#631 2006-f

On-Site Inspection Report

LABORATORY NAME: Summit Environmental Technologies, Inc.

ADDRESS: 595 East Tallmadge Avenue
Akron, OH 44310

CERTIFICATE NO: #631

DATE OF INSPECTION: May 8-9, 2006

TYPE OF INSPECTION: Maintenance

EVALUATOR: Ms. Tonja Springer

LOCAL PERSON CONTACTED: Mr. Ron Gibas

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 lab is congratulated for doing a good job of implementing the Certification program. All
equipment is well maintained. Records are well kept and the data appeared accurate. A few
more quality control measures are needed.

New Policies:

Pre-programmed curve:
REQUIREMENT: Each analyst must have there own daily or annual curve unless a pre-
programmed calibration is used. Pre-programmed calibrations must be verified annually with 5
non-zero standards and a blank. A new calibration verification will need to be performed for
each new lot of digestion solution and each new lot of stock standard. Each analysis day,
thereafter, include at least one reagent blank and CCV (NC Policy defines as mid-range check
standard same source as calibration standards), with each digestion batch. In addition, analyze
one known standard in addition to calibration standards each day samples are analyzed to
document accuracy. Reference: 15A NCAC 2H .0805 (a) (7) (B) and (I); SM 20th Edition
5220D.4c.
SECOND SOURCE STANDARDS
NCLC REQUIREMENT: Analyze one known standard in addition to calibration standards each
day samples are analyzed to 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 B.3.
DEFINITION: LABORATORY CONTROL STANDARD (LCS)
A standard, certified by an outside agency, used to measure the bias in a procedure. For certain
constituents and matrices, use NIST Standard Reference Materials when available. SM 20th
Edition Method 1010C 1.

DEFINITION: QUALITY CONTROL STANDARD (QCS)
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Analyze an externally generated quality control sample of known concentration at least quarterly
and whenever new calibration stock solutions are prepared. Obtain this sample from a source
external to the laboratory or prepare it from a source different from those used to prepare
working standards. Use to validate the laboratory’s working standards both qualitatively and
quantitatively. SM 20th Edition Method 3020 B 2. c.

ACCEPTANCE CRITERIA: Not vary by more than ± 10% for in-house prepared standard. 15A
NCAC 2H .0805 (a) (7) (B), (F).
Vendors limits for purchased QA samples.
In-house calculated limits (control charts) based on internal analyses. SM 20th Edition Method
1020 B 12. a.

Balance Weights:
Requirement: The NC Laboratory Certification Program has a new policy concerning Certified
Analytical Weights. The new policy is as follows: Certified analytical weights, Class S, 1 or 2,
must be recalibrated and recertified a minimum of every 5 years. The laboratory can choose to
send the 3 primary weights that are check quality to meet this requirement.

Thermometers:
Requirement: When checking a thermometer or temperature sensor, the thermometer/meter
readings must be less than or equal to 1ºC from the NIST thermometer reading.

Continuing Calibration Blanks (CCB) and Method Blanks:
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).

DEFINITION: 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.

ELECTRODE SLOPE/EFFICIENCY DOCUMENTATION:
NCLC policy requires that the slope value or efficiency be documented. Slope of ten fold millivolt
change (difference in millivolt readings between one standard and another standard with a
concentration ten times greater than the first standard) should be -54 to -60 mv. The millivolt
change may vary from the given ranges depending on the concentration of the standards used.
Harder to achieve with 0.1 and 1.0 mg/L standards, Should be routine for 1 and 10 mg/L.

REQUIREMENT: For the ammonia analysis a slope calibration should be performed in
accordance with the manufacturer’s recommendations and the slope must be verified to be in
the acceptable range daily. The slope must be recorded daily. This is considered pertinent
information.
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pH meter:
NCLC Requirement: There have been some changes made by the Certification Program
regarding the temperature sensor and the Automatic Temperature Compensator (ATC). Most of
the labs have been following the procedure outlined below (temperature sensor verification) with
a NIST thermometer. This procedure, by itself, is no longer considered sufficient to verify the
internal temperature compensator is operational in the pH meter. The following should be
performed on an annual (12 month) basis:

To check the ATC on the pH meter: 1. Take a buffer solution and cool to below 10ºC and read
the temperature. Analyze the buffer solution at that temperature. Document the temperature
and the measured pH value obtained on the log sheet.
2. Raise the temperature of the buffer solution to approximately 25ºC. Document the
temperature and the measured pH value on the log sheet.
3. Raise the temperature of the buffer solution to approximately 35ºC. Document the
temperature and the measured pH value on the log sheet.
4. Repeat with additional temperature adjustments and pH solution readings as necessary to
ensure the temperature usually measured for samples has been bracketed. As the temperature
increases or decreases the value of the buffer solution should remain approximately the same.

