HomeMy WebLinkAbout#199 2012
INSPECTION REPORT ROUTING SHEET
To be attached to all inspection reports in-house only.
Laboratory Cert. #: 199
Laboratory Name: Archer Daniels Midland Company
Inspection Type: Industrial Maintenance
Inspector Name(s): Todd Crawford
Inspection Date: November 29, 2012
Date Report Completed: December 10, 2012
Date Forwarded to Reviewer: December 10, 2012
Reviewed by: Chet Whiting
Date Review Completed: February 11, 2013
Cover Letter to use: Insp. Initial Insp. Reg.
Insp. No Finding Insp. CP
Corrected
Unit Supervisor: Dana Satterwhite
Date Received: February 13, 2013
Date Forwarded to Linda: February 18, 2013
Date Mailed: February 18, 2013
_____________________________________________________________________
On-Site Inspection Report
LABORATORY NAME: Archer Daniels Midland Company
NPDES PERMIT # : NC0027065
WATER QUALITY PERMIT # : WQ0004500
NC GENERAL PERMIT #: NCG060000
ADDRESS: 1730 Moore Street, S.E.
Southport, NC 28461
CERTIFICATE #: 199
DATE OF INSPECTION: November 29, 2012
TYPE OF INSPECTION: Industrial Maintenance
AUDITOR: Todd Crawford
LOCAL PERSON(S) CONTACTED: Stewart Clarke, Scott Phillips and Jonathan Ward
I. INTRODUCTION:
This laboratory was inspected by a representative of the North Carolina Wastewater/Groundwater
Laboratory Certification (NC WW/GW LC) program 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. The facility has all the equipment necessary to perform the
analyses. A system for traceability of standard and reagent preparation is in place but needs to include
some additional information. Proficiency Testing (PT) samples have been analyzed for all certified
parameters for the 2012 proficiency testing calendar year and the graded results were 100% acceptable.
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
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. 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.
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Contracted analyses are performed by Environmental Chemists, Inc. (Certification #94).
The requirements associated with Findings C, D and M are new policies that have been implemented by
our program since the last inspection.
III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:
Traceability
A. Finding: The laboratory needs to increase the documentation of purchased materials and
reagents.
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.
Quality Control
B. Finding: The analytical balance weights have not been verified against ASTM standard weights
since 4/2/87.
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.
Comment: The weights were tarnished and scratched. The analyst stated that he uses metal
tongs to handle the weights since the plastic tongs have been lost.
Recommendation: It is recommended that the weight set be replaced due to the advanced state
of deterioration and that the lab obtain plastic tongs for handling weights.
Ammonia Nitrogen – Standard Methods, 4500 NH3 D - 1997
Comment: This test is only required quarterly. Samples are subcontracted and there was no regulatory
data to review. If this analysis is again performed in-house, the findings associated with TKN analysis will
apply.
Ammonia Nitrogen – Standard Methods, 4500 NH3 D - 1997
Total Kjeldahl Nitrogen – Standard Methods, 4500 Norg B-1997 (NH3 D - 1997)
C. Finding: A calibration blank and calibration verification standard (mid-range) are not analyzed
initially, after every tenth sample and at the end of the sample group.
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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, 20th Edition, 1020 B. (10) (c), 3020 B. (2) (b), and 4020 B. (2).
Requirement: For analyses requiring a calibration curve, the concentration of method and
reagent blanks must not exceed 50% of the reporting limit, unless otherwise specified by the
reference method. Ref: North Carolina Wastewater/Groundwater Laboratory Certification
Policy.
Comment: The calibration verification standard is prepared from the calibration stock standard
solution.
Ammonia Nitrogen – Standard Methods, 4500 NH3 D - 1997
Total Kjeldahl Nitrogen – Standard Methods, 4500 Norg B-1997 (NH3 D – 1997)
NO2 + NO3 Nitrogen – Standard Methods, 4500 NO3 E - 2000
D. Finding: The laboratory is not analyzing matrix spikes.
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 by calculation necessary. If the spike solution volume 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.
Recommendation: It is recommended that the spike solution constitutes ≤1% of the total MS
volume.
