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General Engineering Laboratory, Inc. On-Site Inspection Report

LABORATORY NAME: General Engineering Laboratory, Inc.

ADDRESS: 2040 Savage Road
Charleston, SC 29407-4731

CERTIFICATE NO: 233

DATE OF INSPECTION: October 23, 24 & 25, 2006

TYPE OF INSPECTION: Maintenance

EVALUATOR: Jeffrey R. Adams, Chet Whiting and Gary Francies

LOCAL PERSON(S) CONTACTED: Nancy Mattern, Denni Grunstra, Carey Bocklet, Pat Steele, Lonnie
Morris, Annaliza Johnson and Bob Pullano.

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 in the process of discontinuing the use of the Konelab instrument. All automated
colorimetric procedures will be analyzed on the new Lachet and the two Lachet instruments previously in
use.
No instances items (notes 1-3) were observed during the inspection. These items were included as
reminders for specific North Carolina Policies.

NOTE 1: Whenever a certified commercial laboratory refers or subcontracts samples to another
certified laboratory for analyses, the referring laboratory must supply the date and time samples were
collected to insure holding times are met. Subcontracted samples must clearly indicate the State of
North Carolina as the collection site on all record transcripts. Laboratories may subcontract sample
fractions, extracts, leachates and other sample preparation products provided that all Rules and
requirements of 15A NCAC 02H .0800 are documented. The initial client requesting the analyses
must receive the original or a copy of the report made by the laboratory that performs the analyses.
Ref: 15A NCAC 02H .0805 (e) 2.

NOTE 2: Records that are stored only on electronic media must be maintained and supported in the
laboratory by all hardware and software necessary for immediate data retrieval and review. Ref: 15A
NCAC 2H .0805 (a) (7) (G).

NOTE 3: At any time a laboratory receives samples that do not meet sample collection, holding
time, or preservation requirements, the laboratory must notify the sample collector or client and
secure another sample if possible. If another sample cannot be secured the original sample may
be analyzed, but the results reported must be qualified with the nature of the infraction(s) and the
laboratory must notify the State Laboratory about the infraction(s). The notification must include a
statement indicating corrective action taken to prevent the problem for future samples. Ref:15A
NCAC 2H .0805 (a) (7) (N).

III. DEFICIENCIES, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:
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Quality Control:

Standard Curves:

A). COMMENT: There are inconsistencies in the Standard Operating Procedure (SOP) regarding the
Calibration Verification Standards (CVS). Not all methods meet North Carolina rules for sources and
acceptance criteria. The following items were noted:

1. Inconsistencies exist in the SOPs regarding the source. For example many indicate the source may
be either primary or secondary. But the Hexavalent Chromium SOP indicates it must be primary.

2. The Lachet methods indicate the CVS concentration may vary.

3. The acceptance criteria are not consistent: Total Phosphorus = ± 15%, TKN and Ammonia Nitrogen
= + 10%, Hexavalent Chromium = ± 20%.

REQUIREMENT: For analyses that require a series of standards, a mid-range standard must be
analyzed with each group of samples to verify the standard curve. This calibration verification standard
(CVS) is made from the same source as the calibration standards. When the mid-range standard varies
by more than ± 10%, or is outside the established control limits, whichever is lower, the analysis is out
of control. The analysis must be terminated and the problem corrected. Ref: 15A NCAC 2H .0805 (a)
(7) (F) and (I).

REQUIREMENT: The blank and mid-range standard (CVS) must be analyzed after every tenth sample
and at the end of each sample group to check calibration drift. Ref: Standard Methods, 20th Edition -
Method 1020 B. 10.c.

Continuing Calibration Blanks and Method Blanks:

B). COMMENT: The SOP is not consistent with the acceptance criteria for inorganic method blanks.
Some acceptance criteria are listed as < the PQL (Reporting Limit Standard) and some say ≤ 50% of
the PQL. In general it appears all the data met the ≤ 50% rule.

