#221 - 9-2011 - FINAL

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NCDENR
North Carolina Department of Environment and Natural Resources
Division of Water Quality
Beverly Eaves Perdue Coleen H. Sullins
Governor Director
November 28, 2011
221
Ms. Pem Carter
CNA Holdings, Inc. — Ticona Facility
2525 Blacksburg Road
Grover, NC 28073-9461
SUBJECT: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC)
Maintenance Inspection
Dear Ms. Carter:
Dee Freeman
Secretary
Enclosed is a report for the inspection performed on September 22, 2011 by Chet Whiting. I apologize for the
delay in getting this report to you. Where finding(s) 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,
Gary Francies
Unit Supervisor
Laboratory Section
CC: Chet Whiting
Gary Francies
Master files
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 27607-6446
Phone: [phone] \ FAX: [phone]
Internet: www.dwglab.org
An Equal Opportunity, Affirmative Action Employer Customer Service:1-877-623-6748 www.ncwaterquality.org

INSPECTION REPORT ROUTING SHEET
To be attached to all inspection reports in-house only.
Laboratory Cert. #:
221
Laboratory Name:
CNA Holdings, Inc. — Ticona Facility
Inspection Type:
Industrial Maintenance
Inspector Name(s):
Chet Whiting
Inspection Date:
September 22, 2001
Date Report Completed:
October 7, 2011
Date Forwarded to Reviewer: October 10, 2011
Reviewed by:
Todd Crawford
Date Review Completed:
October 11 2011
Cover Letter to use: _
Insp. Initial X Insp. Reg. _ Insp. No Finding _ Insp. CP _Corrected
Unit Supervisor:
Gary Francies
Date Received:
10/11/2011
Date Forwarded for mailing:
11/28/2011
Date Mailed: a �.

LABORATORY NAME:
NPDES PERMIT #:
ADDRESS:
CERTIFICATE #:
DATE OF INSPECTION:
TYPE OF INSPECTION:
AUDITOR(S):
LOCAL PERSON(S) CONTACTED:
IkiI"Z 01010Is] 'kF
•n-Site Inspection Report
CNA Holdings, Inc. — Ticona Facility
NC0004952
2525 Blacksburg Road
Grover, NC 28073-9461
221
September 22, 2011
Industrial Maintenance
Chet Whiting
Pem Carter
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 requirements associated with Findings A, B, D and E are new policies that have been implemented
by our program since the last inspection.
r - e; - • r - • �.
A. Finding: The date materials are put in use is not always documented.
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:
North Carolina Wastewater/Groundwater Laboratory Certification Policy.

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#221 CNA Holdings, Inc.—_Ticona Facility_
General Laboratory
B. Finding: Auto-pipettors are not calibrated.
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 and documented. Each liquid -dispensing device must meet the manufacturer's
statement of accuracy. Ref: North Carolina Wastewater/Groundwater Laboratory Certification
Policy.
C. Finding: Standard Operating Procedures (SOPs) have not been updated since 2004 for all of
the parameters included on the laboratory's certificate attachment.
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: The laboratory must have an updated Quality Control/Standard Operating
Procedures document for the parameters included on the certificate attachment by March 31,
2012. This must be submitted for review upon completion.
Comment: The Analytical Quality Control document must include standard operating procedures.
A standard operating procedure describes the method in such detail that an experienced analyst
unfamiliar with the method can obtain acceptable results and meet documentation requirements.
Standard operating procedures must be developed which describe in detail how a method is
performed in that particular laboratory.
Recommendation: It is recommended that SOPs include a revision history with relevant dates
and a brief description of the change(s) made.
Standard Methods,
Recommendation: It is recommended that the laboratory change terminology from time set up and
counted to time in and out of the water bath to clearly demonstrate the required incubation time was
met.
D. Finding: A calibration blank and calibration verification standard (mid -range) 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, 20t" Edition, 1020 B. (10) (c), 3020 B. (2) (b), and 4020 B. (2).
E. Finding: The laboratory is not analyzing matrix spikes.

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#221 CNA Holdings, Inc. —Ticona Facility
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
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.
If the unspiked sample result is in the top 40% of the calibration range, the sample should be
diluted and the matrix spike prepared using the diluted sample. The recovery of the matrix spike
samples must be bracketed by the calibration range.
The volume of spike solution used in matrix spike preparation must in all cases be <_ 10% of the
total matrix spike volume. It is preferable that the spike solution constitutes <_ 1 % of the total
matrix spike volume so that the matrix spike can be considered a whole volume sample with no
adjustment ent by calculation necessary. if the Spike solution volume ie constitutes %1 % of the total
sample volume, the sample concentration or spike concentration must be adjusted by
calculation. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy.
Chemical Oxygen Demand — Standard Methods, 18th Edition, 5220 D
Fecal Coliform — Standard Methods, 18th Edition, 9222 D
Suspended Solids — Standard Methods, 181h Edition, 2540 D
F. Finding: Sample collection time and receipt in the laboratory time are not clearly documented.
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: The samples are collected when the pH sample is collected and are received in the
laboratory when the pH sample is returned for analysis. The samples are received in less than 15
minutes; however this procedure is not documented. This information must be documented or the
laboratory must document thermal preservation (samples received on ice, temperature at
collection and upon receipt.)
Recommendation: The laboratory has an in-house custody document. It is recommended that
sample collection and receipt be documented there.
G. Finding: Chemical preservation (to a pH of < 2) is not documented.
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: 40 CFR Table II, footnote 2 states: Add the preservative to the sample container
prior to sample collection when the preservative will not compromise the integrity of a grab
sample, a composite sample, or an aliquot split from a composite sample; otherwise, preserve

IV.
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#221_CNA Holdings, Inc. — Ticona Facility
the grab sample, composite sample, or aliquot split from a composite sample within 15 minutes
of collection.
Recommendation: The laboratory has an in-house custody document. It is recommended that
the chemical preservation be documented there.
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 the Ticona Plant for May, July, and August 2011. No transcription errors were detected.
The facility appears to be doing a good job of accurately transcribing data.
Correcting the above -cited findings and implementing the recommendations will help this lab to
produce quality data and meet certification requirements. The inspector would like to thank the staff for
its assistance during the inspection and data review process. Please respond to all findings.
Report prepared by: Chet Whiting
Report reviewed by: Todd Crawford
Date: October 7, 2011
Date: October 11, 2011