#544 - 09 - 2010 - FINAL

INSPECTION REPORT ROUTING SHEET
To be attached to all inspection reports in-house only,
Laboratory Cert. #:
544
Laboratory Name:
Water Quality Lab & Operations, Inc.
Inspection Type:
Commercial Maintenance
Inspector Name(s):
Jason Smith, Chet Whiting
Inspection Dater
September 17, 2010
Date Report Completed:
November 2 2010
Date Forwarded to Reviewer:
November 2 2010
Reviewed by:
Chet Whiting
Date Review Completed:
December 15, 2010
Cover Letter to use: _'..Insp.
Initial X Insp. Reg. _ Insp. No Finding — Insp. CP
Unit Supervisor:
I
Gary Francies
Date Received:
12/17/2010
Date Forwarded to Alberta:
12/22/2010
Date Mailed:'nlb

NCDENR
North Carolina Department of Environment and Natural Resources
Division of Water Quality
Beverly Eaves Perdue Coleen H. Sullins
Governor Director
December 23, 2010
544
Mr. Paul Isenhour
Water Quality Lab & Operations, Inc.
P.O. Box 1167
Banner Elk, NC 28604
SUBJECT: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC)
Maintenance Inspection
Dear Mr. Isenhour.
Dee Freeman
Secretary
Enclosed is a report for the inspection performed on September 17, 2010 by Jason Smith and Chet Whiting. I
apologize for the delay in getting this report to you. Where findings) ,are cited in this report, a response is
required. Within 30 days of receipt, please supply this office with a written item for item description of how
these finding(s) were corrected. 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 828-296-4677.
Sincerely,
c
Gary Zancies
Unit Supervisor
Laboratory Section
CC: Jason Smith
Master files
DENR DWQ Laboratory Section NC Wastewater/Groundwater Laboratory Certification Branch One
1623 Mail Service Center, Ralegn, North Carolina 27699-1623 NorthC`irolina
Location: 4405 Reedy Creek Road. Raleigh, North Carolina 27607-64.45 t� �Fytylkr �y f
Phone: [phone] FAX: [phone] (f yt& yxL L
Internet =Av,dvrglab.org
An Epual Opportunity \Affirmative Action Employer Customer Service:1-877-623-6748 www.newaterquality.org

LABORATORY NAME:
ADDRESS:
CERTIFICATE #:
DATE OF INSPECTION:
•
LOCAL PERSON(S) CONTACTED:
Inspection Report
Water Quality Lab & Operations, Inc.
P.O. Box 1167
Banner Elk, NC 28604
544
September 17, 2010
Commercial Maintenance
Jason Smith and Chet Whiting
Paul Isenhour
' 1. INTRODUCTION:
This laboratorywas inspected to verify its compliance with the requirements of 15A NCAC 2H .0800 for
p y p q
the analysis of environmental samples.
if. GENERAL COMMENTS:
The facility has all the equipment necessary to perform the analyses; however better maintenance of the
equipment is required. Additional quality control and documentation needs to be implemented. The
1 laboratory was provided with new policies at the time of the inspection. Findings C, E, F, K, and Y are
new policies that have been implemented by our program since the last inspection.
The previous inspection was an abbreviated inspection of only field parameters. Findings EE, FF, and GG
were cited in the previous report and have not been adequately addressed. It appears that better
oversight corrected the findings for a while, but once regular reviews of benchsheets ended, the issues
reemerged.
III. FINDINGS REQUIREMENTS COMMENTS AND RECOMMENDATIONS:
General Laboratory
A. Finding:. The laboratories Standard Operating Procedures (SOPs) have not been updated
since 2004.
Requirement: Each laboratory shall develop and maintain a document outlining the analytical
quality control practices used for the parameters included in their certification. Supporting
records. _shall be' maintained as evidence that these practices are being effectively carried out.
The quality control document shall be available for inspection by the State Laboratory. Ref: 15A
NCAC 2H..0805 (a) (7).
Comment: Please submit updated SOPs for all certified parameters by June 1, 2011
B. Finding: The sample receiving thermometer and Chemical Oxygen Demand reactor thermometer
were not checked against a NISI certified or NIST traceable thermometer every 12 months.

