NC0005321_Lab Inspection_20010910

Michael F. Easley, Governor
William G. Ross Jr., Secretary
North Carolina Department of Environment and Natural Resources
Gregory J. Thorpe, Ph.D.
Acting Director
Division of Water Quality
September 10, 2001
525
Mr. Bryan A. Laney
Buckeye Lumberton Inc.
P. O. Box 1305
1000 East Noir Street
Lumberton, NC 28359-
SUBJECT: Laboratory Certification Maintenance Inspection
Dear Mr. Laney:
Enclosed is a report for the inspection performed on August 30, 2001 by Mr.
Frederick L. Bone. Within thirty days, please supply this office with a written item for item
description of how these deficiencies were corrected. A response is not required for
comments or recommendations unless specifically requested. If the deficiencies cited
in the enclosed report are not corrected, enforcement actions Will be recommended. For
certification maintenance, your laboratory must continue to carry out the requirements set
forth in 15A NCAC for 2H .0800.
Copies of the checklists completed during the inspectiorn may be requested from
this office. Thank you for your cooperation during the inspection. Please contact us at
919-733-3908, if you have questions or need additional information.
Sincerely,
GU YL4
James W. Meyer
Laboratory Section
Enclosure
cc: Frederick L. Bone
Fayetteville Regional Office
Laboratory Section N. C. Division of Water Quality 1623 Mail Service Center
FAX: [phone] Internet: www.esb.enr.state.nc.us/lab
41
NCDENR
Raleigh, NC 27699-1623 [phone]

On -Site Inspection Report
LABORATORY NAME: Buckeye Lumberton Inc.
ADDRESS:
P.O. Box 1305
1000East Noir Street
Lumberton, NC 28359
CERTIFICATE NO: 525
DATE OF INSPECTION: August 30, 2001
TYPE OF INSPECTION: Maintenance
EVALUATOR: Frederick L. Bone
LOCAL PERSON(S) CONTACTED: Bryan Laney
I. INTRODUCTION:
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 spacious and well equipped. All facilities and equipment are well maintained.
Records are well kept and most data looked good. Some further quality control procedures need to be
implemented.
II{. DEFICIENCIES, RECOMMENDATIONS, REQUIREMENTS, AND COMMENTS:
General:
1. DEFICIENCY: The laboratory is not making the proper temperature corrections on some the
laboratory thermometers. 1 -
REQUIREMENT: All thermometers must meet National Institute of Standards and Technology
(NIST) specifications for accuracy or be checked against a NIST traceable thermometer and proper
corrections made. Ref: 15A NCAC 2H .0805 (a) (7) (o)
A. COMMENT: Some of the mid -range standards used in the laboratory are not analyzed at a
concentration of one-half of the highest calibration standard. As was discussed at the time of the
audit the mid -range is to be defined as on half the concentration of the high standard. (Residual
Chlorine and Ammonia)
REQUIREMENT: The laboratory must adjust the concentrations of the daily mid -range verification
standards to be one half of the highest concentration standard. Verify the standard curve daily by
analyzing one or more standards within the linear range, as specifed in the individual method. The
curve must be updated as set forth in the standard procedures, each time the slope changes by more

