NCD003200383_19930922_Koppers Co. Inc._FBRCERCLA RD_Selection of Dioxin Laboratory - Remedial Design-OCR

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· "6' CHESTER
-. -~---ENVIRONMENTAL
· · . . · Ref. No. 179285-01
Federal Express ·
September 22, 1993
Ms. Beverly Hudson, Remedial Project Manager USEPA Region IV
N. C. North Superfund Remedial Branch Waste Management Division
345 Courtland Street, NE
Atlanta, GA 30365
Dear Beverly:
Re: Selection of Dioxin Laboratory
Former Koppers Plant Remedial Design Morrisville, North Carolina
KtCt\VtU
SEP 2 :.I 199J
sueERfUN~ SECOON
On behalf of Beazer East, Inc. and in accordance with the Unilateral Order, Chester Environmental (Chester) is informing you that Alta Analytical Laboratory has been chosen to perform the dioxin/furan analyses for the Koppers site in Morrisville, North Carolina. ·
Please find enclosed teri (10) copies of Alta Analytical Laboratory's QAM.
Should you need additional information regarding the submittal, please contact Shannon Craig at [phone] or me. ·
Very truly yours,
John Mitsak, P.E.
Manager, Baltimore Operations
Enclosures
cc: Ms. Shannon Craig -Beazer East, Inc. Ms. Cindy Zuch -Beazer East, Inc. Mr. Jim Cook -Beazer East, Inc.
Mr. Bruce Nicholson -NCDEHNR Superfund
3000 Tech Center Drive
Monroeville, Pennsylvania 15146
412-825-9600: Fax [phone]
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I SEP 2 J J99j
SUPERFUN~SfCOON
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I LABORATORY QAM
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DIOXIN/FURAN ANALYSIS
Alta Analytical Laboratory
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FOREWORD
The following document was prepared in accordance with the USEPA guidelines specified in
"Interim Guidelines and Specifications for Preparing Quality Assurance Project Plans" (QAMS-
005/80). It is the intent of Alta Analytical Laboratory (ALTA) to meet or exceed the QNQC
requirements set by USEPA or other appropriate governmental or private entities and to assure
that all analytical data generated are scientifically valid, defensible, comparable and of known
acceptable precision and accuracy.
.;./-27-'13
nf)ohn W. Cornacchia, President
. . 0 ~ I , JL. 11/ 5.,..._.,,.., \~ ~ ;t) I 1' ;. 1 r rt'7 t,, ,r I
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Sharon K. Pierson, Quality Assurance Officer
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TABLE OF CONTENTS
I Section 1. Laboratory Administration
I Section 2. Sample Control
I Section 3. Sources and Preparation of Standards
I Section 4. Analytical Procedures
I Section 5. Initial and Continuing Calibration Procedures
ll Section 6. Internal Quality Control Procedures
flt Section 7. Corrective Actions
ll Section 8. Performance and System Audits
I Section 9. Preventative Maintenance
I Section 10. Quality Assurance Reports to Management
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Section 11. Appendix
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SECTION 1.
Laboratory Administration
Section No. _1
Revision No. 5.0
Date: 3/31/93
Page: _! of ..1..
1. Laboratory Administration
1.1 Organizational Structure
Alta Analytical Laboratory (ALTA) is a privately owned California
corporation providing mass spectrometry services to chemical manufacturers,
environmental engineering firms, the pulp and paper industry as well other
industrial and governmental clients. The organizational structure for ALT A is
shown in Figure 1.1-A.
The management structure of ALTA consists of the laboratory President and
directors. The duties of the management team are as follows:
1.1. l The Laboratory President is responsible for the management of
financial/technical operations as well as implementation of corporate
goals, objectives and policy.
1.1.2 The Director of Financial Services is responsible for all financial and
facility services. The management of the facility includes overseeing
sample control, LIMS, the data archive and building maintenance. The
Director of Financial Services supervises all administrative personnel.
1.1. 3 The Director of High Resolution Mass Spectrometry Services (HRMS)
is responsible for all HRMS instrument operations. This includes study
management, consultative services, sales and marketing, personnel
training and HRMS technology development.
1.1.4 The Director of Liquid Chromatography Mass Spectrometry Services
(LCMS) is responsible for the development and management of all
instrument operations involving LCMS, LC/MS/MS, GCMS (low
resolution) and GC/MS/MS. Studies performed in support of USEPA
FIFRA registration requirements will in most cases be managed by the
Director of LCMS Services. Other responsibilities include TSQ 700
maintenance and training, tandem mass spectrometry technology
development, as well as sales and marketing.
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Section No. _1
Revision No. 5.0
Date: 3/31/93
Page: 2 of.]_
1.1.5 The Director of Technical Services is responsible for management of
the staff and resources associated with the initial phases of analysis by
LCMS and HRGC/HRMS. He provides technical guidance and support
for routine work, methods development, and research and development
projects.
1.1.6 The Director of Air Toxics is responsible for production scheduling and
client managing for the Air Toxics group. He is also responsible for
the final review and interpretation of analytical data and final reports.
1. 1. 7 The Quality Assurance Officer and Safety (QAO) is responsible for
managing the QA activities for the laboratory. The QAO reports
directly to the President and works with management to ensure that the
ALTA QAPP and associated SOP's are followed as written. The QAO
is also responsible for all safety issues and hazardous materials and
waste management.