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#544 Water Quality Lab & Operations, Inc.
Requirement: All thermometers must meet National Institute of Standards and Technology
(NIST) specifications for accuracy or be checked, at a minimum annually (every twelve
months), against a MIST traceable thermometer and corrections made. Ref: 15A NCAC 2H
.0805 (a) (7) (0).
C. Finding: The analytical balance has not been serviced.
Requirement: Laboratory analytical balance(s) must be serviced by a qualified
vendor/technician at a minimum every 12 months to ensure that the balance is functioning
within required tolerances. Documentation that this service has been performed must be
available for review upon request. If the operational capabilities of the balance are in question
at any time during the 12-month period, corrective action must be taken. Ref: North Carolina
Wastewater/Groundwater Laboratory Certification Policy.
D. Finding: The analytical balance weights have not been verified against ASTM standard weights
within five years. The last time this was performed was February, 2005._
Requirement: ASTM Class 1 and 2 weights must be verified at least every 5 years. ASTM
Class 1 weights (20 g to 25 kg) and ASTM Class 2 weights (10 g to 1 mg) are equivalent to the
NBS Class S weights specified in 15A NCAC 2H .0805 (a) (7) (K). Ref: North Carolina
WastewaterlGroundwater Laboratory Certification Policy.
E. Finding: The desiccators are not being properly maintained. The desiccant was pink indicating
that the desiccant needed to be dried or replaced. The gasket on the door of one desiccator
needed to be replaced. The glass top desiccator needed fresh grease applied to maintain an
adeauate seal.
Requirement: Facilities and equipment. Each laboratory requesting certification must contain or
be.. equipped . with the following: Glassware, chemicals, supplies, and equipment required to
perform .all analytical procedures included in their certification. Ref: 15A NCAC 2H .0805 (a) (6)
(H).. .
F. Finding: Auto-pipettors are not calibrated twice per year.
Requirement: Mechanical volumetric liquid -dispensing devices (e.g., fixed and adjustable auto-
pipettors, bottle -top. dispensers, etc.) must be calibrated at least twice per year, approximately
six months apart. Each liquid -dispensing device must meet the manufacturer's statement of
accuracy. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy.
G. Finding: The nitric acid used for metals preservation is not low level metals grade.
Requirement: All acids used for this method must be of ultra high -purity grade or equivalent. EPA
Method 200.7 Revision 4.4 (1994), Section 7, 1.
Comment: The Winston-Salem Regional Office requested that the purity of the nitric acid be
confirmed based upon anomalous metals results. Although this laboratory does not perform
metals analyses, they preserve samples themselves using ACS grade nitric acid. In order to
ensure samples are not contaminated, low level metals grade nitric acid must be used for
preservation.

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##544 Water Quality Lab & Operations, Inc.
Documentation
Recommendation: The date on many benchsheets and logs is only recorded as month and day, with no
indication of year. The year is sometimes listed with the start of a new year or log sheet. If the sheets get
out of order, it may be impossible to determine, the year. it is recommended that the day, month, and year
always be recorded in order to avoid any questionable documentation.
H. Finding: The laboratory needs to increase the documentation of purchased materials and
reagents. The date opened and expiration date is not recorded.
Requirement: All chemicals, reagents, standards and consumabies 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: North Carolina
Wastewater/Groundwater Laboratory Certification Policy.
I. Finding: The system of traceability needs improvement. It is not clear from the benchsheets
.which lot numbers were used for calibration and which were used for verification.
Requirement: See requirement for finding H.
J. Finding Several instances of writing over a number as a means of error correction were
observed..
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: North Carolina Wastewater/
Groundwater Laboratory Certification Policy.
Oil and Grease — EPA Method 1664 A
Recommendation: ,While documented elsewhere, it is recommended that the laboratory document the
recovery of the -Matrix Spike and Ongoing Precision and Recover standard on the benchsheet.
Ammonia Nitrogen — Standard Methods, 181h Edition, 4500 NH3 F
Chemical Oxygen Demand — Standard Methods, 18th Edition, 5220 D
K. Finding: The laboratory is not analyzing matrix spikes.
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 be qualified or the laboratory must