To calibrate check the temperature sensor: To check the temperature sensor read the
temperature of the meter against a NIST thermometer and record the two temperatures. The
thermometer readings must be less than 1ºC from the NIST thermometer reading. REQUIRED
for certified data. (NCLC Policy). In the documentation include the serial number of the NIST
thermometer or traceable thermometer that was used in the comparison. Also document any
correction that applies on both the instrument and on a separate sheet to be filed.

Requirement: The temperature sensor must be calibrated annually even if it is not being
used to report temperature.

A. Comment: Upon completion, please send a copy to our office, of the ATC check and
temperature sensor check for the pH meter and DO meter.

III. DEFICIENCIES, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS,:

Benchsheets:

1. Deficiency: On several of the benchsheets there were instances where the data was not
legible and in other cases there were several instances where there were overwritten entries.
Cited Previously (For example, Phenol, BOD, Ion Chromatography)

Requirement: In the event of an error, draw a single line through the error, write the correct result
near the error or in the margin, and initial the correction. Records should be legible, identifiable,
and retrievable, and protected against damage, deterioration, or loss. All records should be
written in indelible ink.

2. Deficiency: On several of the benchsheets reviewed, the data was incomplete. See the
following:
(a) Oil & Grease 1664- In some instances the blank and the LCS was not calculated out
completely. - In some instances the blank weight was not documented.
- Evaporation Temperature was not documented on some of the benchsheet, a space is
provided on the benchsheet.
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(b) Ion Chromatography- There is no analyst initials on the benchsheet.
(c) TDS/TSS/TS -there is a space provided to document the balance id, oven id, but it is
not always completed.

B. Comment: There is no documentation to show how calibration curves are made. (Example:
Cyanide). All reagents and standards associated with the samples should be documented such
as the lot number and vendor of the stock standard used to make the working standard solution,
along with the amount used to make the series of dilutions. More documentation is needed in
the reagent logbook.

Requirement: The preparation of all reagents, pre-made standards should 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 solution preparation
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 information as well as the vendor,
manufacturer, lot number, and expiration date should be retained for primary standards or
chemicals and reagents used.

Requirement: Supporting records shall be maintained as evidence that these practices are
being effectively carried out. Reference: 15A NCAC 2H .0805 (a) (7).

Comment: It is strongly recommended that the laboratory list the acceptance ranges and true
values for each quality control sample on the benchsheet. This will enable the analyst to
compare the analytical result to the acceptable range in a timely fashion. If the sample is out of
the acceptable range, it can then be reanalyzed immediately and within all holding times.

C. Comment: The laboratory is not always calculating a correlation coefficient for the standard
curve for some of the analyses. The laboratory does not demonstrate statistically that the
analytical curve is linear. Cited Previously.

Requirement: The laboratory must calculate a correlation coefficient for each analytical curve in
order to demonstrate linearity. 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. Reference: 15A NCAC 2H .0805 (a) (7)

Comment: The standardization of the titrant is done on a computer. It is recommended that a
copy of the computer printout be attached to the front of the logbook and referenced on each
benchsheet.

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. The quality
control document shall be available for inspection by the State Laboratory. The following are
requirements for certification and must be included in each certified laboratory's quality control
program. Ref: 15A NCAC 2H .0805 (a) (7).
Requirement: All data and supporting documents must be stored for up to five years. Ref:
NCAC 15A 2H (a) (7) (G).

Comment: Please be advised that documentation requirements of 15A NCAC 2H .0800
regulations are probably not adequate for data that will be used in court. It is our experience that
in litigation particular attention is focused on SOP’s, Chain of Custody documentation, and
quality control documentation. Many comments and recommendations made by this office are
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for the expressed purpose of helping laboratories produce more legally defensible data. It is in
the laboratory’s best interest to conduct periodic evaluations of documentation procedures to
determine what changes will best suit the needs of clients and the laboratory itself.

