NC0003719_Lab Certification_20010829

Michael F. Easley, Governor
William G. Ross Jr., Secretary
' North Carolina Department cif.Environment and Natural Resources
Gregory J. Thorpe, Ph.D.
Acting Director _
Division of Water Quality
August 29, 2001,-
520
Mr. Carl Mumford
Monsanto Fayetteville Plant Laboratory
- P.O. Box 3307
Cedar Creek Road
Fayetteville; NC-28302
SUBJECT: Laboratory Certification Maintenance.•Inspection.
Dear Mr. Mumford:
Enclosed is a report for the inspection performed on August 22, 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 continueto carry out,the requirements set
forth in 15A NCAC for 2H .0800. -
Copies of the checklists 'completed during the inspection may be requested from
this officer Thank you for your, cooperation during the inspection... Please contact us at
919-733-3908, if you have questions or need additional information.,.
Sincerely,
James W. Meyer
Laboratory Section
Enclosure
cc: Frederick L. Bone
Fayetteville Regional Office
Laboratory Section
FAX: [phone].
N. C. Division of Water Quality. - 1623 Mail Service Center Raleigh, NC 27699-1623 [phone]
Internet: www.esb.enr.state.nc.us/lab
° .NCDENR

On -Site Inspection Report
LABORATORY NAME: . . Monsanto Fayetteville:. Plant
ADDRESS:
P.O. Box 3307
Cedar Creek Road,
Fayetteville, NC 28302
CERTIFICATE NO: 520
DATE. OF INSPECTION: August 22, 2001
TYPE:OF INSPECTION: - . ' 'Maintenance
EVALUATOR:
LOCAL PERSON(S) CONTACTED: Curt West, Elaine Frasier, Hope Mills, and Allan Baldwin
' 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: =
Frederick L., Bone
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 qualitycontrol procedures need to be implemented.
III. DEFICIENCIES, RECOMMENDATIONS, REQUIREMENTS, AND COMMENTS:
General:
A.COMMENT: -The laboratory does not, analyze second source QC standards daily.
REQUIREMENT: Analyze one known standard. in addition to calibration standards each: day samples:are
analyzedlo document accuracy: This'LCS (laboratory control standard) must be from a, second source.' For
held curves for colorimetric methods; it must be analyzed. after the initial CCV (continuing calibration
verification standard) is analyzed. It is recommended that this laboratory control standard, like the CCV, have
a mid -range concentration and not vary by more than ± 10%. If 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, 18th Edition - Method 1020 E3.3.
B. COMMENT: Duplicate samples are not clearly labeled' on the laboratory bench'sheets.
RECOMMENDATION: For duplicate samples the sample name should be followed: by the term "Dup": 'or
"Duplicate" to indicate sample duplication. This will clearly delineate the duplicate samples:from other samples
analyzed.
C. COMMENT: The laboratory is using computer -generated benchsheets for some analysis. These benchsheets
are not signed by the analyst..
REQUIREMENT: Whenever a computer -generated benchsheet- is used for data reporting purposes, that the
analyst either signs or initials the computer- generated printout. This will help to clearly identify that the analyst
who performed the analysis is the.actual person that: is listed on the computer -generated forms.