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{ #544 Water Quality Lab & Operations, Inc.
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: North Carolina Wastewater/Groundwater Laboratory Certification Policy.
L. Finding: A calibration blank and calibration verification standard (mid -range same source) are
not analyzed 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 (e.g., repeating sample
determinations since the last acceptable calibration verification, repeating the initial calibration,
etc.). Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy based upon
Standard Methods, 20'h Edition, 1020 B. (10) (c), 3020 B. (2) (b), and 4020 B..(2).
Ammonia Nitrogen — Standard Methods, 181h Edition, 4500 NH3 F
M. Finding: The laboratory's acceptance criterion for blanks is less than the reporting limit.
Requirement: For analyses requiring a calibration curve, the concentration of method and
reagent blanks must not exceed 50% of the reporting limit, unless otherwise specified by the
reference method. Ref: North Carolina Wastewater/Groundwater Laboratory Certification
Policy.:: .
N. Finding: The volume of 1 ON NaOH is not documented.
Requirement: Record volume of 1 ON NaOH added. Ref: Standard Methods, 181h Edition, 4500
NH3 F. (4) (e).
O. Finding: After the addition of the 10 N NaOH, the phi is verified to be greater than 11 with
Ammonia pH Adjusting ISA; however the elevated pH is not documented.
Requirement: Add a sufficient volume of 10N NaOH solution to raise pH above 11. Ref:
Standard Methods, 18't' Edition, 4500 NH3 F. (4) (b).
Requirement: Supporting records shall be maintained as evidence that these practices are being
effectivelycarried out. Ref: 15A NCAC 2H .0805 (a) (7).
Chemical Oxygen Demand — Standard Methods,18'h Edition, 5220 D
P. Finding: The correlation coefficient of the calibration curve is not calculated.
Requirement: When linear regression is used, use the minimum correlation coefficient specified
in the method. If the minimum correlation coefficient is not specified, then a minimum value of
0.995 (or a coefficient of determination, r2, of 0.99) is required. Ref: North Carolina
Wastewater/Groundwater-Laboratory Certification Policy based upon Standard Methods, 20th
Edition, 1020 B. (10) (b).

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4544 Water Quality Lab & Operations, Inc.
Settleable Solids — Standard Methods, 18" Edition, 2540 F
Q. Finding: The start time, forty five minute stir time, and end time of the procedure are 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: 15A NCAC 2H .0805 (a)
(7) (A)
Total Suspended Solids — Standard Methods, 18`h Edition, 2540 D
R. Finding: A minimum dried residue weight gain of 1 mg is used to determine the reporting limit.
Requirement: The minimum reporting value is established at 2.5 mg/L when 1000 mL of sample
is analyzed. The minimum weight gain allowed by any approved method is 2.5 mg. In instances
where the weight gain is less than the required 2.5 mg, the value must be reported as less than
the appropriate value based upon the volume used. For example, if 500 mL of sample is analyzed
and < 2.5 mg of dried residue is obtained, the value reported would be < 5 mg/L. Ref: North
Carolina Wastewater/Groundwater Laboratory Certification Policy based upon Standard Methods,
20th and.215t Editions, 2540 D. (3) (b).
S. Finding:. The time samples are placed in the oven and the time samples are removed 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: 15A NCAC 2H .0805 (a)
(7) (A).
Comment: In order to document the method required one hour minimum drying time and the
drying time that documented constant weight in the last study, it is necessary to document these
times::
T. Finding: The column header on the benchsheet lists the weights as grams; however, results are
recorded in milligrams.
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).
Specific Conductance -- Standard Methods, 18" Edition, 2510 B
U. Finding: Duplicates were not consistently analyzed at the required frequency.
Requirement: Analyze five percent of all samples in duplicate to document precision.
Laboratories analyzing less than 20 samples per month must analyze at least one duplicate
each month samples are analyzed. Ref: 15A NCAC 2H .0805 (a) (7) (C).
Fecal Coliform -- Standard Methods, 18th Edition, 9222 D
V. Finding: The NIST thermometer is graduated in 1 °C increments. This is not acceptable to check
the thermometer used in the fecal incubator.

