#197_2018_0207_JS_FINAL

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To be attached to all inspection reports in-house only.
Laboratory Cert. #:
197
Laboratory Name:
The Quartz Corp. USA — Altapass
Inspection Type:
Industrial Maintenance
Inspector Name(s):
Jason Smith
Inspection Date:
February 7, 2018
Date Forwarded for Initial
Review:
February 16, 2018
Initial Review by:
Anna Ostendorff
Date Initial Review
Completed:
February 21, 2018
Cover Letter to use:
❑ Insp. Initial
❑Insp. No Finding
❑Corrected
❑ Insp. Reg
®Insp. CP
❑Insp. Reg. Delay
Unit Supervisor/Chemist III:
Todd Crawford
Date Received:
February 22, 2018
Date Forwarded to Admin.:
March 7, 2018
Date Mailed:
March 7, 2018
Special Mailing Instructions:

Water Resources
ENVIRONMENTAL. CTllAL'IY
March 7, 2018
197
Mr. James Garofalo
The Quartz Corp. USA - Altapass
P.O. Box 99
Spruce Pine, NC 28777
ROY COOPER
MICHEAL S. REGAN
LINDA CULPEPPER
SUBJECT: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC)
Maintenance Inspection
Dear Mr. Garofalo:
Enclosed is a report for the inspection performed on February 7, 2018 by Jason Smith. 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 findings were corrected and include an implementation
date for each corrective action.
We are concerned with the findings that were cited previously and not corrected. 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.
A copy of the laboratory's Certified Parameter List at the time of the audit is attached. This list will reflect
any changes made during the audit. Copies of the checklists completed during the inspection may be
requested from this office. Thank you for your cooperation during the inspection. If you wish to obtain an
electronic copy of this report by email or if you have questions or need additional information, please
contact me at [phone] ext. 251.
Sincerely,
Todd Crawford
Technical Assistance & Compliance Specialist
NC WW/GW Laboratory Certification Branch
Attachment
cc: Dana Satterwhite, Jason Smith, Master File 197

LABORATORY NAME: The Quartz Corp. USA — Altapass
NPDES PERMIT #: NC0000353 and NC0000400
ADDRESS: 797 Altapass Rd
Spruce Pine, NC 28777
CERTIFICATE : 197
DATE OF INSPECTION: February 7, 2018
TYPE OF INSPECTION: Industrial Maintenance
AUDITOR(S): Jason Smith
LOCAL PERSON(S) CONTACTED: James Garofalo, Teresa Morris, Joe Pittman, Glenn Young, Chris
Gentry and Ryan Fredsall
I. INTRODUCTION:
This laboratory was inspected by a representative of the North Carolina Wastewater/Groundwater
Laboratory Certification (NC WW/GW LC) program to verify its compliance with the requirements
of 15A NCAC 2H .0800 for the analysis of environmental samples.
GENERAL COMMENTS:
A review of laboratory benchsheets, requested by Linda Wiggs, Environmental Senior Specialist
of the NC Department of Environmental Quality Asheville Regional Office, indicated that the
laboratory had not implemented requirements associated with the 2012 and 2017 updates of the
Code of Federal Regulations, Title 40, Part 136. Ms. Wiggs requested that a laboratory inspection
be performed in conjunction with her sampling and facility inspection in order to ensure
compliance with Federal and State regulations.
The laboratory analyzes pH and Temperature in the field for the Quartz Corp. USA — Pine
Mountain facility (NPDES permit number NC000400) in addition to its own samples. The facility
has all the equipment necessary to perform the analyses.
All required Proficiency Testing (PT) Samples have been analyzed and the laboratory has fulfilled
its PT requirements for the 2017 PT Calendar Year.
The laboratory submitted their Quality Assurance (QA) and/or Standard Operating Procedures
(SOP) document(s) in advance of the inspection. These documents were reviewed and editorial
and substantive revision requirements and recommendations were made by this program