Resumes for the management team are presented in the Appendix.
Section No. _I_
Revision No. 5.0
Date: 3/31/93
Page: ..l. of ..l.
William J.
Luksemburg
Director of
HRMS Services
James Hedin
Associate Scientist
Martha Maier
Associate Scientist
Nial Maloney
Associate Scientist
Brad Silverbush
Associate Scientist
Michael Werst
Associate Scientist
NON-GLP
Robert S. Mitzel
Director of
Air Toxics
Phil Hartwick
Associate Scientist
Melanee Schuld
Associate Scientist
Richard Spas
lab Technician
FIGURE 1.1-A
Dr. John W. Cornacchia
President
Scott N. Jimison
Director of
Financial
Services
Ken Flatt
Sample Custodian
Mike Gabbard
Sample Custodian
Cathi Stovall
Admin. Assistant
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Sharon Pierson
Quality Assurance O.fjicer
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Shelly Weagraff
QA Associate/Archivist
GLP
Bob Peterson
Director of
Technical
Services
BobBethem
Director of
LCMS Services
Shannon Bryant
Associate Scientisl
Jeri Frier
Associale Scientist
Jim Lehman
Associate Scientist'
Scott Serl
Associate Scientist
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SECTION 2.
Sample Control
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Section No . ...l.
Revision No. 3.0
Date: 9 /20 /91
Page:_l_ of_]_
2. Sample Control
Sample Control standard operating procedures are designed to ensure the proper
maintenance of samples from acceptance to return. The Director of Financial Services is
the sample custodian and is responsible for the management of Sample Control. All
samples are processed into the laboratory following standard chain-of-custody procedures
and stored in secured areas. Sample Control SOP's cover:
2.1 Complete chain-of-custody (COC) procedures from sample receipt to
return of samples back to the client The ALTA COC is presented in
Figure 2.1-A
2.2 Secured sample storage areas including lockable refrigerators, cabinets and
freezers. The laboratory is equipped with an electronic security system
which is continuously monitored during non-business hours when no staff
are in the facility.
2.3 Sample receiving and log-in procedures documenting sample condition,
identification, preservation and any discrepancies in sample documentation.
Sample log-in data are entered into the ALTA Laboratory Information
Management System (LlMS) to enable sample tracking through the
laboratory.
2.4 Sample maintenance procedures including proper storage conditions,
containers and maximum holding times as specified in published HRMS
analytical methods. Table 2.4-A presents a summary of the sample
maintenance procedures routinely followed by ALTA
2.5 Sample tracking, shipping and return procedures including an· internal
sample check-out and return policy. Most solid samples (except pulps and
tissues) are returned to clients approximately 45 days after delivery of the
final laboratory report.
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FIGURE 2.1-A
Section No. -1..
Revision No. lQ_
Date: 9 /2JJ /91
Page:..l_ of_]_
I Chain of Custody Record
I IA -I ALTA
CHAIN OF CUSTODY RECORD
I Projo::tlD.: ______________ P.0.11: __________ Sampler.
Relinquished by;a..---...-N--)
7
I Rocc.ivcd by. CS.-.u,j"'"'-1"'-1
Relinquished by:~-Pt--,N-J
Rclinquishc:d by:u.c--_,.,__.,.._,
I SHIPTO:
Alta Analytica.l Labontory
Method of Shipmcnc Circle or Add
Aru.l~is( es)
Requ=ed 5070 Rohen J. MatheWl' Parkway. Suiie 2 a.. El Dorado Hills CA 95630
.. TIN: __ _
Scnplc De:.cription
Shipmcru ID:
5-plcID
Nwnbo-Time Description 11
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Special lrutructions/C-OmmczllS: _________________________ _
WHITE-ORIGINAL YELLOW • AROUVE
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Dau::
ConWJI ,,
TAT • Type
Time.:
Time:
TU'llc:
Time:
:A:~~i~/ ;:(1'= ~; /' .:
(:"~;:;.,.;..,~><,:,,,~. /.".
~,},,;.~,.,.,,,,AW-':·:•·•'/ .. '.
,;::.:>..,_.'!»',:,, • .z::_'-._~~-~-,,.;!; -,: ."'
·,--q-•'/,•.'-:..,.0,, .. ,/.
