#171_06_2012_FINAL

INSPECTION REPORT ROUTING SHEET
To be attached to all inspection reports in-house only.
Laboratory Cert. #: 171
Laboratory Name: Domtar Paper Company, LLC.
Inspection Type: Industrial Maintenance
Inspector Name(s): Nick Jones, Gary Francies
Inspection Date: 6/12/2012
Date Report Completed: 7/13/2012
Date Forwarded to Reviewer: 7/13/2012
Reviewed by: Jason Smith
Date Review Completed: 7/19/12
Cover Letter to use: _ Insp. Initial X Insp. Reg. _ Insp. No Finding _
Unit Supervisor:
Date Received:
Date Forwarded to Linda:
Date Mailed:
Gary Francies
7/23/2012
8/2/2012
%�L, I c�_
Insp. CP _ Corrected

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41
North# Department of ! and Natural Resources
Beverly Eaves Perdue
Governor
171
Mr. Alan Barnes
Domtar Paper Company, LLC.
P.O. Box 747
Plymouth, NC 27962
Division of Water Quality
Charles Wakild, P. E.
Director
August 2, 2012
Dee Freeman
Secretary
Subject: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW
LC) Maintenance Inspection
Dear Mr. Barnes:
Enclosed is a report for the inspection performed on June 16, 2012 by Nick Jones and myself. I
apologize for the delay in getting this report to you. 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 finding(s) were 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.
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 us at
828-296-4677.
Sincerely,
G ci�
Gary Francies
Certification Unit Supervisor
Laboratory Section
Enclosure
cc: Washington Regional Office
Nick Jones
Master File
DENR DWO Laboratory Section NO 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
NorthCar®Iin.a
;Vatumllff
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
Domtar Paper Company, LLC.
NC0000680
P.O. Box 747
Plymouth, NC 27962
171
June 16, 2012
Industrial Maintenance
Nick Jones and Gary Francies
Alan Barnes
This laboratory was inspected to verify its compliance with the requirements of 15A NCAC 2H .0800 for
the analysis of environmental samples.
IL GENERAL COMMENTS:
The lab was clean and well organized. All the equipment necessary to perform the certified analyses was
present and appeared well maintained. The system for traceability of standard and reagent preparation is
effective, thorough and easy to follow. Laboratory personnel communicate well with sample collectors
and coordinate sample analyses effectively to manage workload and holding times. Proficiency Testing
(PT) samples have been analyzed for all certified parameters for the 2012 PT calendar year and the
graded results were acceptable except for Chemical Oxygen Demand (COD).
The primary objective of the inspection was to respond to a request by the facility for technical assistance
regarding COD analysis. The time remaining after the technical assistance was used to perform an
abbreviated inspection. The abbreviated inspection consisted of reviewing the checklists completed by
the facility for all certified parameters.
Since the inspection, the facility has chosen to drop certification for COD and contract out that analysis.
An updated certification attachment reflecting this change, effective June 5, 2012, was issued on June
16, 2012.
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.
On May 18, 2012, EPA promulgated changes to the list of Clean Water Act (CWA) methods at 40 CFR
Part 136.3. This action, referred to as the Methods Update Rule (MUR) approves new methods, or

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changes to existing methods, that affects over 100 EPA methods, Standard Methods, ASTM methods,
and other test procedures in Part 136 of Title 40 of the Code of Federal Regulations (CFR). The rule
also contains a number of clarifications relating to approved methods, sample preservation and holding
times, and method modifications. The final rule may be found at:
http://water.epa.gov/scitech/methods/cwa/update index.cfm. The North Carolina
Wastewater/Groundwater Laboratory Certification (NC WW/GW LC) program will be asking certified
laboratories to move toward implementation of the new rule with changes fully implemented by the end
of 2012. Each laboratory will need to review the MUR and evaluate its effect on current laboratory
practices. These changes must be made in the laboratory's Standard Operating Procedures and in
Quality Manuals, as well as any other place where the method is cited, e.g., reports, benchsheets,
logs, etc. During this transition period, inspection reports will refer to the methods employed at the
laboratory at the time of the inspection, but will reference the requirements in the most recently
approved version of the method. Any difficulties encountered with meeting the requirements of these
references by the date due may be addressed in the written corrective action response.
Contracted analyses are performed by Environment 1, Inc. (Certification #10).
The requirements associated with Findings A, B, C, F and G are new policies that have been
implemented by our program since the last inspection or required due to the May 18, 2012 EPA Method
Update Rule.
III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:
Documentation
A. 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 21-1.0805 (a) (7).
Requirement: Laboratories must have a documented plan (this is usually detailed in the
laboratory's Quality Assurance Manual) 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 proficiency testing and any inter -laboratory organized studies, as
applicable. The laboratory must also be able to explain when proficiency testing is not possible for
certain parameters 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 proficiency testing results and related corrective action responses. Laboratory
Standard Operating Procedures (SOPs) must address 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, February 20, 2012, Revision 1.2.
B. Finding: The laboratory is not documenting PT sample analyses in the same manner as
environmental samples.

