#160_2017_0830_JMS_FINAL

INSPECTION REPORT ROUTING SHEET
To be attached to all inspection reports in-house only.
Laboratory Cert. #:
160
Laboratory Name:
Tuckaseigee Water and Sewer Authority
Inspection Type:
Municipal Maintenance
Inspector Name(s):
Jason Smith
Inspection Date:
August 30, 2017
Date Forwarded for Initial
Review:
September 21, 2017
Initial Review by:
Tonja Springer
Date Initial Review
Completed:
September 29, 2017
Cover Letter to use:
❑ Insp. Initial ❑ Insp. Reg
❑Insp. No Finding ❑Insp. CP
❑Corrected ®Insp. Reg. Delay
Unit Supervisor/Chemist III:
Todd Crawford
Date Received:
October 4, 2017
Date Forwarded to Admin.:
October 23, 2017
Date Mailed:
October 23, 2017
Special Mailing Instructions:

Water Resources
ENVIRONMENTAL QUALITY
October 23, 2017
160
Mr. Stan Bryson
Tuckaseigee Water and Sewer Authority
1246 West Main St.
Sylva, NC 28779
ROY COOPER
MICHEAL S. R.E GAN
S. JAY ZIMMERMAN
Subject: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC)
Maintenance Inspection
Dear Mr. Bryson:
Enclosed is a report for the inspection performed on August 30, 2017 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. 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 [phone] ext. 251.
Sincerely,
Todd Crawford
Technical Assistance & Compliance Specialist
NC WW/GW Laboratory Certification Branch
Attachment
cc: Dana Satterwhite, Jason Smith, Master File #160
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: [phone] FAX: [phone]
Internet: httOldeamc.govlabout/division s/water-resou rcestwater-resourees•data/water•sciences•home-pagetiaboratory-certification-branch

LABORATORY NAME:
NPDES PERMIT #:
ADDRESS:
CERTIFICATE #:
DATE OF INSPECTION:
TYPE OF INSPECTION:
AUDITOR(S):
LOCAL PERSON(S) CONTACTED:
INTRODUCTION:
Tuckaseigee Water and Sewer Authority
NC0039578, NC0020214, NC0063321, NCO087602
1871 River Road
Sylva, NC 28779
160
August 30, 2017
Municipal Maintenance
Jason Smith
Stan Bryson, Joyce Hammerly and Sheila Ledford
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 facility is well organized and has all the equipment necessary to perform the analyses.
Benchsheets are well designed, easy to follow and concise. Records are well organized and easy
to retrieve. Staff were forthcoming and seemed eager to adopt necessary changes.
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 September 30, 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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Laboratory Fortified Matrix (LFM) and Laboratory Fortified Matrix Duplicate (LFMD) are also
known as Matrix Spike (MS) and Matrix Spike Duplicate (MSD) and may be used
interchangeably in this report.
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 Pace Analytical Services, LLC - Asheville, NC (Certification
#40).
All required Proficiency Testing (PT) Samples have been analyzed and the laboratory has fulfilled
its PT requirements for the 2017 PT Calendar Year.
III. FINDINGS REQUIREMENTS COMMENTS AND RECOMMENDATIONS:
Documentation
A. Finding: The units of measure are not consistently documented on laboratory worksheets.
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).
Comment: Units of measure were missing on the Whittier Analysis Record, the pH and
Dissolved Oxygen (DO) calibration logs and benchsheets and for pH and Total Residual
Chlorine (TRC) on the chain of custody form.
B. Finding: Error corrections are not properly performed.
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: Error corrections are not dated and some instances of correction fluid were
observed.
C. Finding: The preparation of standards and reagents are not consistently documented in
such a way as to provide traceability from preparation to analysis.
Requirement: 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