REQUIREMENT: NCLC policy requires that the concentration of the blank must not exceed 50% of the
LOQ/MQL/PQL. The lab must obtain a signal in which the constituent concentration in reagent water is
2(1.645)s above the mean of blank analyses (Lower Limit of Detection). The constituent concentration
that produces a signal sufficiently greater than the blank, that it can be detected within specified limits,
by good laboratories, during routine operating conditions, is the Limit of Quantitation. Typically it is the
concentration that produces a signal 10s above the reagent water blank signal. In most cases, this
requires an absorbance value greater than 0.005 units, preferably greater than 0.010 units. Ref:
Standard Methods, 20th Edition - Method 1010 C. and 1030 C.
CCB: As part of calibration verification of the periodic confirmation that instrument response has not
changed significantly from the initial calibration. Verify calibration by analyzing a midpoint calibration
standard and calibration blank at the beginning and end of a sample run, periodically during a run
(normally after each set of ten samples).

METHOD BLANK (MB): A potion of reagent water treated exactly as a sample including exposure to
all equipment, glassware, procedures, and reagents. The MB is used to assess whether analytes or
interference are present within the analytical process or system. NCLC Policy Memo 5/2006.

WALKTHROUGH:
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ANALYTICAL BALANCE:

OBSERVATION: The balance printout did not indicate the balance ID.

RECOMMENDATION: This information is in the computer but not the printout. It is highly recommended
that the printouts identify which balance is being used.

TEMPERATURE:

C). COMMENT: It was observed that the temperature of several of the refrigerators being used
to store samples for organic analyses were outside the required range of 1.0 to 4.0°C.

REQUIREMENT: For sample storage, the temperature of the cooler must be between 1.0 and 4.0°C. For
sample transport, the temperature range is 1.0 to 6.0°C. Ref: USEPA Office of Research and
Development, Environmental Monitoring Systems Laboratory, Cincinnati, OH, Letter January 26, 1995
James W. O'Dell, Jr.

NOTE: It was the laboratorys understanding that a 2°- 6° C temperature range was acceptable for sample
storage. The laboratory indicated that the new adjustments would be made and the refrigerator storage
temperatures corrected.

D). COMMENT: The laboratory is using “Blue Ice” to preserve the samples during shipment.

REQUIREMENT: Although Standard Methods accepts the use of “Blue Ice”, NCLC policy prohibits the
use of blue ice for the preservation of samples being shipped. Ref: NC Policy.

OBSERVATION: It is our experience that the use of “Blue Ice” is not adequate for cooling and
maintenance of temperature during shipment. (NCLC Policy).

INORGANICS:

TKN:
RECOMMENDATION: It is strongly recommended that an organic nitrogen standard be analyzed to
test the efficiency of the digestion procedure.
FECAL COLIFORM (MF):

1). DEFICIENCY: Samples are not verified to be free of residual chlorine.

REQUIREMENT: Samples received for analysis must be verified and documented to have been
properly preserved. Samples containing chlorine must be dechlorinated at the time of sample collection
and treated according to the requirements of the analysis to be performed. Upon receipt in the
laboratory, samples must be checked and documented to be free of chlorine. A variety of testing kits
are considered to be adequate for most chlorine interference checks and a maximum detection limit of
0.5 mg/L is allowed. When samples are received out of compliance, the lab must inform the client and
the State of NC in writing. Ref: 15A NCAC 2H .0805 (a) (1) and (7) (M) and (N).

E). COMMENT: No comparison test is conducted before a new lot of consumables are put into use.

NOTE: A handout explaining this method requirement was provided during the inspection.

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REQUIREMENT: It is required that when a new lot of culture medium, pads, or membrane filters is to
be used, a comparison of the current lot in use, (reference lot) against the new lot (test lot), be made.
As a minimum, make single analyses on five positive samples. Ref: Standard Methods, 18th Edition -
Method 9020 B.3d. (page 9-7)

F). COMMENT: The graduated cylinders are washed but not sterilized.

REQUIREMENT: Apparatus and Materials; graduated cylinders must be covered with aluminum foil or
kraft paper before sterilization. Ref: Microbiological Methods for Monitoring the Environment. Part 111.
Section c. 2.3.5. EPA 1978.