-;:~M'.·:-;:,,,i,:',,;..~-M . .Z: .,:, -:·,·:',;
TAT(An&Jyi;u.1T..,...~Tima)l•1d>y1 2•l<ld.,-. J•2ld.o,-. ◄•2ld•:n
Container Types: C = Core Tube T = Tra..in A .. I Liu:r Amber G "'Glass Jar P = PUF O =Other _____________ _
SE/\.'D DOCUMENTATION AND RESULTS TO: Name: __________________ _
Company: ___________________ _
Addrcss:. __________ ~---------Phone: __________ Fu.: _______ _
PL-.:K ·COPY
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Section No . ...1_
' Revision No. 3.0
Date: 9/20/91
Page: ..l of ..l I
TABLE 2.4-A Sample Containers, Preservatives and Maximum Holding Times
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EPA Method Water 30 Days Extrn Amber Glass 4°C I
8280 45 Days Analysis '11 Bottle (AGB) I Solid 30 Days Extrn Amber Glass 4 °C
45 Days Analysis '11 Jar (AGJ)
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EPA Method Water 30 Days Extrn AGB 4 °C, Dark r
8290 45 Days Analysis '11 I 4 °C, Dark Solid 30 Days Extrn AGJ
45 Days Analysis '11
I Fish/ 30 Days Extrn -20 °C, Dark
Adipose 45 Days Analysis '11
EPA Methods Aqueous 1 Yr. Extrn AGB 0-4°C'31
I 1613 & 1613A 40 Days Analysis '21
Solid 1 Yr. Extrn AGJ o -4°c
40 Days Analysis C2l I
EPA Method Aqueous 7 Days Extrn AGB 4 °C''' Dark I ' 613 40 Days Analysis21
513 Aqueous 90 Days Extrn AGB Ambient, Dark I 40 Days Analysis'2l
EPA Method MM5 Train Train and/ or 0 -4 ° C Dark csi ,
23 AGB I EPA Method PUF 4 °C
T09
CARB Method MM5 Train Train and/or 0 - 4 ° C Dark csi I ,
428 AGB
CARB Methods MM5 Train 7 Days Extrn Train and/ or 4 °C
429 (4) 40 Days Analysis AGB
NCASI 551 C4l All Samples 4 oC(S)
(1) 45 days from collection. CZ) 40 days from extraction (Extm). (3) If residual chlorine is present sodium thiosulfatc is added as per the method.
(4) Holding times and preservation set by ALTA {S) Recommended by ALTA
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SECilON 3.
Sources and Preparation of Standards
Section No . ...l.
Revision No . .....1J!..
Date: 6/01/91
Page:_!_ of...i
3. Sources and Preparation of Standards
ALTA manages the receipt, inventory and preparation of analytical standards (hereafter,
reference substances), stock solutions and reagents based on SOP's which comply with
USEP A Good Laboratory Practices as specified in 40 CFR 160 including:
Reference Substance Inspection and Acceptance,
Logging-in Reference Substances,
Labeling Reference Substances,
Reference Substance Storage,
Reagents and Solutions.
A reference substance is defined as any analytical standard whether it be neat, in
solution or in solution in combination with other analytical standards. The Director of
Operations is responsible for the management of all reference substances.
3.1 Reference Substance Inspection and Acceptance
ALTA accepts reference compounds from traceable sources including commercial
suppliers, chemical manufacturers and the USEP A Criteria for acceptance
includes:
3.1.1 Documentation regarding substance identity, strength, purity,
composition and stability must accompany shipments of reference
substances and must be provided by the source. The source must
be capable of verifying substance characterization. Other pertinent
information including MSDS's and appropriate storage conditions
should be available upon request. ALTA only accepts shipments of
reference substances that are not physically damaged upon delivery
and that are properly labeled.
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3.2 Logging-In Reference Substances
Section No . ..l_
Revision No. 2.0
Date: 6 /01 /91
Page: ..1. of ....i
ALTA logs-in all references substances accepted into the laboratory and maintains
a reference substance database. A log-in form is shown in Figure 3.2-A and
includes the following control features:
3.2.1 A unique eight character log number,
32.2 Substance name or description,
3.2.3 Amount received,
3.2.4 Chemist logging-in substance,
3.2.5 Date received,
3.2.6 Condition of substance as received,
3.2.7 Source, Catalogue No., or Lot/Batch No.,
3.2.8 Solvent and concentration (when applicable),
3.2.9 Date opened and expiration date,
3.2.10 Purity,
3.2.11 Storage location.
The chemist using the reference substance is required to record the amount,
purpose and date of usage as per 40 CFR Section 160 Subpart F. Standard
solutions are logged onto a form similar to that shown in Figure 3.2-A
Section No._]_
Revision No. --1,Q_
Date: 6/01/91
Page: _]_ of _..,i
FIGURE 3.2-A
REFERENCE SUBSTANCE RECEIPT & INVENTORY LOG
LogNo.=L~---
Substance Name: -------------------------
Amount Received: -------Logged By: ________ _
Date Received: _______ _ Condition: _________ _
Received From: --------Catalog No. ________ _
Lot/Batch No.: _______ _ Solvent: ___ Cone.: ____ _
Date Opened: ________ _ Expiration Date: _______ _
Purity:----------Storage Loe. ________ _
Record All Usage With the Appropriate Units Below.
Tare Amount Gross Purpose Initials
Weight Withdrawn Wt./Vol. /Date
After
Withdrawal
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3.3 Labeling Reference Substances
Section No . ..l.
Revision No. _bQ_
Date: 6/01 /91
Page: ....1. of ..2__
All primary reference substances receive labels with the following information:
3.3.1 Name, Case or code number,
3.32 Lot or batch number,
3.3.3 Expiration date (if any),
3.3.4 Storage conditions,
3.3.5 ALTA Log number,
3.3.6 Date,
3.3.7 Initials.
Standard solutions also receive labels which at a minirollro include the solution
ID, solution name and the expiration date.
3.4 Reference Substance Storage
All reference substances and standard solutions are stored in designated freezers,
refrigerators or cabinets based on the manufacturer's (i.e., source) recommended
storage procedures. The temperatures of refrigerators and freezers containing
reference materials are recorded daily. Acceptable temperatures for freezers and
refrigerators range from -5° C to -25~ C and from 1° C to 8° C, respectively.