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outside of this formal report process. Although subsequent revisions were not requested to be
submitted, they must be completed by April 1, 2019.
The laboratory is reminded that any time changes are made to laboratory procedures, the
laboratory must update the QA/SOP document(s) and inform relevant staff. Any changes made
in response to the pre -audit review or to 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 each
approved practice, test, analysis, measurement, monitoring procedure or regulatory
requirement being used in the laboratory. In some instances, the laboratory may need to create
an SOP to document how new functions or policies will be implemented.
The laboratory is also reminded that SOPs are intended to describe procedures exactly as they
are to be performed. Use of the word "should" is not appropriate when describing requirements
(e.g., Quality Control (QC) frequency, acceptance criteria, etc.). Evaluate all SOPs for the proper
use of the word "should".
Laboratory Fortified Matrix (LFM) and Laboratory Fortified Matrix Duplicate (LFMD) are also
known as Matrix Spike (MS) and Matrix Spike Duplicate (MSD) and may be used
interchangeably in this report.
Requirements that reference 15A NCAC 2H .0805 (a) (7) (A), stating "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", are intended to be a requirement to document information pertinent to
reconstructing final results and demonstrating method compliance. Use of this requirement is not
intended to imply that existing records are not adequately maintained unless the Finding speaks
directly to that.
Contracted analyses are performed by Environmental Testing Solutions, Inc. (Certification # 600).
III. FINDINGS REQUIREMENTS COMMENTS AND RECOMMENDATIONS:
General Laboratory
Recommendation: Laboratory personnel have changed at both facilities since the last inspection.
Due to the number of Findings in this report that were cited in the previous report, it is
recommended that the laboratory adopt a formal documented training process for new employees
which includes, at a minimum, documentation of the following:
® staff have the appropriate education, training, experience and/or demonstrated skills, as
required to generate quality control results within method -specified limits
® staff have read the laboratory Quality Assurance Manual and/or applicable SOPs
® staff have obtained acceptable results on unknown performance evaluation samples or
other demonstrations of proficiency
A. Finding: Samples are not thermally preserved within 15 minutes of collection.
Requirement: Except where noted in this Table II [40 CFR Part 136.3] and the method for
the parameter, preserve each grab sample within 15 minutes of collection. For a
composite sample collected with an automated sample (e.g., using a 24-hour composite
sample; 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 <_6 °C, unless specified otherwise in this Table 11 or

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in the method(s), until collection, splitting, and preservation is completed. Ref: Code of
Federal Regulations, Title 40, Part 136; Federal Register Vol. 82, No. 165, August 28,
2017; Table II, Footnote 2.
Comment: Samples must be thermally preserved within 15 minutes unless they are
analyzed within that time. If samples will not be analyzed within 15 minutes, sample
temperature must be measured and documented upon collection and arrival at the
laboratory in order to demonstrate a downward trend in sample temperature.
B. Finding: The analytical balance is not being checked with three weights quarterly. Cited
previously on September 7, 2010.
Requirement: The analytical balance must be checked with one class S, or equivalent,
standard weight each day used and at least three standard weights quarterly. The values
obtained must be recorded in a log and initialed by the analyst. Ref: 15A NCAC 2H .0805
(a) (7) (K).
C. Finding: The analytical balance weights have not been verified against ASTM standard
weights in the past 5 years.
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: NC
WW/GW LC Policy.
D. Finding: Thermometers in ovens and refrigerators are not checked against a National
Institute of Standards and Technology (NIST) traceable thermometer annually.
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: 15 NCAC 2H .0805 (a) (7) (0).
Requirement: All thermometers and temperature measuring devices must be checked
every 12 months against an 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 an 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. The documentation must include the serial number of the NIST certified
thermometer or NIST traceable thermometer that was used in the comparison. Also
document any correction that applies (even if zero) on both the thermometer/meter and
on a separate sheet to be filed. (NOTE: Other certified laboratories may provide
assistance in meeting this requirement.)
NIST traceable thermometers used for temperature measurement must be
recalibrated in accordance with the manufacturer's recalibration date. If no
recalibration date is given, the NIST traceable thermometer must be recalibrated
annually.

