#203_2016_0301_JS_FINAL

To be attached to all inspection reports in-house only.
Laboratory Cert. #:
Laboratory Name:
Inspection Type:
Inspector Name(s):
Inspection Date:
Date Report Completed:
Date Forwarded to Reviewer:
Reviewed by:
Date Review Completed:
Cover Letter to use:
Unit Supervisor/Chemist III:
Date Received:
Date Forwarded to Admin:
Date Mailed:
203
Hickory Regional Laboratory
Municipal Maintenance
Jason Smith Gary Francies, Anna Ostendorff, Tonia Springer, and Beth
Swanson
March 1, 2016
March 28, 2016
April 5, 2016
Beth Swanson
4/6/2016
❑ Insp. Initial ❑ Insp. Reg.
❑ Insp. No Finding ❑ Insp. CP
❑ Corrected ® Insp. Reg. Delay
Todd Crawford
April 6, 2016
April 15, 2016
April 18, 2016

Water Resources
ENVIRONMENTAL QUALITY
April 18, 2016
203
Ms. Susan McNeely
Hickory Regional Laboratory
310 Cloninger Mill Rd.
Hickory, NC 28601
PAT MCCRORY
DONALD R. VAN DER VAART
S. JAY ZIMMERMAN
Subject: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC)
Maintenance Inspection
Dear Ms. McNeely:
Enclosed is a report for the inspection performed on March 1, 2016 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.
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,
ice..
1
Todd Crawford
Technical Assistance & Compliance Specialist
NC WW/GW Laboratory Certification Branch
Attachment
cc: Dana Satterwhite, Jason Smith, Master File
Water Sciences Section
NC wastewaterlGroundwater Laboratory Certification Branch
1623 Mail Service Center, Raleigh, North Carolina 27699-1623
Location: 4405 Reedy Creek Road, Raleigh, North Carolina 27607
Rhone: 919-733-39051 FAX: [phone]
internet http://deq.nc.goviabouUdivisionslwater-resources/water-resources-data/water-sciences-home-paste/laboratorv-certificaV,on-branch

LABORATORY NAME: Hickory Regional Laboratory
NPDES PERMIT : NC0025542, NC0040797, NC0020401, NC0032662 and
NC0081370
ADDRESS: 310 Cloninger Mill Road
Hickory, NC 28601
CERTIFICATE #: 203
DATE OF INSPECTION: March 1, 2016
TYPE OF INSPECTION: Municipal Maintenance
AUDITOR(S): Jason Smith, Gary Francies, Beth Ostendorff, Tonja Springer and
Beth Swanson
LOCAL PERSON(S) CONTACTED: Susan McNeely, David Cox, Paula Prestwood, Jeff Stevens and
Laura Vail
INTRODUCTION:
This laboratory was inspected by a representative of the North Carolina Wastewater/Groundwater
Laboratory Certification (NC WW/GW LC) program to verify its compliance with the requirements
of 15A NCAC 2H .0800 for the analysis of environmental samples.
II. GENERAL COMMENTS:
The facility is neat and 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. Laboratory personnel communicate well with sample collectors and
coordinate sample analyses effectively to manage workload and holding times. Staff was
forthcoming and seemed eager to adopt necessary changes.
Proficiency Testing (PT) samples for the 2016 proficiency testing calendar year have not yet been
analyzed. The laboratory is reminded that these results must be submitted to this office directly
from the vendor by September 30, 2016.
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
Assurance (QA)/Standard Operating Procedures (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.
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.

