NC0005321_Lab Certfication Maintenance Inspection_19980515

NORTH CAROLINA DEPARTMENT OF
ENVIRONMENT !AND I NATURAL RESOURCES
DIVISION OF WATER QUALITY
May 15, 1998
525
Mr. Chuck Oxendine
Buckeye Lumberton Inc.
P. O. Box 1305
1000 East Noir Street
Lumberton, NC 28359-
SUBJECT: Laboratory Certification Maintenance
Dear Mr. Oxendine:
RECEIIVE
1 9. 1998
FAYE �a E'EV L,.LF
AEG. OFFIc
Inspection
Enclosed is a report for the inspection performed on December 4,
1997 by Ms. Harvi C. Cooper. Within thirty days, please supply this office
with a written item for item description of how these violations were
corrected. A response is not required for comments or recommendations
unless specifically requested. We are seriously concerned about the Failure -
to analyze a Check standard for the BOD analysis violation found during the
inspection. Ifthe violations cited in the enclosed report are not corrected,
enforcement actions will be recommended. For cerfiification 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. Please contact us at 919-733-3908 if you have questions or
need additional information.
Sincerely,
Q/ YL 4' �/. i�' C•
James W. Meyer
Laboratory Section
Enclosure
cc: Harvi C. Cooper
Norman L. Good
Fayetteville Regional Supervisor
• LABORATORY SECTION
4405 REEDY CREEK (ROAD, RALEIGH, NORTH CAROLINA 27607-6445
PHONE [phone] FAX [phone]
AN EQUAL OPPORTUNITY / AFFIRMATIVE ACTION EMPLOYER - 50% RECYCLED/10% POST -CONSUMER PAPER

ON -SITE INSPECTION REPORT'
LABORATORY NAME & ADDRESS: Buckeye Lumberton Inc.
1000 East Noir Street
Lumberton, NC 28359-
CERTIFICATE NO.: 525
DATE OF INSPECTION: December 4, 1997
TYPE OF INSPECTION: Maintenance
EVALUATORS: Harvi C. Cooper
LOCAL PERSON CONTACTED: Eric Bolin and Ronald Radford
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 was clean and well organized. Instruments and facilities are
well maintained. Several violations were found and some further quality
control procedures have been recommended. 1
III. VIOLATIONS, REQUIREMENTS RECOMMENDATIONS AND COMMENTS:
BOD
Violation: Lab is not always documenting the time in and out of the
incubator for BOD samples.
Comment: The comment on the BOD checklist indicates that no time is
recorded, but all BODs are initiated and taken off in the morning.
1
Requirement: Lab must document date and time in and out of the incubator for
BOD samples. ref: 15A NCAC 2H .0805 (a)(7)(H) pg 6:
Violation: A GGA check sample was not analyzed with every set of BOD
samples.

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Comment: A GGA check sample was not included in the analytical batches set
up on 10/11, 10/12, 10/25, 10/26, 11/8 or 11/9/97. These dates all represent
weekend shifts. There are no instructions to include a GGA check sample in
the standard operating procedure.
Requirement: A 2% GGA. standard must be analyzed with each set of samples
and the value must be 198 ± 30.5 mg/l. Ref: Standard Methods 18th Edition
5210 B (6) (a)
Violation: Analyst indicated that corrective actions were taken when the GGA
check sample was outside of method established control limits, but the
corrective actions were not documented.
Requirement: Any time quality control results indicate an analytical
problem, the problem must be resolved and any samples involved must be
rerun if the holding time has not expired. ref: 15A NCAC 2H .0805 (a)(7)(F)
pq. 6 Supporting records shall be maintained as evidence that analytical
quality control practices are being effectively carried out. ref: 15A NCAC
2H .0805 (a)(7) pq. 6 The laboratory must document the corrective action
taken as evidence that quality control practices are followed.
Recommendation: Recommend documenting corrective actions on the BOD bench
worksheet.
Total Residual Chlorine
Violation: Corrective actions are not always documented when the control
limits for slope efficiency for the Total Residual Chlorine ion selective
electrode exceeds the control limits of 26 to 30 mVIas stated on the current
bench worksheet.
Comment: The slope documented is often high. Corrective actions are
sometimes noted.
Requirement: The laboratory's current standard operating procedure requires
that corrective actions be taken when .control limits are exceeded. ref: BL-
MP-101 Version 3 Issue B Supporting records Ishall be maintained as
evidence that analytical quality control practices are being effectively
carried out. ref: 15A NCAC 2H .0805 (a)(7) pq. 6 The laboratory must
document the corrective action taken as evidence that quality control
practices are followed.
.Ammonia
Comment: Calibration documentation for the Ammonia ion selective electrode
indicates that manufacturer's criteria for slope efficiency is seldom met
for the 0.1 to 1.0 mg/L calibration range. Most samples analyzed are greater
than 1.0 mg/L and the daily limit on the DMR is approximately 11 mg/L.
Recommendation: Conditioningthe electrode prior to use may be helpful.
Samples are currently analyzed daily immediately following collection.
Conditioning of the electrode would require a greater interval between
analytical batches than daily analysis would allow Laboratory could either