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® NIST certified thermometers must be recalibrated, at a minimum, every five years. A
new certificate must be issued and maintained for inspection upon request.
Ref: NC WW/GW LC Policy.
Documentation
E. Finding: The laboratory does not report results of all tests on the characteristics of the
effluent.
Requirement: The results of all tests on the characteristics of the effluent, including but
not limited to NPDES permit monitoring requirements, shall be reported on the monthly
report forms. Ref: 15A NCAC 2B .0506 (b) (3) (J).
Requirement: If more than one pH concentration has been taken for a particular day,
these values cannot be averaged due to the logarithmic nature of pH concentration. All
values must be reported on the electronic Discharge Monitoring Report (eDMR), either in
the daily cell or the comments section. The following convention must be followed when
deciding which value to report in the daily cell:
® Any value in violation of permit limits must be reported in the daily cell. If multiple
samples yielded noncompliant results, the most extreme noncompliant value must
be reported in the daily cell.
® If all values taken during the day were compliant with the permit limits, the value
closest to the bounds of the limit range (high or low) must be reported in the daily
cell.
Ref: NC WW/GW LC Approved Procedure for the Analysis of pH.
Comment: The laboratory duplicates pH, but does not report the duplicate result if
different than the original.
Comment: Duplicates are not required for Field analyses. If they are analyzed voluntarily,
both values must be reported.
Comment: The laboratory is certified for Temperature, but it is not required in the permit
for the Altapass facility. Temperature is analyzed at the Altapass facility daily along with
pH, but not reported. If analyzed, the Temperature must be reported.
Recommendation: It is recommended that the laboratory not analyze the Temperature of
the effluent at the Altapass facility.
Comment: The laboratory analyzes pH, Fluoride, and Turbidity daily, but only reports one
value weekly as required by the permit. The laboratory stated that the effluent is analyzed
daily for process control and would have difficulty collecting a sample prior to the effluent
that would give them meaningful results. If this practice continues, the results must be
reported.
Comment: The Asheville Regional Office is requiring that the facility amend the eDMRs
for August 2017 — January 2018 to include the unreported results.

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F. Finding: Error corrections are not always properly performed.
Requirement: All documentation errors must be corrected by drawing a single line
through the error so that the original entry remains legible. Entries shall not be obliterated
by erasures or markings. Wite-Out®, correction tape or similar products designed to
obliterate documentation are not to be used. Write the correction adjacent to the error.
The correction must be initialed by the responsible individual and the date of change
documented. All data and log entries must be written in indelible ink. Pencil entries are not
acceptable. Ref: NC WW/GW LC Policy.
Comment: Error corrections are not initialed and dated consistently and occasional use of
correction fluid was noted.
G. Finding: The laboratory needs to increase the traceability documentation of purchased
materials and reagents, as well as documentation of standards and reagents prepared in
the laboratory. Cited previously on September 7, 2010.
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.
Requirement: Supporting records shall be maintained as evidence that these practices
are being effectively carried out. All analytical records must be available for a period of five
years. Ref: 15A NCAC 2H .0805 (a) (7) and (a) (7) (G).
H. Finding: The Field parameter benchsheets for both facilities were lacking pertinent data:
instrument identification and NPDES permit number. This is considered pertinent data.
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).
Requirement: The following must be documented in indelible ink whenever sample
analysis is performed: Facility name, sample site (ID or location), and permit number;
instrument identification (serial number preferred). Ref: NC WW/GW LC Approved
Procedure for the Analysis of pH, NC WW/GW LC Approved Procedure for the Analysis of
Temperature.
I. Finding: The Field parameter benchsheet for Altapass was lacking pertinent data: pH
meter calibration time. This is considered pertinent data.

