#65_0722_FINAL

North Carolina Department of Environmental Quality
Pat McCrory
Governor
September 21, 2015
65
Ms. Alicia Goots
TZ Osborne WRF Laboratory
P.O. Box 3136
Greensboro, NC 27402-3136
Donald R. van der Vaart
Secretary
Subject: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC)
Maintenance Inspection
Dear Ms. Goots:
Enclosed is a report for the inspection performed on July 22, 2015 by staff of the NC WW/GW LC
program. 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 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 us at (828)
296-4677.
Attachment
cc: Beth Swanson
Master File
Sincerely,
COY c�sa-t,
Gary Francies, Technical Assistance/Compliance Specialist
Division of Water Resources
Water Sciences Section
NC Wastewater/Groundwater Laboratory Certification Branch
1623 [fail Service Center, Raleigh, North Carolina 27699-1623
Location: 4405 Reedy Creek Road, Raleigh, North Carolina 27607
Phone: [phone] l FAX: [phone]
Internet: www.dwglab.orq
An Equal Opportunity t Affirmative Action Employer

INSPECTION REPORT ROUTING SHEET
To be attached to all inspection reports in-house only.
Laboratory Cert. #: 65
Laboratory Name: TZ Osborne WRF Laboratory
Inspection Type: Municipal Maintenance
Inspector Name(s): Beth Swanson Gary Francies, Dana
Satterwhite Nick Jones, Todd Crawford
Jason Smith
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 Linda:
Date Mailed:
July 22 2015
August 20 2015
August 20 2015
Nick Jones
September 2 2015
❑ Insp. Initial
❑ Insp. No Finding
❑ Corrected
Gary Francies
® Insp. Reg.
❑ Insp. CP
❑ Insp. Reg. Delay
9/4/2015
9/21 /2015

On -Site Inspection Report
LABORATORY NAME:
NPDES PERMIT #:
ADDRESS:
CERTIFICATE #:
DATE OF INSPECTION:
TYPE OF INSPECTION:
AUDITOR(S):
LOCAL PERSON(S) CONTACTED:
I. INTRODUCTION:
TZ Osborne WRF Laboratory
NC0047384, NCO024325
P.O. Box 3136
Greensboro, NC 27402-3136
65
July 22, 2015
Municipal Maintenance
Beth Swanson, Gary Francies, Dana Satterwhite,
Nick Jones, Todd Crawford, and Jason Smith
Alicia Goots and Martie Groome
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 laboratory was very clean and well organized. Data was readily available and analysts were
knowledgeable and forthcoming. The organizational culture of this laboratory is one that focuses on
quality of data. Everyone we interacted with was interested and willing to adapt their processes to the
required and recommended changes. As shown in the report, the laboratory was proactive in responding
to several Findings.
Proficiency Testing (PT) samples have been analyzed for all certified parameters for the 2015 proficiency
testing calendar year and the graded results were 100% acceptable.
The laboratory is reminded that any time changes are made to laboratory operations; the laboratory must
update the Quality Assurance (QA)/Standard Operating Procedures (SOP) document(s). Any changes
made in response to the 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 approved practice and regulatory requirements. In
some instances, the laboratory may need to create a SOP to document how new functions or policy will
be implemented.
Contracted analyses are performed by Meritech, Inc. (Certification #165).
The requirements associated with Findings B, E, M, N, P, and U have been implemented by our program
since the last inspection.

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III. FINDINGS REQUIREMENTS COMMENTS AND RECOMMENDATIONS:
General
Recommendation: It is recommended that the sample preservation and storage temperature
requirements be changed in accordance with 40 CFR Part 136.3 Table II in all pertinent SOPs and in
practice. The current practice is to store "at 4°C". 40 CFR Part 136.3 Table II allows 56°C for most
inorganic and metals parameters and <10°C for bacterial tests, without evidence of freezing.
Documentation
Recommendation: It is recommended that all records of preventative maintenance performed on
analytical instrumentation be documented in an individual equipment maintenance log book maintained
by the laboratory. All records of corrective action taken or minor troubleshooting and repair performed
should also be documented in the equipment maintenance log. The records may include the following, as
appropriate:
a. The identity of the item of equipment and its software;
b. The manufacturer's name, type identification, and serial number or other unique identifier;
C. The current location;
d. The dates, results and copies of reports and certificates or all calibrations, adjustments,
acceptance criteria, and the due date of the next calibration.
e. The maintenance plan, where appropriate, and maintenance completed date.
f. Documentation of any damage, malfunction, modification, or repair to the equipment.
g. Signature or initials of the person performing the maintenance or troubleshooting.
These records provide an historical reconstruction of the maintenance performed, a reference for
effective troubleshooting in the future, and can also serve as a valuable training tool for new analysts.
Comment: Improper error correction was noted that included the use of correction fluid and crossing out
data with no initial and/or date. NC WW/GW LC policy states: 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-OutO correction tape or similar products desianed 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. Notification of acceptable corrective action
(i.e., on June 24, 2015, staff participated in a meeting detailing the proper procedure for error correction),
was received by email on July 30, 2015 stating that all changes were implemented at that time. No
further response is necessary for this Finding.
Comment: Units of measure were not included on the temperature charts throughout the lab. This is
considered pertinent information. The North Carolina Administrative Code, 15 NCAC 2H .0805 (a) (7) (A)
states: All analytical data pertinent to each certified analysis must be filed in an orderly manner so as to
be readily available for inspection upon request. Notification of acceptable corrective action (i.e., a note
was added to the top of all temperature charts in use stating that all temperatures are in °C) was
received by email on July 30, 2015 and implemented immediately. No further response is necessary
for this Finding.
Comment: The date received for chemicals and consumables was not documented. NC WW/GW LC
policy states: 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). 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

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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. Notification of acceptable
corrective action (i.e., traceability logs for consumables and chemicals received by the laboratory were
created and implemented on August 3, 2015) was received by email on August 3, 2015. No further
response is necessary for this Finding.
Comment: The benchsheet for the analysis of DO, pH, and temperature did not contain instrument
identification. The NC WW/GW LC Approved Procedure for the Analysis of Dissolved Oxygen, NC
WW/GW LC Approved Procedure for the Analysis of pH and NC WW/GW LC Approved Procedure for
the Analysis of Temperature documents state: The following must be documented in indelible ink
whenever sample analysis is performed: Thermometer/Instrument Identification. This requirement is a
new policy that has been implemented by our program since the last inspection. Notification of
acceptable corrective action (i.e., instrument/thermometer ID was added to the benchsheet and
implemented on August 3, 2015) was received by email on August 3, 2015. No further response is
necessary for this Finding.
A. Finding: The temperature correction factor is not always posted on thermometers for corrections of
0°C.
Requirement: 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. Ref: NC WW/GW
LC Policy.
Comment: This was noted on the digital thermometer used for sample receipt temperature
checks. All other thermometers had corrections (both zero and non -zero) posted.
Quality Control
B. Finding: Auto-pipettors are not being 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.
C. Finding: The annual verification of the digital thermometer used for sample receipt temperature
checks cannot be confirmed.
Requirement: All thermometers must meet 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 thermometer is a NIST traceable thermometer but the expiration date was not
legible on the thermometer and no paperwork was found to determine the expiration date. Either the
expiration date information needs to be requested from the manufacturer or the thermometer needs
to be verified against an NIST traceable thermometer.
D. Finding: The thermal preservation of samples from North Buffalo is not being maintained during
transportation.
Requirement: A 15-minute limit to thermally or chemically preserve samples is allowed. The
temperature of a temperature blank or of a representative sample from each cooler must be