D. Comment: Some of the benchsheets have two options listed for the units of measure (mL
or g) but neither is circled. The analyst will need to indicate which units to apply to the samples.

Oil & Grease 1664:

3. Deficiency: The laboratory is not verifying the balance with the weights required by the
method.

Requirement: Calibrate the analytical balance at 2 mg and 1000 mg using class “S” weights.
Calibration shall be within + 10% (i.e. + 0.2 mg) at 2 mg and + 0.5 % (i.e. + 5 mg) at 1000 mg. If
values are not within these limits, recalibrate the balance. Reference: Method 1664 Revision
A, Section 10.1 & 10.2.

E. Comment: There was not documentation of the balance verification before and after
analysis, for the dates of the data reviewed. It was stated at the exit interview that another
balance logbook is used for documenting the Oil & Grease balance checks. Please provide a
copy of the balance logbook for the months of April and May 2006, along with a copies of
any Oil & Grease 1664 benchsheets with data for these two months.

Requirement: Verify calibration of the balance per Section 10 before and after each analytical
batch. If calibration is not verified after measurement of the analytical batch, recalibrate the
balance and reweigh the batch. Reference: Method 1664 Revision A, Section 9.5

Recommendation: It is recommended that the balance verification of the 2 mg and 1000mg
before and after analysis be documented on the benchsheet.

4. Deficiency: Matrix spikes are not analyzed with every batch of 20 samples. Previously
cited.

Comment: The LCS does not satisfy the method requirement for the spike. The method
requires a matrix spike.

Requirement: Collect additional one or two aliquots (1L, additional smaller volume, or both) of
a sample for each set of twenty samples or less for the matrix spike and, if used, the matrix
spike duplicate. Note: For those circumstances requiring the collection of multiple aliquots of
one sample, each aliquot is to be collected in either of the following ways: 1) collect
simultaneously in parallel, if possible, or 2) collect as grab samples in rapid succession.
Reference: Method 1664 Revision A Section 8.2.

Requirement: The laboratory must spike a minimum of 5 percent of all samples from a given
sampling site or, if for compliance monitoring, from a given discharge/waste stream (matrix
spike). The sample aliquot shall be spiked with the hexadecane/stearic acid spiking solution.
The spike must fall within the following acceptance criteria: HEM (78-114), SGT-HEM (64-132).

Requirement: At any time a laboratory receives samples which 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
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notification must include a statement indicating corrective actions taken to prevent the problem
for future samples. Reference: 15A NCAC 2H .0805 (a) (7) (N).

Requirement: Each analytical batch of 20 or fewer samples must be accompanied by a
laboratory blank, an ongoing precision and recovery sample, and a matrix spike, resulting in a
minimum of four analyses (1 sample, 1 blank, 1 OPR, and 1 MS) and a maximum of 23
analyses (20 field samples, 1 blank, 1 OPR, and 1 MS) in the batch. If greater than 20 samples
are to be extracted in a 12-hour shift, the samples must be separated into analytical batches of
20 or fewer samples. Reference: Method 1664 Revision A, Section 18.2.1 & 18.2.2.

5. Deficiency: The laboratory does not perform multiple weighing on the boiling flasks.

Requirement: Repeat the cycle of drying, cooling, desiccating, and weighing until the weight
loss is less than 4 % of the previous weight or less than 0.5 mg, whichever is less. Reference:
Method 1664 Revision A, Selection 11.4.4.

F. Comment: A sample that was extracted on 4/8/06 and was analyzed, appeared to be a
solid sample. (10g sample). If solid samples are to be analyzed, they will need to be analyzed
by 9071B method. (Please clarify in the response).

G. Comment: Solid samples must be analyzed by the method 9071B. On some of the data
reviewed the sample 3308-01 appears to be a soil sample. This sample would need to be
analyzed by the method 9071B. Please clarify in the response how this sample was filtered
if analyzed by 1664.

H. Comment: The true value of the LCS appears to be 20 based on the recoveries noted. If
the true value is 20mg/L, some of the data reviewed for the LCS would be outside the
acceptance criteria for HEM (78-114). The method requires the LCS (OPR) to be 40 mg/L.
(Please clarify in the response the true value of the LCS and the corrective action taken
when the values fall outside the acceptance criteria).

4. Deficiency: Matrix spikes are not analyzed with every batch of 20 samples. Previously
cited.

Comment: The LCS does not satisfy the method requirement for the spike. The method
requires a matrix spike.