Reference substances are stored separately from samples and sample extracts.
3.5 Reagents and Solutions
3.5.1 All reagents are obtained from national suppliers. The suitability of
all reagents is verified through their use in processing method blanks
or analysis prior to use.
3.5.2 Solutions made from reference substances is documented on a
Reference Substance Control Form shown in Figure 3.5-A
Section No . ...l
Revision No. _ll
Date: 6 /01 /91
Page:_i of_i
FIGURE 3.5-A
REFERENCE SUBSTANCE CONTROL FORM
STANDARD SOLUTIONS
Solution ID: ------Expires: ____ _
Solution Name: -------------
Solution Type: Stock Spiking Calibration ( circle one)
Chemist: -------Date Prepared: ___ _
Log/Solution Name Init. Units Amount
ID Cone. Used
Final Volume: Diluent: ------------
Procedure:
. Final
Concentration
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'-SECTION 4.
Analytical Procedures
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Section No . ...1.
Revision No. _b!L
Date: 6/01/91
Page: ..1.. of __1_
4. Analytical Procedures
4.1
4.2
Analytical Methods
ALTA follows USEPA, CARE, NCASI or other validated analytical methods
for the determination of dioxins and furans, PCB's, P AH's, chlorophenols,
cblorobenzenes. Table 4.1-A lists those methods and matrixes routinely
conducted by ALTA
ALTA also performs non-routine method development, method validation and
protocols su brnitted by clients.
Data Collection and Recording
Sample preparation and instrument analytical data are stored in analytical batch
files in secured areas within the laboratory. Sample preparation data are
recorded on laboratory benchsheets which include the analytical batch ID,
extraction date, chemist, sample weights and volume, spike witness and other
pertinent information. Instrument data include all calibration and quantitation
results necessary to calculate sample results.
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PULP
SLUDGE
EFF.
SOIL
TISSUE
WATER
FLY
ASH
MMS X
PUF X
FUEL
OILS
STILL
BOTTOM
Section No . ...1_
Revision No. 2.0
Date: 6/01/91
Page:-1._ of-1._
TABLE 4.1-A HR/LRMS Analytical Procedures
X X X X
X X X X X
X X X X X
X X X X X X
X X X
X X X X X X X
X X X X X
X
X X
X X
• EPA Method 1613A can be modified for any matrix if initial precision and accuracy is successful.
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SECTION 5.
Initial and Continuing Calibration Procedures
Section No. i
Revision No. 2.0
Date: 6/01/91
Page: ..l. of ...l.
5. Initial and Continuing Calibration Procedures
The following calibration procedures are applicable to numerous methods including:
5.1
EPA Methods 23, 613, 8280, 8290 and 1613A,
CARE Methods 428 and 429,
NCASI Technical Bulletin 551,
Other methods designated ·by the Director of HRMS or LCMS Services.
Initial Calibration
5.1.1 Duplicate injections of 5 -7 standards are made to create an initial
calibration at least every six months or whenever the continuing
calibration check falls outside of the acceptable relative response factor
window (Average RRF ± 20%). The concentration range of the
standard curve is that specified by the applicable method.
5.1.2 An initial calibration curve is deemed acceptable if it meets the
following criteria:
5.1.2.1
5.1.2.2
5.1.2.3
The signal-to-noise ratio (s/n) exceeds 10:1 for all ions
monitored,
The ion abundance ratio must be within ± 15% of the
theoretical ratio.
The RSD must be less than 20%.
5.1.3 All data associated with initial calibration curve will be permanently
archived by the QAU along with a data summary.
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5.2
5.3
Section No. _i
Revision No. 2.0
Date: 6 /01 /91
Page: ...l. of ...l.
Continuing Calibration
5.2.1 A continuing calibration check is made every 12 hours by injecting a
mid-range standard from the initial calibration curve and a column
performance standard mix (CPSM).
5.2.2 A continuing calibration check is deemed acceptable if the following
criteria are met:
5.2.2.1
5.2.2.2
Relative response factors for the mid-range standard are
within ±20% of the average RRF from the initial
calibration curve,
Chromatographic resolution must be better than 25%.
Non-routine Initial and Continuing Calibration
For methods that have no established calibration criteria, initial and continuing
calibration schemes are at the discretion of the appropriate Director of HRMS or
LCMS Services.
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SECTION 6.
Internal Quality Control Procedures
Section No._§_
Revision No. 2.0
Date: 6/01/91
Page:....!. of_§_
6. Internal Quality Control Procedures
The following quality control (QC) procedures are routinely followed to evaluate method
performance in terms of accuracy and precision. ALTA's in-house program is designed to
ensure that laboratory data meets or exceeds acceptable data quality criteria specified by the
method or protocol. ALTA's internal quality control procedures include the analysis of
method blanks, duplicate samples, laboratory control samples and matrix spikes.
6.1 Definitions
6.1.1
6.1.2
6.1.3
6.1.4
Accuracy: Accuracy is the nearness of a measurement to the true or
theoretical value. Accuracy is assessed by determining recoveries
from laboratory control samples, matrix spikes or by comparing
values obtained from reference samples.