Page 2
#203 Hickory Regional Laboratory
Current SOPs were reviewed prior to the audit and Findings regarding the SOPs were sent to
the laboratory by email on March 4, 2016. Required SOP revisions from the preaudit review, as
well as revisions in response to Findings in this report, must be completed by May 1, 2017.
Contracted analyses are performed by Pace Analytical Services, Inc. — Asheville (Certification
#40), Blue Ridge Labs (Certification #275), Research & Analytical Laboratories (Certification #34)
and Statesville Analytical, Inc. (Certification #440).
Approved Procedures for the analysis of the facility's currently certified Field parameters were
provided at the time of the inspection.
The Requirements associated with Findings F, G, H, K, L, M, N, P, Q, T, X, BB, HH, JJ, MM, NN,
00 and PP have been implemented by our program since the last inspection.
III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:
Documentation
Recommendation: It is recommended that acceptance criteria for Quality Control be added to all
benchsheets.
Recommendation: It is recommended that method references be added to all benchsheets.
Recommendation: It is recommended that the laboratory define all acronyms in the Quality
Assurance document.
Recommendation: It is recommended that reporting limits be documented on all benchsheets.
Comment: The oven temperature log did not include the units of measure. The North Carolina
Administrative Code, 15 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. Acceptable corrective action (i.e., units of measure for
temperature were added to the log) was performed during the inspection and observed by the
inspector to be adequate. No further response is necessary for this Finding.
A. Finding: The units of measure are not documented consistently.
Requirement: All laboratories must use printed laboratory bench worksheets that
include a space to enter the signature or initials of the an 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: The units of measure are not documented in the following locations:
• BOD benchsheet page 2 - Final BOD result
• BOD pH Record — pH
• Chloride benchsheet - initial buret reading, final buret reading, and blank
• Total Residual Chlorine (TRC) benchsheet — column labeled "Average"
(which is the reported result)
• pH calibration log - pH

Page 3
#203 Hickory Regional Laboratory
® Dissolved Oxygen (DO) benchsheet (calibration section) — Temperature
and DO values
® Suspended Residue benchsheet — initial and final weights
Recommendation: This may not be a comprehensive list of locations of missing units of
measure. It is recommended that the laboratory thoroughly review all benchsheets and
logs to ensure compliance with this requirement.
B. Finding: Error corrections are not always 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: Some instances of writing over errors were observed. Not all errors were
initialed and/or dated.
C. Finding: Documentation of preservation is not complete.
Requirement: Each sample container must be checked upon receipt in the laboratory for
the effectiveness of any required pH adjustment and the results documented. Ref: NC
WW/GW LC Policy.
Comment: Preservation pH is not documented for Ammonia, Metals, COD, Inorganic
Phenols, and MBAS.
D. Finding: The laboratory does not maintain adequate traceability for all parameters.
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 traceability of reagents is not adequately documented for Total
Phosphorus. The Quality Control (QC) standard is the only one with adequate traceability
documentation.
Comment: Suspended Residue filter traceability information is not documented.

Page 4
#203 Hickory Regional Laboratory
Comment: The date reagents are opened is documented on the container, but is not
documented in a log that is maintained for five years. The date put in use is the date
opened for most reagents. The laboratory currently maintains documentation of date put
into use, but not date opened.
Quality Control
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 "chill to 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. Additionally, the holding time for Fecal
Coliform may be extended from 6 hours to 8 hours.
Comment: For laboratory prepared curves that are held, such as MBAS and Inorganic Phenols,
verification with a second source standard is only required when the curve is initially prepared.
The laboratory currently verifies them daily with a second source standard.
Comment: Duplicate analyses are not required for Field parameters (i.e., pH, Total Residual
Chlorine, Dissolved Oxygen, Temperature, and Conductivity).
E. Finding: Quality control results are not consistently calculated and evaluated to
demonstrate meeting the acceptance criteria.
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: 15 NCAC 2H .0805 (a) (7).
Comment: The QC results obtained must be documented and evaluated against the
acceptance criteria to demonstrate that the analyst was aware of any out -of -control
situation and the corrective action that was taken. Any samples not meeting the criteria
must be reanalyzed if possible. If this is not possible, the data must be flagged on the
laboratory reports and Discharge Monitoring Reports (DMR) as all quality control
requirements not met.
Comment: Duplicate Relative Percent Difference (RPD) results are not calculated and
evaluated for Fecal Coliform and Total Phosphorus. Duplicate RPD results and standard
recovery results are not calculated and evaluated for Chloride. Standard recovery results
are not calculated and evaluated for Metals analyses.
F. Finding: Auto-pipettors are not calibrated.
Requirement: Mechanical volumetric liquid -dispensing devices (e.g., fixed and
adjustable auto-pipettors, bottle -top dispensers, etc.), used for critical measurements,
must be calibrated at least twice per year, approximately six months apart and
documented. Each liquid -dispensing device must meet the manufacturer's statement of
accuracy. Ref: NC WW/GW LC Policy.
Comment: Technical assistance for calibration was provided to the laboratory by email on
March 29, 2016.