Requirement: Collect additional one or two aliquots (1L, additional smaller volume, or both) of
a sample for each set of twenty samples or less for the matrix spike and, if used, the matrix
spike duplicate. Note: For those circumstances requiring the collection of multiple aliquots of
one sample, each aliquot is to be collected in either of the following ways: 1) collect
simultaneously in parallel, if possible, or 2) collect as grab samples in rapid succession.
Reference: Method 1664 Revision A Section 8.2.

Requirement: The laboratory must spike a minimum of 5 percent of all samples from a given
sampling site or, if for compliance monitoring, from a given discharge/waste stream (matrix
spike). The sample aliquot shall be spiked with the hexadecane/stearic acid spiking solution.
The spike must fall within the following acceptance criteria: HEM (78-114), SGT-HEM (64-132).

Requirement: At any time a laboratory receives samples which 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
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notification must include a statement indicating corrective actions taken to prevent the problem
for future samples. Reference: 15A NCAC 2H .0805 (a) (7) (N).

Requirement: Each analytical batch of 20 or fewer samples must be accompanied by a
laboratory blank, an ongoing precision and recovery sample, and a matrix spike, resulting in a
minimum of four analyses (1 sample, 1 blank, 1 OPR, and 1 MS) and a maximum of 23
analyses (20 field samples, 1 blank, 1 OPR, and 1 MS) in the batch. If greater than 20 samples
are to be extracted in a 12-hour shift, the samples must be separated into analytical batches of
20 or fewer samples. Reference: Method 1664 Revision A, Section 18.2.1 & 18.2.2.

I. Comment: The evaporation temperature on the benchsheet reviewed was typically around
62 ºC. On the checklist the analyst answered yes on the following question: “Is the flask dried
30-45 minutes in a 70 + 2ºC oven, then desiccated at least 30 minutes before weighing?”
Please clarify in the response what the evaporation temperature is set on for this
procedure.

6. Deficiency: On the data reviewed there were several instances where the collected sample
volume was below the method requirement of one liter. In some cases, for example, the sample
volume was 610 mls, 670 mls, 710 mls, and 770 mls. If the required volume is not submitted
the data must be qualified.

Requirement: Collect approximately one liter of representative sample in a glass bottle
following conventional sampling practices, except that the bottle must not be pre-rinsed with
sample before collecting. To allow for potential QC failures, it is recommended that additional
sample aliquots be collected. Reference: Method 1664 Revision A, Section 8.1. Note:

Recommendation: It is suggested that the laboratory obtain a QCS from a source different
from the source for the hexadecane and stearic acid used routinely in this method (Sections 7.8
and 7.9), and that the QCS be used for verification of the concentrations of HEM and SGT-HEM
using the procedure given in the note in Section 7.10.3. The QCS should be analyzed monthly
by laboratories performing routine analyses and less frequently by laboratories performing these
analyses intermittently. Reference: Method 1664 Revision A, Section 9.7.

Phenol/BOD:

7. Deficiency: Duplicates were not always analyzed. Duplicates were not analyzed on the
following dates of the data reviewed for Phenols: 2/14/06, 2/15/06, and 2/20/06. Cited
Previously for BOD.

Requirement: Analyze 5% or more of the samples in duplicate. Analyze duplicates and known
additions in matrices representative of the samples analyzed in the laboratory. Reference:
Standard Methods 18th Edition; 1020B Section 6.

Requirement: Except for Oil & Grease (413.1), settleable solids or where otherwise specified
in an analytical method, analyze five percent of all samples in duplicate to document precision.
Laboratories analyzing less than 20 samples per month must analyze at least one duplicate
each month samples are analyzed. Reference: 15A NCAC 02H .0805 (a) (7) (C).

Phenol / Ion Chromatography:

8. Deficiency: Units are needed on the benchsheet.

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,
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volume of sample analyzed, value from the measurement system, factor and final value to be
reported and each item must be recorded each time sample are analyzed. Reference: 15A
NCAC 02H .0805 (a) (7) (H).

BOD:

J Comment: The laboratory does not check the calibration of the DO meter during each
sample set with sufficient frequency. The laboratory should verify the DO Meter calibration
every 10 readings (to include dilutions), and at the end of the sample set. If the meter drifts
more than 0.20 mg/L then recalibrate meter and reanalyze all samples since the last drift
check.