Analytical Batch: An analytical batch is a set of samples of the same
matrix which are analyzed together with the same method, reagents
and standards within the same time period. QC results associated
with individual analytical batches such as laboratory control samples,
method blanks, matrix spike samples, and duplicate samples are
evaluated together to assess data quality.
Clean-up Recovery Standard: A clean-up recovery standard is a
reference substance that is an isotopically labelled analyte which is
added to the sample extract prior to any clean-up procedures. This
standard is used to quantitatively assess losses occurring through the
clean-up process.
Control/Warning Limits: Warning and control limits are limits used
in laboratory control charts tracking average recovery and relative
percent difference. For a Means Chart, typical warning and control
levels are ± 2 and ± 3 standard deviations (s) from the central line
(i.e., average mean recovery), respectively. Similarly, the warning
and control limits for a RPD Chart are usually set at + 2s and + 3s
above the mean RPD, respectively.
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Section No . ...Q.
Revision No. 2.0
Date: 6/01/91
Page: ...l. of ...Q.
6.1.5 Duplicate Sample (DS): Duplicate samples are two separate aliquots
taken from the same source. Duplicate samples are analyzed
independently to assess laboratory precision.
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6.1.6 Internal Standards: An internal standard is a reference substance
that is an isotopically labelled analyte which is added to the sample
prior to extraction and used in the quantitation and identification of
native analytes.
6.1.7 Laboratory Control Sample (LCS1/LCS2): A laboratory control
sample is prepared by adding a known quantity of native standards to
an interferant free matrix. A pair of laboratory control samples are
analyzed to assess method performance (precision and accuracy) in a
well characterized matrix.
6.1.8 Method Blank (MB): A method blank is a sand or distilled water
preparation that is free of native analyte or interferants that has been
prepared and analyzed using the same procedures followed for the
rest of the analytical batch. The method blank is used to determine
the level of background laboratory contamination, if present.
6.1.9 Method Ouantitation Limit (MOL): The method quantitation limit is
defined as the quantity of native analyte that corresponds to the
lowest concentration of the calibration curve.
6.1.10 · Matrix Spike(MS/MSD): A matrix spike sample is prepared by
adding a known quantity of native standards to a sample matrix prior
to extraction. Matrix spike concentration levels will vary according to
the matrix encountered and study objectives.
6.1.11 Native Standard: A native standard is a reference substance that is a
non-isotopically labelled analyte. Native standards are used in
conjunction with internal standards to determine response factors and
quantitatively assess accuracy.
6.1.12 Precision: Precision is the agreement between a set of replicate
measurements. RPD is used as the principal measure of precision
and is based on the analysis of duplicate quality control samples.
Section No._§_
Revision No. 2.0
Date: 6/01/91
Page: _J_ of_§_
6.2
6.1.13 Pre-Spike Standards: A pre-spike standard is an isotopically labeled
analyte that is spiked into a MM5 resin cartridge prior to sampling.
The recoveries of pre-spike standards provide a measure of the air
sampling efficiency for native analytes.
6.1.14 Quality Control Sample: Quality control samples are analyzed to
access the various aspects of the analytical process in order to
monitor quality within the laboratory. The most frequently used QC
samples are method blanks, duplicates, matrix spikes, matrix spike
duplicates and LCS pairs.
6.1.15 Recovery Standard: A recovery standard is a reference substance
that is an isotopically labelled analyte which is added to the sample
extract after clean-up and prior to injection. This standard is used to
quantitatively assess the absolute recoveries of the internal and clean-
up recovery standards.
6.1.16 Resin QC: A resin QC is a XAD-2 preparation that is analyzed to
assess possible background contamination
originating from the resin.
Calculations
62.1 Percent Recovery(%R): Recovery of native standards from LCS or
matrix spike analyses is a measure of accuracy and is calculated
according to the following expression:
%R = (Amount Found)-(Amount Background) X 100 (Amount Spiked')
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6.2.2
6.2.3
6.2.4
Section No._§_
Revision No. 2.0
Date: 6/0l /91
Page: ...1. of_§_
Relative Percent Difference (RPD): Percent Recovery (%R) from
duplicate LCS or matrix spike analyses are used to calculate RPD
using the following expression:
Similarly, the RPD for duplicate sample analyses, is calculated as
follows:
IC1 -C2I RPDDS = ----X 100
(Cl + C2)
2
Control Limits:
6.2.4.1
6.2.4.2
6.2.43
6.2.4.4
The initial warning and control limits for internal
standard recoveries 60% and 100%, and 40% and 120%,
respectively.
The initial warning and control limits for the nature
recoveries from LCS samples are 75% and 125%, and
50% and 150%, respectively for analytes other than
OCDD and OCDF. The respective limits for both OCDD
and OCDF are 70% and 130%, and 40% and 160%.
The initial warning and control limits for LCS RPD
values are 30 and 50%, respectively.
The RPD control limits for MS/MSD and laboratory
duplicate samples are 25% and 20%, respectively.
Section No._§_
Revision No. 2.0
Date: 6/01/91
Page: __i of_§_
6.3 Procedures
6.3.1
6.3.2
Method Blanks:
6.3.1.1
6.3.1.2
63.1.3
6.3.1.4
6.3.1.5
A method blank is run with each analytical batch or 20
samples (whichever is less) per method and matrix type.
