#623 - 03 - 2011- FINAL

Beverly Eaves Perdue
Governor
623
Mr. Rick Singleton
Unimin— Crystal Plant
136 Crystal Drive
Spruce Pine, NC 28777
NCDENR
North Carolina Department of Environment and Natural Resources
Division of Water Quality
Coleen H. Sullins
Director
July 15, 2011
SUBJECT: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC)
Maintenance Inspection
Dear Mr. Singleton:
Dee Freeman
Secretary
Enclosed is a report for the inspection performed on March 29, 2011 by Jason Smith. I apologize for the delay
in getting this report to you. No findings are cited in this report, a response is not required. We appreciate the
fine job you and your staff are doing. As a certification requirement, 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,
L
Gary Francies
Unit Supervisor
Laboratory Section
CC Jason Smith
Gary Francies
Master File
DENR DWQ Laboratory Section NC Wastewater/Groundwater Laboratory Certification Branch One
1623 Mail Service Center, Raleigh, North Carolina 27699-1623 NorthCarOlina
Location: 4405 Reedy Creek Road. Raleigh, North Carolina 27607-6445
Phone: [phone] \ FAX: [phone] Naturally
Internet: www.dwglab.org
An Equal opportunity \ Affirmative Action Employer Customer Service:1-877-623-6748 www.ncwaterquality.org

LABORATORY NAME:
NPDES PERMIT M
ADDRESS:
CERTIFICATE M
DATE OF INSPECTION:
TYPE OF INSPECTION:
AUDITOR(S):
LOCAL PERSON(S) CONTACTED
I. INTRODUCTION:
Unimin — Crystal Plant
NC0084620
136 Crystal Drive
Spruce Pine, NC 28777
623
March 29, 2011
Industrial Maintenance
Jason Smith
Rick Singleton and Denny Buchanan
This laboratory was inspected to verify its compliance with the requirements of 15A NCAC 2H .0800 for the
analysis of environmental samples.
11. GENERAL COMMENTS:
The laboratory was clean and well organized. The facility has all the equipment necessary to perform the
analyses. The laboratory has not analyzed samples for compliance purposes since obtaining certification. The
effluent is discharged to another facility for further treatment prior to discharge. The inspection was performed
by reviewing data generated by the voluntary analysis of the process control samples (i.e. effluent samples that
are not reported). The laboratory requested an inspection due to the possibility the facility may begin to
discharge and the need to analyze samples.
General Laboratory
Comment: The laboratory's Standard Operating Procedures (SOPs) had not been reviewed nor updated since
their original creation in June, 2000. The North Carolina Administrative Code, 15A 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. Notification of acceptable corrective action (i.e., the
laboratory reviewed, revised, and submitted a copy of the SOPs) was received by email on April 4, 2011. No
further response is necessary for this finding.
Comment: The laboratory's analytical balance had not been serviced annually. North Carolina
Wastewater/Groundwater Laboratory Certification Policy based upon Standard Methods 20th Edition, 9020. (3)
(b) states: 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 manufacturer's specifications. 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.
Notification of acceptable corrective action (i.e., the laboratory had the analytical balance serviced and has
scheduled this to be performed annually) was received by email on April 4, 2011. No further response is
necessary for this finding.

