#381 2006-f

On-Site Inspection Report

LABORATORY NAME: Analytical Services, Inc.

ADDRESS: 110 Technology Parkway
Norcross, GA 30092

CERTIFICATE NO: 381

DATE OF INSPECTION: May 22, 23 & 24, 2006

TYPE OF INSPECTION: Maintenance

EVALUATOR: Jeffrey R. Adams

LOCAL PERSON(S) CONTACTED: Ms. Pam Varner, Ms. Karen Greene, Mr. Richard Fox, Mr. William
Dyer and Mr. G. Wyn Jones

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 staff is congratulated for doing a good job of maintaining the laboratory certification program. The
laboratory is spacious and well equipped. All facilities and equipment appeared to be well maintained.
Records are well kept and most data looked good. All issues had been corrected that were noted in the
previous inspection, although some further quality control procedures need to be implemented. The
inspector would like to thank the staff for their assistance in the inspection and data review process.

Comment: For all benchsheets, it is recommended that the lab indicate which edition of the method is
being referenced. This will aid the analysts, when method changes are promulgated by EPA, to
maintain adequate documentation of their data.

III. DEFICIENCIES, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:

Inorganics:

COD, Cyanide, Hexavalent Chromium, MBAS, Phenols, Sulfide, Total Organic Carbon.

1). Deficiency: It was observed that for the majority of the inorganic and colorimetric calibration curves
were being forced through “zero” by using the blank in the calibration curves.

Requirement: The laboratory must not force curves through the origin. As a minimum, measure three
different dilution’s of the standard when an analysis is initiated. A blank does not contain a measurable
amount of standard; therefore zero or the origin cannot be considered in the calibration curve. Ref:
Standard Methods, 18th Edition - Method 1020 B Pg. 1-5.

Desiccators:

2). Deficiency: It was observed during the “walk through” inspection, that the laboratory is using
Phosphorous Pentoxide as the desiccant and indicator. When expired, it turns from a solid to a liquid.
Unfortunately all of the desiccators contained “liquefied” Phosphorous Pentoxide, indicating that the
desiccant had expired and needed to be changed.
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Requirement: A dessicator must be maintained and the desiccant kept fresh as indicated by a color
indicator of moisture concentration or an instrumental indicator. Ref: Standard Methods 18th Edition
2540 B Total Solids at 103-105° C section (2) d p2-54.

Comment: The laboratory uses a humidity indicator rather than color indicating desiccant in the
desiccator used for total suspended solids samples.

Recommendation: It is recommended that the laboratory include color indicating desiccant as a
backup (i.e. Drierite or silica gel) to the humidity indicator that is currently being used in the desiccator.
Thermometers:

A). Comment: One of the thermometers was broken on “sample cooler” #2. This thermometer was
replaced during the inspection.

Balances:

B). Comment: The analytical balance level checks were very close to indicating being unlevel by the
bubble being located on the far edge of the circle, and not being centered.

Recommendation: It is recommended that the analysts observe the balance levels more carefully when
performing the daily calibration checks.

BOD:

A). Comment: The laboratory is using a (4) DO probe automated system. Although the GGA recoveries
and blank data were within the acceptable control limits, it was observed that majority of the gold plating
was gone or tarnished on each of the probes.

Requirement: The gold cathode should be bright and have fine scratches covering the entire surface. Do
not attempt to create a “glass smooth surface on the cathode, because the absence of scratches will
prevent accurate readings from being measured. The gold cathode can become plated with silver from the
anode and tarnished from the use with wrinkled membranes or after contact with known interfering gases
such as hydrogen sulfide. Ref: YSI Model 5905 or 5910 BOD Probe Manufacturers Manual.

Note: In order to service the gold cathode, follow the instructions using the sanding disk provided in the
Cap Membrane Kit, item # 5906 that was included with the YSI 5905 or 5010 BOD probes.

B). Comment: Although the GGA standards had no expiration date and all of the observed GGA results
were within the acceptable control limits, but due to the “opened date of 5/22/99” posted on the GGA
standard containers and since these were being used for quality control standards rather than for reagent
solutions, the inspector felt that they need to be replaced with a new lot and an “old vs. new” comparison
check be performed and documented.

Requirement: Chemicals must be used within the expiration period stated by the manufacturer.
Chemicals exceeding the expiration date can no longer be considered reliable. Ref: Standard Methods,
18th Edition - Method 1070 C.3c.

Recommendation: Although not stated by EPA, it is highly recommended and a general “rule of good
laboratory practice” to replace any chemical or reagent (even if no expiration date is posted) after 5
years.

Recommendation: It is highly recommended that the GGA standards be desiccated at all times.

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COD:

C). Comment: Although the %recoveries and RPDs are being performed and documented in the QC
Summary Report, the laboratory is not always listing the “true value” and the RPD for duplicate
analyses on the benchsheets.

Recommendation: The inspector recommends that the laboratory include the “true value” and the
RPD of any duplicate analysis on the benchsheet.