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preparation, the volume or weight of standard(s) used, the solvent and final volume of the
solution. Ref: NC WW/GW LC Policy.
Comment: The laboratory does not consistently document the volume or weight of
standard(s) used and final volume of the solution.
D. Finding: The Whittier Analysis Record does not clearly identify the sample
collection/analysis time.
Requirement: Sample identification must be associated with the date and time of sample
collection and analysis. The time elapsed between sampling and analysis must be
documented to determine if hold times are met. Ref: NC WW/GW LC Policy.
Comment: Samples are analyzed immediately upon collection. A footnote may be added
to indicate this or the column labeled "Time" may be updated to "Collection/Analysis Time".
E. Finding: The analyst is not signing or initialing the Whittier Analysis Record.
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).
Quality Control
F. 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: The laboratory stopped qualifying data when they began using the eDMR.
Data qualifiers must be reported in the "Comment' section of the eDMR.
General Laboratory
G. Finding: Temperature corrections of thermometers used in laboratory equipment are not
being properly performed.
Requirement: All thermometers and temperature measuring devices must be checked
every 12 months against a NIST certified or NIST traceable thermometer and the process
documented. To check a thermometer or the temperature sensor of a meter, read the
temperature of the thermometer/meter against a NIST certified or NIST traceable
thermometer and record the two temperatures. The calibration must be performed at a
temperature that corresponds to the temperature used by the incubator, refrigerator,
freezer, etc. In the case of temperature measuring devices used to perform variable
temperature readings the calibration must be performed at a temperature range that
approximates the range of the samples. The thermometer/meter readings must be less

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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 make any corrections to the
data and document any correction that applies (even if zero) on both the
thermometer/meter and on a separate sheet to be filed. (NOTE: Other certified
laboratories may provide assistance in meeting this requirement.) Ref: NC WW/GW LC
Policy.
Requirement: All thermometers must meet National Institute of Standards and
Technology (NIST) specifications for accuracy or be checked, at a minimum annually,
against a NIST traceable thermometer and proper corrections made. Ref: 15A NCAC 2H
.0805 (a) (7) (0).
Comment: The laboratory changes the acceptable temperature range of the incubator,
oven or refrigerator on the log based on the thermometers' temperature correction factors
and records the observed uncorrected temperature. While this results in the instruments
being in the correct temperature range, the documentation on the temperature log lists an
incorrect range based on the correction being applied to the acceptable range rather than
the observed value. The correction is not documented on the log and it must be cross
referenced with the annual thermometer verification to determine if the temperature results
are acceptable. Temperature corrections must be made on each reading and the adjusted
temperature documented. Thermometer correction factors must also be documented on
the thermometer.
H. Finding: Laboratory thermometers are not replaced if the reading is >1 °C different from
the NIST certified thermometer.
Requirement: All thermometers and temperature measuring devices must be checked
every 12 months against a NIST certified or NIST traceable thermometer and the
process documented. The thermometer/meter readings must be less than or equal to 1
°C from the NIST certified or NIST traceable thermometer reading. Ref: NC WW/GW
LC Policy.
I. Finding: The analytical balance weights have not been verified against ASTM standard
weights in the past 5 years.
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: NC
WW/GW LC Policy.
Comment: The weights have not been verified since they were put into use in June 2009.
Comment: Please refer to the attached NC WW/GW LC Policy.
J. Finding: For chemicals/reagents/consumables that do not have an expiration date, the
laboratory has not established a policy for assigning expiration dates.
Requirement: Adherence to manufacturer expiration dates is required. If no expiration
date is given, the laboratory must have a policy for assigning an expiration date. Ref: NC
WW/GW LC Policy.

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K. Finding: SOPs have not been developed for Proficiency Testing Samples or Vector
Attraction Reduction: Option 8.
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.
Chlorine, Total Residual — Standard Methods, 4500 Cl G-2000 (Aqueous)
L. Finding: The reagent blank analyzed when verifying the curve for the Odyssey 2500
meter was unacceptable.
Requirement: The concentration of reagent blanks must not exceed 50% of the reporting
limit (i.e., the lowest calibration or calibration verification standard concentration), unless
otherwise specified by the reference method, or corrective action must be taken. Ref: NC
WW/GW LC Approved Procedure for the Analysis of Total Residual Chlorine. Please
submit a copy of a new curve verification for the Odyssey 2500 with the reply to this
report.
Comment: The reporting limit is 20 pg/L and the value obtained for the blank was 13 pg/L.
Dissolved Oxygen — Standard Methods, 4500 O G-2001 (Aqueous)
M. Finding: The elevation at which the meter is calibrated is not documented.
Requirement: Calibration documentation must include the following, where applicable to
the instrument used and the type of calibration performed: elevation, temperature,
barometric pressure (in mmHg), salinity, slope, or %efficiency. Ref: NC WW/GW LC
Approved Procedure for the Analysis of Dissolved Oxygen.
Dissolved Oxygen — Standard Methods, 4500 O G-2001 (Aqueous)
pH — Standard Methods, 4500 H+ B-2000 (Aqueous)
N. Finding: The laboratory benchsheet was lacking pertinent data: instrument identification.
Requirement: The following must be documented in indelible ink whenever sample
analysis is performed: instrument identification. Ref: NC WW/GW LC Approved Procedure
for the Analysis of Dissolved Oxygen and NC WW/GW LC Approved Procedure for the
Analysis of pH.