Page 5
#203 Hickory Regional Laboratory
Proficiency Testing
G. 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
samples would satisfy the documentation requirement,
H. Finding: The laboratory is not analyzing PT samples in the same manner as compliance
samples.
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's common practice was to analyze a known standard along
with the metals PT sample as additional quality control. Since this is not performed with all
compliance samples, it is considered additional quality control. However, known samples
are recommended when analyzing remedial PT samples as part of the troubleshooting
and corrective action process.
Bacteria - Coliform Fecal — Standard Methods, 9222 D-1997 (MF) (Aqueous)
Finding: The laboratory is using a total 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://'w .v. o\c /mercy / lternatives.htm.
Comment: If the thermometer is not able to be properly submerged, a partial immersion
thermometer or the digital thermometer on the incubator must be used.
J. Finding: Laboratory personnel were not evaluating consumables testing acceptance
criteria as stated in the SOP.
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: 15 NCAC 2H .0805 (a) (7).

Page 6
#203 Hickory Regional Laboratory
Comment: The SOP established an acceptance criterion for consumable materials testing
that was unnecessarily restrictive and data were not being evaluated by that criterion.
Some of the new materials should not have been put into use based upon the established
acceptance criterion, had it been applied. However, a reasonable acceptance criterion
would have shown that the materials were acceptable for use.
Recommendation: It is recommended that the laboratory use an acceptance criterion
three times the standard deviation of the mean of past results, a set value like 20% RPD,
or the laboratories established acceptance criteria. This criterion needs to be evaluated to
determine if the materials are fit for use and included in the SOP revision.
K. Finding: The time that the sample is filtered is not recorded on the benchsheet to show
that no more than 30 minutes has passed before filters are placed into the incubator.
Requirement: Place all prepared cultures in the water bath within 30 minutes after
filtration. Ref: Standard Methods, 9222 D-1997. (2) (d).
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).
L. Finding: Incubator temperature is only checked one time per day.
Requirement: When incubator is in use, monitor and record calibration -corrected
temperature twice daily. Ref: Standard Methods, 9020 B-2005. (4) (n).
M. 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 13-
2005. (9) (a).
N. Finding: The laboratory is not monitoring the quality of the reagent water used in fecal
coliform analysis.
Requirement: 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. Ref: NC WW/GW LC Policy and Standard Methods 9020 B-2005.
(5) (f)-
BOD — Standard Methods, 5210 B-2001 (Aqueous)
O. Finding: Initial DO concentrations are not always brought to the required range of 7 - 9
mg/L.

Page 7
#203 Hickory Regional Laboratory
Requirement: The working range is equal to the difference between the maximum initial
DO (7 to 9 mg/L) and minimum DO residual of 1 mg/L corrected for seed, and multiplied
by the dilution factor. Ref. Standard Methods, 5210 B-2001. (8) (b).
Requirement: Samples supersaturated with DO — Samples containing DO concentrations
above saturation at 20 °C may be encountered in cold waters or in water where
photosynthesis occurs. To prevent loss of oxygen during incubation of such samples,
reduce DO to saturation by bringing sample to about 20 ± 3 °C in partially filled bottle while
agitating by vigorous shaking or by aerating with clean, filtered compressed air. Ref:
Standard Methods, 5210 B-2001. (4) (b) (4).
P. Finding: Multiple dilution water blanks are being analyzed, but the results are not
averaged to determine acceptability.
Requirement: Multiple dilution water blanks in the same batch using the same dilution
water are to be treated as replicates and averaged. The averse 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.
Chlorine, Total Residual — Standard Methods, 4500 Cl G-2000 (Aqueous)
Comment: The laboratory is currently using liquid reagents and the pour-thru cell. The laboratory
may use DPD powder and discontinue use of the pour-thru cell, but must verify the curve using
the DPD powder prior to implementation.
Comment: A second lot of Potassium Permanganate is used to make a 30 pg/L standard for the
annual curve verification. This is not required and all standards for the curve verification may be
from the same lot of Potassium Permanganate. Additionally, the laboratory meets the five -point
calibration verification requirement without using the 30 pg/L standard.
COD — Hach 8000 (Aqueous)
Recommendation: It is recommended that the digestion temperature be documented on the
benchsheet in addition to the digestion log.
Conductivity — Standard Methods, 2510 B-1997 (Aqueous)
Q. Finding: Meter calibration time is not documented.
Requirement: The following must be documented in indelible ink whenever sample
analysis is performed: Meter calibration and meter calibration time(s). Ref: NC WW/GW
LC Approved Procedure for the Analysis of Specific Conductance (Conductivity).
R. Finding: The Automatic Temperature Compensation (ATC) verification was not properly
performed.
Requirement: The ATC must be verified annually (i.e., every twelve months) and the
process documented. The ATC must be verified by analyzing a standard at 25 °C (the
temperature that conductivity values are compensated to) and a temperature(s) that brackets
the temperature ranges of the samples to be analyzed. This may require the analysis of a
third temperature reading that is > 25 'C. Ref: NC WW/GW LC Approved Procedure for the
Analysis of Specific Conductance (Conductivity).