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Requirement: All PT sample analyses must be recorded in the daily analysis records as for any
environmental sample. This serves as the permanent laboratory record. Ref: Proficiency
Testing Requirements, February 20, 2012, Revision 1.2.
C. Finding: The preparation of PT samples is not documented.
Requirement: 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. Ref: Proficiency Testing Requirements, February 20,
2012, Revision 1.2.
General Laboratory
D. Finding: The analytical balance weights have not been verified against ASTM standard
weights.
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
Wastewater/Groundwater Laboratory Certification Policy. See attachment for additional
guidance.
Residue, Suspended (TSS) — Standard Methods 2540D
Comment: The facility performs a quarterly drying study to determine the minimum drying time
needed. North Carolina allows for an annual drying study.
E. Finding: No maximum filtration time has been observed or set for Total Suspended Solids (TSS).
Requirement: If complete filtration takes more than 10 min, increase filter diameter or decrease
sample volume. Ref: Standard Methods, 2540 D-1997 (3) (b).
Biochemical Oxygen Demand (BOD) — Standard Methods 5210 B
Recommendation: Analyzing a seeded blank is recommended to demonstrate proper analyst
techniques and homogeneity of seeding material. The seeded blank should be within 0.2 mg/L of the
calculated seed correction. However, it is not to be used to determine the seed correction value.
F. Finding: The pH of BOD samples were not being adjusted according to the requirements of the
approved method promulgated in the May 18, 2012 EPA Method Update Rule.
Requirement: All samples — Check pH; if it is not between 6.0 and 8.0, adjust sample
temperature to 20 + 3°C, then adjust pH to 7.0 to 7.2 using a solution of sulfuric acid (H2SO4) or
sodium hydroxide (NaOH) of such strength that the quantity of reagent does not dilute the
sample by more than 0.5%. Exceptions may be justified with natural waters when the BOD is to
be measured at in -situ pH values. The pH of dilution water should not be affected by the lowest
sample dilution. Always seed samples that have been pH adjusted. Ref: Standard Methods,
5210 B-2001. (4) (b) (1).
G. Finding: Extra nutrient, mineral, and buffer solutions are not added to the Biochemical Oxygen
Demand (BOD) bottles containing more than 67% (i.e., > 201 mL) sample.

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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: Standard Methods, 5210 B-2001, (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.
Chemical Oxygen Demand (COD) — Standard Methods 5220 C
Comment: The facility was using mid -range (0-1500 ppm, Cat# 25651) Hach COD Mercury -free
digestion vials. The low -range (0-150 ppm, Cat# 21258-25) Hach COD digestion vials, being an order
of magnitude lower in concentration, would allow the facility to analyze samples more accurately within
the range for which they are concerned. The facility was in possession of the low -range vials. It is
believed that the unacceptable result obtained for the analysis of the PT sample was due to the
decreased sensitivity caused by the use of the higher concentration potassium dichromate digestion
vials.
Also, according to the Code of Federal Regulations, Title 40, Part 136; Federal Register Vol. 72, No.
47, March 12, 2012, mercury -free COD vials are not approved for NPDES compliance monitoring by
the EPA because of the possibility of chloride interference.
The facility had not yet implemented the new matrix spiking policy for COD samples. No response is
necessary for this finding.
IV. PAPER TRAIL INVESTIGATION:
No paper trail was performed.
V. CONCLUSIONS:
Correcting the above -cited findings and implementing the recommendation 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: Nick Jones Date: July 13, 2012
Report reviewed by: Jason Smith Date: July 19, 2012

Weight Verification (NC WW/GW LC Policy 05/23/2008)
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). Verification may be accomplished by:
1. Sending laboratory weights back to the manufacturer for recertification - reference weights shall
be calibrated by a body that can provide traceability to ASTM specifications, or
2. Checking laboratory weights against certified reference weights (i.e., weights that have been
recertified as above) and found to be within ASTM Class 1 or Class 2 tolerances (see table
below) - often the balance service technician may provide this service.
Note: Although some manufacturers will assign a one-year calibration due date, 5 years is considered
an acceptable calibration interval due to the limited use of the reference weight set.
Documentation of weight verifications or recertification must be maintained for 5 years. If the condition
of a weight(s) is in question at any time due to damage (e.g., corrosion, nicks, scratching, etc.), the
laboratory must have that weight(s) re -verified as described above.
Maximum tolerances (Ref. ASTM E 617-97, 2003)
Denomination
Maximum tolerance for
ASTM Class 1 and 2
weights, (± mg)
500 g
1.2
300 g
0.75
200 g
0.50
100 g
0.25
50 g
0.12
30 g
0.074
20 g
0.074
log
0.074
5 g
0.054
3 g
0.054
2 g
0.054
1 g
0.054
500 mg
0.025
300 mg
0.025
200 mg
0.025
100 mg
0.025
50 mg
0.014
30 mg
0.014
20 mg
0.014
10 mg
0.014
5 mg
0.014
3 mg
0.014
2 mg
0.014
1 mg
0.014