HomeMy WebLinkAbout#222_2017_1012_BS_FINALINSPECTION REPORT ROUTING SHEET
To be attached to all inspection reports in-house only.
Laboratory Cert. #:
222
Laboratory Name:
"Pilot Creek" c/o City of King's Mountain
Inspection Type:
Municipal Maintenance
Inspector Name(s):
Beth Swanson and Jason Smith
Inspection Date:
October 12, 2017
Date Forwarded for Initial
Review:
October 23, 2017
Initial Review by:
Jason Smith
Date Initial Review
Completed:
October 30, 2017
Cover Letter to use:
❑ Insp. Initial
❑Insp. No Finding
❑Corrected
® Insp. Reg
❑Insp. CP
❑Insp. Reg. Delay
Unit Supervisor/Chemist III:
Dana Satterwhite
Date Received:
October 30, 2017
Date Forwarded to Admin.:
November 17, 2017
Date Mailed:
November 17, 2017
Special Mailing Instructions:
Email to wes.bell@ncdenr.gov
November 17, 2017
222
Mr. Jason Davis
"Pilot Creek" c/o City of King's Mountain
P.O. Box 429
Kings Mountain, NC 28086
ROB' COOPER
Governor
MICHAEL S. REGAN
LINDA CULPEPPER
imerim Director
Subject: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC)
Maintenance Inspection
Dear Mr. Davis:
Enclosed is a report for the inspection performed on October 12, 2017 by Beth Swanson. 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.
A copy of the laboratory's Certified Parameter List at the time of the audit is attached. This list will
reflect any changes made during the audit. 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. 202.
Sincerely,
Dana Satterwhite, Environmental Program Supervisor
Division of Water Resources
Attachment
cc: Beth Swanson, Master File #222
On -Site Inspection Report
LABORATORY NAME:
NPDES PERMIT #:
ADDRESS:
CERTIFICATE #:
DATE OF INSPECTION:
TYPE OF INSPECTION:
AUDITOR(S):
LOCAL PERSON(S) CONTACTED:
I. INTRODUCTION:
"Pilot Creek" c/o City of King's Mountain
NCO020737
200 Potts Creek Road
King's Mountain, NC 28086
222
October 12, 2017
Municipal Maintenance
Beth Swanson and Jason Smith
Jason Davis, Richelle Meek, Kathy Moses and Lee Bailey
This laboratory was inspected by representatives 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 is neat and well -organized. The analysts were forthcoming and expressed interest
in the inspection process.
All required Proficiency Testing (PT) Samples have been analyzed and the laboratory has fulfilled
its PT requirements for the 2017 PT Calendar Year.
The laboratory submitted their Quality Assurance (QA) and/or Standard Operating Procedures
(SOP) document(s) in advance of the inspection. These documents were reviewed and editorial
and substantive revision requirements and recommendations were made by this program
outside of this formal report process. Although subsequent revisions were not requested to be
submitted, they must be completed by December 8, 2018.
The laboratory is reminded that any time changes are made to laboratory procedures, the
laboratory must update the QA/SOP document(s) and inform relevant staff. Any changes made
in response to the pre -audit review or to Findings, Recommendations or Comments listed in this
report must be incorporated to insure the method is being performed as stated, references to
methods are accurate, and the QA and/or SOP document(s) is in agreement with each
approved practice, test, analysis, measurement, monitoring procedure or regulatory
requirement being used in the laboratory. In some instances, the laboratory may need to create
an SOP to document how new functions or policies will be implemented.
The laboratory is also reminded that SOPs are intended to describe procedures exactly as they
are to be performed. Use of the word "should" is not appropriate when describing requirements
(e.g., Quality Control (QC) frequency, acceptance criteria, etc.). Evaluate all SOPs for the proper
use of the word "should".
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#222 "Pilot Creek" c/o City of King's Mountain
Requirements that reference 15A NCAC 2H .0805 (a) (7) (A), stating "All analytical data pertinent
to each certified analysis must be filed in an orderly manner so as to be readily available for
inspection upon request", are intended to be a requirement to document information pertinent to
reconstructing final results and demonstrating method compliance. Use of this requirement is not
intended to imply that existing records are not adequately maintained unless the Finding speaks
directly to that.
Contracted analyses are performed by K & W Laboratories (Certification # 559).
Approved Procedure documents for the analysis of the facility's currently certified Field
Parameters were provided at the time of the inspection.
III. FINDINGS REQUIREMENTS COMMENTS AND RECOMMENDATIONS:
Documentation
A. Finding: Laboratory thermometers are not consistently labeled with their respective
correction factors.
Requirement: The thermometer/meter readings must be less than or equal to 1°C 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 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: Temperature corrections of zero are not being documented on the
thermometers.
B. Finding: The weights used to check the balance are not documented to be Class S or
equivalent. This is considered pertinent data.
Requirement: The analytical balance must be checked with one class S, or equivalent,
standard weight each day used and at least three standard weights quarterly. The values
obtained must be recorded in a log and initialed by the analyst. 15A NCAC 2H .0805 (a)
(7) (K)•
Requirement: All analytical data pertinent to each certified analysis must be filed in an
orderly manner so as to be readily available for inspection upon request. Ref: 15 NCAC
2H .0805 (a) (7) (A).
Comment: Per NC WW/GW LC Policy, ASTM Class 1 weights (20 g to 25 kg) and ASTM
Class 2 weights (10 g to 1 mg) are equivalent to the NBS Class S weights specified in 15A
NCAC 2H .0805 (a) (7) (K).