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#623 Unimin — Crystal Plant
Documentation
Comment: The laboratory was not recording the temperature of the refrigerator used to store samples. The
North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (J) states: 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. Notification of
acceptable corrective action (i.e., the laboratory has added the refrigerator temperature to the daily benchsheet
and is recording it) was received by email on April 4, 2011. No further response is necessary for this
finding.
Comment: The laboratory is not documenting all required information for materials received and reagents
prepared. North Carolina Wastewater/Groundwater Laboratory Certification 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). 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, 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. Notification of acceptable corrective action (i.e., a log recording all required
information) was received by email on April 4, 2011. This is a new policy that has been implemented by our
program since the last inspection. No further response is necessary for this finding.
Quality Control
Comment: The laboratory did not have duplicate acceptance criteria established for Turbidity and Total
Suspended Solids. The North Carolina Administrative Code, 15A 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. The quality control document shall be available for inspection by the
State Laboratory. Notification of acceptable corrective action (i.e., the laboratory has established the duplicate
acceptance criteria at 10%) was received by email on April 4, 2011. No further response is necessary for
this finding.
Total Suspended Solids — Standard Methods, 20th Edition, 2540 D
Comment: Filters were not weighed to constant weight prior to sample analysis, nor was a dry filter blank
analyzed with each set of samples. North Carolina Wastewater/Groundwater Laboratory Certification Policy
based upon Standard Methods, 20th Edition, 2540 D. (3) (a) states: If pre -prepared filters are not used, the
method requires that filters must be weighed to a constant weight after washing. Repeat cycle of drying,
cooling, desiccating, and weighing until a constant weight is obtained or until weight change is less than 4% of
the previous weighing or 0.5 mg, whichever is less. In lieu of this process, it is acceptable to analyze a single
daily dry filter blank to fulfill the method requirement of drying all filters to a constant weight prior to analysis.
This is a new policy that has been implemented by our program since the last inspection. Notification of
acceptable corrective action (i.e., the laboratory is now analyzing a dry filter blank with each set of samples)
was received by email on April 4, 2011. No further response is necessary for this finding.
Comment: The laboratory was using an incorrect reporting limit. North Carolina Wastewater/ Groundwater
Laboratory Certification Policy based upon Standard Methods, 20th and 21st Editions, 2540 D. (3) (b) states:
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. This is a new policy that has been implemented by our program since the last inspection.

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#623 Unimin — Crystal Plant
Notification of acceptable corrective action (i.e., the laboratory is now using 2.5 mg of weight gain to determine
the reporting limit) was received by email on April 4, 2011. No further response is necessary for this
finding.
Comment: The samples were not weighed to constant weight, nor was an annual multiple weighing study, to
verify the adequacy of the drying time, performed. North Carolina Wastewater/Groundwater Laboratory
Certification Policy based on Standard Methods 20th Edition, 2540 D. (3) (c), 2540 B. (3) (b), and 2540 C.
(3) (d) states: Constant weights must be documented. The approved methods require the following: "Repeat
the cycle of drying, cooling, desiccating, and weighing until a constant weight is obtained or until the weight
change is less than 4% of the previous weight or 0.5 mg, whichever is less." In lieu of this, an annual study
documenting the time required to dry representative samples to a constant weight may be performed. Verify
minimum daily drying time is greater than or equal to the time used for the initial verification study drying
cycle. Drying cycles must be a minimum 1 hour for verification. Notification of acceptable corrective action
(i.e., the laboratory is now performing an annual drying study on the effluent) was received by email on April 4,
2011. No further response is necessary for this finding.
Comment: The laboratory was not analyzing a known standard quarterly. The North Carolina Administrative
Code, 15A NCAC 2H .0805 (a) (7) (B) states: Excluding Oil and Grease, all residue parameters, leachate
extractions, residual chlorine, and coliform, analyze one known standard in addition to calibration standards
each day samples are analyzed to document accuracy. Analyze one suspended residue, one dissolved
residue, one residual chlorine and one oil and grease standard quarterly. For residual chlorine, all calibration
standards required by the approved procedure in use and by EPA must be analyzed. Notification of acceptable
corrective action (i.e., a standard was purchased and will be analyzed on a quarterly basis) was received by
email on April 4, 2011. No further response is necessary for this finding.
Settleable Solids — Standard Methods, 201h Edition, 2540 F
Comment: The laboratory was not documenting the end time of the analysis or the gentle stirring or spinning
of the Imhoff cone. The North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) and 15A NCAC 2H
.0805 (a) (7) (A) state: Supporting records shall be maintained as evidence that these practices are being
effectively carried out. 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., an
updated benchsheet with all required documentation) was received by email on April 4, 2011. No further
response is necessary for this finding.
pH — Standard Methods, 20th Edition, 4500 H+ B
Comment: The laboratory was reporting pH to two decimal places. Standard Methods, 20th Edition, 4500 H+ B.
(6) states: A variance of ± 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., reporting of pH to one decimal place) was received
by email on April 4, 2011. No further response is necessary for this finding.
Comment: The laboratory was not documenting units of measure for pH. The North Carolina Administrative
Code, 15A NCAC 2H .0805 (a) (7) (H) states: All laboratories must use printed laboratory bench worksheets
that include a space to enter the signature or initials of the analyst, date of analyses, sample identification,
volume of sample analyzed, value from the measurement system, factor and final value to be reported and
each item must be recorded each time samples are analyzed. The date and time BOD and coliform samples
are removed from the incubator must be included on the laboratory worksheet. Notification of acceptable
corrective action (i.e., an updated benchsheet documenting units of measure) was received by email on April
4, 2011. No further response is necessary for this finding.

