#166 - 2012 Insp - final

INSPECTION REPORT ROUTING SHEET

To be attached to all inspection reports in-house only.

Laboratory Cert. #: 166

Laboratory Name: Global Nuclear Fuel – Americas, LLC (GNF)

Inspection Type: Industrial Maintenance

Inspector Name(s): Todd Crawford and Jeff Adams

Inspection Date: February 29, 2012

Date Report Completed: March 15, 2012

Date Forwarded to Reviewer: March 15, 2102

Reviewed by: Chet Whiting

Date Review Completed: March 19, 2012

Cover Letter to use: Insp. Initial X Insp. Reg. Insp. No Finding __ Insp. CP___ Corrected

Unit Supervisor: Dana Satterwhite

Date Received: March 19, 2012

Date Forwarded to Linda: March 20, 2012

Date Mailed: March 20, 2012

_____________________________________________________________________

On-Site Inspection Report

LABORATORY NAME: Global Nuclear Fuel – Americas, LLC (GNF)

NPDES PERMIT # NC0001228, WQ0031317

ADDRESS: PO Box 780
Mail Code H-92
Wilmington, NC 28402

CERTIFICATE #: 166

DATE OF INSPECTION: February 29, 2012

TYPE OF INSPECTION: Industrial Maintenance

AUDITOR(S): Todd Crawford and Jeff Adams

LOCAL PERSON(S) CONTACTED: Dengwei (David) Huo and Shawn O’Connor

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. The facility has all the equipment necessary to perform the
analyses. A system of traceability for prepared reagents and standards was in place for the main lab,
however, a system of traceability for purchased reagents and consumable supplies used for Field analyses
needs to be initiated.

The requirements associated with Findings B, J and L are new policies that have been implemented by our
program since the last inspection.

III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:

Quality Control

A. Finding: The thermometers in the drying oven and sample storage refrigerator have not been
calibrated against a NIST certified or traceable thermometer in the past 12 months.

Requirement: All thermometers and temperature measuring devices must be checked every
12 months against a NIST certified or NIST traceable thermometer and the process
documented. To check a thermometer or the temperature sensor of a meter, read the
temperature of the thermometer/meter against a NIST certified or NIST traceable thermometer
and record the two temperatures. The calibration must be performed at a temperature that
corresponds to the temperature used by the incubator, refrigerator, freezer, etc. In the case of
temperature measuring devices used to perform variable temperature readings the calibration
must be performed at a temperature range that approximates the range of the samples. The
thermometer/meter readings must be less than or equal to 1ºC from the NIST certified or NIST
traceable thermometer reading. The documentation must include the serial number of the NIST
certified thermometer or NIST traceable thermometer that was used in the comparison. Also
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make any corrections to the data and document any correction that applies (even if zero) on
both the thermometer/meter and on a separate sheet to be filed.

• NIST traceable thermometers used for temperature measurement must be recalibrated
in accordance with the manufacturer’s recalibration date. If no recalibration date is
given, the NIST traceable thermometer must be recalibrated annually.

• NIST certified thermometers must be recalibrated, at a minimum, every five years. A
new certificate must be issued and maintained for inspection upon request.
Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy.

Documentation

B. Finding: The laboratory needs to increase the documentation of purchased materials and
reagents used for field analyses.

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.

C. Finding: Several instances of writing over a number as a means of error correction were
observed in Sanitary Waste Treatment data.

Requirement: All documentation errors must be corrected by drawing a single line through the
error so that the original entry remains legible. Entries shall not be obliterated by erasures or
markings. Wite-Out®, correction tape or similar products designed to obliterate documentation
are not to be used. Write the correction adjacent to the error. The correction must be initialed by
the responsible individual and the date of change documented. All data and log entries must be
written in indelible ink. Pencil entries are not acceptable. Ref: North Carolina Wastewater/
Groundwater Laboratory Certification Policy.

pH - Standard Methods, 18th Edition, 4500 H+ B

D. Finding: Data values for pH are reported on the Discharge Monitoring Report to 0.01 S.U. instead
of 0.1 S.U., as required by the method.

Requirement: A variance of ± 0.1 pH unit represents the limit of accuracy under normal
conditions, especially for measurement of water and poorly buffered solutions. For this reason,
report pH values to the nearest 0.1 pH unit. Ref: Standard Methods, 18th Edition, 4500 H+ B. (6).
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pH - Standard Methods, 18th Edition, 4500 H+ B
Dissolved Oxygen - Standard Methods, 18th Edition, 4500 O G

E. Finding: The times that pH and DO meters are calibrated are not being documented. This is
considered pertinent information.

Requirement: All analytical data pertinent to each certified analysis must be filed in an orderly
manner so as to be readily available for inspection upon request. Ref: 15A NCAC 2H .0805 (7)
(A).

F. Finding: The pH and DO meters used for field analyses are not labeled with their respective
temperature correction factors.

Requirement: All thermometers, or temperature sensing devices on field meters must meet
NIST specifications for accuracy or must be calibrated against a NIST certified or NIST
traceable thermometer annually (every 12 months) and proper corrections made and
documented. A correction factor must be posted on the meter even if that correction factor is
0ºC. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy.