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#65 TZ Osborne WRF Laboratory
recorded upon receipt in the laboratory. Occasionally, samples that are collected and delivered to
the lab within a short period of time may not have time to cool to less than or equal to 6°C (less than
10' C for Bacteriological analyses) before they arrive at the laboratory. If these samples are placed
in ice immediately after collection and are shipped on ice or in ice slurry (NOTE: frozen or blue ice
packs are not acceptable) the sample collectors have complied with these requirements to the best
of their ability and the samples will be accepted. Documentation of the actual sample temperature at
the time of collection and upon receipt at the laboratory must exhibit a downward trend and will
complete the preservation documentation requirements. Ref: NC WW/GW LC Policy
Comment: The samples from North Buffalo are composite samples which are placed into a
refrigerator for several hours until they are transported to the TZ Osborne facility. However, the
samples are not transported on ice, and the temperature upon receipt exhibits an upward trend from
the temperature taken at the time of collection.
E. Finding: Chemical preservation is not being conducted within 15 minutes of sample collection.
Requirement: Except where noted in this Table II and the method for the parameter, preserve
each grab sample within 15 minutes of collection. For a composite sample collected with an
automated sampler (e.g., using a 24-hour composite sampler; see 40 CFR 122.21 (g) (7) (i) or 40
CFR Part 403, Appendix E), refrigerate the sample at :56 °C during collection unless specified
otherwise in this Table II or in the method(s). For a composite sample to be split into separate
aliquots for preservation and/or analysis, maintain the sample at :56 °C, unless specified
otherwise in this Table II or in the method(s), until collection, splitting, and preservation is
completed. Add the preservative to the sample container prior to sample collection when the
preservative will not compromise the integrity of a grab sample, a composite sample, or an
aliquot split from a composite sample; otherwise, preserve the grab sample, composite sample,
or aliquot split from a composite sample within 15 minutes of collection. Ref: Code of Federal
Regulations, Title 40, Part 136; Federal Register Vol. 72, No. 47, March 12, 2007; Table II.
SOP
Recommendation: It is recommended that all SOPs be reviewed and evaluated for use of the word
"should". SOPs are intended to describe procedures exactly as they are to be performed. While some
uses of the word "should" versus "must" are noted in Finding I, not all have been listed in this report.
Recommendation: It is recommended that SOPs include a revision and review history with relevant
dates (e.g., effective, review and revision dates) and a brief description of the change(s) made.
Recommendation: It is recommended that acronyms and terms for Quality Assurance/Quality Control
(QA/QC) elements (e.g., LRL or PQL, LRB, CAL BILK, FRB, etc.) be defined in the Metals SOP and used
consistently across the data and SOP.
Recommendation: It is recommended that the Metals SOP state the minimum purity of the Argon used.
Recommendation: It is recommended that section C of the Metals SOP state examples of when the
reporting limit would be adjusted (e.g., dilution and dropping the lowest standard).
Recommendation: It is recommended that the quality control section of the Total Residual Chlorine
(TRC) SOP only include items that apply to the low range procedure. For instance, the DPD is only used
with the LaMotte 1200 colorimeter that is used for TRC screening in ammonia and CBOD samples.
Comment: An inconsistency and/or omission was noted between the Standard Operating Procedure
(SOP) and laboratory practice as follows: personnel were not following procedures as stated in the

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#65 TZ Osborne WRF Laboratory
Laboratory's SOP, the method reference in the SOP is not correct, the SOP is in direct conflict with
method and/or regulatory requirements, and the SOP does not describe in detail how the method is
performed (observations are listed below). The North Carolina Administrative Code, 15 NCAC 2H .0805
(a) (7) states: 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. Demonstration of
acceptable corrective action (i.e., updated SOPs were submitted) was received by email on July 30, 2015.
No further response is necessary for this finding.
Residue, Suspended (SM 2540 D-1997)
o The SOP did not state that wide bore pipettes were being used as required by the method.
o The SOP referenced the 18th Edition of Standard Methods rather than Standard Methods
Committee approval year.
o The SOP did not state that the volume of sample is chosen to yield between 2.5 and 200
mg of dried residue.
o The SOP did not state that a dry filter blank was analyzed daily.
• Proficiency Testing
o The laboratory did not have an SOP to detail the analysis of PT samples.
Bacteria- Coliform Fecal (SM 9222 D-1997)
o The SOP referenced the 18th Edition of Standard Methods rather than Standard Methods
Committee approval year.
o The SOP included preservation and hold time language from Standard Methods, but this
would not apply as the requirements in 40 CFR Part 136.3, Table II takes precedent.
o The SOP incorrectly included the word "should" versus "must" in various sections.
o The SOP stated that the buffered dilution water could be kept indefinitely instead of 6
months.
o The SOP did not clearly describe the acceptance criterion for duplicate analyses.
F. Finding: An inconsistency and/or omission was noted between the Standard Operating
Procedure (SOP) and laboratory practice as follows:
The method reference in the SOP is not correct.
o Dissolved Oxygen (SM 4500 G-2001) — The SOP references SM 4500 O G- 1998
18th Edition.
o Phosphorous, Total (SM 4500 P E-1997) —The SOP references the 18th Edition of
Standard Methods rather than Standard Methods Committee approval year.
o COD (SM 6220 D-1997) — The SOP references the 18th Edition of Standard Methods
rather than Standard Methods Committee approval year.
o BOD/CBOD (SM 5210 B-2001) —The SOP references the 18th Edition of Standard
Methods rather than Standard Methods Committee approval year.
o Nitrogen, Ammonia (SM 4500 NH3 D-1997) —The SOP references the 18th Edition of
Standard Methods rather than Standard Methods Committee approval year.
Personnel were not following procedures as stated in the Laboratory's SOP.
o Metals (EPA 200.8, Rev 5.4, 1994) —The SOP states that the duplicate acceptance
criterion is 10% RPD, but the analyst uses 20% RPD.
o Metals (EPA 200.8, Rev 5.4, 1994) —The SOP states that a sample duplicate is being
analyzed instead of a Laboratory Fortified Matrix Duplicate (LFMD).
The SOP does not describe in detail how the method is performed.