For any method involving the determination of native
2,3,7,8-substituted isomers except hepta-or octa-
PCDD/PCDF, the levels measured in the_method blank
must be less than the MQL, or ten times lower than the
concentration found in any sample within the analytical
batch.
For any method involving the determination of native
HpCDD/HpCDF or OCDD/OCDF, the levels measured
in the method blank must be less than five times the
MQL, or ten times lower than the concentration found in
any sample within the analytical batch.
All samples within an analytical batch are re-extracted
and analyzed if the method blank associated with that
batch do not meet internal standard recovery criteria or
contamination limits specified above.
Any series of five consecutive R values above the mean,
or three consecutive R values outside the warning limits
for any internal standard requires that corrective action
be taken by HRMS managers to improve laboratory
performance.
Laboratory Control Samples
6.3.2.1 A pair of LCS is analyzed and associated with groups of
clients' samples, not exceeding 20 samples or within 2
weeks from the last pair of LCS analyzed.
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6.3.3
6.3.4
6.3.5
Section No . ..Q.
Revision No. 2.0
Date: 6/01/91
Page: ..Q. of ..Q.
All samples within an analytical batch are re-extracted and analyzed
if the native or internal standard recoveries from the LCS do not fall
within the acceptable control range for accuracy, or if the RPD is
greater than 50% (UCL).
6.3.3.1 A series of five consecutive %R values above the mean,
or three consecutive %R values outside the warning limits
for any native standard require that corrective action be
taken by HRMS managers to improve laboratory
performance.
Matrix Spike and Duplicate Sample Analyses
6.3.4.1
6.3.4.2
6.3.4.3
A MS, MS/MSD or duplicates are analyzed upon client
request, method requirements or at the discretion of the
Director of HRMS.
If the RPD from duplicate field samples or MS/MSD
exceeds 20 and 25% respectively, corrective action will be
taken as 'directed in the method ( e.g., EPA Method 8290
(draft))
If the RPD from sample duplicate analyses are greater
than 50% then both duplicate samples will be reanalyzed.
Quality Control Charts
Selected Quality Control charts will be generated in the near future
and handled as follows. Quality control data are recalculated on a
periodic basis by the QAU and distributed to the Director of HRMS
Services. A set of current QC Charts is kept in the HRMS Services
and Operations departments to monitor QC trends on a real time
basis. Original copies of the QC charts and any associated tabular
data are stored in the QC archives. QC control charts can be made
available upon written request of clients or regulatory agencies or
may be viewed during facility audits.
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SECTION 7.
Corrective Actions
Section No. -1..
Revision No. 2.0
Date: 6/01/91
Page: -1.. of 1
7. Corrective Actions
7.1
7.2
Instrument Calibration
HRMS operators will retune their instruments and create a new initial
calibration curve when the relative response factors from the continuing
calibration check (CCC) fall outside ±20% of the average RRF. The
operator follows trouble shooting and maintenance procedures
recommended in the instrument operating manual.
Quality Control Samples
7.2.1 Method Blanks:
When the method blanks from consecutive analytical batches exceed
acceptable limits of contamination (refer to Section 6), the Operation
department will initiate an investigation to determine the source of the
contamination. Potential sources of contamination include but are not
limited to reagents, glassware and laboratory equipment. A Corrective
Action Report is completed and filed with the QAU pending the outcome
of the investigation (Figure 7.2-A).
7.2.2 Laboratol}' Control Samples
The HRMS or LCMS Services groups will initiate method performance
studies when Laboratory Control Sample recoveries do not fall within
acceptable warning and control limits for accuracy and precision. For
example, successive LCS replicate recoveries that fall outside warning
limits are often indicative of decreasing performance trends and will be
cause to re-evaluate standard and reagent stability as well as other
potential factors. Recoveries outside of allowable control limits for
accuracy or precision may also cause laboratory management to review
chemist method performance as well as the condition of reagents,
standards or instrument calibration. The results of the investigation will be
presented in a Corrective Action Report and submitted to the QAU.
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Section No . ..1..
Revision No. 2.0
Date: 6/01/91
Page: ..1. of ..1.
FIGURE 7.2-A
CORRECTIVE ACTION REPORT
Batch ID: Sample No.: ___ _ Analtyical Method: __ _
Date Rec.: Date Prep'd.: ___ _ Date Anl.: _____ _
Description of problem or anomaly:
Reported by:. _____ _ Date:'-----
Corrective action taken:
Completed by:'-------Date:. ___ _ QAU Approval:'-----
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SECTION 8.
Review of Analytical and Quality Control Data
Section No. __§_
Revision No . ..1:Q.
Date: 4/26/93
Page: _I of i.
8. Performance and System Audits
Performance, System, and External audits are conducted to verify conformance with ALTA's
quality assurance program, to determine the effectiveness of the QA program, and to
continually improve ALTA's data quality.
8.1 Performance Audits are conducted as single blind assay samples. This
performance sample (PE) is analyzed at least once a year as part of the U.S.
EPA Water Supply (WS) study. The analyst is not provided with the
acceptable result for the PE until after the experimental result is reported.
Other externally originated PEs are analyzed when supplied by the client as
either a single blind or as a double blind sample and are scheduled through the
laboratory as routine samples.