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Requirement: All analytical data pertinent to each certified analysis must be filed in an
orderly manner so as to be readily available for inspection upon request. Ref: 15A NCAC
2H .0805 (a) (7) (A).
Comment: The laboratory identifies the TRC meters by model. It is recommended that all
meters be identified by both model and serial number. This will make it possible to
determine when a new meter is put into use if it is replacing the same model.
Chlorine, Total Residual — Standard Methods, 4500 Cl G-2000 (Aqueous)
Dissolved Oxygen — Standard Methods, 4500 O G-2001 (Aqueous)
pH — Standard Methods, 4500 H+ B-2000 (Aqueous)
O. Finding: The laboratory benchsheet was lacking pertinent data: meter calibration time.
Requirement: The following must be documented in indelible ink whenever sample
analysis is performed: meter calibration time. Ref: NC WW/GW LC Approved Procedure
for the Analysis of Total Residual Chlorine, NC WW/GW LC Approved Procedure for the
Analysis of Dissolved Oxygen and NC WW/GW LC Approved Procedure for the Analysis
of pH.
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).
Bacteria — Fecal Coliform — Standard Methods, 9222 D-1997 (Aqueous)
P. Finding: The laboratory is not sterilizing the phosphate buffer and magnesium chloride
solutions.
Requirement: Stock phosphate buffer solution Sterilize by filtration or autoclave. Store
stock solution under refrigerated conditions and discard if turbidity develops. Ref: Standard
Methods, 9050 C-2005. (1) (a) (1).
Requirement: Magnesium chloride stock solution — Sterilize and store stock solution
under refrigerated conditions, discarding if solution becomes turbid. Ref: Standard
Methods, 9050 C-2005. (1) (a) (2).
Q. Finding: The laboratory was not documenting their use of heat -indicating tape. This is
considered pertinent information.
Requirement: Use heat -indicating tape to identify supplies and materials that have been
sterilized. Ref: Standard Methods 9020 B-2005. (4) (h).
Requirement: Each laboratory shall develop and maintain a document outlining the
analytical quality control practices used for the parameters included in their certification.
Supporting records shall be maintained as evidence that these practices are being
effectively carried out. Ref: 15A NCAC 2H .0805 (a) (7).
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).

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R. Finding: The total run-time and actual time period at sterilization temperature of the
autoclave is not documented.
Requirement: Record items sterilized and sterilization temperature along with total run-
time (exposure to heat), actual time period at sterilization temperature, set and actual
pressure readings, and initials of responsible person for each cycle. Ref: Standard
Methods 9020 B- 2005. (4) (h).
S. Finding: Sample bottle sterility is not verified.
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.
T. Finding: The Fecal Coliform incubator bath temperature is not being monitored and
recorded twice daily.
Requirement: When incubator is in use, monitor and record calibration -corrected
temperature twice daily. Ref: Standard Methods, 9020 B - 2005. (4) (n).
U. Finding: The laboratory is not monitoring the quality of the reagent water used in fecal
coliform analysis.
Requirement: At a minimum, reagent water used to prepare buffered dilution/rinse water
or media must be analyzed at least every twelve months for the following parameters:
Specific Conductance, Total Organic Carbon, Cadmium, Chromium, Copper, Nickel, Lead,
and Zinc.
Maximum Acceptable Limits are:
Total Organic Carbon < 1.0 mg/L
Specific Conductance < 2 pmhos/cm
Heavy Metals, single element < 0.05 mg/L
Heavy Metals, Total of cited elements < 0.10 mg/L
If the facility is using vendor purchased dilution/rinse water this testing is not required as
long as the Certificate of Analysis from the manufacturer meets these requirements and is
kept on file. Ref: NC WW/GW LC Policy.
V. 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, initiate investigation and any necessary corrective action. Ref: Standard
Methods, 9020 B-2005. (9) (a).