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o Dissolved Oxygen (SM 4500 G-2001) — The SOP contains use of the word "should"
instead of "must" in the sections of Sampling and Holding Time.
o pH (SM 4500 H+ B-2000) — The SOP contains use of the word "should" instead of
"must" in the Holding Time section.
o pH (SM 4500 H+ B-2000) — The SOP does not state the check standard buffer
acceptance criterion (i.e., ±0.1 SU).
o Phosphorous, Total (SM 4500 P E-1997) — The cell path length and wavelength are
not specified in the SOP.
o Phosphorous, Total (SM 4500 P E-1997) — The SOP does not include the sample
digestion procedure.
o Phosphorous, Total (SM 4500 P E-1997) — The spectrophotometer set-up section
lacks detail about instrument warm up.
o Phosphorous, Total (SM 4500 P E-1997) — Sections 3.a.1 and 3.a.2 of the SOP are
lacking units (i.e., 5.0 Second Source Standard).
o Phosphorous, Total (SM 4500 P E-1997) — The SOP does not include the calibration
blank acceptance criterion.
o Phosphorous, Total (SM 4500 P E-1997) — The SOP does not include the
acceptance criterion for LFM recovery.
o Phosphorous, Total (SM 4500 P E-1997) — The SOP does not include the addition of
30 mL of ascorbic acid to the single acid reagent.
o BOD/CBOD (SM 5210 B-2001) — Section D.5. of the SOP does not detail how the
residual chlorine of samples is checked.
o BOD/CBOD (SM 5210 B-2001) — Section D.9. of the SOP does not include directions
to seed the sample if it is greater than 6 hours past collection.
o BOD/CBOD (SM 6210 B-2001) — The SOP does not specify the CBOD acceptance
criterion. This may be set at 164 ± 30.7 mg/L [allowed by EPA for CBOD] or 198 ±
30.5 mg/L [specified in the method]; however, one range must be chosen and
consistently used.
o BOD/CBOD (SM 5210 B-2001) — The SOP does not state that nitrification inhibitor is
added to the CBOD GGA standards.
o BOD/CBOD (SM 6210 B-2001) — Section EA. specifies the number of dilutions for
influent and effluent samples but not pretreatment/industry samples.
o Metals (EPA 200.8, Rev 5.4, 1994) — The SOP does not specify what type of bottle
(i.e., polypropylene) is used for sample collection.
o Metals (EPA 200.8, Rev 5.4, 1994) — The SOP does not describe the manufacturer
recommended operating conditions of the ICP/MS instrument.
o Metals (EPA 200.8, Rev 5.4, 1994) — Section E.7 of the SOP has instances where
"should" is used in place of "must".
o Metals (EPA 200.8, Rev 6.4, 1994) — Section C of the SOP does not state the
strength of HNO3 used (i.e., 1+1).
o Metals (EPA 200.8, Rev 5.4, 1994) — The SOP does not include reagent and standard
preparation instructions (e.g., 1+1 HNO3, LFM, etc).
o Metals (EPA 200.8, Rev 6.4, 1994) — The SOP does not state the manufacturer's
conditions for an acceptable tune to evaluate against the requirements in Section
10.2.2 of the method.
o Metals (EPA 200.8, Rev 5.4, 1994) — The SOP does not state which specific internal
standards are used.
o Metals (EPA 200.8, Rev 5.4, 1994) — The SOP does not state that samples are
preserved with HNO3 to pH <2 at least 24 hours prior to analysis.
o Metals (EPA 200.8, Rev 5.4, 1994) — The SOP does not include the 18 om water
rinse in the glassware instructions.

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#65 TZ Osborne WRF Laboratory
o Metals (EPA 200.8, Rev 5.4, 1994) — The SOP does not state the masses being
monitored.
o Metals (EPA 200.8, Rev 5.4, 1994) — The SOP does not describe the sample results
reporting scheme (e.g., For all sample analyses, a minimum of three replicate
integrations are reported for data acquisition. Use the average of the integrations for
data reporting.).
o Metals (EPA 200.8, Rev 5.4, 1994) — The SOP does not state the frequency (e.g.,
quarterly) and acceptance criterion (i.e., ±10%) for the Quality Control Standard
(QCS).
o Metals (EPA 200.8, Rev 5.4, 1994) — The SOP does not describe how to calculate
and report sample results (e.g., use of significant figures, dilution factors, units, etc.).
o Metals (EPA 200.8, Rev 5.4, 1994) — The SOP does not state that an initial
demonstration of performance, consisting of a determination of the linear calibration
range, analysis of quality control samples and determination of method detection
limits, must be performed prior to analyses conducted and any time a change in
instrument hardware or operating conditions are made.
o Metals (EPA 200.8, Rev 5.4, 1994) — The SOP does not state the acceptance criteria
for blanks (e.g., continuing calibration blanks, laboratory reagent blank)
o Nitrogen, Ammonia (SM 4500 NH3 D-1997) — The SOP does not state how the
sample is checked for total residual chlorine.
o Nitrogen, Ammonia (SM 4500 NH3 D-1997) — The SOP does not include the
calculation needed when differing amounts of NaOH are added to calibration
standards and samples.
o Nitrogen, Ammonia (SM 4500 NH3 D-1997) — The SOP does not explicitly state that
a LFMD is being analyzed although it does give an acceptance criterion for precision
(i.e., relative percent difference).
o Chlorine, Total Residual (SM 4500 CI G- 2000) — The SOP does not state the
acceptance criterion for the annual calibration curve verification.
o Chlorine, Total Residual (SM 4500 Cl G- 2000) — The SOP does not state what
standard concentrations are used to verify the factory -set calibration.
o Chlorine, Total Residual (SM 4500 CI G- 2000) — The calculation section of the SOP
does not state that the blanking reagent value is subtracted from the sample result.
o Chlorine, Total Residual (SM 4500 CI G- 2000) — The SOP does not state to record
the calibration time.
o COD (SM 5220 D-1997) — The SOP for COD held little to no description of the quality
control elements for the parameter. This includes but may not be limited to; the
reporting limit, the 5-point calibration curve, LCS, duplicates, blanks, QC acceptance
criteria, and the spiking procedure.
The SOP is in direct conflict with the method and/or a regulatory requirement.
o pH (SM 4500 H+ B-2000) — The SOP does not state that the 4 SU check buffer is
analyzed after calibration with 7 SU and 10 SU buffers. This means the sample values
would not be bracketed with calibration and/or check buffers..
o Phosphorous, Total (SM 4500 P E-1997) — The SOP states that the single reaction
reagent can be stored at 40C and is stable for one week, but the method states it is
only stable for 4 hours.
o BOD/CBOD (SM 6210 B-2001) — Section C of the SOP includes holding time
information from Standards Methods, but this would not apply as 40 CFR Part 136.3,
Table II takes precedent.
o BOD/CBOD (SM 5210 B-2001) — Section D.6. does not include instructions to titrate
the sample aliquot to the end point and then add the appropriate amount of sodium
sulfite to the sample.