Page 8
#203 Hickory Regional Laboratory
Comment: The most recent verification included a standard at 23.2 °C. The standard must
be 25 ± 0.5 °C in order to demonstrate the result when temperature compensation is not
performed by the meter.
S. Finding: The benchsheet does not specify which standard is used for calibration and
which is used for calibration verification.
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: 15 NCAC 2H .0805 (a) (7).
Requirement: The following must be documented in indelible ink whenever sample
analysis is performed: True value of the standard used for calibration and true value of the
calibration verification check standard. Ref: NC WW/GW LC Approved Procedure for the
Analysis of Specific Conductance (Conductivity).
Dissolved Oxygen — Standard Methods, 4500 O G-2001 (Aqueous)
Recommendation: Some instances of the altitude not being documented for calibration were
noted. It is recommended that this be permanently typed on the sheet since the meter is always
calibrated at the same altitude.
Recommendation: The calibration log includes columns labeled "theoretical" and "found". The
"theoretical" value recorded is the meter reading prior to calibration. It is recommended that this
be removed since it is not required to document this information.
T. Finding: A post analysis verification is not performed.
Requirement: When performing analyses away from the certified laboratory's primary
location, a post analysis calibration verification must be analyzed at the end of the run. It is
recommended that a mid -day calibration verification be performed when samples are
analyzed over an extended period of time. The calculated DO value must verify the meter
reading within ±0.5 mg/L. If the meter verification does not read within ±0.5 mg/L of the
theoretical DO, corrective action must be taken. Ref: NC WW/GW LC Approved
Procedure for the Analysis of Dissolved Oxygen.
MBAS — Standard Methods, 5540 C-2000 (Aqueous)
U. Finding: The molecular weight of the LAS used for the calibration curve is not
documented.
Requirement: From the calibration curve (5540C.4a) read micrograms of apparent LAS
(mol wt _) corresponding to the measured absorbance. Ref: Standard Methods, 5540
C-2000. (5).
V. Finding: A curve is not prepared with each new lot of LAS.
Requirement: For colorimetric analyses, a series of five standards for a curve prepared
annually or three standards for curves established each day or standards as set forth in
the analytical procedure must be analyzed to establish a standard curve. The curve
must be updated as set forth in the standard procedures, each time the slope changes
by more than 10 percent at midrange, each time a new stock standard is prepared, or at