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BOD —Standard Methods, 5210 B-2001 (Aqueous)
W. Finding: The laboratory is not seeding samples over six hours old.
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 h 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).
X. 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).
Nitrogen, Ammonia — USGS 1-3520-85 (Aqueous)
Recommendation: The concentration of standard used to spike the sample is subtracted from
the MS result. The resulting sample concentration calculated from the MS is averaged with the
unspiked result to determine the value to be reported. It is recommended that only the unspiked
sample result be reported. The spiked sample is considered a quality control sample and does not
fall under the reporting requirements of 15A NCAC 2B .0506 (b) (3) (J). Please refer to the
attached NC WW/GW LC Policy regarding Matrix Spikes.
Y. Finding: Duplicate analyses are not performed.
Requirement: 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. Ref: 15A NCAC 2H .0805 (a) (7) (C).
Comment: The analysis of an MSD fulfills this requirement and is recommended when the
sample concentration is low.
Z. Finding: The distillation study was not properly performed and the results were not
acceptable.
Requirement: Samples must be spiked according to the NC WW/GW LC Matrix Spike
Policy, in duplicate, to allow for a meaningful statistical comparison. It is recommended
that samples are spiked to yield a value within the verified calibration range so that sample
dilution is not needed. Comparisons between the matrix spike and matrix spike duplicate,
as well as between distilled and undistilled samples must meet a 20% RPD acceptance
criterion. Both the distilled and undistilled samples must be analyzed using the same
method technology used to report compliance data for the permitted facility. It is
recommended that both the distilled and undistilled portions of the sample be analyzed by
the same laboratory. Per 15A NCAC 2H .0805 ()(2), it would be permissible to have a
contract lab distill the samples and send the distillates back to the permittee for analysis
within the prescribed holding time. It is the responsibility of the permittee to ensure that

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when only the distillation portion is contracted, that samples are distilled into the proper
receiving solution required by the analytical method to be used. That means when the
titration method will be employed, samples must be distilled into a boric acid solution.
When the phenate method will be employed, samples must be distilled into a sulfuric acid
solution.
The following frequencies are required:
Initially, compare a minimum of 9 samples, spiked in duplicate, both with and without the
distillation step (a total of 36 samples), to evaluate the need for distillation.
Subsequently, each year analyze a minimum of 2 samples, spiked in duplicate,
approximately 6 months apart, both with and without the distillation step (a total of 8
samples). If effluent characteristics change (e.g., contributing industries are added or lost,
major change in plant processes, etc.), or if the laboratory changes to another analytical
method that requires the comparison, a minimum of two additional samples must be
spiked in duplicate and analyzed, both with and without the distillation step, to demonstrate
that that distillation is still not required
Comment: A comparison was performed using only one spiked sample from each effluent
annually. The results from TWASA #1, TWASA #2 and Whittier did not meet the
acceptance criterion of 20% RPD. This may be due to the laboratory analyzing the
undistilled samples using a different technology than the distilled samples analyzed by
their contract laboratory.
IV. PAPER TRAIL INVESTIGATION:
The paper trail consisted of comparing original records (e.g., laboratory benchsheets, logbooks,
etc.) and contract lab reports to electronic Discharge Monitoring Reports (eDMRs) submitted to
the North Carolina Division of Water Resources. Data were reviewed for TWASA #1 (NPDES
permit #NC0039578) for February 2017. No transcription errors were observed. 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 their assistance during the inspection and data review process. Please
respond to all Findings and include supporting documentation and implementation
dates for each corrective action.
Report prepared by: Jason Smith Date: September 21, 2017
Report reviewed by: Tonja Springer Date: September 29, 2017