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#65 TZ Osborne WRF Laboratory
o BOD/CBOD (SM 5210 B-2001) — The SOP states that only 2 glucose glutamic acid
(GGA) checks are analyzed.
o BOD/CBOD (SM 5210 B-2001) — The SOP states that data is qualified when the
dilution water blank depletes >0.2 mg/L, but the requirement is >0.20 mg/L.
o BOD/CBOD (SM 5210 B-2001) — Section B of the SOP states that 2 dilutions are
analyzed per sample, but the method requires at least three dilutions per sample.
o BOD/CBOD (SM 5210 B-2001) — The SOP states that the meter is recalibrated after
every 10 samples. This is only required if the drift check is unacceptable (i.e., not
within ±0.2 mg/L).
o Bacteria- Coliform Fecal (SM 9222 D-1997) — The SOP does not state that reagent
water testing is performed yearly as required by Standard Methods, 9020 B-2005.
Table 9020:11. NC WW/GW LC Policy only requires the testing of certain analytes in
the referenced table. These include conductivity, TOC, Cadmium, Chromium, Nickel,
Lead, and Zinc.
o Nitrogen, Ammonia (SM 4500 NH3 D-1997) — The SOP states that the meter is
performing a blank correction, which is not allowed by the method.
o Nitrogen, Ammonia (SM 4500 NH3 D-1997) — The SOP states that the acceptance
criterion for the second source laboratory control standard (LCS) is ±20% recovery, but
the method states ±15%. The checklist completed by the laboratory states that ±10%
is used.
o Nitrogen, Ammonia (SM 4500 NH3 D-1997) — The SOP only lists one concentration
for the LCS (i.e., 0.05 mg/L). An additional 0.5 mg/L LCS is required and is analyzed
on the high range curve.
The laboratory does not have an SOP for the certified parameter.
o Temperature (SM 2550 B-2000)
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). Please submit updated SOPs with the items listed above addressed
by December 1, 2015.
Residue, Suspended — Standard Methods, 2540 D-1997
G. Finding: The verified thermometer reading varied more than 1 °C from the NIST traceable
thermometer reading.
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 than or equal to 1°C from the NIST certified or NIST
traceable thermometer reading. Ref: NC WW/GW LC Policy.
Comment: The thermometer used in the suspended residue oven has a correction of + 2°C.

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#65 TZ Osborne WRF Laboratory
Phosphorous, Total — Standard Methods, 4500 P E-1999
Comment: The laboratory performs an acid wash on the glassware once a month. The method implies
glassware is acid washed before each use. Once the analysis of a method blank is implemented (see
Finding H), monitor the blank values on randomly selected glassware to determine if more frequent acid
washing is required.
Recommendation: The laboratory is adding 0.5 mg of ammonium persulfate during digestion but section
5.c of Standard Methods, 4500 P B-1997 states to use 0.4 mg. Since the ammonium persulfate is used
as a catalyst, it is unlikely that this negligible difference will affect the results. No issues were evident in
the recovery of the digested standards for the data reviewed. Despite this, we recommend the laboratory
start using 0.4 mg of ammonium persulfate as stated in the method.
Comment: The laboratory was not analyzing 6 non -zero standard concentrations in the calibration curve.
The instrument (i.e., Thermo Scientific Genesys 20) was not able to store a calibration curve, so each day
the analyst was unknowingly performing a one standard calibration instead of analyzing a check standard
against a stored calibration curve. Standard Methods, 4500 P E-1999. (4) (c) states: Prepare individual
calibration curves from a series of six standards within the phosphate ranges indicated in 4500 P.E.1 c.
Notification of acceptable corrective action (i.e., the laboratory is analyzing samples using a Hach
DR3900 meter with a 6 non -zero point curve that the analyst constructed on August 3, 2015 and is
stored in the meter) was received by email on September 21, 2015, "with implementation of sample
analysis on August 20, 2015. No further response is necessary for this Finding.
Comment: The laboratory submitted notification on July 30, 2015, that all samples for total phosphorous
analysis are being sent to a contract lab until calibration issues have been satisfactorily resolved.
H. Finding: The laboratory is not analyzing a method blank.
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-2009, Rev. 2011. (2) (d).
Requirement: A reagent blank (method blank) consists of reagent water and all reagents (including
preservatives) that normally are in contact with a sample during the entire analytical procedure. Ref:
Standard Methods, 1020 B-2011. (5).
Finding: A calibration blank is not analyzed initially after calibration.
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. Ref: NC WW/GW LC Policy.
J. Finding: A calibration blank and mid -range standard are not analyzed at the end of analysis.
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. Ref: NC WW/GW LC Policy.
K. Finding: Documentation of the time samples are placed into the autoclave and autoclave maximum
temperature and pressure are not linked to the applicable batch of samples. This is considered
pertinent information.

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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: 15 NCAC 2H .0805 (a) (7)
(A).
Requirement: Each day an incubator, oven, waterbath or refrigerator is used, the temperature
must be checked recorded, and initialed. During each use the autoclave maximum temperature
and pressure must be checked recorded, and initialed. Ref: 15 NCAC 2H .0805 (a) (7)
Requirement: Alternately, heat for 30 min in an autoclave or pressure cooker at 98 to 137 kPa.
Ref: Standard Methods, 4500 P B-1999. (5) (c).
Recommendation: The laboratory's autoclave prints a log of time, temperature and pressure
during each use. It is recommended that the log printed each time samples are autoclaved be
initialed and attached to the total phosphorous benchsheet to satisfy the documentation
requirement.
L. Finding: The laboratory is using the wrong spike concentration when calculating the LFM recovery.
Requirement: LFM recovery:
(CSXfj — C X 100 = %Recovery LFM or LFMD
S
where:
CS = LFM concentration determined experimentally,
f= spike dilution correction,
C = concentration of sample before spiking, and
S = concentration of spike.
NOTE: f should be greater than 0.95. More than 5% dilution due to spiking changes the matrix
significantly. Ideally keep f to above 0.99 (equivalent to 1 % dilution of sample due to spike
addition), in which case f can be ignored and the equation simplified to eliminate f.
Ref: Standard Methods, 4020 B-2009, Rev. 2011. (3) (a).
Comment: Instead of using the true concentration of the spike that is added to the LFM, the
laboratory is using the experimentally determined concentration obtained for the LFB.
Comment: The note above from Standard Methods states that the volume of spike should be <5%
of the total, but as a reminder, NC WW/GW LC policy allows up to 10% as long as spike volumes
above 1 % are corrected through calculation.
M. Finding: The laboratory is not analyzing a LFMD.
Requirement: Include at least one LFM/LFMD daily or with each batch of 20 or fewer samples. Ref:
SM 4020 B-2009, Rev. 2011, Table 4020:1 and (2) (g).
Comment: LFM and LFMD are also known a Matrix Spike (MS) and Matrix Spike Duplicate (MSD).
Comment: Analysis of the LFMD (or MSD) is acceptable to satisfy the sample duplicate
requirement listed in North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (C).