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Requirement: All thermometers must meet National Institute of Standards and Technology
(NIST) specifications for accuracy or be checked, at a minimum annually (every twelve
months), against a NIST traceable thermometer and corrections made. Ref: 15A NCAC 2H
.0805 (a) (7) (0).
--� Comment: A thermometer igraduated in 0.1 °C increments must be used.
W. Finding: Only two analyses are performed for consumable comparison testing.
Requirement: It is required that when a new lot of culture medium, pads, or membrane fitters 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. Ref: Standard
Methods, 18th Edition, 9020 B. (3) (d).
Biochemical OnMen Demand— Standard Methods, 184h Edition, 5210 B
Recommendation: The 21s' Edition of Standard Methods requires that the dilution water blank Dissolved
Oxygen (DO) uptake in 5 days must not be more than 0.20 mg/L and preferably not more than 0.10 mg/L.
It is recommended that the laboratory read the DO, measurements to two decimal points in order to clearly
document this method criterion.
X. Finding: The majority of bottles in the incubator had very large air bubbles possibly indicating a
significant loss of DO during the incubation period that did not result from the oxidation of
organic matter by the bacteria present. This may result in a false high BOD value. No air
bubbles should be present during incubation.
Requirement: Fill bottles with enough dilution water, seeded if necessary, so that insertion of
stopper will,displace all air, leaving no bubbles. Determine initial DO ... and replace any displaced
contents with dilution water to fill the bottle. Stopper tightly, water -seal, and incubate for 5 days at
20 °C. Ref: Standard Methods, 18'h Edition, 5210 B. (4) (f) (2).
Comment: The stirrer on the DO probe Is no longer functioning. In order to stir the sample, a stir
bar is placed in the bottle during DO measurement. It appears that there is not enough dilution
water added to the bottle after removal of the stir bar and/or the water seal is not adequate and
evaporation is occurring.
Y. Finding: Extra nutrient, mineral, and buffer solutions are not added to the Biochemical Oxygen
Demand (BOD) bottles containing more than 67% (> 201 mL) sample.
Requirement: When a bottle contains more than 67% of the sample after dilution, nutrients
may .be limited in the diluted sample and, subsequently, reduce biological activity. In such
samples, add the nutrient, mineral, and buffer solutions (3a through e) directly to individual
BOD bottles at a rate of 1 mL/L (0,33 mL/300-mL bottle) or use commercially -prepared
solutions designed to dose the appropriate bottle size. Ref: North Carolina
Wastewater/Groundwater Laboratory Certification Policy based upon Standard Methods, 20th
Edition, 5210 B, (4) (f) and Standard Methods, 215' Edition, 5210 B. (5) (c) (2).
Comment: Dilution water prepared as normal with nutrient, mineral, and buffer solutions would
still be used in the BOD bottles. For the bottles containing more than 67% sample, extra
nutrient, mineral, and buffer solutions would be added in addition to the dilution water.
Recommendation: Rather than pipetting 0.33 mL of each reagent into the BOD bottle, it is
recommended that commercially prepared nutrient buffer pillows for 300 mL bottles be used.

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#544 Water Quality Lab & Operations, Inc.
Field Testing
Recommendation: Rather than recording the amount of drift that occurs when analyzing midday and
end of day pH standards, record the actual pH obtained at these times.
Z. Finding: The laboratory needs to increase the documentation of purchased materials and
reagents used by field personnel.
Requirement: See requirement for finding H
AA. Finding: The pH and DO meters temperature sensors were not checked against a NIST certified
or NIST traceable thermometer every 12 months. This was last performed in February, 2009.
Requirement: All thermometers must meet National Institute of Standards and Technology
(NIST) specifications for accuracy or be checked, at a minimum annually (every twelve
months), against a NIST traceable thermometer and corrections made. Ref: 15A NCAC 2H
.0805 (a) (7) (0).
BB. Finding: The Total Residual Chlorine (TRC) meters have not had their internal curves verified
.. every 12 months. This was last performed in February, 2009.
Requirement: For analytical procedures requiring analysis of a series of standards, the
concentrations of these 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. For metals by AA or ICP, a series of at least three
standards must be analyzed along with each group of samples. 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 mid -range, each time a new stock standard is
prepared, or at least every twelve months. Each analyst performing the analytical procedure
must produce a standard curve. Ref: 15A NCAC 2H .0805 (a) (7) (1).
CC. Finding: The gel standards used to verify the TRC calibration curves daily have not been
assigned.new true values every 12 months. This was last performed in February, 2009.
Requirement: Purchased "Gel -type" or sealed liquid ampoule standards may be used for daily
calibration verification only. These standards must be verified initially and every 12 months
thereafter, with the standard curve. The assigned values will be used for the next twelve
months, or until a new curve verification is performed. The gel standard verification must be
performed.for each instrument on which they are to be used. If multiple instruments and/or
standard sets are used, each must have assigned values specific for the instrument and
standard set..Ref:. Technical Assistance for Field Analysis of Total Residual Chlorine.
DD. Finding:, Gel standard values were consistently outside of the acceptable range for one
meter/operator. This was not addressed nor resolved.
Requirement: Any time quality control results indicate an analytical problem, the problem must
be.resoived and any samples involved must be rerun if the holding time has not expired. Ref:
15A NCAC 2H .0805 (a) (7) (F).