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than 10 percent at midrange. Ref: Standard Methods 18th Edition 1020 B. Quality Control section 5
p. 1-5, and Ref: 15A NCAC 2H .0805 (a) (7) (i).
B. COMMENT: The thermometer in the drying oven is currently reading the internal air temperature
and not the sample matrix temperature.
RECOMMENDATION: The thermometer in the drying oven should be placed in a beaker of sand or
other solid matrix. This ensures that the proper matrix temperature ismeasured as well as providing
a more stable temperature environment for the thermometer readings.
C. COMMENT: Some of the daily logs and benchsheets used by the laboratory do not contain all of
the necessary labeling information. Units of measure were not associated with some of the data
values listed in the logbooks and benchsheets.
REQUIREMENT: The laboratory should review all of their benchsheets and log books to make sure
that every entry is marked with the appropriate unit of measure. Every number recorded on a
benchsheet or logbook must have an appropriate unit assigned to it.
D. COMMENT: The laboratory is not making corrections to the data in an approved manner. The
laboratory is writing over data results.
REQUIREMENT: If an error is made in data recording the error must be removed by making a single
line through the incorrect entry, recording the correct entry beside error, and initialing and dating the
error. Ref: SW 846 Sept 1994 Test Methods for Evaluating Wastes Chapter One pg. 13.
E. COMMENT: The laboratory is not weighing a weight in the Tess than one gram range quarterly.
REQUIREMENT: An analytical balance capable of weighing 0.1 mg is required for certification. Ref:
15A NCAC 2H .0805 (a) (6) (d). The balance must be calibrated with class "S" weights to bracket the
range of the instrument.
F. COMMENT: The laboratory does not keep a log for the preparation of standards and reagents.
REQUIREMENT: The laboratory must have a written record of all standards and reagents on file for
a period of at least three years. A standard reagent log will help the laboratory to meet this
requirement. A standards logbook will also enable the laboratory to document exactly when, by
whom, and how each reagent was prepared.
Residual Chlorine:
G. COMMENT: The laboratory does not analyze a second source QC standard daily for this parameter.
REQUIREMENT: Analyze one known standard in addition to calibration standards each day that
samples are analyzed to document accuracy. This laboratory control standard must be from a
second source. For held curves for colorimetric methods, it must be analyzed after the calibration
verification standard is analyzed. It is recommended that this laboratory control standard, like the
calibration verification standard, have a mid -range concentration and not vary by more than ± 10%. If

Page 3
it does the analysis is out of control. The analysis must be terminated and the problem corrected.
Ref: 15A NCAC 2H .0805 (a) (7) (B), (F), and Standard Methods,18thrEdition - Method 1020 B.3.
Residual Chlorine and Ammonia:
H. COMMENT: The laboratory reports the value of the analytical blanks as < 0.0001 mg/L. This is
well below the lowest standard in the analytical curve.
REQUIREMENT: The laboratory must report blank values as less than the lowest standard in the
analytical curve.
Residual Chlorine and pH:
I. COMMENT: The laboratory is not recording the time sampled and the time analyzed for pH and
Residual Chlorine samples on the General Worksheets.
Note: This information is important to document that the holding times were met for these analyses.
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).
pN.:
J. COMMENT: The laboratory does not record the pH electrode calibration information on the same
benchsheet with" the sample data. The calibration information is logged on a separate pH calibration
log.
RECOMMENDATION: It is strongly recommended that the laboratory record all calibration
information on the same benchsheet as the. sample data. This allows for ease of data verification as
well as eliminating the possibility of data becoming separated from essential calibration information.
K. COMMENT: The laboratory is calibrating the pH meter with a 4 and 7' buffer an reading a pH 10
buffer to verify this calibration.
REQUIREMENT: The laboratory must calibrate the pH meter with at least two buffers and read a
third buffer below pH 10, approximately 3 pH units different from the second buffer and the reading
should be within 0.1 pH units from the expected value. Ref: Standard methods 18th Edition 4500-H
B.(4) (a) p4-68.
Total Suspended Solids:
2. DEFICIENCY: The laboratory is not analyzing a sample of sufficient size to yield 1.0 mg of residue
on each filter.
REQUIREMENT: The lab must filter enough sample to achieve >1.0 mg residue on the filter. Ref:
EPA 600/4 - 79•-020, Revised Method 1983 Method 160.2 pg. 2-1.