8.2 System Audits evaluate the operational components of ALTA's QA program.
8.3
8.4
This audit is conducted on a quarterly basis, at a minimum, by the QAU.
Items audited include but is not limited to sample tracking, chain of custody
procedures, standard preparation, general laboratory equipment maintenance,
safety, method detection limit, standard operating or analytical procedures,
notebook use and maintenance, and any unique client specific data or
procedure requirements. Any problems or deficiencies are documented in a
report and are submitted to management for prompt corrective action.
External Audits are performed on an on-going basis by clients, regulating
agencies (State and Federal), or other third party auditors. These audits are
pre-scheduled with the client and QA U to ensure that the appropriate
laboratory personnel are available to address all audit inquiries. All deviations
or deficiencies noted during the audit are to be addressed in the time frame
provided by the auditor.
Data Audits at ALTA utilize a three tier data review system involving
laboratory directors, client managers and the QAU.
8.4.1 Tier 1. In the initial phase, the analyst, defined as the instrument
operator, completes final data calculations, enters the data and submits
the results to a laboratory director for review. In the case of
anomalies, the laboratory director may require the analyst to prepare a
corrective action report (CAR) discussing the potential causes for the
problems encountered as well as the recommended corrective action.
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8.5
Section No.~
Revision No . ...1&.
Date: 4/26/93
Page: ..1.. of ..i..
Both the analyst as well as the laboratory director reviewing the data
sign and date the final data sheets and any CAR's (if applicable).
8.4.2 Tier 2. The second tier review requires the project manager, defined
as the laboratory director signing the cover letter of the final report, to
review and approve the data package. The project manager examines
the data for completeness and assesses whether the package as a whole
meets the data quality objectives set by the client. The project manager
is required to discuss or explain any data anomalies in the text of the
cover letter.
8.4.3 Tier 3. The third tier review is performed by the QAU. The QAO or
staff designated by the QAO will audit approximately 5 % of the data
packages and reviews all aspects of the data package covered during the
second and third tier reviews. The QA U review may result in a
request to the laboratory director for additional information regarding
the data set and if necessary, re-analysis of selected samples.
For convenience, checklists shown in Figures 8 .4-A and 8 .4-B are used to
determine completeness of client files.
Section No . ...li.__
Revision No . .lQ..
Date: 4/26/93
Page: ..l.. of 2_
FIGURE 8.4-A
QA/QC Check-list
Completeness and Problems (rp-5/20/91)
Batch ID/Auditor/Date __________________ _
DATA FOLDER:
y N
y N
y N
y N
y N
y N
y N
y N
RAW DATA:
y N
y N
1. Client Information Page.
2. Batch Data Page.
3. Correspondence/letters/phone conversations.
4.
5.
6.
7.
8.
9.
C-O-C.
Picture.
Invoice.
Login-checklist.
Sample Inventory Sheet.
Process Sheets/Method Summaries
10. Work Sheets:
A. Standards
Y N B. Method Blanks
Y N C. LCS's/MS & MSD
Y N D. Samples
REPORT:
Y N 11. Cover Letter
12. Results
Y N A. Method Blanks
Y N B. LCS's/MS & MSD
Y N C. Samples
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FIGURE 8.4-B
QA/QC CHECKLIST
Batch Data Folder
Batch ID/ Auditor/Date
1. Completeness
a.
b.
C.
d.
e.
f.
g.
h.
sample analysis data
sample inventory
client C-O-C
benchsheet I
benchsheet II
injection log
quan file summary I & 2
I. standard quan file and chromatogram
2. sample quan file and chromatogram
3. matrix spike quan file and chromatogram
Comments:
Section No . .1...
Revision No . .1.Jl..
Date: 4/26/93
Page: ..1.. of 2._
Section No. ~
Revision No . .l.:.Q_
Date: 4/26/93
Page: ..i_ of ..i_
2. Transcription
a.
b.
C.
d.
e.
sample ID
composite weights
dates
depths
prep weights
Comments:
Batch ID/ Auditor/Date
3. Calculations
a. average response factor
b. Eq.l: % moisture
c. Eq.3: cone. (ppm)
d. Eq.2: raw cone. (ppm)
e. Eq.4: total (ug)
f. significant figures
·calculations:
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SECTIONS 9 & 10.
Instrument Maintenance Logbook & Good Laboratory Practices
Section No._9_
Revision No.-1,Q_
Date: 4/26/93
Page:_!_ of _I
9. Preventative Maintenance
Routine preventative maintenance allows the laboratory to generate a high quality of reliable
data. Preventative instrument maintenance is the responsibility of the analysts using the
instruments. Preventative maintenance and emergency repairs that cannot be performed by
ALTA are contracted out to either the instrument manufacturer or an authorized maintenance
vendor.
9.1
9.2
9.3
Instrument Maintenance Logbook are maintained for laboratory equipment
including analytical instruments, balances, freezers, refrigerators and other
equipment in operation. Each logbook contains separate sections for calibrations
(where applicable), routine maintenance, non-routine maintenance/service reports
and part numbers. Logbooks contain the instrument name, model, serial number,
SOP, operator's instrument manual, or the appropriate references to the manual.