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secure a second instrument and alternate use to allow time for conditioning,
or preserve and batch the ammonia samples. If' these options are not
desirable, we recommend calibrating from 1.0 to 10.0 mg/L and using 1.0 mg/L
as the lower reporting "concentration. Another alternative would be
calibrating from 0.5 to 5.0 mg/L using 0.5 mg/L as the lower reporting
concentration.
Requirement: Check electrode sensing element performance according to
manufacturer's instructions to make sure that electrode is operating
properly. ref: Standard Methods 18th Edition 4500-NH3 F. (4)(b)and (d) pq.
4-82 Lab must maintain documentation of calibration verification. All
analytical records must be available for a period ol,f three years. ref: 15A
NCAC 2H .0805 (a)(7)(G) pq. 6 Please submit a copy of the laboratory's
calibration documentation for ammonia. Also include a:copy of the section
of the laboratory's ion selective electrode manual with the manufacturer's
acceptance range for slope efficiency.
pH
Violation: Control limits used for the calibration
than ± 0.1 pH unit.
check buffer are greater
Comment: Lab is currently calibrating the pH meter with buffers at 4 and.7
pH units and checking the calibration with a buffer at,10 pH units. The
lower and upper control limits used are 9.85 and 10,.15'pH units
respectively. None of the values recorded for the check buffer were greater
than 0.1 unit different from 10.0 units.
Requirement: To validate calibration, immerse electrodes in a third buffer
below pH 10, approximately 3 pH units different from the second calibration
buffer; the reading should be within 0.1 unit for the pH of the third
buffer. ref: Standard Methods 18th Edition Method 4500-H± (4)(a) pg. 4-68
Total Suspended Solids
Comment: Lab is currently filtering from 25 to 50
effluent monitoring.
mis of sample for
Recommendation: Recommend filtering larger volumes ofisample to ensure that
at least 1.0 mg residue is retained on the filter. The recommendations for
selection of filter and sample sizes from Standard Methods 18th Edition are
as follows: Choose sample volume to yield between 10 and 200 mg dried
residue. If more than 10 minutes are required to complete filtration,
increase filter size or decrease sample volume. When very low total
suspended solids are encountered (less than 10 mg/L), less dried residue
may be collected; compensate by using a high -sensitivity balance (0.002
mg). ref: Standard Methods 18th-Edition Method 2540 D. (3)(b) pq. 2-56
General
Recommendation: Recommend increasing the documentation of reagent and
standard preparation. Recommend the preparation of all reagents, standards
and media be documented in a preparation log or logs. Traceable identifiers
should link solution preparation information to analytical batches in which
the solutions are used. Documentation of solutionlpreparation should
include the analyst's initials, date of preparation, the volume or weight
of standard used, the solvent and final volume of:the solution. This

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information as well as the vendor, manufacturer, lot number, and expiration
date should be retained for primary standards or chemicals used.
Comment: Lab checklists indicate that control limits have not been
established for duplicate sample results. Duplicate values reviewed were
within guidelines established in Table 1020:I in Standard Methods for the
Examination of Water and Wastewater, 18th edition. ,
Recommendation: Table 1020:I in Standard Methods for the Examination of
Water and Wastewater, 18th edition may be used as aiguide to determine
whether the analysis of duplicates indicates an analytical problem.
Recommend establishing statistical control limits for BOD.GGA check
standard results as set forth in Standard Methods 1020B and 1030C.
Recommendation: Recommend lab document the true value (including units of
measure) of the accuracy check standard on all bench worksheets. Also
recommend calculating the percent recovery as a system for documenting the
validityof calibration. Another system for documenting the validity of
accuracy check standards would be to calculate and 'document the range of
acceptable concentrations for the accuracy check standards. Recommend the
acceptance criteria for accuracy check standards be documented on the bench
worksheets.
IV. DATA REVIEW:
Data review consisted of a review of the Chain of dustody procedure for
North Carolina Wastewater/Groundwater samples to check for adherence to
required preservation and hold times. Bench sheets land analytical reports
for randomly selected dates from October 1996 through November 1997 were
reviewed and compared to Discharge Monitoring Reports for the parameters on
the laboratory's discharge permit number NC0005321.' Analytical reports were
also reviewed for monitoring. required by land application permit number
WQ0002932. No problems in properly calculating or transcribing data were
detected.
V. CONCLUSION:
Five violations were cited. Three of the five violations cited relate to
three supplemental requirements of the Laboratory Certification Program
Administrative Code 15A NCAC 2H .0800. The laboratory's analytical quality
assurance document must be updated to incorporate administrative code
requirements. Two violations cited are method req4rementswhich must be
included in the standard operating procedure for the specific analyses. One
of the two method violations was minor and results; reported were still
within method quality control limits. One of the method violations resulted
in the method quality control check sample to be omitted from the
analytical batch on six occasions. Enforcement action in the form of a
civil penalty is will be recommended in relation tc this violation if it is
found to have occurred again. Lab must submit evidence of corrective
actions taken for all violations. Correction of the above cited violations
should help this lab document the quality of data produced, and meet North
Carolina certification requirements. Several of the recommendations are
aimed at improving legal admissibility of data.
Report prepared by: Harvi C. Cooper Date: February 20, 1998
Reviewed by: Norman L. Good
Date: May 8, 1998