Recommendation: If the duplicate sample value is near or below the reporting limit, it is
recommended that a Matrix Spike Duplicate (MSD) be analyzed. The MSD fulfills the duplicate
required by 15A NCAC 2H .0805 (a) (7) (C). This would result in better statistical results to
monitor method and analyst precision.
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NO2 + NO3 Nitrogen – Standard Methods, 4500 NO3 E - 2000
E. Finding: A second source standard is not analyzed.
Requirement: When a standard curve is manually prepared (as opposed to a factory-set
calibration), it is required to analyze one known standard in addition to calibration standards
each day samples are analyzed to document accuracy.
This standard must be prepared from materials obtained from a source independent from the
one used for preparing the calibration standards (often referred to as a second source standard
or external reference standard). A second source standard may be:
• a quality control standard obtained from a vendor,
• a standard prepared from primary standards obtained from a second vendor, or
• a standard made from primary standards from the same vendor but from a
different lot number (i.e., an independent lot) as those used to make the
calibration standards.
Second source standards must be evaluated using one of the following: vendor supplied
criteria, method-defined acceptance criteria, in-house calculated acceptance limits that are
statistically-derived from historical data based on three standard deviations from the mean in
the detectable range or other statistically viable evaluation criterion. If the results fall outside of
acceptance limits, the analysis is out of control. The analysis must be terminated and the
problem corrected prior to sample analysis. Ref: North Carolina Wastewater/Groundwater
Laboratory Certification Policy based upon 15A NCAC 2H .0805 (a) (7) (B), (a) (7) (F), and
Standard Methods, 20th Edition, 1020 B. (2) and (5).
F. Finding: The method blank analysis is not documented.
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: For analyses requiring a calibration curve, the concentration of method and
reagent blanks must not exceed 50% of the reporting limit, unless otherwise specified by the
reference method. Ref: North Carolina Wastewater/Groundwater Laboratory Certification
Policy.
G. Finding: The calibration curve does not always bracket the concentration of the samples.
Requirement: For analytical procedures requiring analysis of a series of standards, the
concentrations of those standards must bracket the concentration of the samples analyzed. One
of the standards must have a concentration equal to the laboratory’s lower reporting concentration
for the parameter involved. Ref: 15A NCAC 02H .0805 (a) (7) (I).
Comment: Samples analyzed on 10/24/12 and 11/14/12 were documented to have
concentrations that exceeded the concentration of the highest calibration standard of 1.0 mg/L
and corrective action was not taken.
Comment: The proper corrective action in this case would have been to either dilute the sample
and reanalyze or extend the high end of the curve.
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Conductivity – Standard Methods, 2510 B - 1997
H. Finding: The Automatic Temperature Compensator (ATC) was not verified initially and every 12
months thereafter.
Requirement: The ATC must be verified annually (i.e., every twelve months) and the process
documented. The ATC must be verified by analyzing a standard at 25 °C (the temperature that
conductivity values are compensated to) and a temperature(s) that brackets the temperature
ranges of the samples to be analyzed. This may require the analysis of a third temperature
reading that is > 25 °C. Ref: North Carolina Wastewater/Groundwater Laboratory Certification
Policy.
I. Finding: The true values of the calibration standard and the calibration check standards are not
correctly labeled on the bottles or on the Conductivity Standards Preparation sheet.
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).
Residue, Total Suspended – Standard Methods, 2540 D - 1997
Comment: Although all observed data was correctly calculated and reported, the benchsheet
incorrectly states the minimum required weight gain as 10 mg. The minimum weight gain allowed by the
approved method is 2.5 mg. Choose sample volume to yield between 2.5 and 200 mg dried residue.
This establishes a minimum reporting value of 2.5 mg/L when 1000 mL of sample is analyzed. Please
submit a revised benchsheet.
J. Finding: Filters are not weighed to constant weight prior to sample analysis, nor is a dry filter
blank analyzed with each set of samples.
Requirement: If pre-prepared filters are not used, the method requires that filters must be
weighed to a constant weight after washing. Repeat cycle of drying, cooling, desiccating, and
weighing until a constant weight is obtained or until weight change is less than 4% of the previous
weighing or 0.5 mg, whichever is less. In lieu of this process, it is acceptable to analyze a single
daily dry filter blank to fulfill the method requirement of drying all filters to a constant weight prior to
analysis. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy based
upon Standard Methods 20th Edition 2540 D. (3) (a).
