue. If volume filtered fails to meet minimum yield, increase sample volume up
to 1 L. Ref: Standard Methods, 2540 D-1997 (3) (b).
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Comment: The benchsheet states residue yield needs to be 1-200 mg.
Residue, Total – Standard Methods, 2540 G-1997
O. Finding: The benchsheet references the incorrect method.
Requirement: Laboratory Procedures. Analytical methods, sample preservation,
sample containers and sample holding times shall conform to those requirements
found in 40 CFR-136.3. Ref: 15A NCAC 2H .0805 (a) (1).
Comment: The benchsheet references SM 2540 B-1997. The laboratory is not
analyzing any aqueous Total Residue samples by SM 2540 B-1997 and only non-
aqueous samples analyzed by SM 2540 G-1997 are documented on the sheet.
P. Finding: The drying time study does not have a start time documented. This is
considered pertinent data.
Requirement: All analytical data pertinent to each certified analysis must be filed
in an orderly manner so as to be readily available for inspection upon request.
Ref: 15A NCAC 2H .0805 (a) (7) (A) states:
Requirement: Constant weights must be documented. The approved methods
require the following: “Repeat the cycle of drying, cooling, desiccating, and
weighing until a constant weight is obtained or until the weight change is less than
4% of the previous weight or 0.5 mg, whichever is less.” In lieu of this, an annual
study documenting the time required to dry representative samples to a constant
weight may be performed. Verify minimum daily drying time is greater than or
equal to the time used for the initial verification study drying cycle. Drying cycles
must be a minimum 1 hour for verification. Ref: NC WW/GW LC Policy.
Comment The most recent annual drying time study was conducted on October
6, 2015.
Phosphorus, Total – Standard Methods, 4500 P E-1999
Nitrate + Nitrite, Nitrogen – Standard Methods, 4500 NO 3 - E-2000
Recommendation: It is recommended that the laboratory not use ± 20% across the
board as the acceptance criterion for back calculated calibration standards. Standard
Methods states that back-calculated and true concentrations should agree within ±10%,
unless different criteria are specified in an individual method. At the lower limit of the
operational range, acceptance criteria are usually wider. Such criteria must be defined in
the laboratory’s QA plan.
Ammonia, Nitrogen – Standard Methods, 4500 NH 3 D-1997
Recommendation: It is recommended that the benchsheet be rearranged to clearly
reflect the sequential order of the analysis. The benchsheet should accurately
demonstrate that the sample results are appropriately bracketed by proper QC.
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Recommendation: It is recommended that the laboratory monitor and calculate matrix
spike recovery even when the parent sample has a value which is less than the reporting
limit. Assume there is no contribution for the sample when calculating the spike %
recovery.
Nitrogen, Total Kjeldahl – Standard Methods, 4500 Norg C-1997 (Standard Methods,
4500 NH3 D-1997)
Q. Finding: A calibration blank is not analyzed at the end of the sample group.
Requirement: Verify calibration by periodically analyzing a calibration standard and
calibration blank during a run—typically, after each batch of ten samples and at the
end of the run. Ref: Standard Methods, 4020 B-2011. (2) (b).
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:
NC WW/GW LC Policy.
R. Finding: Data that does not meet quality control requirements is not qualified on
the Discharge Monitoring Report.
Requirement: When quality control (QC) failures occur, the laboratory must
attempt to determine the source of the problem and must apply corrective action.
If data qualifiers are used to qualify samples not meeting QC requirements, the
data may not be useable for the intended purposes. A notation must be made on
the Discharge Monitoring Report (DMR) form, in the comment section or on a
separate sheet attached to the DMR form, when any required sample quality control
does not meet specified criteria, and another sample cannot be obtained. Ref: NC
WW/GW LC Policy.
Comment: The laboratory was not consistently transcribing data qualifiers from the
contract laboratory reports to the DMR. The following error was noted: On
10/19/2015 the MS/MSD failed established QC criteria. The sample was reported
on the DMR without qualification of QC failure. The same MS/MSD sample was
reanalyzed on 10/22/2015 and passed established QC criteria. However, on
10/22/2015 the MS/MSD was analyzed alone without any other QC or the unspiked
environmental sample. This second analysis of the MS/MSD would not be
indicative of, or applicable to, the analytical conditions on 10/19/2015.