Page 9
#203 Hickory Regional Laboratory
least every twelve months. Each analyst performing the analytical procedure must
produce a standard curve. Ref: 15A NCAC 2H .0805 (a) (7) (1).
Comment: The curve prepared April 22, 2014 used LAS solution that expired July,
2014. A new curve was not prepared with the LAS solution put into use in July, 2014.
W. Finding: The curve prepared on 4/22/2014 was not verified with a second source
standard.
Requirement: If the LFB is not prepared from a second source to confirm method
accuracy, (unless the method specifies otherwise) the laboratory must also verify the
accuracy of its standard preparation by analyzing a mid -level second source calibration
standard whenever a new initial calibration curve is prepared. Ref: Standard Methods,
5020 B-2010. (2) (b).
X. Finding: The laboratory is not analyzing a standard at the reporting limit and a value
above the expected concentration of samples.
Requirement: Provided that linearity is demonstrated over the range of interest (r=0.995
or better) run daily check standards at the reporting limit and a concentration above the
expected samples' concentration. Check standard results should be within 25% of original
value at the reporting limit and 10% of original value for all others. Ref: Standard Methods,
5540 C-2000. (4) (a).
Metals — Standard Methods, 3111 B-1999 (Aqueous)
Comment: The laboratory chooses to analyze all three calibration standards after calibration and
has established the acceptance criterion at ± 10% of the true value. The method requires analysis
of the reporting limit standard and an Initial Calibration Verification (ICV); however, analysis of a
third calibration standard is not required.
Y. Finding: The digested reagent blank is not properly evaluated.
Requirement: For analyses requiring a calibration curve, the concentration of reagent,
method and calibration blanks must not exceed 50% of the reporting limit or as
otherwise specified by the reference method. Ref: NC WW/GW LC Policy.
Comment: The laboratory evaluates the reagent blank based on the absorbance rather
than the concentration. The absorbance is not converted to concentration to evaluate it
against the reporting limit.
Z. Finding: The acceptance criterion for the ICV is greater than what the method allows.
Requirement: For regulatory compliance purposes, use acceptance criteria of between
95 and 105% of the expected value. Ref: Standard Methods, 3020 B-2005. (2) (c).
Comment: The laboratory set the acceptance criterion for the ICV at 90-110%. The
method only allows a 90-110% acceptance criterion for Continuing Calibration Verification
(CCV) results.
Comment: The method allows the ICV and Second Source Calibration Verification
(SSCV) standard to be the same standard if prepared from a second source. SM 3020 13-
2005 (2) (c) states in part: Initial Calibration Verification: A calibration check solution (CCS)

Page 10
#203 Hickory Regional Laboratory
may be prepared from a different stock solution than was used to prepare the calibration
standard(s) or from the same stock solution. If the CCS is prepared from a second source,
the SSCV and ICV may be combined into a single step and check solution.
AA. Finding: The laboratory is not analyzing field blanks.
Requirement: A field blank is a portion of reagent water placed into a sample bottle and
taken out into the field during sample collection. Use the same type of bottle used to
collect the sample and treat [field blank] FB exactly the same as the sample. Ref:
Standard Methods, 3020 B-2005. (2) (g).
BB. Finding: The analyst(s) has not performed an Initial Demonstration of Capability (IDOC).
Requirement: Verify analyst capability before analyzing any samples and repeat
periodically (annually or when there is a new analyst, whichever is more frequent) to
demonstrate proficiency with the analytical method. Test analyst capability by analyzing at
least four well -characterized samples with a concentration of the analyte of interest that is
unknown to the analyst. Ref: Standard Methods, 3020 B-2005. (1) (a).
Nitrogen, Ammonia — Standard Methods, 4500 NH3 D-1997 (Aqueous)
Recommendation: It is recommended that a column for dilution factors be added to the
benchsheet.
CC. Finding: The benchsheet does not specify which standards are used for calibration and
which are used for calibration verification. This is considered pertinent information.
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: 15 NCAC 2H .0805 (a) (7).
Comment: Currently the benchsheet lists 100, 50, 10, 1.0 and 0.10 mg/L under the
heading "Standards" and 5.0 mg/L under the header "QC Standard". The meter is
calibrated with the 1.0 and 50 mg/L standards and the rest are analyzed as QC standards.
DD. Finding: The slope is not documented on the benchsheet.
Requirement: It is required that the slope value or efficiency be documented for ion
selective electrode meter calibrations. Ref: NC WW/GW LC Policy.
EE. Finding: The sample volume is not documented.
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: Ref: 15A NCAC 2H .0805 (a) (7) (H).