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Total Suspended Solids:
D. COMMENT: The laboratory is not analyzing water blanks for the Total Suspended Solids analysis. The
laboratory must filter a volume of DI water (equal to the maximum sample volume used) as a method blank each
analysis day.
REQUIREMENT: Blanks must be analyzed in order to determine bias in each sample batch. Ref: Standard
Methods 18th Edition - Method 1020B pg. 1-5.
E.COMMENT: The benchsheet for the total suspended solids analysis is missing some of the necessary
labeling information. No units of measure are associated with some of the data entries.
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 .0800 (a) (7) (h).
F. COMMENT: The laboratory lists process control data . and other non -reportable data on the same
benchsheet as the reportable data. This listing of data gives the impression that the 10% sample duplication
criteria are not being meet.
RECOMMENDATION: It is recommended that data not intended to meet certification requirements, such as
process control data, be clearly labeled as "non -certified" or "not meant to meet certification requirements" on
the laboratory benchsheet. This will clearly demonstrate which data is to be reviewed as meeting the
laboratory certification requirements. It is further recommended that the laboratory analyze one duplicate
sample each analysis day. This will ensure that the laboratory is within the proper duplication requirements.
BOD:
G. COMMENT: The laboratory is averaging values that do not meet the acceptance criteria of the method with
values that do,meet method criteria to report results. The laboratory was not using the proper acceptance
criteria for calculating seed controls.
REQUIREMENT: For seed corrections, only values that meet the 0.6-1.0 mg/L may be used to compute the
averaged seed correction factor. Only data that meets the 2 mg/L used 1 mg/L remainingcriteria can be
averaged to obtain a final BOD result. Only GGA standards that fall within the range of 198 ± 30.5 mg/L can
be averaged to obtain passing GGA results. Data that does not meet the method criteria must not be
averaged with acceptable data to obtain an acceptable result. Ref: Standard Methods, 18 Edition - Method
5210 B pg. 5-3,4.
H. COMMENT: The laboratory does not perform a titrametric analysis to determine the chlorine content and
neutralization for all seeded BOD samples.
Note: If the laboratory can demonstrate that .the chlorine level is Tess than 20ug/L per day neutralization is
unnecessary. Some samples contained greater than 20µg/L of chlorine and were not neutralized with sodium
sulfite.
REQUIREMENT: The laboratory must perform a titrametric analysis to determine the chlorine content and
neutralization for all seeded samples. This is required by the method, in order to determine the amount of
sodium sulfite or Potassium Bi-iodate that is needed to neutralize the samples. The laboratory must perform
the titrametric test for the removal of residual chlorine, as described in. Standard Methods, 18th Edition p 5-4.

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pH: ( done in Satellite laboratory )
1: DEFICIENCY: The laboratory is not verifying the automatic temperature compensation of the pH meter on
an annual basis.
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).
I. COMMENT: The laboratory is not performing sufficient quality control for it's duplicate sample analyses. The
laboratory must calculate either the relative percent difference, or the absolute difference for each duplicate
pair analyzed. This value is then used to establish control charts or other appropriate acceptance criteria. This
type of data is necessary to demonstrate that the data is within acceptable control limits. The. %RPD must be
listed on the inorganic bench sheets so that the analyst will be able to immediately confirm whether or not the
data falls within acceptable limits.
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).
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.
Residual Chlorine:
2. DEFICIENCY: The laboratory is not analyzing a blank daily for the residual chorine analysis.
REQUIREMENT: Analyze reagent blanks whenever new reagents are used and as often as required in
specific methods. Analyze a minimum of 5% of the sample load as reagent blanks; this monitors purity of
reagents and the overall procedural' blank. Analyze a reagent .blank after any sample with a concentration
greater than that of the highest standard or that might result in carryover from one sample to the next. Ref:
Standard Methods 18th Edition 1020B Quality Control (4).p
Residual Chlorine and COD:
3. DEFICIENCY: Each analyst that performs analysis of Residual Chlorine and COD samples does not
produce a standard curve on an annual basis.
REQUIREMENT: Each analyst performing the analytical procedure must produce a standard curve. Ref: 15A
NCAC 2H .0800 (a) (7) (I).
K. COMMENT: The standard that the laboratory is currently analyzing, as a mid -point check standard is not at
the mid -point of the calibration curve. The actual mid -point of the analytical curve for residual chlorine in this
laboratory is 1.0 mg/L. The laboratory is analyzing a standard at 0.5mg/L. As was discussed at the time of the
audit the mid -range is to be defined as one half the concentration of the high standard.

•Page 4
Note: The mid -range check standard must be prepared from the same stock standards as the analytical curve.
A second source laboratory control standard (LCS) must be analyzed in addition to the mid range check
standard daily. A second source LCS sample does not constitute daily mid -range verification. .:
REQUIREMENT: Verify the standard curve daily by analyzing one'or more standards within thelinear range,,
as specified in the individual method. The curve must be updated as set forth in the standard procedures,
each time the slope changes by more 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).
L. COMMENT:. The laboratory does not demonstrate linearity of the analytical curves. The laboratory is not
calculating correlation coefficients for the standard curves.
REQUIREMENT: The laboratory must calculate a correlation coefficient for each analytical curve in order to
demonstrate linearity. Analytical Quality Control Program. 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. The quality control document shall be available for inspection by the State Laboratory. Ref: 15A
NCAC 2H .0805 (a) (7).
Residual Chlorine and pH:
M. COMMENT: The laboratory does not record the time sampled. and the time analyzed for pH and Residual
Chlorine samples on the laboratory benchsheets. 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).
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: August 27, 2001