C. Finding: There is no documentation of the weight verification. This is considered pertinent
data.
Requirement: ASTM Class 1 and 2 weights must be verified at least every 5 years. ASTM
Class 1 weights (20 g to 25 kg) and ASTM Class 2 weights (10 g to 1 mg) are equivalent
to the NBS Class S weights specified in 15A NCAC 2H .0805 (a) (7) (K). Ref: INC
WW/GW LC Policy.
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#222 "Pilot Creek" c/o City of King's Mountain
Requirement: All analytical data pertinent to each certified analysis must be filed in an
orderly manner so as to be readily available for inspection upon request. Ref: 15 NCAC
2H .0805 (a) (7) (A).
Comment: The laboratory stated that weights are verified by a balance technician
annually, but the documentation is not maintained.
D. Finding: The laboratory needs to increase the traceability documentation of purchased
materials and reagents, as well as 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: NC WW/GW LC
Policy.
Comment: The laboratory was not maintaining a supply receipt log or including weights or
volumes of reagents in the preparation log. An example of a receipt log was given to the
laboratory during the inspection.
E. Finding: Units of measure are not consistently documented. This is considered pertinent
information.
Requirement: All laboratories must use printed laboratory bench worksheets that include
a space to enter the signature or initials of the analyst, date of analyses, sample
identification, volume of sample analyzed, value from the measurement system, factor and
final value to be reported and each item must be recorded each time samples are
analyzed. Ref: 15A NCAC 2H .0805 (a) (7) (H).
Requirement: 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: The following must be documented in indelible ink whenever sample
analysis is performed: units of measure. Ref: NC WW/GW LC Approved Procedure for
the Analysis of Specific Conductance (Conductivity) and NC WW/GW LC Approved
Procedure for the Analysis of pH.
Comment: Units of measure were not documented in the following places:
• BOD benchsheet columns labeled as follows - Initial DO, 5th day DO, 02, Seed
Correction, Corrected 02 and C12.
Conductivity benchsheet - conductivity obtained value column.
pH calibration log - all pH values
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#222 "Pilot Creek" c/o City of King's Mountain
Proficiency Testing
F. Finding: The laboratory does not have a documented plan for PT procedures.
Requirement: Each laboratory shall develop and maintain a document outlining the
analytical quality control practices used for the parameters included in their certification.
Supporting records shall be maintained as evidence that these practices are being
effectively carried out. Ref: 15A NCAC 2H .0805 (a) (7).
Requirement: Laboratories must have a documented plan (this is usually detailed in the
laboratory's Quality Assurance Manual or may be a separate Standard Operating
Procedure (SOP) of how they intend to cover the applicable program requirements for
Proficiency Testing per their scope of accreditation. This plan shall cover any commercially
available PT Samples and any inter -laboratory organized studies, as applicable. The
laboratory must also be able to explain when PT Sample analysis is not possible for
certain methods and provide a description of what the laboratory is doing in lieu of
Proficiency Testing. This shall be detailed in the plan. The plan must also address the
laboratory's process for submission of PT results and related Corrective Action Reports
(CARs). Ref: Proficiency Testing Requirements, May 31, 2017, Revision 2.0.
Requirement: SOPs must address situations where the instructions from the Accredited
PT Provider for the preparation, analysis or result calculations would constitute a deviation
from the laboratory's routine procedure. Examples of this may include how low-level
samples will be analyzed, including concentration of the sample or adjustment of the
normality of a titrant. These instructions shall be followed when the concentration of a PT
sample falls below the range of their routine analytical method. Instructions shall also be
included in the laboratory's SOP for how high-level samples will be analyzed, including
preparation of multiple dilutions of the sample. These instructions will be followed when the
concentration of a PT falls above the range of their routine analytical method. Ref:
Proficiency Testing Requirements, May 31, 2017, Revision 2.0.
G. Finding: The laboratory is not documenting PT Sample analyses in the same manner as
routine Compliance Samples.
Requirement: As specified in 15 NCAC 2H .0800, in order to meet the minimum
standards for Certification, laboratories must use acceptable analytical methods. The
acceptable methods are those defined or referenced in the current State and federal
regulations for the environmental matrix being tested. All samples, (including PT
Samples) that are, or that may, be used for Certification purposes, must be analyzed using
approved methods only. 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. Laboratories must document any exceptions. All PT Sample analyses must be
recorded in the daily analysis records as for any Compliance Sample. This serves as the
permanent laboratory record. Ref: Proficiency Testing Requirements, May 31, 2017,
Revision 2.0.
Quality Control
Recommendation: The sample storage refrigerator temperature often reaches 6 °C. It is
recommended that the operating temperature be set to a lower temperature to avoid violations in
case of larger variations.
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#222 "Pilot Creek" c/o City of King's Mountain
H. Finding: Data that does not meet all QC requirements is not qualified on the electronic
Discharge Monitoring Report (eDMR).
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 electronic Discharge Monitoring
Report (eDMR) 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: Fecal Coliform duplicates not meeting the acceptance criterion are not
qualified. The laboratory established acceptance limit for Relative Percent Difference
(RPD) of duplicates is 10%, which is often not met and the results are not qualified.
Recommendation: It is recommended that the laboratory increase the RPD above 10 %
for duplicates with plate counts of >_ 20 cfu and establish a criterion of plus or minus a
certain number of colonies for plates with less than 20 colonies. In this case, a criterion for
duplicate plates that are not within the same acceptance range (e.g., 16 and 22 cfu) would
also need to be established.
Comment: Data is not qualified when the average of BOD dilution water blank values are
>0.20 mg/L.
Bacteria — Coliform Fecal — Standard Methods, 9222 D-1997 (MF) (Aqueous)
I. Finding: Consumable materials used for the Fecal Coliform MF method are not properly
tested.
Requirement: Before a new lot of consumable materials are used for the Fecal Coliform
MF method, those materials must be tested and compared to those currently in use to
ensure they are reliable. Consumable materials included in this requirement are:
membrane filters and/or pads (often packaged together) and media. It is recommended
that only one consumable be tested at a time. At a minimum, make single analyses on
five positive samples that will yield 20-60 colonies for both the current lot and the new lot.
There are two options for determining acceptance of results:
Option 1: Follow the acceptance criteria described in Standard Methods 9020 B-2005 5. (�
(2) (a) and (b).
Option 2: Compare the average colony count of each five -sample set and evaluate against
your routine sample duplicate acceptance criterion. Ref: NC WW/GW LC Policy. Please
obtain (i.e., purchase or borrow) a new lot of media and perform the consumable
testing on your current media and submit the results of this study with your
response to this report.
Comment: The laboratory conducts a comparison of the filter and pad packaged together,
but not the media. In addition, the comparison test is not performed per NC WW/GW LC
Policy. Dilutions of 1, 5, 100 and 100 mL are analyzed for the old and new lot. This does
not provide five dilutions of the same volume to compare and the resulting plate counts are
often not within 20-60 colonies.
J. Finding: The Fecal Coliform incubator temperature is not being monitored and recorded
twice daily.
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#222 "Pilot Creek" c/o City of King's Mountain
Requirement: When incubator is in use, monitor and record calibration -corrected
temperature twice daily. Ref: Standard Methods, 9020 B- 2005 (4) (n).
Comment: The incubator temperature is checked and recorded once per day.
K. Finding: The laboratory is not checking and documenting the pH of prepared media. This
is considered pertinent information.
Requirement: All analytical data pertinent to each certified analysis must be filed in an
orderly manner so as to be readily available for inspection upon request. Ref: 15 NCAC
2H .0805 (a) (7) (A).
Requirement: 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: Rehydrate product in 1 L water containing 10 mL 1 % rosolic acid in 0.2 N
NaOH. Heat to near boiling, promptly remove from heat, and cool below 50 'C. If agar is
used, dispense 5- to 7-mL quantities to 50 x 12-mm petri plates and let solidify. Final pH
should be 7.4 ± 0.2. Ref: Standard Methods, 9222 D-1997. (1) (a).
L. Finding: Heat -indicating tape is not used with all materials each sterilizing cycle.
Requirement: Use heat -indicating tape to identify supplies and materials that have been
sterilized. Ref: Standard Methods 9020 B-2005. (4) (h).
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: This is considered pertinent information and documentation must be
maintained.
M. Finding: The laboratory is not checking the autoclave operating temperature weekly with
a minimum/maximum thermometer.
Requirement: Record items sterilized temperature, pressure and time for each run.
Optimally use a recording thermometer. Check operating temperature weekly with a
minimum/maximum thermometer. Ref: Standard Methods, 9020 B-2005. Table 9020:1.
Requirement: Each laboratory requesting certification must contain or be equipped with
the glassware, chemicals, supplies and equipment required to perform all analytical
procedures included in their certification. Ref: 15A NCAC 02H .0805 (a) (6) (H).
Comment: The laboratory does not own a maximum registering thermometer.
N. Finding: The laboratory does not document all required information in the autoclave log.
Requirement: Record items sterilized and sterilization temperature along with total run-
time (exposure to heat), actual time period at sterilization temperature, set and actual
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#222 "Pilot Creek" c/o City of King's Mountain
pressure readings, and initials of responsible person for each cycle. Ref: Standard
Methods 9020 B- 2005. (4) (h).
Comment: The laboratory documents the items sterilized, time the autoclave was started
and set temperature and pressure of the autoclave. In addition to the items listed in the
requirement, autoclave logs must document that the heat -indicating tape was positive and
the temperature of the maximum reading thermometer when used.
O. Finding: The purchased Phosphate Buffer is not documented by the manufacturer or
verified by the laboratory to be pH 7.2 ± 0.5 S.U. This is considered pertinent information.
Requirement: Stock phosphate buffer solution — Adjust to pH 7.2 ± 0.5 with 1 N sodium
hydroxide (NaOH). Ref: Standard Methods, 9050 C-2005. (1) (a) (1).
Requirement: All analytical data pertinent to each certified analysis must be filed in an
orderly manner so as to be readily available for inspection upon request. Ref: 15 NCAC
2H .0805 (a) (7) (A).
Comment: The laboratory may either check the pH of the Phosphate Buffer upon receipt
or obtain a copy of the Certificate of Analysis from the manufacturer.
P. Finding: Fecal bottle sterility is not documented by the manufacturer or verified by the
laboratory. This is considered pertinent information.
Requirement: Minimally test for sterility one sample bottle per batch sterilized in the
laboratory, or at a set percentage such as 1 to 4%. This is performed by adding sterile
dilution/rinse water to the bottle after sterilization and then subsequently analyzing it as a
sample. Document results. If sample bottles or bags are purchased pre -sterilized,
verification of sterilization is not required if the laboratory maintains copies of the
Certificate of Analysis from the vendor. Ref: NC WW/GW LC Policy.