Dissolved Oxygen:

3). Deficiency: The samples taken for dissolved oxygen are not measured immediately upon sample
collection, but are transported to the laboratory for analysis.
Requirement: All dissolved oxygen measurements must be taken immediately at the site of collection.
Ref: 40CFR Ch.1 (7-1-95) p. 644 table II.

D). Comment: All DO data being reported must be qualified as being analyzed “out of hold time and
results are not usable for regulatory purposes”.

Total Residual Chlorine:

4). Deficiency: The laboratory does not meet the 15 min. holding time for residual chlorine analysis.
Requirement: The maximum holding time for residual chlorine samples is 15 min. Ref: 40CFR Ch.1 (7-
1-95) p. 644 table II.

E). Comment: The laboratory is currently using the FAS titration method for its residual chlorine
analysis. All data observed indicated all samples being analyzed were out of the required “15 minute”
hold time. All residual chlorine data being reported must be qualified as being analyzed “out of hold
time and results are not usable for regulatory purposes”.

Total and Ortho Phosphate:

F). Comment: The laboratory is not always recording the “true value” and the RPD values on the
benchsheet.

Recommendation: The inspector recommends that the laboratory include the “true values” and RPD
for all duplicate analysis on the benchsheets.

ORGANICS:

G). Comment: The laboratory is currently using The “Rule of Huge Error” in the electronic monitoring
of its internal quality control criteria for inorganic and organic analyses. Supposedly this allows the
system to “reject” and not include any obvious outliers, thus eliminating analysts or personal data
validation and judgment error. (Ref: John Keenan Taylor. Statistical Techniques for Data Analysis.)

Note: The “Rule of Huge Error” is expressed as:

M = Suspect – Mean
σ

Where M denotes the deviation from the mean as a multiple of the standard deviation σ. Normally if

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M > 4 the suspect can be considered an outlier.

Comment: The inspector viewed (2) data packs of all organic parameters and observed all matrix
spikes, duplicate analyses and laboratory control spikes to fall within the ± 2 σ standard deviations from
the laboratory generated mean. The QA officer assured the inspector that the “Rule of Huge Error”
equation was only being implemented for gross and obvious outliers.

Recommendation: After a thorough review of SW-846 EPA Method 8000B, 8000C and Standard
Methods the inspector highly recommends that the laboratory abolish the “Rule of Huge Error” from the
construction of its control charts and data acceptance criteria and to follow the conventional ± 3σ
standard deviations to insure a 95% confidence limit in its control charts data acceptance criteria and
when these limits are exceeded corrective action must be implemented.

EDB:

5). Deficiency: The laboratory is not analyzing a Laboratory Fortified Blank every 10 samples
analyzed.
Requirement: The laboratory must demonstrate that the measurement system is in control by
analyzing LFB (s) of the analysis at 0.25 µg/L concentration level for each analyte. This must be
demonstrated on a frequency equivalent to 10% of the sample load or one (1) per batch of samples
extracted, whichever is greater. Ref: EPA Method 504.1- 9.1.4, 9.3 Rev.1, (1995)

BNA’s Method 8270

H). Comment: The laboratory is currently using the following points of 10, 40, 60, 80, 120, and 160
mg/L in the calibration curve.

Recommendation: Although not required, it is a general rule not to exceed more than twice the
concentration between points when constructing a calibration curve. The inspector highly recommends
that the 20 mg/L standard be inserted into the lower range of the calibration curve and possibly
dropping the 60 mg/L standard.

Other Organic Parameters: Methods 8151A, 8081A, 8080-EPA-608,

I). Comment: After a thorough review of the organic data the inspector found that the laboratory was
using “Linear Weighted Averaging” in the construction of the above stated organic analytical curves and
calculating the data based on these curves. This data was reviewed by (4) different inspectors of varying
experience and expertise and of the several calibration curves reviewed several did not exhibit the need
for the “Linear Weighted Averaging”.

Recommendation: Even though SW-846 Method 8000C permits the use of this type of curve, it doesn’t
recommend its use under normal laboratory operating conditions. It is generally observed that when it is
necessary to use “Linear Weighted Averaging”, there is the concern that there possibly could be “masking”
of analytical problems, i.e. dirty detectors, leaking septums, columns being depleted and possibly analysts
error, therefore is not usually accepted as the “norm”. It is highly recommended that the laboratory re-
evaluate these stated organic parameters and to follow 8000C and Methods specific rules in determining
the methods of calibration and the establishing of the various parameter control limits. It is generally
recommended that the construction of the analytical curves not to exceed a second order quadratic
regression fit, with a correlation coefficient of R2= ≥0.99 or a first order Linear Least Squares regression of
R= ≥0.995.

IV. PAPER TRAIL INVESTIGATION:

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The inspector reviewed (2) data packs from 2005 and 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 inspector found no
computation errors on the data packs reviewed and data appeared accurate and easily accessible to
the inspector.

V. CONCLUSIONS:

Correcting the above cited deficiencies and comments and implementing the
requirements/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: Jeffrey R. Adams Date: June 28, 2006