METALS:

OBSERVATION: The laboratory is checking the hot block digester temperature, but is not documenting
the “grid hole” position.
RECOMMENDATION: It is highly recommended that the laboratory construct a template of the digester
block grid and alter the position each time the temperature is checked and documented. This will enable
the monitoring of the heat uniformity of the digester over time. This is recommended for any hot block
digester.

G). COMMENT: The instrument did not print out the calculated calibration curves and correlation
coefficients.
REQUIREMENT: Supporting records shall be maintained as evidence that these practices are being
effectively carried out. All analytical records must be available for a period of five years. Ref: 15A NCAC
2H .0805 (a) (7) and (a) (7) (G).

RECOMMENDATION: It is highly recommended that the software be configured to calculate and print a
plot of the calibration curves and correlation coefficients. This will greatly aid in the data review process in
future inspections.

MERCURY: Method 1631E:

2). DEFICIENCY: The laboratory is not analyzing a field or trip blank with each batch (10 Samples Max.)
of low level mercury samples.

NOTE: Field blanks are used to demonstrate that samples have not been contaminated by the sample
collection and transport activities.

REQUIREMENT: Analyze the field blank(s) shipped with each set of samples (samples collected from
the same site at the same time, to a maximum of 10 samples). Analyze the blank immediately before
analyzing the samples in the batch. (10% from the same site at the same time) Ref: EPA Method
1631E, 9.4.5

TSS:

3). DEFICIENCY: The samples are not dried at the proper temperature range.

NOTE: A temperature range of 103 ± 50 C is used. The SOP indicates the correct range of 103-1050 C.

REQUIREMENT: Dry for at least one hour at 103 to 1050 C in an oven until a constant weight is
obtained. Ref: Standard Methods, 20th Edition – Method 2540 D. 3c.
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H). COMMENT: The method and SOP requirement regarding time allowed for sample volume filtration
is not being followed. Currently the sample is allowed to filter for however long it takes.

REQUIREMENT: If complete filtration takes more than 10 minutes increase filter diameter or decrease
sample volume. Ref: Standard Methods, 20th Edition – Method 2540 D.3b.

TDS:

I). COMMENT: The samples are not evaporated in a steam bath or drying oven prior to drying in the
1800 C oven. This must be performed at a lower temperature to ensure the sample does not splatter
out of the evaporating dish. Ref: Standard Methods, 20th Edition – Method 2540 C.3d.

NOTE: The SOP contains ambiguous language about doing this procedure if needed to prevent
splattering but gives no guidance on how to determine the need.

REQUIREMENT: Samples are to be evaporated to dryness on a steam bath or in a drying oven. Then
dry evaporated samples for at least one hour in an oven at 180 ± 20 C.

COD:

J). COMMENT: The following are not documented: 1). the reactor temperature and 2). the time
samples are digested. (that is the time on and off.)

NOTE: It must be documented that the samples are digested at 1500 C for two hours.

REQUIREMENT: Supporting records shall be maintained as evidence that these practices are being
effectively carried out. All analytical records must be available for a period of five years. Ref: 15A NCAC
2H .0805 (a) (7) and (a) (7) (G).

FLUORIDE:
K). COMMENT: Samples are not distilled nor is a distillation study on file.

REQUIREMENT: Commercial Laboratories shall analyze one sample distilled and undistilled yearly
from all waste types. Additional samples must be analyzed comparatively if the above samples results
do not indicate approximately the same values for distilled and undistilled samples. Ref: Federal
Register, October 23, 2002; 40 CFR 136; Fluoride Footnote 6.

RECOMMENDATION: It is highly recommended that the facility discontinue certification by the
electrode method and retain certification by the Ion chromatography (IC) method only. This would
eliminate the need for a distillation study each year.
MBAS:

L. COMMENT: Each analyst does not generate his or her own standard curve.

REQUIREMENT: Each analyst performing the analytical procedure must produce a standard curve.
Ref: 15A NCAC 2H .0805 (a) (7) (I).
4). Deficiency: There were major problems with traceability of held standard curves. It appeared that
incorrect dates of curves were documented. The staff was very helpful in attempting to sort out the dates
but was not entirely successful.
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REQUIREMENT: Supporting records shall be maintained as evidence that these practices are being
effectively carried out. All analytical records must be available for a period of five years. Ref: 15A NCAC
2H .0805 (a) (7) and (a) (7) (G).