Requirement: Check one or two points frequently to confirm original calibration. If calibration
changes, the new calibration should be parallel to the original, provided that the same
membrane material is used. Ref: Standard Methods, 18th Edition - Method 4500-O G 1a. p4-
104.

K. Comment: It is strongly recommended that the laboratory analyze a seeded blank. A
seeded blank is a bottle of dilution water with the same amount of seed in it as the sample. The
seeded blank should be around 0.2 mg/L of the calculated seed control. The seeded blank can
let you know if you have the right ratio of seed in the sample to seed in seed controls. It can
also let you know when your seed is weak. It can be a very good source for problem solving.

L. Comment: Occasionally the dilution water blank is not <0.2 mg/L.

Recommendation: It is strongly recommended that at least 2 dilution water blanks are analyzed
with each batch. A dilution water blank would be the dilution water without the seeded material.
The dilution water blank must be <0.2 mg/L or must be qualified. If more than one is analyzed
and one is within the acceptance criteria, the data does not have to be qualified.

M. Comment: Occasionally the initial DO values are around 8.0 mg/L. This is still in the
acceptance criteria but it is running close to the edge. The supersaturated samples should be
vigorous shaken to remove the excess oxygen.

Requirement: Samples containing more than 9 mg DO/L at 20°C may be encountered in cold
water or in water where photosynthesis occurs. To prevent loss of oxygen during incubation of
such samples, reduce DO to saturation at 20°C by bringing samples to about 20°C in partially
filled bottle while agitating by vigorous shaking or by aerating with clean, filtered compressed
air. Reference: 18th Edition Standard Methods 5210B (4) (e) (4) pg 5-5.

Recommendation: It is recommended that additional columns be added and other columns
shifted around to document the following in this order: the amount of oxygen used (prior to the
seed correction), corrected BOD after the seed correction column, column for the dilution factor
and reported BOD column. This will allow anyone reading the data to follow the process a lot
easier. (Note: There is a column for the dilution factor but it is not being used to document the
dilution factor).

N. Comment: A GGA standard is not always analyzed with each batch.

Requirement: Check dilution water quality, seed effectiveness, and analytical technique by making
BOD measurements on pure organic compounds and samples with known additions. If control
limits are outside the range of 198 ± 30.5, reevaluate the control limits and investigate source of the
problem. If measured BOD for a glucose-glutamic acid check is outside the accepted control limit
range, corrective action must be taken and the data qualified. If one is within the acceptance limits
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the data does not need to be qualified. Reference: 18th Edition Standard Methods 5210B (4)
(c) pg 5-3.

Recommendation: If is recommended that at least 2 GGA are analyzed with each batch. Only
average the GGA standards that are within the acceptance criteria of + 198 mg/l.

O. Comment: Sometimes seed dilutions that do not deplete at least 2.0 mg/L are used in the
average to calculate the seed control.

Requirement: Only data that meets the 2 mg/L used 1 mg/L left criteria can be averaged to
obtain a final BOD result. Data that does not meet the method criteria must not be averaged
with acceptable data to obtain a final result. Ref: Standard Methods, 18 Edition - Method 5210 B
pg. 5-3.

Requirement: The seed dilution used in calculating the seed control must met the “2” to “1” rule of
use 2 .0 mg/L, leave 1 mg/L, and must be between 0.6 mg/L -1.0 mg/L.

P. Comment: The calculated average seed control is not always used as the value to subtract
from the samples. Sometimes the lowest value calculated is used.

Requirement: All seed controls that meet the criteria would be average the same criteria as
the samples.

Requirement: Determine BOD of the seeding material as for any other sample. Ideally, make
dilution of seed such that the largest quantity results in at least 50% DO depletion. Reference:
Standard Methods 18th Edition- Method 5210B (4) (d) (2).

Q. Comment: Sometimes the pH values were outside the range of 6.5-7.5 and no adjustment
was made. For example one sample the pH was 1.22 and there was not documentation of an
adjustment to the pH of the sample.

Requirement: Neutralize samples to pH 6.5 to 7.5 with a solution of sulfuric acid or sodium
hydroxide of such strength that the quantity of reagent does not dilute the sample by more than
0.5%. Reference: Standard Methods 18th Edition 5210B (3) (e) (1).