Dissolved Oxygen - Standard Methods, 18th Edition, 4500 O G

G. Finding: The unit of measure is not documented on the benchsheets used for the Sanitary
Waste Treatment facility.

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. The date and time
BOD and Coliform samples are removed from the incubator must be included on the laboratory
worksheet. Ref: 15A NCAC 2H .0805 (a) (7) (H).

H. Finding: The time of the analysis is not documented on the benchsheet used for the Sanitary
Waste Treatment facility. This is considered pertinent information.

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”.

Temperature - Standard Methods, 18th Edition, 2550 B

I. Finding: The unit of measure is not documented on the benchsheets used for the Process
Waste Treatment facility.

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. The date and time
BOD and Coliform samples are removed from the incubator must be included on the laboratory
worksheet. Ref: 15A NCAC 2H .0805 (a) (7) (H).
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Total Suspended Solids - Standard Methods, 18th Edition, 2540 D

J. Finding: The laboratory is not basing the reporting limit on the minimum weight gain required by
the method.

Requirement: The minimum weight gain allowed by any 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. If complete filtration takes
more than 10 minutes increase filter diameter or decrease sample volume. In instances where
the weight gain is less than the required 2.5 mg, the value must be reported as less than the
appropriate value based upon the volume used. Ref: North Carolina Wastewater/Groundwater
Laboratory Certification Policy based upon Standard Methods, 20th and 21st Editions, 2540 D.
(3) (b).

Comment: The facility was using a reporting limit of 10.0 mg/L based on a 500 ml sample. If
500 mL of sample is analyzed and < 2.5 mg of dried residue is obtained, the value reported would
be < 5.0 mg/L.

Ammonia Nitrogen - Standard Methods, 18th Edition, 4500 NH3 C

K. Finding: Samples are not being distilled prior to analysis and no distillation study is on file.

Requirement: The titration method requires all samples to be distilled. For all other methods,
manual distillation is not required if comparability data on representative effluent samples are on
file to show that this preliminary distillation step is not necessary; however, manual distillation
will be required to resolve any controversies. In the case of low concentration effluents, the
samples must be spiked to allow for a meaningful statistical comparison. It is recommended that
samples with a concentration < 1.0 mg/L be spiked to yield a value in the 1 – 5 mg/L range.
Comparisons performed in this concentration range should check within 20% RPD. Additional
samples must be analyzed comparatively if the results do not indicate approximately the same
values for distilled and undistilled samples. It is recommended that both the distilled and undistilled
portions of the sample be analyzed by the same laboratory using the same methodology. The
following frequencies are required:

Municipal and Industrial Laboratories shall analyze initially four samples distilled and undistilled
from each discharge and; thereafter, analyze two samples a year from each effluent. Submit
analytical results for four samples, distilled and undistilled, from each discharge within 60
days of receipt of this report.

Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy based upon Code
of Federal Regulations, Title 40, Part 136; Federal Register Vol. 72, No. 47, March 12, 2007;
Table IB Footnote 6.

Recommendation: It is recommended that the distilled and undistilled sample portions be
analyzed by the same lab, using the same instrument, technology and methodology to minimize
uncertainty introduced by the analysis, yielding a truer representation of the effect of matrix and
the distillation process on sample results.

L. 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
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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.

M. Finding: A new calibration curve is not prepared for each new batch of Nessler reagent.

Requirement: Redetermine complete calibration curve for each new batch of Nessler reagent.
Ref: Standard Methods, 18th Edition, 4500 NH3 C. (4) (c).

Metals – EPA Method 200.7

N. Finding: The laboratory is not analyzing matrix spikes.

Requirement: The laboratory must add a known amount of each analyte to a minimum of 10%
of the routine samples. In each case the Laboratory Fortified Matrix (LFM) aliquot must be a
duplicate of the aliquot used for sample analysis and for total recoverable determinations added
prior to sample preparation. For water samples, the added analyte concentration must be the
same as that used in the laboratory fortified blank (Section 7.10.3). Ref: EPA Method 200.7
Rev. 4.4 (1994), Section 9.4.2.

O. Finding: The laboratory is not analyzing a calibration blank immediately following the
Instrument Performance Check (IPC) standard.

Requirement: For all determinations the laboratory must analyze the IPC solution (Section
7.11) and a calibration blank immediately following daily calibration, after every 10th sample (or
more frequently, if required) and at the end of the sample run. Ref: EPA Method 200.7 Rev. 4.4
(1994), Section 9.3.4.

IV. PAPER TRAIL INVESTIGATION:

The paper trail consisted of comparing field testing records and contract lab reports to Discharge
Monitoring Reports (DMRs) submitted to the North Carolina Division of Water Quality. Data for Field
parameters were reviewed for October, November and December, 2011. Data for metals were
reviewed for January, February, May and October, 2011. No transcription errors were detected. The
facility appears to be doing a good job of accurately transcribing data.
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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: Todd Crawford Date: March 15, 2012
Report reviewed by: Chet Whiting Date: March 19, 2012