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#544 Water Quality Lab & Operations, Inc.
Comment: It appears that due to a personnel change, the gel standards were switched between
meters without changing the acceptable range on the benchsheet. It seems that the gel standard
values were acceptable; however there is no documentation to confirm this.
Recommendation: It is recommended that the gel standards used be identified by lot number on
the benchsheets and/or calibration logs in order to avoid this situation.
EE. Finding: Analyst initials are not consistently documented on calibration logs.
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 .08D5 (a) (7)
(H).
FF. Finding: Sample collection and analysis times continue to not be consistently documented. Cited
previously on February 19, 2009.
Requirement: See requirement for finding DD.
GG. Finding: The documented time of pH, DO, and TRC meter calibrations continue to occasionally
be later than sample analysis times. Cited previously on February 19, 2009.
Requirement: The meter must be calibrated prior to the analysis of samples. Ref: Technical
Assistance for Field Analysis of pH and Technical Assistance for Field Analysis of Dissolved
Oxygen.—
. .:..:......
Requirement: Instruments are to be calibrated or a calibration check must be performed prior to
analysis of samples each day compliance monitoring is performed. Ref: Technical Assistance for
Field Analysis of Total Residual Chlorine.
HH. Finding: Post calibration checks and/or recalibrations for DO, pH, and TRC continue to not be
consistently performed. Cited previously on February 19, 2009.
Requirement: When performing analysis at multiple sampling locations, re -calibrations) must be
performed every four hours. Ref: Technical Assistance for Field Analysis of Dissolved Oxygen.
Requirement: If compliance samples are analyzed throughout the day, a post calibration check
must be analyzed mid -day and at the end of the run (i.e., roughly every 4 hours based on an eight
hour -day); -::Ref: Technical Assistance for Field Analysis of Total Residual Chlorine and Technical
Assistance for Feld Analysis of pH.
IV. PAPER TRAIL INVFSTiGATION:
The paper. trailconsisted of comparing field testing records and contract lab reports to Discharge
Monitoring Reports (DMRs) submitted to the North Carolina Division of Water Quality. Data were
reviewed :for Town of Crossnore (NPDES permit #NC0026654) and Jonas Ridge (NPDES permit
#NC0060224) for January, 2010, Hawksnest Utilities (NPDES permit #NC0058891), Gamp Broadstone
(NPDES permit #NC©032166), Willow Valley (NPDES permit #NC0061425), and Mill Ridge (NPDES
permit #NC0030473) for June, 2010. The following errors were noted:

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#544 Water Quality Lab & Operations, Inc.
Date
Parameter
Location
Value on
Benchsheet
Value on DMR
6-8-10
Total Residual Chlorine
Camp Broadstone Effluent
No value.
<15 pg/L
6-29-10
Total Residual Chlorine
Camp Broadstone Effluent
No value.
<15 pg/L
In order to avoid questions of legality, it is recommended that you contact the appropriate Regional,
Office for guidance as to whether an amended Discharge Monitoring Report will be required. A copy of
this report will be forwarded to the Regional Office.
V. CONCLUSIONS:
i We are concerned with the findings that were cited previously and not corrected.
C Laboratory Decertification Ref: 15A NCAC 2H .0807 (a) (1), (13) and (14):
A laboratory may be decertified for any or all parameters for up to one year for any or all of the
following infractions:
(1) Failing to maintain the facilities, or records, or personnel, or equipment, or quality control
program as set forth in the application, and these Rules; or
(14) Failing to comply with any other terms, conditions, or requirements of this Section or of a
Laboratory certification.
Correcting the above -cited findings and implementing the recommendations will help this lab to
produce quality data and meet certification requirements, The inspectors would like to thank the staff
for its assistance during the inspection and data review process. Please respond to all findings.
Report prepared by Jason Smith Date: November 2, 2010
Report reviewed by: Chet Whiting Date: December 15, 2010