Comment: The DO meter is set to read %, it is recommended that it be adjusted to read in
mg/L.

Recommendation: When anomalies occur that require additional information, we suggest
that you contact Gary Francies at the Asheville Regional Office for assistance. He can be
reached at 828-296-4677 ([e-mail]).

COD:

9. Deficiency: Blanks were not always analyzed with each batch.

Requirement: If the reagent blank is used to zero the instrument, the same reagent blank must
be read back as the CCB after the mid-range standard, after every ten samples and at the end
of the run.

Recommendation: It is recommended that a copy of the calibration curve be included at the
front of the logbook, if it is in another logbook.

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R. Comment: The check sample at the end of analysis does not always have the % recovery
documented.

Recommendation: It is recommended that the % recovery, true value and acceptance criteria
for all the QC standards be documented on the benchsheet. This will allow anyone observing
the data, to see if it is within the acceptance criteria.

S. Comment: On the data reviewed, the low check standard was outside the acceptance
criteria of + 10% but it was not reanalyzed.

Requirement: Corrective action would require that the batch be reanalyze or the data be
qualified.

Cyanide:

10. Deficiency: The preparation of the working standard cyanide solution, Chloramine T and
the color reagent was not documented in a logbook. The last documentation of the Chloramine
T was on 4/4/06.

Requirement: The laboratory needs to increase the documentation of reagents used, made, and
standard preparation. The preparation of all reagents, standards and media should 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 solution preparation 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 information as well as the vendor, manufacturer, lot number,
and expiration date should be retained for primary standards or chemicals and reagents used.

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).

Requirement: Reagents must be dated and initialed when prepared. Reference: 15A NCAC
2H .0805 (a) (7) (L).

Requirement: Dissolve 1.0g of white, water soluble Chloramine T in 100 ml of distilled water
and refrigerate until ready to use. Prepare fresh daily. Reference: EPA Method 335.2
Section 7.12.
Pyridine-Barbituric Acid Reagent: This reagent is stable for approximately six months if stored in
cool, dark place. Reference: EPA Method 335.2 Section 7.13.1.

pH:

11. Deficiency: The analyst did not meet the 15 minute holding time for pH and it was not
qualified on the client report. This was a NC project # 0509457. It was received on 10/12/06
and analyzed on 10/17/06.
Requirement: The analyst must meet the 15-minute holding time for all parameters listed for
“immediate”
analysis in the Federal Register. Ref: Federal Register, October 26, 1984; 40 CFR 136; Table II.
Required Containers, Preservation Techniques, and Holding Times.

Requirement: At any time a laboratory receives samples which 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
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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 actions taken to prevent the problem
for future samples. Reference: 15A NCAC 2H .0805 (a) (7) (N).

Recommendation: It is recommended that the collection time and collection date be
documented on the
benchsheet to act as a visual reminder of the holding time.

T. Comment: Sometimes samples are above a pH of 10. The samples should be bracketed
with the pH
buffers. Another buffer higher than a pH10 will need to be check whenever there is higher pH
sample.

Requirement: For analytical procedures requiring analysis of a series of standards, the
concentrations of these standards must bracket the concentration of the samples analyzed.
Reference: 15A NCAC 2H .0805 (a) (7) (I).

U. Comment: It was noted during the inspection that sometimes pH paper is used to verify the
pH of samples that are higher than a pH 10. Please clarify in the response this procedure.
The method requires that a pH meter be used to analyze the samples.

Comment: On the checklist the acceptance criteria for the third pH buffer check was noted as
being 0.5 pH units. The method states the acceptance criteria for the third pH buffer as + 0.1
pH units.

Requirement: For routine work use a pH meter accurate and reproducible to 0.1 pH unit with a
range of 0 to 14 and equipped with a temperature compensation adjustment. Ref: Standard
Methods, 18th Edition - Method 4500 - H+ B (2) and (4) (a) and Ref: 15A NCAC 2H .0805 (a)
(7).

Chain of Custody:

12. Deficiency: At the time of receipt the temperature for the NC project #0509457 was 12ºC
but there was not indication that the client had been contacted that the sample was outside the
required temperature.

Requirement: A record of date collected, time collected, sample collector, and use of proper
preservatives must be maintained for all samples. Reference: 15A NCAC 2H .0805 (a) (7)
(M). The acceptable temperature range of samples during transport is 4 ±2°C, and during
storage and for stored sample extracts, is 1.0 - 4.4°C. Ref: Federal Register, July 1, 1995; 40
CFR 136; Table II. Required Containers, Preservation Techniques, and Holding Times.
EPA letters of January and February 1995.

Requirement: At any time a laboratory receives samples which 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 actions taken to prevent the problem
for future samples. Reference: 15A NCAC 2H .0805 (a) (7) (N).

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504.1:

V. Comment: It was noted on the checklist that Field Reagent Blanks are only analyzed if
submitted. This is a method requirement. If the field reagent blank is not submitted the data
must be qualified. (Please clarify this response in the reply).

Requirement: The minimum requirements of this program consist of an initial demonstration of
capability and an ongoing analysis of field reagent blanks (FRB), laboratory reagent blanks
(LRB), laboratory fortified blanks (LFB), laboratory fortified sample matrix (LFM), and quality
control samples (QCS) to evaluate and document data quality. Reference: 504.1 Section 9.1.
Each day, the analyst must analyze a laboratory reagent blank and a field blank, if applicable, to
demonstrate that interferences from the analytical system are under control before any samples
are analyzed. Reference: 504.1 Section 9.1.3.

W. Comment: It was noted on the checklist that the requirement of samples being analyzed
within 24 hours of extraction is for North Carolina samples and is not required by the method.
This is not only a NC but a method requirement. (Please clarify this response in the reply).

Requirement: Because 1,2,3-trichloropropane has been added to the analyte list in this
method and has been found to have a 14-day maximum holding time in studies conducted by
Method 524.24, all samples must be extracted within 14 days of collection. Samples not
analyzed within this period must be discarded and replaced. Because of the potential for
solvent evaporation, it is preferred that extracts be analyzed immediately following preparation.
When necessary, extracts may be stored in tightly capped vials (Section 6.2) at 4º C or less for
up to 24 hours. Reference 504.1 Section 8.3.2.

1631:

X. Comment: It was noted on the checklist that the field blanks are analyzed if submitted by
the client. As a reminder, field blanks are a method requirement. A memo was submitted to all
certified labs from our office, on July 5, 2005 concerning field blanks. As stated in the memo,
the determination of the NC Certification Program is that the certified laboratories are not to
accept and/or analyze any samples for this analysis without the accompanying field blanks. (A
copy of this memo is enclosed). (Please clarify in the response the laboratory’s policy).

6020:

Y. Comment: It was noted on the checklist that the Instrument Detection Limits (IDL) is not
determined
every 3 months as required by the method but is performed annually.

Requirement: Instrument Detection Limits (IDL) must be determined at least every 3 months
and kept with the Instrument’s log book. Reference: Method 6020 Section 8.2.

Z. Comment: It was noted on the checklist that samples that are more concentrated than the
highest
standard analyzed in the curve are not diluted and reanalyzed. Instead, the linear range is used
for these samples.

Requirement: For analytical procedures requiring analysis of a series of standards, the
concentrations of these 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.
Reference: 15A NCAC 02H .0805 (a) (7) (I).
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General Requirements

Our regulation requires that a standard curve consisting of a blank and five standards must be
analyzed. For colorimetric analyses this curve must be checked each time samples are analyzed
with a blank and a medium level standard. In lieu of a standard curve, a three point (low, medium
and high standard) may be analyzed with each group of samples. For metals analyses the
standard curve must be analyzed each time samples are analyzed along with a medium level
quality control standard. The standards for the standard curve should bracket the range of samples
being analyzed, i.e. if you choose to have a lower detection or reporting limit of 5 µg/l for a
particular metal parameter , you must analyze a 5 µg/l standard for that metal parameter and report
lower samples as <5 µg/l. If you choose 1000 µg/l for the top of your standard curve, you must
analyze a 1000 µg/l standard and all samples above this limit must be diluted and reanalyzed to fall
within the curve.

6010B:

AA. Comment: On the data reviewed the reporting limit was not demonstrated in the run. The
data reviewed was not a NC sample. This is a requirement for NC samples.

Requirement: For analytical Procedures requiring analysis of a series of standards, the
concentrations of these 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 2H .0805 (a) (7) (I)

See General Requirements above.

BB. Comment: On the data reviewed the pH of preserved metals samples was not documented
to be pH <2 either at receiving or at the bench.