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#623 Unimin — Crystal Plant
Fluoride — Standard Methods, 20t" Edition, 4500 F" C
Comment: The laboratory was not analyzing a blank and was not analyzing a mid -range standard at the end
of each sample set. North Carolina Wastewater/Groundwater Laboratory Certification Policy based upon
Standard Methods, 20th Edition, 1020 B. (10) (c), 3020 B. (2) (b), and 4020 B. (2) states: 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.).
Notification of acceptable corrective action (i.e., the laboratory is analyzing a blank and mid -range standard at
the beginning and end of each sample group) was received by email on April 4, 2011. This laboratory does not
analyze more than ten samples in a sample group. This is a new policy that has been implemented by our
program since the last inspection. No further response is necessary for this finding.
Comment: The laboratory had only performed a distillation study on one sample. North Carolina
Wastewater/ Groundwater Laboratory Certification Policy based upon Code of Federal Regulations, Title
40, Part 136; Federal Register Vol. 72, No. 47, March 12, 2007; Table IB Footnote 6 states: The titration
method requires all samples to be distilled. For all other methods, manual distillation is not required if
comparability data on representative effluent samples are on file to show that this preliminary distillation
step is not necessary; however, manual distillation will be required to resolve any controversies. Municipal
and Industrial Laboratories shall analyze initially four samples distilled and undistilled from each discharge
and; thereafter, analyze two samples a year from each effluent. Notification of acceptable corrective action
(i.e., an acceptable distillation study with three additional samples) was received by email on June 1, 2011. No
further response is necessary for this finding.
Comment: The laboratory was not performing Matrix Spike (MS) analyses. North Carolina Wastewater/
Groundwater Laboratory Certification Policy states: 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 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. Notification of acceptable corrective action (i.e.,
the laboratory has implemented MS analyses) was received by email on June 1, 2011. This is a new policy
that has been implemented by our program since the last inspection. No further response is necessary for
this finding.
IV. PAPER TRAIL INVESTIGATION:
No paper trail performed since no data has been reported.
All findings noted during the inspection were adequately addressed prior to the completion of this report.
The inspector would like to thank the staff for its assistance during the inspection and data review process. No
response is required.
Report prepared by: Jason Smith Date: July 6, 2011
Report reviewed by: David Livingston Date: July 11, 2011

INSPECTION REPORT ROUTING SHEET
To be attached to all inspection reports in-house only.
Laboratory Cert. #:
623
Laboratory Name:
Unimin — Crystal Plant
Inspection Type:
Industrial Maintenance
Inspector Name(s):
Jason Smith
Inspection Date:
March 29, 2011
Date Report Completed:
July 6, 2011
Date Forwarded to Reviewer: July 6, 2011
Reviewed by:
David Livingston
Date Review Completed:
July 11, 2011
Cover Letter to use: _
Insp. Initial _ Insp. Reg. _ Insp. No Finding _ Insp. CP X Corrected
Unit Supervisor:
Gary Francies
Date Received:
7/14/2011
Date Forwarded to Linda
7/15/2011
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Date Mailed:
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