A description of the maintenance performed, date of service or maintenance,
person preforming the service or maintenance, type and reason for service or
maintenance is recorded. When the repair or service is performed by the
manufacturer, a copy of the service record is maintained in the appropriate
logbook.
Instrument Maintenance and Repair guidelines is provided in the technical
reference or instrument manual. Typical HRMS preventative maintenance may
include but is not limited to changing the instrument septa twice daily, cleaning of
injection liner, column cutting to improve chromatography, cleaning of injection
port (weekly), syringe replacement, cleaning of filament and slits, and when
required bake-out of flight tube. An example of non-routine maintenance would
be the replacement of the flight tube when normal maintenance does not provide
the desired sensitivity and peak shape.
Spare Parts are maintained in the laboratory by the responsible person listed in the
instrument logbook. Typical spare parts for the HRMS instruments may include:
filaments, additional clean sources, spare electronic boards, ion gauges, columns,
pirani gauges, injection liners, syringes, septa, source heater, ferrules, extra fuses,
transfer lines, and inlet jets.
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Section No._!Q__
Revision No . ..:LQ_
Date: 4/26/93
Page:_!_ of _I
10. Quality Assurance Reports to'Management
Corrective Action Reports (CAR) are completed and filed with the QA U as stated in Section 7.
When the next System audit is perfonned after the filing of the CAR, QA U will investigate the
anomaly to determine if any corrective action has been instituted and will assess its effectiveness.
If the corrective action has either not been instituted or is not effective both the HRMS Director
and the President of the laboratory is notified in a written report.
Other QA reports to are issued and responses circulated to management as follows:
8.1
8.2
8.3
8.4
Perfonnance Audit results are distributed by QAU to the HRMS Director for
review and deficiency responses as requested by the submitting agency.
System Audit summaries is issued by QAU to the Laboratory President and all
effected Laboratory Directors. Each Director is given two weeks to determine the
most appropriate course of corrective action for all deficiencies or deviations noted
in the audit summary, to include revision of laboratory procedures if necessary.
External Audit summaries issued by clients or other regulating agencies for
ascertaining compliance with program specific requirements are distributed by the
QAU to the appropriate section supervisor and director for review and corrective
action response. After QA U receives acceptable corrective action responses back
for all deviations or deficiencies, a response is then written to the client or
regulating agency.
Data Audits of HRMS data are reviewed by QAU for completeness, transcription
errors, calculation errors, and operational procedures. The QA U review may
result in a request to the appropriate Laboratory Director for additional
information or corrective action.
The "Table of Contents" from ALTA Standard Operating Procedures (SOP) Manual is
presented in the Appendix. The SOP manual provides information to the general
laboratory staff for the reporting of QA activities to QAU and management as well as
instrument operating procedures.
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► SECTION 11.
Appendix
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EDUCATION
Ph.D.
B.S.
EXPERIENCE
Present
1989 -1990
1987 -1989
1986 -1987
John W. Cornacchia, Ph.D.
President
Ecology, University of California, Davis, CA (1982)
Animal Science, University of California, Davis, CA (1975)
President, ALTA Analytical Laboratory
Dr. Cornacchia is co-founder, CEO, and a member of the Board of
Directors of ALTA. He is responsible for the management of business
planning including venture funding, sales and marketing and the review of
laboratory operations. He participates in the planning of agrochemical
studies, particularly field dissipation studies and groundwater monitoring
projects.
Senior Program Administrator, Enseco-Cal Lab
Responsible for managing USEPA-FIFRA Environmental Fate Studies
conducted for Fortune 500 chemical companies and government agencies.
Also was responsible for all sales and marketing of LCMS and LCMS/MS
services for the USEPA-FIFRA pesticide residue testing market.
Director of Production Planning & Control/Director of Information
Services, Enseco-Cal Lab
Coordinated the scheduling and planning of laboratory production capacity
and managed the Information Services Group (ISG) for the largest
commercial laboratory in California. His ISG functions included the
operation of the Sample Control Department, Data Control Group and the
Computer Group. In addition, he managed analytical services programs
supporting large-scale terrestrial field dissipation studies, groundwater
monitoring investigations, and surface water surveys.
Technical Manager, Enseco-Cal Lab
Provided consultative services to agrochemical clients responding to the
California Groundwater Contamination Prevention Act (AB2021) including
the preparation of terrestrial field dissipation study reports. Managed
analytical programs in support of aquatic field dissipation studies.
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1981 -1986 Senior/Associate Environmental Specialist, Division of Water Quality,
California Water Resources Control Board.
As a member of the Pollutant Investigations Branch Special Studies Unit,
Dr. Cornacchia designed, implemented and managed large-scale pesticide
and water quality monitoriq.g projects and aquatic bioassay studies. As part
of the Pesticide Registration and Evaluation Unit/Priority Chemicals Unit,
he performed statewide chemical risk assessments of agrochemicals
including malathion, molinate, and thiobencarb.
QUALIFICATIONS
Dr. Cornacchia has over nine years of experience in environmental research examining the
fate and effects of agrochemicals in aquatic and terrestrial systems. He spent the first five
years as a regulator performing aquatic risk assessments regarding pesticide usage in
California, and the last four years developing analytical programs in support USEPA FIFRA
Environmental Fate Studies and governmei;ital water quality assessments. