#152 - 04 - 2012 - FINAL

Beverly Eaves Perdue Charles Wakild, P. E. Dee Freeman
Govemor Director Secretary
June 4, 2012
152
Mr. Steve Wilson
Unimin Quartz Feldspar Operations
P.O. Box 588
Spruce Pine, NC 28777
SUBJECT: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC)
Maintenance Inspection
Dear Mr. Wilson:
Enclosed is a report for the inspection performed on April 12, 2012 by Jason Smith. Since the
finding(s) cited during the inspection were all corrected prior to the completion of the enclosed
report, a response is not required. The staff is commended for taking the initiative in correcting
the findings in such a timely manner. 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 electronic mail, or if you have questions or need additional information please
contact me at 828-296-4677.
Sincerely,
Gary Francies
Certification Unit Supervisor
Laboratory Section
CC: Jason Smith
DENR DWQ Laboratory Section NC Wastewater/Groundwater Laboratory Certification Branch
1623 Mail Service Center, Raleigh, North Carolina 27699-1623
Location: 4405 Reedy Creek Road. Raleigh, North Carolina 27607-6445
Phone: [phone] \ FAX: [phone]
Internet: www.dwglab.org
An Equal Opportunity \ Affirmative Action Employer

LABORATORY NAME:
NPDES PERMIT #:
ADDRESS:
CERTIFICATE #:
DATE OF INSPECTION:
TYPE OF INSPECTION:
AUDITOR(S):
LOCAL PERSON(S) CONTACTED:
INTRODUCTION:
On -Site Inspection Report
Unimin Quartz Feldspar Operations
NC0000175
P.O. Box 588
Spruce Pine, NC 28777
152
April 12, 2012
Industrial Maintenance
Jason Smith
Steve Wilson
This laboratory was inspected to verify its compliance with the requirements of 15A NCAC 2H .0800 for
the analysis of environmental samples.
II. GENERAL COMMENTS:
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.
III. FINDINGS REQUIREMENTS COMMENTS AND RECOMMENDATIONS:
Documentation
Comment: Reagent preparation procedures were not documented. 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 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. This requirement is a new policy that has been implemented by our program
since the last inspection. Notification of acceptable corrective action (i.e., the reagent preparation log
has been updated to include a description of reagent preparation procedures) was received by email
on April 18, 2012. No further response is necessary for this finding.

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Comment: The laboratory has not qualified Quality Control failures on the Discharge Monitoring Report.
North Carolina Wastewater/Groundwater Laboratory Certification Policy based upon Standard Methods,
20th Edition,1020 B. (14) states: When quality control (QC) failures occur, the laboratory must attempt to
determine the source of the problem and must apply corrective action. If data qualifiers are used to
qualify samples not meeting QC requirements, the data may not be useable for the intended purposes. A
notation must be made on the Discharge Monitoring Report (DMR) form, in the comment section or on a
separate sheet attached to the DMR form, when any required sample quality control does not meet
specified criteria, and another sample cannot be obtained. No instances of QA failures were noted during
the inspection, however the laboratory was not aware of this requirement. This requirement is a new
policy that has been implemented by our program since the last inspection. Notification of acceptable
corrective action (i.e., QC failures will be documented on the DMR) was received by email on April 18,
2012. No further response is necessary for this finding.
Comment: Proficiency Testing (PT) sample preparation was not documented. The North Carolina
Wastewater/Groundwater Laboratory Certification document Proficiency Testing Requirements, February
20, 2012, Revision 1.2. states: PT samples received as ampules must be diluted according to the PT
provider's instructions. The preparation of PT samples must be documented in a traceable log or other
traceable format. The diluted PT sample becomes a routine environmental sample and is added to a
routine sample batch for analysis. This requirement is a new policy that has been implemented by our
program since the last inspection. Notification of acceptable corrective action (i.e., PT preparation will
be documented) was received by email on April 18, 2012. No further response is necessary for this
finding.
Comment: The correct method codes were not reported for PT samples. The North Carolina
Wastewater/Groundwater Laboratory Certification document Proficiency Testing Requirements, February
20, 2012, Revision 1.2. states; Laboratories must also be careful to designate the correct method code(s)
being used for each PT sample result. To ensure that you are reporting the correct method, review your
certificate attachment (i.e., certified parameter list). The method must include the entire method reference
as is written on your certificate attachment (i.e., certified parameter list). You must also indicate the
correct edition or revision of a method (e.g., 20th edition) where listed on your certificate attachment (i.e.,
certified parameter list). This requirement is a new policy that has been implemented by our program
since the last inspection. Notification of acceptable corrective action (i.e., proper method codes will be
reported for PT samples) was received by email on April 18, 2012. No further response is necessary
for this finding.
Temperature — Standard methods, 20th Edition 2550 B
Comment: Temperature analyses for stream samples were not performed within the EPA holding time.
Samples were collected and analyzed within 15 minutes. The Code of Federal Regulations, Title 40, Part
136; Federal Register Vol. 72, No. 47, March 12, 2007; Table it states that immediate analysis is
required. Notification of acceptable corrective action (i.e., temperature samples are now measured
immediately upon collection) was received by email on April 18, 2012. No further response is
necessary for this finding.
Total Suspended Residue — Standard Methods, 20th Edition, 2540 D
Comment: The laboratory had not established acceptance criteria for the quarterly check standard. 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., an acceptance range of ± 10% has been