Requirement: All analytical data pertinent to each certified analysis must be filed in an
orderly manner so as to be readily available for inspection upon request. Ref: 15 NCAC
2H .0805 (a) (7) (A).
Comment: Pre -sterilized bottles are purchased but a Certificate of Analysis is not
obtained from the vendor and a sterility test is not performed.
Q. Finding: Culture positive plates are not analyzed with each batch of prepared media.
Requirement: A culture positive must be analyzed with each batch of prepared media and
once per week for purchased ready -to -use media. A sample volume that yields a
countable plate must be analyzed so that individual colonies may be verified to have
proper morphology (i.e. color, shape, size, surface appearance). Ref: NC WW/GW LC
Policy.
R. Finding: Plate comparison counts are not being performed.
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,
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#222 "Pilot Creek" c/o City of King's Mountain
initiate investigation and any necessary corrective action. Ref: Standard Methods, 9020 B-
2005. (9) (a).
Comment: The primary analyst will recount one plate monthly and compare the two
values and any auxiliary analysts will count the same plate twice comparing the two values
and compare the values with the main analyst. If any comparisons do not agree with the
established criteria, retraining may be necessary. All counts must be documented.
BOD — Standard Methods, 5210 B-2001 (Aqueous)
Recommendation: It is recommended that the column labeled "Sample W, which is used to
document seed volume, be renamed to "Seed Volume".
Comment: The column of mercury in the BOD incubator thermometer was separated. North
Carolina Administrative Code, 15A NCAC 02H .0805 (a) (6) (H) states: Each laboratory requesting
certification must contain or be equipped with the following: Glassware, chemicals, supplies, and
equipment required to perform all analytical procedures included in their certification. Acceptable
corrective action (i.e., the broken thermometer was replaced with a properly verified non -mercury
thermometer) was performed by the laboratory and approved by the auditor during the inspection.
No further response is necessary for this Finding.
S. Finding: The seed correction value is not consistently documented. This is considered
pertinent information.
Requirement: All analytical data pertinent to each certified analysis must be filed in an
orderly manner so as to be readily available for inspection upon request. Ref: 15A NCAC
2H .0805 (a) (7) (A).
Comment: The seed correction value is not documented for all seeded samples. Only
dilutions that are used to report a result have the seed correction applied to it, which
makes it appear the other dilutions are not seeded.
T. Finding: The laboratory does not use sodium sulfite to neutralize residual chlorine.
Require: If residual chlorine is present, dechlorinate sample. In some samples chlorine will
dissipate within 1 to 2 h of standing in the light. This dissipation often occurs during
sample transport and handling. For samples in which chlorine residual does not dissipate
in a reasonably short time. Destroy chlorine residual by adding Na2SO3 solution. Ref:
Standard Methods, 5210 B-2001. (4) (b) (2).
Comment: Chlorine neutralization is not needed very often but when needed, the
laboratory uses sodium thiosulfate instead of sodium sulfite. The procedure for
determining the amount of sodium sulfite that must be added to each sample is attached
at the end of this report.
U. Finding: The laboratory is not seeding all disinfected wastes and wastes having pH values
less than 6 or greater than 8 S.U.
Requirement: Some samples (for example, some untreated industrial wastes, disinfected
wastes, high -temperature wastes, wastes having pH values' less than 6 or greater than 8,
or wastes stored more than 6 In after collection) do not contain a sufficient microbial
population. Seed such samples by adding a population of suitable microorganisms. Ref:
Standard Methods, 5210 B-2001. (4) (d).
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#222 "Pilot Creek" c/o City of King's Mountain
Requirement: Check pH; if it is not between 6.0 and 8.0, adjust sample temperature to 20
± 3 °C, then adjust pH to 7.0 to 7.2 using a solution of sulfuric acid or sodium hydroxide of
such strength that the quantity of reagent does not dilute the sample by more than 0.5%.
The pH of dilution water should not be affected by the lowest sample dilution. Always seed
samples that have been pH adjusted. Ref: Standard Methods, 5210 B-2001. (4) (b) (1).
Comment: The laboratory only seeds samples stored more than 6 hours after collection.
To keep the process simpler, it is acceptable to seed all samples, even if they do not fall
into one of the above categories.
V. Finding: Extra nutrient, mineral, and buffer solutions are not added to the 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 (0.30 mL/300-mL bottle) or use commercially -
prepared solutions designed to dose the appropriate bottle size. Ref: Standard Methods,
5210 B-2001. (5) (c) (2).
W. Finding: The Dissolved Oxygen (DO) meter is not properly checked for drift at the end of
the analytical series.
Requirement: If the membrane electrode method is used, take care to eliminate drift in
calibration between initial and final DO readings. Ref: Standard Methods, 5210 B-2001. (5)
(g)•
Requirement: Immediately after calibration, measure the DO of a BOD bottle of dilution
water. Stopper the bottle. Document the concentration on the benchsheet (day one initial
drift check). At the end of the sample set reanalyze the drift check bottle and document the
concentration (day one final drift check). The laboratory should verify the DO Meter
calibration throughout the sample set if needed. Repeat process on Day 5. If the meter
drifts more than 0.20 mg/L, recalibrate meter and reanalyze all samples since the last drift
check. Ref: NC WW/GW LC Policy.