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3. DEFICIENCY: The laboratory does not properly verify drying times ;for the total suspended solids
on an annual basis. The laboratory must show that the length of the drying time is sufficient for the
type of samples analyzed.
REQUIREMENT: Dry evaporated sample for at least 1 hour in an oven at 103 the 105°C, cool in
desiccator to balance temperature, and weigh. Repeat cycle of drying, cooling, desiccation, and
weighing until a constant weight is obtained, or until weight change is less than 4% of previous
weight or 0.5 mg, whichever is less. Ref: Standard Methods 18th Edition 2540 D Total Suspended
Solids at 103-105° C section (3) c p2-56.
L. COMMENT: The laboratory must filter a volume of DI water (equal to the maximum sample volume
used) as a method blank each analysis day.
Note: The laboratory is currently analyzing blanks for this analysis, but the volume of the blank is not
equal to the maximum sample volume used.
REQUIREMENT: Blanks must be analyzed in order to determine bias in each sample batch. Ref:
Standard Methods 18th Edition - Method 1020B pg. 1-5.
M. COMMENT: The laboratory does not record the time that the samples were placed into the oven
or removed from the oven on the benchsheet.
REQUIREMENT: The time in and out of the drying oven must be documented to verify drying time is
adequate.
BOD:
4. DEFICIENCY: The initial DO for BOD of some samples is above 9.0 mg/L.
REQUIREMENT: Samples that are supersaturated with DO must be brought to 20°C and vigorously
shaken or aerated with clean compressed air to bring the sample to an initial DO below 9.0 mg/L. The
initial accepted DO range is 7 - 9 mg/L. Ref: Standard Methods, 18th Edition 5210B (6)b p.5-6.
5. DEFICIENCY: The laboratory does not document the pH of each sample.
REQUIREMENT: Samples must be neutralized to a pH of 6.5 - 7.5. Ref: Standard Methods, 18th
Edition - Method 5210 B (4) (e) (1). pg.5-4.
6. DEFICIENCY: The laboratory does not document the pH of the buffered dilution water to be 7.2.
REQUIREMENT: The pH of the buffered dilution water should be 7.2 with out further adjustment.
Ref: Standard Methods, 18 Edition - Method 5210 B (3) (a). pg. 5-3
Ammonia:
7. DEFICIENCY: The laboratory is not checking the removal of residual chlorine or documenting the
pH preservation of ammonia samples.

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REQUIREMENT: The laboratory must document that all residual chlorine has been removed and
that the pH of all samples has been properly adjusted. A record of date collected, time collected,
sample collector and use of proper preservatives must be maintained. Ref: 15A NCAC 2H .0805 (a)
(7) (M)•
Conductivity:
N. COMMENT: The laboratory does not verify the automatic cell constant adjustment for the
conductivity meter on an annual basis.
REQUIREMENT: The laboratory must verify the automatic cell constant on an annual basis. The
procedure for doing the cell constant can be found in Standard Methods, 18th Edition 2510B.4a. p. 2-
45.
8. DEFICIENCY: The laboratory does not bracket all samples analyzed .for this parameter. Some -
sample values are above the highest standard analyzed daily.
COMMENT: The lab may choose to make a higher standard using .the chart in Standard Methods,
18 Edition- Method 2510 Table 2510:1. pg. 2-43 to bracket the higher sample values.
REQUIREMENT: For analytical procedures requiring a series of standards, the concentrations of
these standards must bracket the concentration of the samples analyzed, and one of the standards
must have a concentration equal to the laboratory's lower reporting limit. 1 Ref: 15A NCAC 2H .8005
(a) 97) (1)
IV. PAPER TRAIL INVESTIGATION:
This consisted of comparing data reported on DMR's submitted to this Division] with the values obtained on
laboratory bench worksheets. Data reviewed for the months of January, March,' and May 2001 indicated no
problems in proper data reporting.
V. CONCLUSIONS:
Correcting the above deficiencies and comments should help them to; produce quality- data and meet -
certification requirements.
Please respond to all numbered Deficiencies and lettered Comments cited in this report.
Report prepared by: Frederick L. Bone Date: September 4, 2001