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N. Finding: The laboratory is exceeding 1 % sample volume with spike solution when preparing matrix
spikes and is not using the proper correction factor when calculating the final result.
Requirement: The volume of spike solution used in matrix spike preparation must in all cases be
<_ 10% of the total matrix spike volume. It is preferable that the spike solution constitutes <_ 1 % of
the total matrix spike volume so that the matrix spike can be considered a whole volume sample
with no adjustment 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. Ref: NC WW/GW LC Policy.
Recommendation: It is recommended that the spike solution constitutes :51 % of the total LFM
volume. The laboratory is currently preparing LFMs with 4% spike volume.
BOD/CBOD — Standard Methods, 5210 B-2001
Comment: The laboratory may choose to adopt the less stringent duplicate acceptance criterion of 30%
RPD as prescribed in the method.
Comment: The laboratory is reminded that data does not need to be flagged for seed control factors
(SCF) above 1.0 mg/L as long as there is evidence to show that a higher SCF is necessary to obtain an
acceptable GGA recovery. This may also be removed from the benchsheet.
Comment: The laboratory is reminded that the meter does not need to be calibrated at the end of
analysis.
Recommendation: It is recommended that a seeded blank be analyzed with industrial samples as is
being done with the facility's influent and effluent samples.
Comment: The laboratory was only setting up one GGA standard with industrial samples. Standard
Methods, 5210 B-2001. (6) (b) states: Add sufficient amounts of standard glucose-glutamic acid solution
(¶ 3h) to give 3.0 mg glucose/L and 3.0 mg glutamic acid/L in each of three test bottles (20 mL GGA
solution/L seeded dilution water or 6.0 mU300-mL bottle). Demonstration of acceptable corrective action
(i.e., an industrial waste COC/analysis benchsheet with 3 GGA standards typed permanently on the
benchsheet was received by email on July 30, 2015 and implemented on August 3, 2015. No further
response is necessary for this Finding.
O. Finding: The laboratory is only duplicating the influent sample.
Requirement: Duplicates: When appropriate (Table 5020:1), randomly select routine samples to be
analyzed twice. Ref: Standard Methods, 5020 B- 2010. (2) (f).
Residue, Suspended — Standard Methods, 2540 D-1997
Comment: The laboratory was not seating the filter with water prior to filtering the sample. Standard
Methods, 2540 D-1997. (3) (c) states: Assemble filtering apparatus and filter and begin suction. Wet filter
with a small volume of reagent -grade water to seat it. Demonstration of acceptable corrective action (i.e.,
an updated SOP with the filter seating step added) was received by email on July 30, 2015, with a stated
implementation date of August 3, 2015. No further response is necessary for this Finding.
Comment: The laboratory was filtering longer than the method allowed maximum of 10 minutes.
Laboratory practice was to filter between 15 and 20 minutes. Standard Methods, 2540 D-1997. (3) (b)
states: If complete filtration takes more than 10 minutes increase filter diameter or decrease sample

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volume. Standard Methods, 2540 D-1997. (1) (b) states: Prolonged filtration times resulting from filter
clogging may produce high results owing to increased colloidal materials captured on the clogged filter.
Demonstration of acceptable corrective action (i.e., an updated SOP with directions to decrease sample
volume if filtration takes longer than 10 minutes) was received by email on July 30, 2015, with a stated
implementation date of August 3, 2015. No further response is necessary for this Finding.
Comment: The laboratory was not adjusting the reporting limit for the amount of sample analyzed when
less than 2.5 mg of dried residue was obtained on volumes less than 1000mL. NC WW/GW LC Policy
states: 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 pain is less than the required 2.5
mg the value must be reported as less than the appropriate value based upon the volume used.
Demonstration of acceptable corrective action (i.e., an updated SOP stating the proper adjustment of the
reporting limit and a statement that it was implemented in practice as of August 3, 2015) was received by
emails on July 30, 2015 and August 6, 2015. No further response is necessary for this Finding.
Bacteria- Coliform Fecal — Standard Methods, 9222 D-1997
Comment: The fecal water bath temperature was only being checked once per day. Standard Methods,
9020 B-2005. (4) (n) states: When incubator is in use, monitor and record calibration -corrected
temperature twice daily. This is a new method requirement since the last inspection. Notification of
acceptable corrective action (i.e., an updated SOP stating temperatures are checked twice daily and a
statement that it was implemented in practice as of August 3, 2015) was received by emails on July 30,
2015 and August 6, 2015. No further response is necessary for this Finding.
Comment: A total immersion thermometer was being used in the fecal water bath improperly. The
Environmental Protection Agency's (EPA) guidance website titled "Selecting Alternatives to Mercury -Filled
Thermometers" states: 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. Notification of
acceptable corrective action (i.e., a statement that a NIST traceable partial immersion thermometer with
corrections of 0.06°C at 40°C and 0.00°C at 500C was ordered and received and is being used in the
fecal water bath immersed to the specified immersion line) was received by email on July 30, 2015 and
September 18, 2015 with implementation on July 29, 2015. No further response is necessary for this
Finding.
Comment: The laboratory was not testing a culture positive weekly for purchased MFC broth. Standard
Methods, 9020 B-2005. (9) (b) states: Use certified reference cultures. For each lot of medium received,
each laboratory prepared batch of medium, and each lot of purchased prepared medium, verify
appropriate response by testing with known positive and negative control cultures for the organism(s)
under test. Record results. This is a new method requirement since the last inspection. Demonstration of
acceptable corrective action (i.e., an updated SOP stating that a culture positive is tested weekly with the
purchased MFC broth and an updated benchsheet with a space for the weekly culture positive check)
was received by email on July 30, 2015, with implementation of the practice on August 3, 2015. No
further response is necessary for this Finding.
Comment: The laboratory was not sterilizing the magnesium chloride solution. Standard Methods, 9050
C-2006. (1) (a) (2) states: Magnesium chloride stock solution: Add magnesium chloride (38 g/L MgC12 or
81.1 9 MgC12 - 6H2O) to 1 L reagent grade water. Sterilize and store stock solution under refrigerated