Page 11
#203 Hickory Regional Laboratory
FF. Finding: The volume of Ion Strength Adjusting (ISA) solution added is not documented.
Requirement: Record volume of 10N NaOH added. Ref: Standard Methods, 4500 NH3 D-
1997. (4) (e).
Comment: The analyst stated that no samples have required more ISA than the
standards (i.e., 2 mQ, which makes calculation adjustment unnecessary. If the volumes of
ISA solution used in samples differ from that used in standards, the result must be
adjusted based on the formula in Standard Methods, 4500 NH3 D-1997. (5).
Comment: A statement such as "Unless otherwise noted, 2 mL of ISA is added to all
samples, standards, and blanks" may be added to the benchsheet.
GG. Finding: The laboratory is not replacing 10 N NaOH with 10 N NaOH/EDTA for samples
containing mercury.
Requirement: If the presence of silver or mercury is possible, use NaOH/EDTA solution in
place of NaOH solution. Ref: Standard Methods, 4500 NH3 D-1997. (4) (b).
HH. Finding: Verification of pH adjustment to >11 S.U. 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. Ref: Standard Methods, 4500 NH3 D-1997. (4) (b).
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).
pH — Standard Methods, 4500 H+ B-2000 (Aqueous)
II. Finding: The result of the check standard is not documented.
Requirement: The following must be documented in indelible ink whenever sample
analysis is performed: Value obtained for the check standard buffer (verification of ± 0.1
S.U.). Ref: NC WW/GW LC Approved Procedure for the Analysis of pH.
JJ. Finding: A post analysis verification standard is not analyzed.
Requirement: When performing analyses away from the certified laboratory's primary
location, a post analysis calibration verification using the check standard buffer must be
analyzed at the end of the run. It is recommended that a mid -day check standard buffer be
analyzed when samples are analyzed over an extended period of time. The post analysis
check standard buffer(s) must read within ±0.1 S.0 or corrective actions must be taken.
Ref: NC WW/GW LC Approved Procedure for the Analysis of pH.
KK. Finding: All effluent results are not reported on the Discharge Monitoring Report (DMR).
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 2B .0506 (b) (3) (J).

Page 12
#203 Hickory Regional Laboratory
Comment: Duplicate analyses are not required for field parameters.
Comment: Duplicates are analyzed occasionally, but the duplicate results are not
reported. If duplicates are analyzed, the results cannot be averaged since pH is a
logarithmic value. Each duplicate result must be reported.
Phosphorus, Total — EPA 365.3, 1978 (Aqueous)
ILL. Finding: The sample volume is not documented.
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).
Residue, Suspended — Standard Methods, 2540 D-1997 (Aqueous)
Recommendation: The balance is checked with 20 g and 100 g weights daily and 0.2 g, 20 g,
and 100 g weights monthly. It is recommended that the 1 g weight be used daily since it is closer
to the weight of residue sample filters.
Chlorine, Total Residual — Standard Methods, 4500 Cl G-2000(Aqueous)
Conductivity —Standard Methods, 2510 B-1997 (Aqueous)
Dissolved Oxygen — Standard Methods, 4500 O G-2001 (Aqueous)
pH — Standard Methods, 4500 H+ B-2000 (Aqueous)
Temperature — Standard Methods, 2550 B-2000 (Aqueous)
MM. 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 Total Residual Chlorine, NC WW/GW LC Approved
Procedure for the Analysis of Dissolved Oxygen, NC WW/GW LC Approved Procedure for
the Analysis of pH, NC WW/GW LC Approved Procedure for the Analysis of Specific
Conductance (Conductivity) and NC WW/GW LC Approved Procedure for the Analysis of
Temperature.
COD — Hach 8000 (Aqueous)
Inorganic Phenols — EPA 420.1, Rev. 1978 (Aqueous)
MBAS — Standard Methods, 5540 C-2000 (Aqueous)
Metals — Standard Methods, 3111 B-1999
Phosphorus, Total — EPA 365.3, 1978 (Aqueous)
NN. Finding: A calibration blank and/or calibration verification standard (mid -range) are not
analyzed initially, at the end of the sample group, and/or after every tenth sample.
Requirement: The calibration blank and calibration verification standard (mid -range)
must be analyzed initially (i.e., prior to sample analysis), after every tenth sample and at
the end of each sample group to check for carry over and calibration drift. If either fall
outside established quality control acceptance criteria, corrective action must be taken