Comment: The laboratory places the DO probe back in the air calibration bottle at the
end of analysis and compares the value to the meter reading obtained immediately after
calibration.
Recommendation: It is recommended that drift be checked throughout the sample run for
larger sets since all bottles must be reanalyzed since calibration (or last acceptable drift
check) if the check is unacceptable.
X. Finding: Multiple dilution water blanks are being analyzed, but not averaged.
Requirement: Multiple dilution water blanks in the same batch using the same dilution
water are to be treated as replicates and averaged. The average of the dilution water
blanks in a batch must not be >0.20 mg/L. Ref: "BOD Multiple Dilution Water Blanks",
Standard Methods Joint Editorial Board memorandum dated August 1, 2014.
Y. Finding: The laboratory reports <2 mg/L without qualification when no 300-mL dilution is
analyzed and no dilution depletes at least 2 mg/L.
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#222 "Pilot Creek" c/o City of King's Mountain
Requirement: The reporting limit for BOD5/CBOD5 is 2 mg/L. Only bottles giving a
minimum Dissolved Oxygen (DO) depletion of 2.0 mg/L and a residual DO of 1.0 mg/L
after 5 days of incubation are considered to produce valid data. It is not acceptable to
elevate the reporting limit and report as less than the value that would have been obtained
if the dilution had depleted the required 2.0 mg/L. It is required that the data be flagged as
a quality control failure if it does not deplete the 2.0 mg/L. The only exception to this is
when a 100% sample does not deplete 2.0 mg/L. In this case, report the value as <2.0
mg/L without qualification. Ref: NC WW/GW LC Policy.
Comment: Instead of reporting samples as
with the most sample is to be reported with
deplete 2 mg/L.
<2 mg/L, the calculated result of the dilution
qualification stating that the sample did not
Recommendation: It is recommended that the laboratory analyze a 100% (i.e., 300 mL)
sample dilution so that qualification of results is not necessary. The largest volume of
sample currently analyzed is usually 250 mL.
Z. Finding: Documentation does not demonstrate that the initial DO is measured within 30
minutes of sample preparation. This is considered pertinent data.
Requirement: After preparing dilution, measure initial DO within 30 min. Ref: Standard
Methods, 5210 B-2001. (5) (g).
Requirement: All analytical data pertinent to each certified analysis must be filed in an
orderly manner so as to be readily available for inspection upon request. Ref: 15 NCAC
2H .0805 (a) (7) (A).
AA. Finding: BOD bottles are not filled to approximately two-thirds full with dilution water or
sample prior to adding seed.
Requirement: Fill each BOD bottle approximately two-thirds full with dilution water. Add
appropriate amounts of seed suspension (¶ d below) and nitrification inhibitor (¶ a below)
to the, individual BOD bottles. Ref: Standard Methods, 5210 B-2001. (5) (c) (2).
Comment: Seed is being added to bottles containing only GGA or small amounts of
sample before adding a sufficient volume of dilution water.
BB. Finding: The laboratory does not decant the supernatant after seed preparation.
Requirement: Decant the supernatant to another clean container (after preparation),
carefully leaving the bran behind. For the remainder of the test, gently stir and pipette
aliquots to BOD bottles from the supernatant. Ref: PolySeed® Manufacturer's Instructions.
Comment: Bran often gets incorporated into the seeding material that is added to BOD
bottles.
CC. Finding: PolySeed® material is used greater than 6 hours after preparation.
Requirement: The PolySeed® solution will remain active for up to 6 hours. If your test
runs over 6 hours, it is necessary to prepare fresh solution. Ref: PolySeed® FAQs. How
long is the prepared PolySeed® good for?
Ref: http:// oiyseed.com/fags/fags poiyseed.h�.
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#222 "Pilot Creek" c/o City of King's Mountain
Comment: The laboratory would use one batch of PolySeed® throughout the week until
the material was gone.
DD. Finding: Glucose and glutamic acid reagents are not dried at 103 °C for 1 hour before
use.
Requirement: Glucose-glutamic acid solution: Dry reagent -grade glucose and reagent -
grade glutamic acid at 103 °C for 1 h. Ref: Standard Methods, 5210 B-2001. (3) (h).
Nitrogen, Ammonia — Standard Methods, 4500 NH3 D-1997 (Aqueous)
Comment: At the time of the inspection, the laboratory was Decertified for this parameter due to
two consecutive unacceptable PT results. The laboratory completed all Recertification
requirements and was Recertified effective October 30, 2017.
Comment: The laboratory does not need to confirm the pH of samples with pH strips after NaOH
addition since it contains color indicator.
EE. Finding: The volume of 10N NaOH added to standards and samples is not documented.
This is considered pertinent information.
Requirement: Add a sufficient volume of 10N NaOH solution (1 mL usually is sufficient) to
raise pH above 11. If the presence of silver or mercury is possible, use NaOH/EDTA
solution in place of NaOH solution. If it is necessary to add more than 1 mL of either
NaOH or NaOH/EDTA solution, note volume used, because it is required for subsequent
calculations. Ref: Standard Methods, 4500 NH3 D-1997. (4) (b).
Requirement: Measurement of samples: Dilute if necessary to bring NH3-N concentration
to within calibration curve range. Place 100 mL sample in 150-mL beaker and follow
procedure in ¶ b above. Record volume of 10N NaOH added. Ref: Standard Methods,
4500 NH3 D-1997. (4) (e).
Requirement: All analytical data pertinent to each certified analysis must be filed in an
orderly manner so as to be readily available for inspection upon request. Ref: 15 NCAC
2H .0805 (a) (7) (A).
Comment: The laboratory's normal procedure is to add 2 mL of the color indicating NaOH
to each standard and sample.
Recommendation: It is recommended that a statement be added to the benchsheet
stating: 2 mL of NaOH added to standards and samples unless otherwise noted.
FF. Finding: The laboratory does not check and then document the pH of samples upon
receipt to verify preservation.
Requirement: A record of date collected, time collected, sample collector, and use of
proper preservatives must be maintained. Each sample must clearly indicate the State of
North Carolina collection site on all record transcriptions. Ref: 15 NCAC 2H .0805 (a) (7)
M.
Requirement: Basic documentation requirements to verify that sample preservation and
hold time requirements are met include: Preservation status; temperature and chemical
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#222 "Pilot Creek" c/o City of King's Mountain
preservative(s) used (i.e., name of preservative, pH<2, pH>9, etc., where pH is not
adequately adjusted document the measured pH). Ref: NC WW/GW LC Policy.
GG. Finding: A calibration blank and calibration verification standard (mid -range) are not
analyzed.
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.
HH. Finding: A method blank is not analyzed.
Requirement: Method blank (MB): Include at least one MB daily or with each batch of 20
or fewer samples, whichever is more frequent. Ref: Standard Methods, 4020 B-2011. (2)
(d).
Requirement: A reagent blank (method blank) consists of reagent water (see section
1080) and all reagents (including preservatives) that normally are in contact with a sample
during the entire analytical procedure. The reagent blank is used to determine whether,
and how much, reagents and the preparative analytical steps contribute to measurement
uncertainty. Ref: Standard Methods, 1020 B-2011. (5).
II. Finding: A laboratory -fortified blank (LFB) is not analyzed.
Requirement: Include at least one LFB daily or per each batch of 20 or fewer samples.
Ref: Standard Methods, 4020 B-2011. (2) (e).
Requirement: A laboratory -fortified blank [laboratory control standard (LCS)] is a reagent
water sample (with associated preservatives) to which a known concentration of the
analyte(s) of interest has been added. An LFB is used to evaluate laboratory performance
and analyte recovery in a blank matrix. Ref: Standard Methods, 1020 B-2011. (6).
Comment: The laboratory analyzed an LFB with the remedial PT in October, but was not
analyzing them with compliance samples prior to Decertification.
JJ. Finding: The laboratory is not evaluating the recoveries of the back -calculated standards.
Requirement: Each laboratory shall develop and maintain a document outlining the
analytical quality control practices used for the parameters included in their certification.
Supporting records shall be maintained as evidence that these practices are being
effectively carried out. Ref: 15A NCAC 2H .0805 (a) (7).
Requirement: The 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. Ref: Standard Methods, 4020 B-2011. (2) (a).
Comment: The standards were back -calculated because it was automatically performed
by the spreadsheet the laboratory is using. They were not evaluating the recoveries
against any acceptance criteria and the data showed that recoveries were not always
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#222 "Pilot Creek" c/o City of King's Mountain
within 10%, which it should be for concentrations above the lower limit of the operational
range.
Residue, Dissolved 180 C — Standard Methods, 2540 C-1997 (Aqueous)
Comment: The laboratory does not analyze Compliance Samples for this parameter. They
analyze mixed liquor for process control.
Residue, Suspended — Standard Methods., 2540 D-1997 (Aqueous)
Comment: It is recommended that QC acceptance criteria be printed on the benchsheet.
KK. Finding: The laboratory does not report results of all tests on the characteristics of the
effluent.
Requirement: The results of all tests on the characteristics of the effluent, including but
not limited to NPDES permit monitoring requirements, shall be reported on the monthly
report forms. Ref: 15A NCAC 213.0506 (b) (3) (J).
Comment: The laboratory analyzes the composite effluent sample as stated in their
permit for reporting purposes. An effluent grab sample, collected at the permitted location,
is also analyzed but not reported.
Recommendation: It is recommended that a grab sample be collected immediately prior
to the last control device. The sample would then be considered process control and not
be required to be reported.
ILL. Finding: The laboratory is not analyzing a volume of sample to yield a minimum of 2.5
mg dried residue.
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).
Comment: Typically, 300 mL of sample is analyzed and the minimum of 2.5 mg is not
consistently obtained.
Comment: The range of measurement for Suspended Residue is determined by the
optimum solids loading on the filter, which can be controlled by adjusting the volume of
sample filtered. The method -defined reporting limit for Suspended Residue is 2.5 mg/L
when filtering 1 L of sample. This sample volume may not be necessary to demonstrate
compliance with regulatory limits; however, it is not acceptable to routinely report less -than
results using a reporting limit greater than 2.5 mg/L. A copy of this report will be shared
with the regional office.
MM. 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
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#222 "Pilot Creek" c/o City of King's Mountain
reported as less than the appropriate value based upon the volume used. Ref: NC
WW/GW LC Policy.
Residue, Dissolved 180 C — Standard Methods, 2540 C-1997 (Aqueous)
Residue, Suspended — Standard Methods, 2540 D-1997 (Aqueous)
NN. Finding: The samples are not weighed to constant weight, nor is an annual multiple
weighing study to verify the adequacy of the drying time, performed.
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.
Chlorine, Total Residual — Standard Methods, 4500 Cl G-2000 (Aqueous)
00. Finding: The annual 5-standard calibration curve verification did not pass the individual
standard recovery criteria.
Requirement: The values obtained must not vary by more than 10% of the known value
for standard concentrations greater than or equal to 50 mg/L and must not vary by more
than 25% of the known value for standard concentrations less than 50 mg/L. The overall
correlation coefficient of the curve must be >_0.995. Ref: NC WW/GW LC Approved
Procedure for the Analysis of Total Residual Chlorine. Please submit a passing curve
verification with the report reply.
Comment: Two different analysts prepared standard concentrations of 15, 50, 200, 500,
1000 and 2000 pg/L and verified the factory curve separately. One curve failed the 15 pg/L
(i.e., 22 pg/L), 200 pg/L (i.e., 150 pg/L) and 500 pg/L (i.e., 446 pg/L) standards. The other
curve failed the 50 pg/L (i.e., 33 mg/L) and 500 pg/L (i.e., 423 pg/L) standards.
Comment: Only one curve verification needs to be performed per year.
Recommendation: It is recommended that the laboratory verify the curve at the following
concentrations: 15, a concentration between 15 and 50, 50, 200 and 400 pg/L.
PP. Finding: The laboratory is not analyzing a reagent blank with prepared standards.
Requirement: Reagent Blank: A reagent blank (sometimes also referred to as a method
blank) is only required when laboratory water is used to make quality control and/or
calibration standards. If you are using a sealed standard (e.g., gel) for your daily check
standard, a reagent blank would only be analyzed when preparing the annual 5-point
calibration curve or 5 annual calibration curve verification standards. Ref: NC WW/GW LC
Approved Procedure for the Analysis of Total Residual Chlorine.
Comment: A reagent blank is made from the same laboratory water source used to make
QC and/or calibration standards with DPD. The concentration of reagent blanks must not
exceed 50% of the reporting limit (i.e., the lowest calibration or calibration verification
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#222 "Pilot Creek" c/o City of King's Mountain
standard concentration), unless otherwise specified by the reference method, or corrective
action must be taken.
Conductivity —Standard Methods, 2510 B-1997 (Aqueous)
QQ. Finding: The laboratory does not calibrate the meter prior to analysis of samples each
day compliance monitoring is performed.
Requirement: Instruments are to be calibrated according to the manufacturer's calibration
procedure prior to analysis of samples each day compliance monitoring is performed. For
most meters, this is a one -point calibration. Ref: NC WW/GW LC Approved Procedure for
the Analysis of Specific Conductance (Conductivity).
Comment: The laboratory checks the conductivity meter with a 100 pmho/cm standard
each day and did not know that the conductivity meter could be calibrated. The
instructions for calibrating the instrument can be found in Section 4.1 Cell Calibration, in
the YSI 3100 instrument manual.
Comment: An additional standard was also checked, but it was the 100 pmho/cm
standard diluted 1:1 and the laboratory thought it was 50 pmho/cm. It was explained that
conductivity standards cannot be diluted in that way. The analyst noted they will
purchase an additional standard.
RR. Finding: The Automatic Temperature Compensator (ATC) check is not being properly
performed.
Requirement: The ATC must be verified prior to initial use and annually (i.e., 12 months)
thereafter at two temperatures by analyzing a standard or sample at 250C (i.e., the
temperature to which conductivity values are reported) and a temperature(s) that brackets
the temperature ranges of the environmental samples routinely analyzed. This may require
the analysis of a third temperature reading that is > 25°C (see #3 below). The manner in
which the ATC is verified may depend upon the meter's capabilities and the
manufacturer's instructions. The following is one option.
1. Pour an adequate amount of conductivity standard or sample into a beaker or
other container and analyze at 25°C. Document the temperature and conductivity
value.
2. Lower the temperature of the standard or sample (e.g., by placing the container in
a refrigerator or ice chest) to less than the lowest anticipated sample temperature
and analyze. Document the temperature and conductivity value.
3. If samples greater than 250C are to be analyzed, perform the following additional
step: Raise the temperature above 250C to greater than the highest anticipated
sample temperature (e.g., by placing the container in a hot water bath) and
analyze. Document the temperature and conductivity value.
As the temperature increases or decreases, the value of the conductivity standard or
sample must be within ±10% of the true value of the standard or ±10% of the value of the
sample at 25°C. If not, corrective action must be taken. Ref: NC WW/GW LC Approved
Procedure for the Analysis of Specific Conductance (Conductivity).
Comment: The laboratory checks a 100 and 1000 pmho/cm standard at one
temperature and the temperature is not documented.
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#222 "Pilot Creek" c/o City of King's Mountain
Dissolved Oxygen — Standard Methods, 4500 O G-2001 (Aqueous)
Comment: The laboratory was analyzing samples and reporting data for DO with a
Luminescence Dissolved Oxygen (LDO) meter without North Carolina
Wastewater/Groundwater Certification. North Carolina Administrative Code, 15A NCAC 2H
.0804 (a) states: Municipal and Industrial Laboratories are required to obtain certification for
parameters which will be reported to the State to comply with State surface water monitoring,
groundwater, and pretreatment Rules. The laboratory stopped using the meter the day of the
inspection and certification for DO by Hach 10360-2011, Rev. 1.2 (LDO) was granted effective
October 20, 2017. No further response is necessary for this Finding.
SS. Finding: Calibration documentation does not include all applicable information.
Requirement: Calibration documentation must include the following, where applicable
to the instrument used and the type of calibration performed: barometric pressure (in
mmHg). Ref: NC WW/GW LC Approved Procedure for the Analysis of Dissolved Oxygen.
Comment: A new meter (i.e., Thermo Orion RDO) had been purchased within the last
month and it uses the temperature and pressure for calibration. Only the temperature is
documented.
pH — Standard Methods, 4500 H+113-2000 (Aqueous)
Recommendation: It is recommended that the check standard acceptance criterion (i.e., ± 0.1
S.U.) be printed on the calibration log.
TT. Finding: Values were reported that exceed the method specified accuracy of 0.1 units.
Requirement: By careful use of a laboratory pH meter with good electrodes, a precision
of ±0.02 unit and an accuracy of ±0.05 unit can be achieved. However, ± 0.1 pH unit
represents the limit of accuracy under normal conditions, especially for measurement of
water and poorly buffered solutions. For this reason, report pH values to the nearest 0.1
PH unit. Ref: Standard Methods, 4500 H+ B-2000. (6).
Recommendation: It is recommended that the laboratory continue to record the result on
the benchsheet to the nearest 0.01 pH unit.
Residue, Settleable — Standard Methods, 2540 F-1997 (Aqueous)
Comment: The laboratory only analyzes process control samples for this parameter.
Comment: Due to the type of sample analyzed, the analyst does not stir at 45 minutes because
they say it will not settle. Since it is a timed test, it is acceptable for some particulates to hang in
suspension. The PT Sample is stirred at 45 minutes.
Comment: The sample volume analyzed is not documented on the benchsheet.
IV. PAPER TRAIL INVESTIGATION:
The paper trail consisted of comparing original records (e.g., laboratory benchsheets, logbooks,
etc.) and contract lab reports to eDMRs submitted to the North Carolina Division of Water
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#222 "Pilot Creek" c/o City of King's Mountain
Resources. Data were reviewed for "Pilot Creek" c/o City of King's Mountain (NPDES permit #
NC0020737) for January, April and August 2017. The following errors were noted:
Date
Parameter
Location
Value on
Benchsheet
Value on DMR
1/3/2017
pH
Downstream
6.38 SU
6.09 SU
1/11/2017
Nitrogen, Ammonia
Effluent
0.31 mg/L
<0.1 mg/L
8/30/2017
Residue, Suspended
Effluent
6.7 mg/L
7 mg/L
To avoid questions of legality, it is recommended that you contact the appropriate Regional Office
for guidance as to whether an amended eDMRs will be required. A copy of this report will be
made available to the Regional Office.
V. CONCLUSIONS:
Correcting the above -cited Findings and implementing the Recommendations will help this
laboratory to produce quality data and meet Certification requirements. The inspector would like to
thank the staff for their assistance during the inspection and data review process. Please
respond to all Findings and include supporting documentation, implementation dates and
steps taken to prevent recurrence for each corrective action.
Report prepared by: Beth Swanson
Report reviewed by: Jason Smith
Date: October 23, 2017
Date: October 30, 2017
Neutralizing Total Residual Chlorine in BOD Samples
It is acceptable to screen samples with DPD powder for the presence of Total Residual Chlorine
(use pillows appropriate for the volume of sample tested). Generally total residual chlorine test
strips are not adequate; however, these may be used for samples where interference with DPD
precludes their use. If DPD yields no pink color, chlorine is absent. Document and proceed to set
sample. If pink color is observed, chlorine is present. In those cases, the titration procedure
outlined below must be used to determine the proper amount of Sodium Sulfite needed to
neutralize chlorine in the sample.
Chemicals:
Sodium Sulfite solution - Dissolve 0.1575 g Na2SO3 in 100 mL distilled water. Prepare
fresh daily.
2. 2% H2SO4 -Add 2 mL concentrated H2SO4 to 100 mL distilled water.
3. Potassium Iodide (KI) solution - Add 10 g KI to 100 mL distilled water. Initially this solution
will be clear, but in a few days it will turn greenish yellow. That's ok.
4. Starch - Commercially available or see SM 4500 O C (2) (d)-2001.
Procedure:
To 100 mL of sample, add approximately 1 mL of 2% H2SO4, 1 mL KI solution, and 1 mL starch.
If the solution remains clear, no chlorine is present. Document this on the bench sheet and
proceed to set up the sample for BOD analysis.
If the solution turns blue, chlorine is present. Add the Sodium Sulfite solution, drop by drop, while
stirring the sample, until the sample is clear again. Count the drops of Sodium Sulfite solution
needed to neutralize the 100-mL sample. Add the relative volume of Sodium Sulfite solution to the
volume of sample needed. For example, if it took 6 drops to neutralize the 100-mL sample volume
and you need 300 mL of sample to set the dilutions you want, add 18 drops of Sodium Sulfite
solution to 300 mL of sample. Document this on the bench sheet. Wait about 15 minutes and
recheck the sample to verify the chlorine has been neutralized. Proceed to set up the sample.
Note: If the blue color returns after a few seconds, do not add more Sodium Sulfite solution.
Recheck with DPD to verify that returning blue color is not caused by chlorine still in sample. If no
chlorine is still present, add amount of Sodium Sulfite solution equivalent to when blue color first
disappears. Adding an excessive amount of Sodium Sulfite solution creates an oxygen demand
and will result in a false high BOD value.
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