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#65 TZ Osborne WRF Laboratory
conditions, discarding if solution becomes turbid. Demonstration of acceptable corrective action (i.e., an
updated SOP stating the magnesium chloride solution is sterilized) was received by email on July 30,
2015, with implementation of the practice on August 3, 2015. No further response is necessary for this
Finding.
Comment: The filtration start and end times were not being documented. This is considered pertinent
information to assure plates are placed into the incubator within 30 minutes of filtration. The North
Carolina Administrative Code, 15 NCAC 2H .0805 (a) (7) (A) states: All analytical data pertinent to each
certified analysis must be filed in an orderly manner so as to be readily available for inspection upon
request. Standard Methods 9222 D-1997. (2) (d) states: Place all prepared cultures in the water bath
within 30 min after filtration. Demonstration of acceptable corrective action (i.e., an updated SOP and
updated benchsheet with spaces to enter the filtration start and end times) was received by email on July
30, 2015, with implementation of the practice on August 3, 2015. No further response is necessary for
this Finding.
Comment: The laboratory was not conducting comparison testing on new lots of consumables (i.e.,
membrane filters, pads, and media). NC WW/GW LC Policy states: When a new lot of culture medium,
pads, or membrane filters is to be used, a comparison of the current lot in use (reference lot) against the
new lot (test lot), be made. As a minimum, make single analyses on five positive samples. Demonstration
of acceptable corrective action (i.e., an updated SOP including the comparison testing on new lots of
consumables) was received by email on July 30, 2015, with implementation of the practice on August 3,
2015. Please submit the first comparison test that is completed.
Comment: The laboratory was not conducting a monthly recount of a positive plate by one analyst and
comparison counts between analysts. Standard Methods, 9020 B-2005. (9) (a) states: 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. Demonstration of acceptable corrective action
(i.e., an updated SOP including monthly recounts of a positive plate by one analyst and comparison
counts between analysts) was received by email on July 30, 2015, with implementation of the practice on
August 3, 2015. No further response is necessary for this Finding.
P. Finding: Heat indicating autoclave tape is not used on all materials with 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).
Q. Finding: The pH of the stock phosphate buffer solution is not documented. This is considered
pertinent information to show that the pH is 7.2 ± 0.5 s.u.
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: Stock phosphate buffer solution - Dissolve 34.0 g potassium dihydrogen phosphate
(KH2PO4) in 500 mL reagent grade water, adjust to pH 7.2 ± 0.5 with 1N NaOH and dilute to 1 L
with reagent grade water. Ref: Standard Methods, 9050 C-2006. (1) (a) (1).

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Nitroaen. Ammonia — Standard Methods, 4500 NH3 D-1997
Comment: The SOP only lists one acceptance criterion for the calibration blank (i.e., <_ 0.05 mg/Q. This
is correct for the low range curve, but the calibration blank acceptance criterion for the high range curve
can be up to <_ 0.5 mg/L.
Comment: Calibration time for the low range and high range curve was being documented, but the
analysis time of the low range samples was not. This is considered pertinent information to show that
analysis is conducted after calibration. The North Carolina Administrative Code, 15 NCAC 2H .0805 (a)
(7) (A) states: All analytical data pertinent to each certified analysis must be filed in an orderly manner so
as to be readily available for inspection upon request. Demonstration of acceptable corrective action (i.e.,
a benchsheet including a space for low range sample analysis time) was received by email on July 30,
2015, with implementation on August 3, 2015. No further response is necessary for this Finding.
R. Finding: Samples are not being checked for total residual chlorine (TRC) and treated, if necessary,
at time of collection.
Requirement: Residual Chlorine reacts with ammonia; remove by sample pretreatment. If a sample
is likely to contain residual chlorine, immediately upon collection, treat with dechlorinating agent as
in 4500-NH3.B.3d. Ref: Standard Methods, 4500 NH3 A-1997. (2).
Comment: Samples are checked and treated for TRC immediately prior to sample analysis. Once
the Finding is corrected, the laboratory is reminded that dechlorinating agents used at the time of
sampling must be documented to have been effective upon receipt in the laboratory.
S. Finding: Samples are not allowed to come to room temperature before analysis.
Requirement: Place 100 mL sample in 150 mL beaker and follow procedure in ¶ 4b above. Ref:
Standard Methods, 4500 NH3 D-1997. (4) (e).
Requirement: Maintain the same stirring rate and a temperature of about 250C through calibration
and testing procedures. Ref: Standard Methods, 4500 NH3 D-1997. (4) (b).
T. Finding: The true value of the LFM is not documented.
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).
Comment: The true value of quality control samples and percent recovery obtained must be
documented on the benchsheet and evaluated against established acceptance criteria to
demonstrate that the analyst was aware of any out -of -control situation.
U. Finding: Preservation acid is not being added to the method blank and LFB.
Requirement: A reagent blank (method blank) consists of reagent water (see Section 1080) and all
reagents (including preservative) that normally are in contact with a sample during the entire
analytical procedure. Ref: Standard Methods, 1020 B-2011. (5).
Requirement: A laboratory -fortified blank [laboratory control standard (LCS)] is a reagent water
sample (with associated preservatives) to which a known concentration of the analytes(s) of interest
has been added. Ref: Standard Methods, 1020 B-2011. (6).

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V. Finding: The LFM is only performed on the TZO Primary (process control) sample.
Requirement: To prepare an LFM, add a known concentration of analytes (ideally from a second
source) to a randomly selected routine sample without decreasing its volume by more than 5%. Ref:
Standard Methods 4020 B- 2009, Rev. 2011. (2) (g).
Comment: The LFM needs to be rotated through all types of samples, including industry, to
demonstrate there is no bias contributed to the analytical results by any matrix encountered for
routine samples.
W. Finding: The volume of NaOH (ISA solution) used to raise the pH > 11 is not documented. This is
considered pertinent information.
Requirement: Add a sufficient volume of 1 ON 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: 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).
Metals — EPA Method 200.8, Rev. 5.4, 1994
Comment: When the use of Kinetic Energy Discrimination (KED) is implemented for chloride and other
halide ion interference reduction, perform a study to demonstrate that it does not cause magnification of
other interferences (which may happen in some effluents) and to demonstrate that sensitivity is not
reduced. Include instruction for KED use and a validation study in the SOP. This validation study may
either be attached to the SOP or kept on file. The study must consist of analyzing a minimum of 10
samples and standards side -by -side with and without the KED. It is recommended that the KED be used
for all analyses to reduce the number of curves that would have to be run. If not used routinely, you must
analyze a curve that reflects this addition, when in use. This study is a new requirement by EPA Region 4.
Recommendation: It is recommended that the sequential run log be printed daily.
Recommendation: It is recommended that the laboratory periodically prepare and analyze a field blank
that is placed in a sample container in the laboratory and treated as a sample in all respects, including
shipment to the sampling site, exposure to the sampling site conditions, storage, preservation, and all
analytical procedures.
Recommendation: It is recommended that instructions for saving electronic batch files be added to the
SOP.
X. Finding: The laboratory was not documenting sample pH and ID, acid lot numbers, or rotating cell
temperature checks. 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).