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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: 15A NCAC
2H .0805 (a) (7) (A).
Requirement: The following must be documented in indelible ink whenever sample
analysis is performed: Meter calibration and meter calibration time(s). Ref: NC WW/GW
LC Approved Procedure for the Analysis of pH.
J. Finding: The laboratory benchsheet for Altapass was lacking pertinent data: NPDES
permit number. This is considered pertinent data.
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).
Requirement: The following must be documented in indelible ink whenever sample
analysis is performed: Facility name, sample site (ID or location), and permit number. Ref:
NC WW/GW LC Approved Procedure for the Analysis of Settleable Residue.
K. Finding: The sample volume and 45-minute stir time are not documented for Settleable
Residue. Cited previously on September 7, 2010.
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).
Requirement: Settle for 45 minutes, gently agitate sample near the sides of the cone with
a rod or by spinning, settle 15 min longer, and record volume of settleable solids in the
cone as milliliters per liter. Ref: SM 2540 F-2011 (3) (a).
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. 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).
Requirement: The following must be documented in indelible ink whenever sample
analysis is performed: Volume of sample analyzed; 45-minute stir time (use of a check box
is acceptable). Ref: NC WW/GW LC Approved Procedure for the Analysis of Settleable
Residue.
L. Finding: The benchsheets for Altapass were lacking pertinent data: Units of measure.
This is considered pertinent data.
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).
Requirement: The following must be documented in indelible ink whenever sample
analysis is performed: Units of measure. Ref: NC WW/GW LC Approved Procedure for

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the Analysis of pH and NC WW/GW LC Approved Procedure for the Analysis of
Temperature.
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).
Comment: The benchsheets were missing units of measure for pH, Turbidity and
Temperature.
M. Finding: The slope is not documented for Fluoride after calibration. This is considered
pertinent data.
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).
Requirement: It is required that the slope value or efficiency be documented for ion
selective electrode meter calibrations. Efficiency and slope of a ten -fold millivolt change
should be within manufacturer's specifications. The millivolt change may vary from the
given ranges depending on the concentration of the standards used. For example, the
specifications will be harder to achieve with 0.1 and 1.0 mg/L standards than with 1 and 10
mg/L standards. Ref: NC WW/GW LC Policy.
Proficiency Testing
Comment: When PT Sample results are reported, the NC WW/GW LC laboratory number is
reported as the EPA lab code and the EPA lab code is not reported. The vendor refers to these as
EPA ID and Agency ID. Contact the PT Sample provider to have your account updated to reflect
the correct EPA ID (NC00982) and Agency ID (197).
N. Finding: The laboratory does not have a documented plan for PT procedures.
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).
Requirement: Laboratories must have a documented plan (this is usually detailed in the
laboratory's Quality Assurance Manual or may be a separate SOP) of how they intend to
cover the applicable program requirements for Proficiency Testing per their scope of
accreditation. This plan shall cover any commercially available PT Samples and any inter -
laboratory organized studies, as applicable. The laboratory must also be able to explain
when PT Sample analysis is not possible for certain methods and provide a description of
what the laboratory is doing in lieu of Proficiency Testing. This shall be detailed in the plan.
The plan must also address the laboratory's process for submission of PT results and
related Corrective Action Reports (CARs). Ref: Proficiency Testing Requirements, May 31,
2017, Revision 2.0.
Requirement: SOPs must address situations where the instructions from the Accredited
PT Provider for the preparation, analysis or result calculations would constitute a deviation