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established for Total Suspended Residue standards) was received by email on April 18, 2012. No
further response is necessary for this finding.
Fluoride — Standard Methods, 201h Edition, 4500 F" C
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. This requirement is a new policy
that has been implemented by our program since the last inspection. Notification of acceptable corrective
action (i.e., MS analyses are performed on 5% of samples) was received by email on April 18, 2012.
No further response is necessary for this finding.
Comment: Samples with concentrations greater than the largest calibration standard were not diluted to
fall within the calibration range. The North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (1)
states: For analytical procedures requiring analysis of a series of standards, the concentrations of these
standards must bracket the concentration of the samples analyzed. Notification of acceptable corrective
action (i.e., samples above the calibration range are diluted to fall within the calibration range) was
received by email on April 18, 2012. No further response is necessary for this finding.
Comment: A distillation study has not been performed since 2008. North Carolina Wastewater/
Groundwater Laboratory Certification Policy based upon the Code of Federal Regulations, Title 40, Part
136; Federal Register Vol. 72, No. 47, March 12, 2007: Table 1 B Footnote 6 states: 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. In the case of low concentration effluents, the samples must be spiked to allow for a
meaningful statistical comparison. It is recommended that samples with a concentration < 1.0 mg/L be
spiked to yield a value in the 1 - 5 mg/L range. Comparisons performed in this concentration range should
check within 20% RPD. Additional samples must be analyzed comparatively if the results do not indicate
approximately the same values for distilled and undistilled samples. It is recommended that both the
distilled and undistilled portions of the sample be analyzed by the same laboratory using the same
methodology. The following frequencies are required:
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.
Due to the length of time since the last distillation study was performed, the laboratory will be required to
perform a distillation study on four samples this year. Notification of acceptable corrective action (i.e.,
the first of four acceptable distillation study samples was submitted with the understanding that the
other three distillation studies will be performed within the next six weeks) was received by fax on May
15, 2012. For future reference, please note that all samples for the distillation study may be analyzed
at the same time. Please submit all four distillation study sample results by August 31, 2012.
Comment: The laboratory was not analyzing a blank. 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) 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

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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., a blank is now analyzed at the required interval) was received by email on April
18, 2012. No further response is necessary for this finding.
Comment: North Carolina Wastewater/Groundwater Laboratory Certification Policy states: 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.
IV. PAPER TRAIL INVESTIGATION:
The paper trail consisted of comparing laboratory benchsheets and contract lab reports to Discharge
Monitoring Reports (DMRs) ,submitted to the North Carolina Division of Water Quality. Data were
reviewed for Unimin Quartz Feldspar Operations (NPDES permit #NC0000175) for February and April
2011. No transcription errors were detected. The facility appears to be doing a good job of accurately
transcribing data.
V. CONCLUSIONS:
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 inspection report response is required; however the Fluoride distillation study
results must be submitted by August 31, 2012.
Report prepared by: Jason Smith Date: May 2, 2012
Report reviewed by: Todd Crawford Date: May 2, 2012