Requirement: The pH of preserved metals samples must be documented to be less than 2. Ref:
Federal Register; Vol. 49, p. 43234 (October 26, 1984) Table II.

Requirement: The laboratory must document that the pH of all samples has been properly
adjusted. A record of date collected, time collected, sample collector and use of proper
preservatives must be maintained. Ref: 15A NCAC 2H .0805 (a) (7) (M).

TCLP:

CC. Comment: On the checklist it was stated that there is no corrective action if matrix spike
results fall outside established control limits or indicate an analytical problem. Please clarify
this response in the report reply.

Requirement: Method states the purpose of the matrix spike is to monitor the performance of
the analytical method used, and to determine whether matrix interferences exit. Use of other
internal calibration methods, modification of the analytical methods, or use of alternate analytical
methods may be needed to accurately measure the analyte concentration in the TCLP extract
when the recovery of the matrix spike is below the expected analytical method performance.
Reference: SW846 Method 1311 Section 8.2.3.

Residue:

DD. Comment: On the data reviewed there were some days when there was no
documentation that the balance had been verified on that day.
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Requirement: The analytical balance must be checked with one class S, or equivalent,
standard weight each day used and at least three standard weights quarterly. The values
obtained must be recorded in a log and initialed by the analyst. Reference: 15A NCAC 02H
.0805 (a) (7) (K).

Organics:

12. Deficiency: There is no documentation to show that a check for residual chlorine is being
done.

Requirement: Samples containing chlorine must be dechlorinated at the time of sample
collection and treated according to the requirements of the analysis to be performed. For any
sample that requires the removal of residual chlorine, (Ammonia, TKN, TPH-Gasoline, and
Diesel, Cyanide, Purgeables, Pesticides, PCB’s and PAH’s) the laboratory must check to
ensure that the chlorine has been removed. The residual chlorine check must be performed to
verify that the residual chlorine level is below 0.5 mg/L. Commercially available starch iodide
paper can be used to perform this determination. Reference: Federal Register, July 1, 1995;
40 CFR 136 for most methods and EPA SW-846; Chapter 4 table4-1 page four-7.Test
methods for Evaluating Solid Waste.

Requirement: At any time a laboratory receives samples which 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 in writing. The notification must
include a statement indicating corrective actions taken to prevent the problem for future samples.
Reference: 15A NCAC 2H .0805 (a) (7) (N).
Requirement: The laboratory must document that all residual chlorine has been removed and
that the pH of all samples has been properly adjusted. A record of date collected, time collected,
sample collector and use of proper preservatives must be maintained. Ref: 15A NCAC 2H .0805
(a) (7) (M).

IV. PAPER TRAIL INVESTIGATION:

A paper trail was conducted at this facility. This consisted of comparing laboratory bench data
with client reports. There were no transcription errors detected.

V. CONCLUSIONS:

We are concerned with the deficiencies that were cited previously and not corrected. Failure to
correct the deficiencies cited in this report will lead to enforcement action.

Ref: 15A NCAC 2H .0807 (a) (1) and (14)

Laboratory Decertification:

A laboratory may be decertified for any or all parameters for up to one year for any or all of the
following infractions:

(1) Failing to maintain the facilities, or records, or personnel, or equipment, or quality control
program as set forth in the application, and these Rules; or
(14) Failing to comply with any other terms, conditions, or requirements of this Section or of a
Laboratory certification.
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Correcting the above cited deficiencies and comments and implementing the recommendations
will help this lab to produce quality data and meet certification requirements. Please respond to
all numbered deficiencies and lettered comments.

Report prepared by: Tonja Springer Date: June 21, 2006

NORTH CAROLINA DENR/DWQ
WASTEWATER/GROUNDWATER
LABORATORY CERTIFICATION

MEMORANDUM

DATE: July 5, 2005

TO: All labs certified for EPA Method 1631

FROM: James W. Meyer

SUBJECT: Field Blanks

It has come to our attention that samples for this analysis are being submitted without the
accompanying required field blanks. The Method clearly states in Section 9.4.5 that “Field blanks
are used to demonstrate that samples have not been contaminated by the sample collection and
transport activities.” 9.4.5.1 states “Analyze field blanks 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.”

The determination of this office is that the certified laboratories are not to accept and/or analyze
any samples for this analysis without the accompanying field blanks. The samples are to be
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rejected by the laboratory and the client requested to resample and resubmit the samples with
proper field blanks.