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Comment: The sample pH and ID, acid lot numbers, and rotating cell temperature checks can be
added to the newly developed digestion log.
Y. Finding: The laboratory is only spiking the effluent sample.
Requirement: Unless otherwise specified by the data user, laboratory or program, the following
laboratory fortified matrix (LFM) procedure (Section 9.4.2) is required. Ref: Method 200.8, Rev. 5.4
(1994), Section 9.4.1.
Requirement: Over time, samples from all routine sample sources should be fortified. Ref: EPA
Method 200.8, Rev. 5.4 (1994), Section 9.4.2.
Z. Finding: Raw data printed from ICP/MS analyses is not initialed by the analyst.
Requirement: All laboratories must use printed bench worksheets that include a space to enter
the signature or initials of the analyst, date of analyses, sample identification, volume of samples
analyzed, value from the measurement system, factor and final value to be reported and each
item must be recorded each time samples are analyzed. The date and time BOD and coliform
samples are removed from the incubator must be included on the laboratory worksheet. Ref: 15A
NCAC 2H .0805 (a) (7) (H).
Comment: The analyst must initial the raw data printed from ICP/MS analyses to verify the data
produced.
AA. Finding: The analyst does not consistently document sample dilution factors.
Requirement: All laboratories must use printed bench worksheets that include a space to enter the
signature or initials of the analyst, date of analyses, sample identification, volume of samples
analyzed, value from the measurement system, factor and final value to be reported and each item
must be recorded each time samples are analyzed. The date and time BOD and coliform samples
are removed from the incubator must be included on the laboratory worksheet. Ref: 15A NCAC 2H
.0805 (a) (7) (H).
BB. Finding: The temperature of the hot block during acid digestion is not 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: 15 NCAC 2H .0805 (a) (7)
(A).
Requirement: To the beaker add 4 mL of (1+1) HNO and 10 mL of (1+4) HCl. Cover 3 the lip of the
beaker with a watch glass. Place the beaker on a hot plate for reflux extraction of the analytes. The
hot plate should be located in a fume hood and previously adjusted to provide a reflux temperature
of approximately 950C. (See the following note.) Note: For proper heating adjust the temperature
control of the hot plate such that an uncovered Griffin beaker containing 50 mL of water placed in
the center of the hot plate can be maintained at a temperature approximately but no higher than
85°C. (Once the beaker is covered with a watch glass the temperature of the water will rise to
approximately 200.8-26 95°C.) Also, a block digester capable of maintaining a temperature of 95°C
and equipped with 250 mL constricted volumetric digestion tubes may be substituted for the hot
plate and conical beakers in the extraction step. Ref: EPA Method 200.8, Rev. 5.4 (1994), Section
11.3.3.

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#65 TZ Osborne WRF Laboratory
CC. Finding: The laboratory is not applying an acceptance criterion (i.e., :550% of the reporting limit) to
the blanks.
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 analyst noted that he does monitor the blank values.
DD. Finding: The laboratory has not completed all components of the method required Initial
Demonstration of Performance.
Requirement: The initial demonstration of performance is used to characterize instrument
performance (determination of linear calibration ranges and analysis of quality control samples) and
laboratory performance (determination of method detection limits) prior to analyses conducted by
this method.
Comment: The instrument is currently shut down while the air handling system in that unit is being
upgraded. An Initial Demonstration of Performance will be required prior to analyzing samples. The
NC WW/GW LC linear calibration/dynamic range policy is attached to the end of this report.
EE. Finding: The laboratory lacks traceability for the preparation of calibration standards, quality control
standards, consumables and reagents.
Requirement: All chemicals, reagents, standards and consumables used by the laboratory must
have the following information documented: Date received, Date Opened (in use), Vendor, Lot
Number, and Expiration Date (where specified). A system (e.g., traceable identifiers) must be in
place that links standard/reagent preparation information to analytical batches in which the solutions
are used. Documentation of solution preparation must include the analyst's initials, date of
preparation, the volume or weight of standard(s) used, the solvent and final volume of the solution.
This information as well as the vendor and/or manufacturer, lot number, and expiration date must
be retained for primary standards, chemicals, reagents, and materials used for a period of five
years. Consumable materials such as pH buffers, lots of pre -made standards and/or media, solids
and bacteria filters, etc. are included in this requirement. Ref: NC WW/GW LC Policy.
FF. Finding: When checking the sample pH to verify pH <2, the value, time, and date are not being
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: 15 NCAC 2H .0805 (a) (7)
(A).
Comment: This information is needed to verify that 24 hours have passed between time of proper
preservation and analysis.
GG. Finding: The laboratory reagent blank (LRB) and LFB are not filtered through the digifilter before
analysis.
Requirement: Laboratory Fortified Blank (LFB) - An aliquot of LRB to which known quantities of the
method analytes are added in the laboratory. The LFB is analyzed exactly like a sample, and its
purpose is to determine whether the methodology is in control and whether the laboratory is capable
of making accurate and precise measurements. Ref: EPA Method 200.8, Rev. 5.4 (1994), Section
3.8.

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#65 TZ Osborne WRF Laboratory
Requirement: Laboratory Reagent Blank (LRB) - An aliquot of reagent water or other blank
matrices that are treated exactly as a sample including exposure to all glassware, equipment,
solvents reagents and internal standards that are used with other samples. Ref: EPA Method
200.8, Rev. 5.4 (1994), Section 3.10.
HH. Finding: The laboratory is not performing the method defined tune procedure.
Requirement: Precalibration routine - The following precalibration routine must be completed prior
to calibrating the instrument until such time it can be documented with periodic performance data
that the instrument meets the criteria listed below without daily tuning. 10.2.1 Initiate proper
operating configuration of instrument and data system. Allow a period of not less than 30 minutes
for the instrument to warm up. During this process conduct mass calibration and resolution checks
using the tuning solution. Resolution at low mass is indicated by magnesium isotopes 24, 25, and
26. Resolution at high mass is indicated by lead isotopes 206, 207, and 208. For good performance
adjust spectrometer resolution to produce a peak width of approximately 0.75 amu at 5% peak
height. Adjust mass calibration if it has shifted by more than 0.1 amu from unit mass. 10.2.2
Instrument stability must be demonstrated by running the tuning solution (Section 7.7) a minimum of
five times with resulting relative standard deviations of absolute signals for all analytes of less than
5%. Ref: EPA Method 200.8, Rev. 5.4 (1994), Section 10.2.
Comment: The laboratory was conducting the Perkin Elmer (PE) Performance Check; however,
this performance check was not always repeated if a target failure occurred.
II. Finding: The recovery and precision for quality control elements is not consistently documented.
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 21-1.0805 (a) (7).
Comment: The true value of quality control samples and percent recovery obtained must be
documented on the benchsheet and evaluated against established acceptance criteria to
demonstrate that the analyst was aware of any out -of -control situation.
Chlorine, Total Residual — Standard Methods, 4500 Cl G- 2000
Comment: There does not seem to be an official copy of the benchsheet in use. Reviewing past data
showed that the date of the calibration curve verification was not consistent. One of the most recent
benchsheets listed a calibration curve verification date of 7/29/2011.
Comment: The TRC benchsheet did not contain chemical, reagent, or consumable traceability
information, instrument identification, or meter calibration verification time. The Approved Procedure for
the Analysis of Total Residual Chlorine document states: The following must be documented in indelible
ink whenever sample analysis is performed: Meter calibration and meter calibration time(s), Traceability
for chemicals, reagents, standards, and consumables, and Instrument identification. Demonstration of
acceptable corrective action (i.e., an updated benchsheet with spaces to enter traceability information,
instrument identification and meter calibration verification time) was received by email on July 30, 2015
and implemented on August 3, 2015. No further response is necessary for this finding.
JJ. Finding: The annual calibration curve verification does not bracket the concentration of the annual
Proficiency Testing (PT) samples.