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from the laboratory's routine procedure. Examples of this may include how low-level
samples will be analyzed, including concentration of the sample or adjustment of the
normality of a titrant. These instructions shall be followed when the concentration of a PT
sample falls below the range of their routine analytical method. Instructions shall also be
included in the laboratory's SOP for how high-level samples will be analyzed, including
preparation of multiple dilutions of the sample. These instructions will be followed when the
concentration of a PT falls above the range of their routine analytical method. Ref:
Proficiency Testing Requirements, May 31, 2017, Revision 2.0.
O. Finding: The laboratory is not documenting PT Sample analyses in the same manner as
routine Compliance Samples.
Requirement: All PT Sample analyses must be recorded in the daily analysis records as
for any Compliance Sample. This serves as the permanent laboratory record. Ref:
Proficiency Testing Requirements, May 31, 2017, Revision 2.0.
Comment: The analysis of PT Samples is designed to evaluate the entire process used to
routinely report Compliance Sample results; therefore, PT Samples must be analyzed and
the process documented in the same manner as Compliance Samples.
P. Finding: The laboratory is not documenting the preparation of PT Samples,
Requirement: PT Samples received as ampules are diluted according to the Accredited
PT Sample Provider's instructions. It is important to remember to document the
preparation of PT Samples in a traceable log or other traceable format. The diluted PT
Sample then becomes a routine Compliance Sample and is added to a routine sample
batch for analysis. No documentation is needed for whole volume PT Samples which
require no preparation (e.g., pH), but it is recommended that the instructions be
maintained. Ref: Proficiency Testing Requirements, May 31, 2017, Revision 2.0.
Comment: Dating and initialing the instruction sheet for each prepared PT Sample would
satisfy the documentation requirement.
Quality Control
Q. Finding: Precision (e.g., relative percent difference) and accuracy (e.g., percent recovery)
of QC results are not calculated, documented and evaluated to demonstrate the analytical
process is in control and the established acceptance criteria are met. Cited previously on
September 7, 2010.
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 precision and accuracy of QC results must be documented and
evaluated against the prescribed acceptance criteria to demonstrate that the analytical
process is in control. Any samples associated with QC not meeting the criteria must be
reanalyzed if possible. If this is not possible, the data must be flagged on the laboratory
reports and eDMR as all quality control requirements not met and giving a brief
description of the QC exceedance that occurred.

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Fluoride — Standard Methods, 4500 F- C-2011 (Aqueous)
R. Finding: A standard is not analyzed at the concentration of the lower reporting limit.
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. Ref: 15A NCAC 2H .0805 (a) (7) (1).
Comment: For effluent samples, the concentration of the lowest calibration standard is
0.2 mg/L and the laboratory reporting limit is 0.5 mg/L. If the calibration standard
concentrations are not changed, the reporting limit would be 0.2 mg/L.
S. Finding: A calibration blank is not analyzed initially, after every tenth sample (if applicable)
and at the end of the sample group.
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: NC WW/GW LC Policy.
T. Finding: A calibration verification standard is not analyzed after every tenth sample (if
applicable) and at the end of the sample group.
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: NC WW/GW LC Policy.
Comment: The calibration verification standard is prepared from the same source as the
calibration standards. The acceptance criterion is ± 10%.
U. Finding: A Laboratory Fortified Blank (LFB) is not analyzed with each sample group.
Requirement: Include at least one LFB daily or per each batch of 20 or fewer samples.
Ref: Standard Methods, 4020 B-2011 (2) (e) and Table 4020:1.
Comment: If the LFB is prepared from a different source than the calibration standards, it
will also fulfill the requirement for Finding V. The acceptance criterion of the LFB is ± 15%.
V. Finding: A second source standard is not analyzed each day samples are analyzed.
Requirement: When a standard curve is manually prepared (as opposed to a factory -set
calibration), it is required to analyze one known standard in addition to calibration
standards each day samples are analyzed to document accuracy. This standard must be
prepared from materials obtained from a source independent from the one used for
preparing the calibration standards (often referred to as a second source standard or
external reference standard). A second source standard may be:

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• a quality control standard obtained from a vendor,
• a standard prepared from primary standards obtained from a second vendor, or
• a standard made from primary standards from the same vendor but from a different
lot number (i.e., an independent lot) as those used to make the calibration standards.
Laboratory control standards are evaluated to assess whether the lab is in control of the
processes involved in the preparation and analysis of specific tests. Laboratory control
standards must be similar in composition to the environmental samples. They must
contain known concentrations of all analytes of interest and undergo the same preparatory
and determinative procedures as the environmental samples.
Second source standards must be evaluated using one of the following: vendor supplied
criteria, method -defined acceptance criteria, in-house calculated acceptance limits that are
statistically -derived from historical data based on three standard deviations from the mean
in the detectable range or other statistically viable evaluation criterion. If the results fall
outside of acceptance limits, the analysis is out of control. The analysis must be
terminated and the problem corrected prior to sample analysis. Ref: NC WW/GW LC
Policy.
W. Finding: The laboratory is not analyzing an LFM and LFMD. Cited previously on
September 7, 2010.
Requirement: When appropriate for the analyte (Table 4020:1), include at least one
LFM/LFMD daily or with each batch of 20 or fewer samples. To prepare an LFM, add a
known concentration of analytes (ideally from a second source) to a randomly selected
routine sample without increasing its volume by more than 5%. Ref: SM 4020 B-2011,
Table 4020:1 and (2) (g).
Comment: The LFMD fulfills the State's requirement for analyzing a sample duplicate so
the laboratory may stop performing unspiked sample duplicate analyses when this
requirement is implemented.
X. Finding: Distillation studies are not performed at the required frequency.
Requirement: The following frequencies are required:
Subsequently, each year analyze a minimum of 2 samples, spiked in duplicate,
approximately 6 months apart, both with and without the distillation step (a total of 8
samples). If effluent characteristics change (e.g., contributing industries are added or lost,
major change in plant processes, etc.), or if the laboratory changes to another analytical
method that requires the comparison, a minimum of two additional samples must be
spiked in duplicate and analyzed, both with and without the distillation step, to demonstrate
that that distillation is still not required. Ref: NC WW/GW LC Policy.
Comment: The laboratory performs a distillation study on two samples once each year,
rather than twice approximately six months apart.
Y. Finding: Distillation studies are not performed properly.
Requirement: Samples must be spiked according to the NC WW/GW LC Matrix Spike
Policy, in duplicate, to allow for a meaningful statistical comparison. It is recommended
that samples are spiked to yield a value within the verified calibration range so that sample
dilution is not needed. Comparisons between the matrix spike and matrix spike duplicate,

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as well as between distilled and undistilled samples must meet a 20% RPD acceptance
criterion. Both the distilled and undistilled samples must be analyzed using the same
method technology used to report compliance data for the permitted facility. It is
recommended that both the distilled and undistilled portions of the sample be analyzed by
the same laboratory. Per 15A NCAC 2H .0805 (e) (2), it would be permissible to have a
contract lab distill the samples and send the distillates back to the permittee for analysis
within the prescribed holding time. Ref: NC WW/GW LC Policy. Please submit the
results of a distillation study properly performed by July 31, 2018.
Comment: The samples used for the distillation study were not spiked.
Residue, Suspended — Standard Methods, 2540 D-2011 (Aqueous)
Z. Finding: The laboratory is not analyzing a volume of sample to yield a minimum of 2.5 mg
dried residue.
Requirement: Choose sample volume to yield between 2.5 and 200 mg dried residue. If
volume filtered fails to meet minimum yield, increase sample volume up to 1 L. Ref:
Standard Methods, 2540 D-1997 (3) (b).
Comment: Typically, 300 mL of sample is analyzed for effluent samples and 500 mL of
sample is analyzed for stream samples. The minimum of 2.5 mg is not consistently
obtained for stream samples. All effluent samples reviewed met the minimum 2.5 mg gain.
Comment: The range of measurement for Suspended Residue is determined by the
optimum solids loading on the filter, which can be controlled by adjusting the volume of
sample filtered. The method -defined reporting limit for Suspended Residue is 2.5 mg/L
when filtering 1 L of sample. This sample volume may not be necessary to demonstrate
compliance with regulatory limits; however, it is not acceptable to routinely report less -than
results using a reporting limit greater than 2.5 mg/L. A copy of this report will be shared
with the regional office.
Comment: If the minimum weight gain of 2.5 mg is not met, filter additional sample up to
1 L. If this is not possible, the reporting limit must be adjusted based on the sample
volume used and results must be qualified.
AA. Finding: The samples are not weighed to constant weight after sample analysis, nor is an
annual multiple weighing study to verify the adequacy of the drying time, performed. Cited
previously on September 7, 2010.
Requirement: 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. Ref: NC WW/GW LC
Policy.
Comment: North Carolina allows for an annual drying study in lieu of the requirement
above to repeat the drying cycle for every sample. A random full set of samples should be
used for the drying study. The repeated drying time in the oven should be at least 1 hour