K. Finding: The samples are not weighed to constant weight, nor is an annual multiple weighing
study to verify the adequacy of the drying time, performed.
Requirement: Constant weights must be documented. The approved method requires the
following: “Repeat the cycle of drying, cooling, desiccating, and weighing until a constant weight
is obtained or until the weight change is less than 4% of the previous weight or 0.5 mg,
whichever is less.” In lieu of this, an annual study documenting the time required to dry
representative samples to a constant weight may be performed. Verify minimum daily drying
time is greater than or equal to the time used for the initial verification study drying cycle. Drying
cycles must be a minimum 1 hour for verification. Ref: North Carolina Wastewater/Groundwater
Laboratory Certification Policy based on Standard Methods 20th Edition, 2540 D. (3) (c), 2540 B.
(3) (b), and 2540 C. (3) (d).
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Comment: North Carolina allows for an annual drying study in lieu of the requirement above to
repeat the drying cycle for every sample. A random full set of samples should be used for the
drying study. The repeated drying time in the oven should be at least 1 hour long. The time
used for the annual drying study is the minimum time that samples are to be dried until a new
drying study is performed.
COD – Standard Method, 5220 D – 1997
Comment: Only one calibration curve verification is required every 12 months. Each analyst is not
required to perform a calibration curve verification when samples are being analyzed against a factory-
set calibration curve.
Comment: A new calibration curve verification would be required prior to the 12 month requirement if a
new lot of tubes is put into use, the slope changes by more than 10% at the mid-point or a new stock
standard is prepared.
Comment: Two mid-range standards from separate sources are not required when samples are being
analyzed against a factory-set calibration curve. Any standard would be considered to be from a
second source when analyzed against a factory-set curve. Therefore, only one mid-range standard is
required initially (i.e., prior to sample analysis), after every tenth sample and at the end of each sample
group to check calibration drift.
Fecal Coliform – Standard Method, 9222 C E – 2000 (MPN)
L. Finding: Duplicate analyses are not analyzed.
Requirement: Duplicate analyses – Perform duplicate analyses on 10% of samples and on at
least one sample per test run. A test run is defined as an uninterrupted series of analyses. If the
laboratory conducts less than 10 tests/week, make duplicate analyses on at least on sample
each week. Ref: Standard Methods, 9020 B. (8) (4).
BOD – Standard Method, 5210 B – 2001
M. 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.
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 (0.30 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 0.30 mL of each reagent into the BOD bottle, it is
recommended that commercially prepared nutrient buffer pillows for 300 mL bottles be used.
Dissolved Oxygen – Standard Methods, 4500 O G – 2001
N. Finding: Sample collection time is not documented.
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Requirement: Sample identification must be associated with the date and time of sample
collection and analysis. The time elapsed between sampling and analysis must be documented to
determine if hold times are met. Ref: North Carolina Wastewater/Groundwater Laboratory
Certification memorandum dated June 20, 2007, “Required Documentation for Sampling
Preservation and Hold Time”.
Comment: The DO sample was being collected at the same time as the pH sample but the
documentation did not indicate that.
pH – Standard Methods, 4500 H+ B - 2000
Recommendation: It is recommended that the time of the meter calibration be documented. This
will soon be required by North Carolina Wastewater/Groundwater Laboratory Certification
Policy.
O. Finding: The calibration check buffer is not documented to the tenths place to show that it is
within the ± 0.1 Standard Units acceptance criterion.
Requirement: If the meter response shows a difference greater than 0.1 pH unit from the
expected value, look for trouble with the electrodes or the potentiometer. Ref: Standard
Methods, 4500 H+ B.-2000 (4) (a).
IV. PAPER TRAIL INVESTIGATION:
No paper trail performed. The Wilmington Regional Office’s Linda Willis performed a paper trail
investigation in June of 2012.
V. CONCLUSIONS:
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: Todd Crawford Date: December 10, 2012
Report reviewed by: Chet Whiting Date: February 11, 2013