BOD:

NOTE: Due to problems with the BOD test, particularly low recoveries for the Glucose- Glutamic Acid
standard (GGA), the laboratory has voluntarily discontinued analyzing samples in house and is currently
contracting the analyses to another lab. The staff has done a good job of troubleshooting the problems
and attempting to correct them. Technical assistance was provided during the inspection. Some
suggestions were made regarding the preparation of the seeding material that may help with the GGA
recoveries.

L). COMMENT: The D. O. meter is not checked for drift during, and at the end of the analytical
series.

REQUIREMENT: When analyzing BOD samples with a membrane electrode, the laboratory must check
one or two points frequently after the initial calibration, and at the end, to confirm the original calibration.
This check must be performed and documented on both day one and day five. The drift should be no more
than 0.2 mg/l. Ref: Standard Methods, 18th Edition - Method 5210 B. 4g, Method 4500-O G. 1a, and Ref:
15A NCAC 2H .0805 (a) (7).

RECOMMENDATION: It is strongly recommended that a seeded blank be analyzed with each set of
samples. Its value should be compared with the calculated seed correction value to help judge the
consistency of the seeding material. Generally an overall difference of 0.2 mg/L or less is an indication
of consistent seed material and good analyst technique.

M). COMMENT: The GGA standard is not a 2% solution as required.
REQUIREMENT: Determine the 5- day 200 C BOD of a 2% dilution of the glucose-glutamic acid standard
check solution. Adjust concentrations of commercial mixtures to give 3 mg/L glucose and 3 mg/L glutamic
acid in each GGA test bottle. Ref: Standard Methods, 20th Edition – Method 5210 B. 4c.

RECOMMENDATION: It is strongly recommended that the lab consider using a commercial GGA
prepared at the strength specified in the method, which is a 2% solution.

ORGANICS:

RECOMMENDATION (GENERAL): Several instances of manual integration were observed during the
review of organics section data. “Before and “after” chromatographs were included in the data packs. It
was not always clear why manual integration was used and no notations were made. Since manual
integration is likely to draw inquiry during outside data reviews we strongly recommend that a footnote
of explanation be included with the data.

NOTE: The laboratory indicated it may request deletion from their certificate for method 6640B.

EDB/DBCP Method EPA 504.1:

4). DEFICIENCY: The laboratory is not analyzing a “Trip Blank” with each sample set.
REQUIREMENT: Replicate Reagent Blanks (FRB) – Must be handled along with each sample set, which
is composed of the samples collected from the same general sampling site at approximately the same
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time. At the laboratory, fill a minimum of two sample bottles with reagent water, seal, and ship to the
sampling site along with sample bottles. Wherever a set of samples is shipped and stored, the FRB must
accompany it. Ref: EPA Method 504.1 Section 8.1.1.

IV. PAPER TRAIL INVESTIGATION:

The inspectors reviewed several data packs from August 22 to September 20, 2006 for all parameters
listed on the laboratory’s certificate. This consisted of comparing data with the values obtained on
laboratory bench worksheets (for both water and soil analysis) including calibrations, quality control charts,
surrogate and duplicate recoveries and statistical calculations performed on duplicate analysis monitoring
precision and accuracy. With the exception of the above statements, the inspectors found no computation
errors on the data packs reviewed and data appeared accurate and easily accessible to the inspector.

V. CONCLUSIONS:

Correcting the above deficiencies and comments and implementing the recommendations should help
this laboratory produce quality data and meet certification requirements. The inspectors would like to
thank the laboratory staff for their great co-operation in the inspection and data review process.
Please respond to all numbered Deficiencies and lettered Comments cited in this report.

Report prepared by: Jeffrey R. Adams Date: December 1, 2006
Report Reviewed by: Gary Francies Date: December 5, 2006
Report Reviewed by: Chet Whiting Date: December 11, 2006