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#197 The Quartz Corp. USA - Altapass
long. The time used for the annual drying study is the minimum time that samples are to
be dried until a new drying study is performed.
BB. Finding: A quarterly check standard is not being analyzed. Cited previously on
September 7, 2010.
Requirement: Analyze one suspended residue, one dissolved residue, one residual
chlorine and one oil and grease standard quarterly. Ref: 15A NCAC 2H .0805 (a) (7) (B).
pH — Standard Methods, 4500 H+ B-2011 (Aqueous)
Recommendation: It is recommended that the 7.0 S.U. buffer be used as a check buffer instead
of the 10.0 S.U. buffer since it is closer to the pH of compliance samples.
CC. Finding: The laboratory is not analyzing a post -analysis check standard buffer when
analyses are performed at multiple locations.
Requirement: When performing analyses at multiple sample sites, a post -analysis
calibration verification using the check standard buffer must be analyzed at the end of the
run. The post -analysis check standard buffer(s) must read within ±0.1 S.U. or corrective
actions must be taken. If recalibration is necessary, all samples analyzed since the last
acceptable calibration verification must be reanalyzed, if possible. If samples cannot be
reanalyzed, the data must be qualified. Ref: NC WW/GW LC Approved Procedure for the
Analysis of pH.
Temperature — Standard Methods, 2550 B-2010 (Aqueous)
DD. Finding: The temperature sensor on the pH meter used to obtain reported temperature
values has not been checked against an NIST traceable thermometer.
Requirement: All compliance temperature -measuring devices without a valid NIST
certificate must be checked initially and every 12 months against an NIST traceable
temperature -measuring device and the process documented. Documentation must include
the serial number of the device being checked. The serial number, stated accuracy and
expiration date of the NIST traceable temperature -measuring device used in the
comparison must also be documented. Verification data must be kept on file and be
available for inspection for 5 years. (NOTE: Vendors or other Certified laboratories may
provide assistance in meeting this requirement. When a vendor or other Certified
laboratory provides this assistance, they must provide a copy of their NIST Certificate or
the serial number, accuracy and calibration expiration date.) Ref: NC WW/GW LC
Approved Procedure for the Analysis of Temperature.
IV. PAPER TRAIL INVESTIGATION:
The paper trail consisted of comparing original records (e.g., laboratory benchsheets, logbooks,
etc.) and contract lab reports to eDMRs submitted to the North Carolina Division of Water
Resources. Data were reviewed for The Quartz Corp. USA - Altapass (NPDES permit #
NC0000353) for January, February and August 2017. The following errors were noted:

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#197 The Quartz Corp. USA - Altapass
Date
Parameter
Location
Value on Renchsheet
Value on eDMR
1/2/2017
Suspended
Residue
Effluent
22 mg/L = 168 lb/day
22 lb/day
1/9/2017
Suspended
Residue
Effluent
48 mg/L = 961 lb/day
48 lb/day
1/16/2017
Suspended
Residue
Effluent
25 mg/L = 549 lb/day
25 lb/day
1/24/2017
Suspended
Residue
Effluent
30 mg/L = 582 lb/day
30 lb/day
To avoid questions of legality, it is recommended that you contact the appropriate Regional
Office for guidance as to whether an amended eDMR(s) will be required. A copy of this report
will be made available to the Regional Office.
V. CONCLUSIONS:
We are concerned with the Findings that were cited previously and not corrected. The number
and severity of the Findings may make much of the data reported by the laboratory appear
questionable to third parties.
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
(13) Failing to respond to requests for information by the date due; or
(14) Failing to comply with any other terms, conditions, or requirements of this Section or of a
Laboratory certification.
Correcting the above -cited Finding(s) and implementing the Recommendation(s) will help this
laboratory to produce quality data and meet Certification requirements. The inspector would like
to thank the staff for its assistance during the inspection and data review process. Please
respond to all Findings and include supporting documentation and implementation
dates for each corrective action.
Report prepared by: Jason Smith
Report reviewed by: Anna Ostendorff
Date: February 16, 2018
Date: February 21, 2018

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