North Carolina Wastewater/Groundwater Laboratory Certification
Matrix Spiking Policy and Technical Assistance (05/11/2012)
Policy Statement
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 (MS) each
month samples are analyzed. If MS 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 MS 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.
When spiking with multi -component standards, if the method does not specify the spiking components,
the Laboratory Control Spike (LCS) and MS must contain all analytes that are reported.
If the unspiked sample result is in the top 40% of the calibration range, the sample should be diluted and
the MS prepared using the diluted sample. The recovery of the MS samples must be bracketed by the
calibration range.
The volume of spike solution used in MS preparation must in all cases be <_ 10% of the total MS volume. It
is preferable that the spike solution constitutes <_ 1% of the total MS volume so that the MS can be
considered a whole volume sample with no adjustment (i.e., volume correction) by calculation necessary.
If the spike solution volume constitutes >1 % of the total sample volume, the sample concentration or spike
concentration must be adjusted by calculation.
Technical Assistance
Spike Preparation
The spike concentration may be set at either 5 to 50 times the Method Detection Limit (as determined by
the Method Detection Limit or MDL study) for the analyte, or at 1 to 10 times the ambient level (average
concentration) of the analyte in samples. There are several options for preparing spikes, for example:
Option 1 (Recommended - easiest) - If the spike solution volume is equal to 1% or less of the
total sample volume, direct subtraction of the unspiked sample is allowed. When the volume of
the standard solution spiked into a sample or a sample extract is less than 1 % of the total volume
then the final concentration need not be adjusted (e.g., 10 pL of spike solution added to a 1 mL
final extract results in only a negligible 1 % change in the final extract volume).
Option 2 - Adjust spike solution to a known volume with sample. In this case the sample
concentration must be adjusted. When the volume of spike solution exceeds 1% of the total MS
volume the sample concentration must be adjusted prior to determining spike recovery.
The general equation for spike recovery is as follows:
% R = amt. of target in spiked sample — amt. of target in unspiked sample
(conc. or mass) (conc. or mass) x 100
amt. of target spiked into the sample
(conc. or mass)
To apply this to the sample preparation schemes described above, refer to the following examples.

Spike Preparation Examples
Option 1 - If the spike solution volume is equal to 1 % or less of the total sample volume, direct subtraction
of the unspiked sample is allowed.
Option 1 Example:
0.5 mis of a 1000 mg/L standard spike added to 100 mis of sample has a theoretical value of 5
mg/L.
(A) The spiked sample recovery is 5.1 mg/L
(B) If the unspiked sample result is 0.5 mg/L
(C) Theoretical value is 5.0 mg/L
The Percent Recovery = spiked sample recovery (A) — unspiked sample result (B) divided by
theoretical value (C) X 100 or
5.1 — 0.5 X 100 = 92% recovery
5.0
A — B X 100 = Percent recovery
C
Option 2 - Adjust spike solution to a known volume with sample. In this case the sample concentration
must be adjusted.
Option 2 Example 1:
10 mis of spike (concentration 50 mg/L) brought to 100 mis with sample the theoretical MS value is
5 mg/L.
(A) The spiked sample recovery is 5.1
(B) If the unspiked sample result is 0.5 mg/L
(C) % sample is 0.90 (sample volume used (90) divided by final volume (100))
(D) Theoretical value is 5.0 mg/L
The Percent Recovery = spiked sample recovery (A) — (unspiked sample result (B) x % sample
(C)) divided by theoretical value (D) X 100 or
5.1 — (0.5 x 0.9) X 100 = 93% recovery A — B x Q X 100 = Percent recovery
5.0 D
Option 2 Example 2: Larger spike volume
25 mis of spike (concentration 50 mg/L) brought to 250 mis with sample the theoretical MS value
is 5 mg/L.
(A) The spiked sample recovery is 5.6
(B) If the unspiked sample result is 0.5 mg/L
(C) % sample is 0.90 (sample volume used (225) divided by final volume (250))
(D) Theoretical value is 5.0 mg/L
The Percent Recovery = spiked sample recovery (A) — (unspiked sample result (B) x % sample
(C)) divided by theoretical value (D) X 100 or
5.6 — (0.5 x 0.9) X 100 = 103% recovery A — (B x C) X 100 = Percent recovery
5.0 D
Corrective Action/Qualifications for MS