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#65 TZ Osborne WRF Laboratory
Requirement: For analytical procedures requiring analysis of a series of standards, the
concentrations of those standards must bracket the concentration of the samples analyzed. One of
the standards must have a concentration equal to the laboratory's lower reporting concentration for
the parameter involved. Ref: 15A NCAC 02H .0805 (a) (7) (1).
Recommendation: The concentrations used to verify the most recent curve are 14, 50, 100, 150
and 200 pg/L. The assigned value of the 2015 PT sample was 224 pg/L. It is recommended that
the laboratory verify the internal curve with a standard concentration between the lowest standard
and 50 pg/L and up to 400 pg/L. This will verify the analytical range used to measure Proficiency
Testing (PT) samples as well as environmental samples.
KK. Finding: Results were not qualified for a sample analyzed outside of hold time.
Requirement: At any time a laboratory receives samples which do not meet sample collection,
holding time, or preservation requirements, the laboratory must notify the sample collector or client
and secure another sample if possible. If another sample cannot be secured, the original sample
may be analyzed but the results reported must be qualified with the nature of the infraction(s) and
the laboratory must notify the State Laboratory about the infraction(s). The notification must include
a statement indicating corrective actions taken to prevent the problem for future samples. Ref: 15A
NCAC 2H .0805 (a) (7) (N).
Comment: On January 9, 2015, the North Buffalo effluent was collected at 8:50 am and analyzed
at 9:15 am, which exceeded the holding time of 15 minutes.
ILL. Finding: The laboratory is not analyzing a reagent blank with the standard curve verification nor the
daily sample analyses.
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 quality
control 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 standard
concentration), unless otherwise specified by the reference method, or corrective action must be
taken.
MM. Finding: The laboratory is filtering samples for TRC analysis.
Requirement: Compensate for color and turbidity by using sample to zero photometer. Ref:
Standard Methods, 4500 Cl G-2000. (1) (b).
Comment: The laboratory is currently following the procedure as described in the Hach 10014 ULR
method. Standard Methods, 4500 CI G- 2000, the method for which the laboratory is certified, does
not allow for filtering of samples. However, if the laboratory chooses to update their certificate to cite
Hach 10014 ULR, they would be required to continue filtering the sample.

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PH — Standard Methods, 4500 H+ B-2000
Comment: Values were reported that exceed the method specified accuracy of 0.1 units. Standard
Methods, 4500 H+ B-2000, (6) states in part: 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. Notification of acceptable corrective action (i.e., a
statement that pH results would be reported to 0.1 units) was received by e-mail on July 30, 2015 with
a stated implementation date of August 3, 2015. No further response is necessary for this Finding.
Temperature — Standard Methods, 2550 B-2000
Comment: The benchsheet did not document the time of sample analysis. The North Carolina
Administrative Code, 15 NCAC 2H .0805 (g) (1) states: Data pertinent to each analysis must be
maintained for five years. Certified Data must consist of date collected, time collected, sample site,
sample collector, and sample analysis time. The field bench sheets must provide a space for the
signature or initials of the analyst, and proper units of measure for all analyses. Demonstration of
acceptable corrective action (i.e., an updated benchsheet with a space to enter analysis time) was
received by email on July 30, 2015 and implemented on August 3, 2015. No further response is
necessary for this Finding.
Dissolved Oxycien — Standard Methods, 4500 O G-2001
Comment: The benchsheet did not include units of measure for the DO meter calibration. This is
considered pertinent information. The North Carolina Administrative Code, 15A NCAC 02H .0805 (g) (1)
states: Data pertinent to each analysis must be maintained for five years. Certified Data must consist of
date collected, time collected, sample site, sample collector, and sample analysis time. The field bench
sheets must provide a space for the signature or initials of the analyst, and proper units of measure for
all analyses. Demonstration of acceptable corrective action (i.e., an updated benchsheet with units of
measure for the DO meter calibration) was received by email on July 30, 2015 and implemented on
August 3, 2015. No further response is necessary for this Finding.
COD —Standard Methods, 5220 D-1997
Comment: The laboratory does not analyze COD samples except for the yearly PT sample. The
laboratory had indicated that they may request to drop the parameter from their certificate, but it has not
been requested at this time. The SOP for COD did not contain any mention of quality control elements
including: the reporting limit, the calibration curve, LCS, duplicates, blanks, acceptance criteria, or matrix
spiking. If the laboratory decides to maintain certification for COD the SOP will have to be revised and
submitted. Please respond in writing as to whether COD certification will be dropped or
maintained.
NN. Finding: No QC standards are analyzed.
Requirement: The following are requirements for certification and must be included in each
certified laboratory's quality control program. (D) Any quality control procedures required by a
particular approved method shall be considered as required for certification for that analysis.
(E) All quality control requirements in these Rules as set forth by the State Laboratory. Ref:
15A NCAC 2H .0805 (a) (7) (D) and (E).
Comment: The only data available to check was the analysis of the PT.

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#65 TZ Osborne WRF Laboratory
00. Finding: The laboratory is only documenting the final calculated result of the PT sample and
no other supporting data to allow historical reconstruction of the final result.
Requirement: All laboratories must use printed bench worksheets that include a space to
enter the signature or initials of the analyst, date of analyses, sample identification, volume of
samples analyzed, value from the measurement system, factor and final value to be reported
and each item must be recorded each time samples are analyzed. The date and time BOD
and coliform samples are removed from the incubator must be included on the laboratory
worksheet. Ref: 15A NCAC 2H .0805 (a) (7) (H).
PP. Finding: The PT sample was analyzed with a factory curve that has not been verified.
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 more than
ten percent at mid -range, each time a new stock standard is prepared, or at least every
twelve months. Ref: 15A NCAC 2H .0805 (7) (1).
IV. PAPER TRAIL INVESTIGATION:
A paper trail was not conducted during this inspection. On April 23, 2015, Mike Mickey of the Winston-
Salem Regional Office performed a Compliance Evaluation Inspection of the NPDES wastewater
discharge from the T.Z. Osborne facility. Part of this inspection included reviewing Discharge Monitoring
Reports (DMRs) for the period March, 2014 through February, 2015.
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. Please respond to all Findings and include an implementation
date for each corrective action.
Report prepared by: Beth Swanson Date: August 20, 2015
Report reviewed by: Nick Jones Date: September 2, 2015