Ammonia, Nitrogen – Standard Methods, 4500 NH 3 D-1997
Nitrogen, Total Kjeldahl – Standard Methods, 4500 Norg C-1997 (Standard Methods,
4500 NH3 D-1997)
Comment: The laboratory uses two drops of 10N NaOH to adjust sample/ standard pH to
>11. If a different volume would need to be added to samples vs. standards, then the
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laboratory would need to use measured volumes in mL or determine the mL equivalent of
a drop in order to adjust the concentration per the calculation in section 5 of the method.
Ammonia, Nitrogen – Standard Methods, 4500 NH 3 D-1997
Nitrate + Nitrite, Nitrogen – Standard Methods, 4500 NO 3 - E-2000
Nitrogen, Total Kjeldahl – Standard Methods, 4500 Norg C-1997 (Standard Methods,
4500 NH3 D-1997)
Phosphorus, Total – Standard Methods, 4500 P E-1999
Comment: The matrix spike stock standard concentration was not documented on the
Spike Sample Identification/Description Document. This is considered pertinent
information. The North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (A)
states: All analytical data pertinent to each certified analysis must be filed in an orderly
manner so as to be readily available for inspection upon request. Notification of
acceptable corrective action (i.e., a revised Spike Sample Identification/Description
Document which includes the matrix spike stock standard concentration) was received
by email on 1/22/2016 with an implementation date of 1/25/2016. No further response
is necessary for this Finding.
S. Finding: The laboratory is not rotating the range of the spike concentrations.
Requirement: Also, rotate the range of spike concentrations to verify performance
at various levels. Ref: Standard Methods, 4020 B-2011. (2) (g).
Metals – EPA Method, 200.8, Rev. 5.4, 1994
Recommendation: It is recommended that the laboratory begin analyzing bottle blanks
since sample bottles are cleaned and reused without an acid rinse.
Comment: Metals samples were not always preserved at <2 s.u. for a minimum of 24
hours before digestion was performed. The Code of Federal Regulations, Title 40, Part
136, Vol. 77, No. 97, May 18, 2012, Table II, footnote 19 states: An aqueous sample may
be collected and shipped without acid preservation. However, acid must be added at least
24 hours before analysis to dissolve any metals that adsorb to the container walls.
Notification of acceptable corrective action (i.e., a statement that metals samples will sit
preserved for at least 24 hours before digestion) was received by email on 1/22//2016 with
an implementation date of 2/2/2016. No further response is necessary for this Finding.
T. Finding: The laboratory is conducting sample digestion at 95°C.
Requirement: The hot plate should be located in a fume hood and previously
adjusted to provide evaporation at a temperature of approximately but no higher
than 85°C. Ref: EPA Method 200.8, Rev. 5.4, (1994), Section 11.2.3.
U. Finding: A calibration blank is not analyzed at the end of the sample group.
Requirement: The calibration blank and calibration verification standard (mid-
range) must be analyzed initially (i.e., prior to sample analysis), after every tenth
sample and at the end of each sample group to check for carry over and
calibration drift. If either fall outside established quality control acceptance criteria,
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corrective action must be taken (e.g., repeating sample determinations since the
last acceptable calibration verification, repeating the initial calibration, etc.). Ref:
NC WW/GW LC Policy.
Comment: The analyst is setting up a calibration blank at the end of each sample
group. The instrument is not recognizing it as an actual blank to be qualitatively and
quantitatively analyzed. It is only recognizing it as an instrument blank for cleaning
purposes.
Recommendation: It is recommended that the final calibration blank be identified
in the software as another environmental sample. Then treat it as a blank for
analysis and QC evaluation.
IV. PAPER TRAIL INVESTIGATION:
The paper trail consisted of comparing original records (e.g., laboratory benchsheets,
logbooks, etc.) and contract laboratory reports to Discharge Monitoring Reports (DMRs)
submitted to the North Carolina Division of Water Resources. Data were reviewed
for South Cary WRF (NPDES permit # NC0065102) for October, November and
December, 2015. No transcription errors were detected. The facility appears to be doing
a good job of accurately transcribing data.
V. CONCLUSIONS:
Correcting the above-cited Findings and implementing the Recommendations will help
this laboratory to produce quality data and meet certification requirements. The
inspector would like to thank the staff for its assistance during the inspection and data
review process. Please respond to all Findings and include an implementation date
for each corrective action.
Report prepared by: Nick Jones Date: February 11, 2016
Report reviewed by: Beth Swanson Date: February 11, 2016