Spike accuracy is usually based on a range of percent recovery (e.g., 80-120%). Refer to the method of
choice for specific acceptance criteria for the matrix spikes until the laboratory develops or adopts
statistically valid, laboratory -specific performance criteria for accuracy. If a MS fails, and the LCS is
acceptable, qualify the data for the MS sample. Repeated failures for a specific matrix may require use of
an alternate method or method of standard addition. Base the sample batch acceptance on the results of
the LCS analyses (and other quality control results) rather than the MS alone, because the matrix of the
spiked sample may interfere with the method performance. If a MS and the associated LCS fail, re -
prepare and reanalyze affected samples.
Post Digestion Spikes (PDS)
Post Digestion Spikes (PDS) are used for some analyses (e.g., metals) to assess the ability of a method
to successfully recover target analytes from an actual sample matrix after the digestion process has been
performed. The PDS results are used with MS results to evaluate matrix interferences. The MS and PDS
should be prepared from the same environmental sample. A PDS is not to be analyzed in place of a MS.
Post Digestion Spikes must be reported as post -digested and must not be misrepresented as pre-
digested spikes. (Exception: TCLP and SPLP samples are always spiked post digestion.)
Corrective Action/Qualifications for Post Digestion Spikes
In general, if the MS recovery for an analyte does not fall within the quality control acceptance range but
the PDS recovery is acceptable, then a matrix affect (associated with the preparatory process) should be
suspected and the unspiked sample results must be qualified on the basis of the matrix spike recovery.
However, when historical data for the effect does not exist, the laboratory would normally be expected to
perform a second digestion and reanalysis of the MS to confirm the result. The result would be confirmed
if the MS recoveries and PDS recoveries for both sets of analyses were similar in magnitude and bias.
When both the MS recovery and PDS recovery for a particular analyte falls outside of quality control
acceptance range in the same manner (i.e., the PDS and MS failures are of similar magnitude and the
direction of bias is the same), confirmatory analyses are unnecessary but the data must be qualified.
Parameters Excluded from MS Requirements
Acidity
BOD/CBOD
Chlorophyll
Color — ADMI
Conductivity
Ignitability
Paint Filter Test
pH
Salinity
Total Residual Chlorine
Alkalinity
Aquatic Humic Substances
All Bacteriological Parameters
Color - PtCo
Dissolved Oxygen
All Residues
Turbidity
Temperature
Sulfite
Vector Attraction Reduction (All Options)
(Field Laboratories and Field Setting analyses are exempt.)

Weight Verification (NC WW/GW LC Policy 05/23/2008)
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). Verification may be accomplished by:
1. Sending laboratory weights back to the manufacturer for recertification - reference
weights shall be calibrated by a body that can provide traceability to ASTM
specifications, or
2. Checking laboratory weights against certified reference weights (i.e., weights that
have been recertified as above) and found to be within ASTM Class 1 or Class 2
tolerances (see table below) - often the balance service technician may provide this
service.
Note: Although some manufacturers will assign a one-year calibration due date, 5 years is
considered an acceptable calibration interval due to the limited use of the reference weight set.
Documentation of weight verifications or recertification must be maintained for 5 years. If the
condition of a weight(s) is in question at any time due to damage (e.g., corrosion, nicks,
scratching, etc.), the laboratory must have that weight(s) re -verified as described above.
Maximum tolerances (Ref. ASTM E 617-97, 2003)
Denomination
Maximum tolerance for ASTM
Class 1 and 2 weights, ± m
500 g
1.2
3009
0.75
200 g
0.50
100 g
0.25
50 g
0.12
30 g
0.074
20 g
0.074
log
0.074
5 g
0.054
3 g
0.054
2 g
0.054
1 g
0.054
500 mg
0.025
300 mg
0.025
200 mg
0.025
100 mg
0.025
50 mg
0.014
30 mg
0.014
20 mg
0.014
10 mg
0.014
5 mg
0.014
3 mg
0.014
2 mg
0.014
1 mg
0.014

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