Page 13
#203 Hickory Regional Laboratory
(e.g., repeating sample determinations since the last acceptable calibration verification,
repeating the initial calibration, etc.). Ref: NC WW/GW LC Policy.
Comment: An initial blank is analyzed for Total Phosphorus, but the results are not
documented.
Comment: The post analysis blank for Metals is not properly analyzed. The instrument
is zeroed with it rather than it being analyzed as a sample.
Comment: No blanks are analyzed for COD.
Comment: A blank and calibration verification standard are not analyzed at the end of
the sample group for Inorganic Phenols and MBAS. The initial blank is analyzed but not
documented.
Chloride — Standard Methods, 4500 Cl- C-1997 (Aqueous)
Metals — Standard Methods, 3111 B-1999
Nitrogen, Ammonia — Standard Methods, 4500 NH3 D-1997 (Aqueous)
00. Finding: The laboratory is not analyzing a LFM and LFMD.
Requirement: Use LFM (also known as matrix spike) and LFM duplicate to evaluate the
accuracy and precision, respectively, of the method as influenced by a specific matrix.
Include one LFM/LFMD for every 20 samples in an analytical batch, or include more
LFM/LFMDs if appropriate. Ref: Standard Methods, 3020 B-2005. (2) (h).
Requirement: Use LFMs exactly as above (3020B.2h) except that the sample should be
fortified before sample preparation. Ref: Standard Methods, 3020 B-2005. (3) (c).
Requirement: When appropriate for the analyte (Table 4020:1), include at least one
LFM/LFMD daily or with each batch of 20 or fewer samples. Ref: Standard Methods, 4020
B-2009. (2) (g).
Comment: Analysis of the LFMD (or MSD), at the required frequency, is acceptable to
satisfy the sample duplicate requirement listed in North Carolina Administrative Code, 15A
NCAC 21-1.0805 (a) (7) (C).
Comment: A copy of the MS/MSD Technical Assistance document was emailed to the
facility on March 29, 2016.
COD — Hach 8000 (Aqueous)
Inorganic Phenols — EPA Method 420.1, Rev. 1978 (Aqueous)
MBAS — Standard Methods, 5540 C-2000 (Aqueous)
Phosphorus, Total — EPA 365.3, 1978 (Aqueous)
PP. Finding: The laboratory is not analyzing a MS.
Requirement: Unless the referenced method states a greater frequency, spike 5% of
samples on a monthly basis. Laboratories analyzing less than 20 samples per month
must analyze at least one matrix spike each month samples are analyzed. Prepare the
matrix spike from a reference source different from that used for calibration unless
otherwise stated in the method. If matrix spike results are out of control, the results must

Page 14
#203 Hickory Regional Laboratory
be qualified or the laboratory must take corrective action to rectify the effect, use
another method, or employ the method of standard additions. When the method of
choice specifies matrix spike performance acceptance criteria for accuracy, and the
laboratory chooses to develop statistically valid, laboratory -specific limits, the laboratory -
generated limits cannot be less stringent than the criteria stated in the approved
method. Ref: NC WW/GW LC Policy.
Requirement: When appropriate for the analyte (Table 5020:1), include at least one
LFM/LFMD daily or with each batch of 20 or fewer samples. Ref: Standard methods, 5020
B-2010. (2) (g).
Comment: Analysis of a MSD is not required for these parameters. However, the
laboratory may choose to analyze a MSD in place of the sample duplicate.
No paper trail performed because Division Regional Office staff conducted a paper trail in January
2016.
V. CONCLUSIONS:
Correcting the above -cited Findings and implementing the Recommendations will help this lab
to produce quality data and meet Certification requirements. The inspector would like to thank
the staff for its assistance during the inspection and data review process. Please respond to
all Findings and include an implementation date for each corrective action.
Report prepared by: Jason Smith Date: April 5, 2016
Report reviewed by: Beth Swanson Date: April 6, 2016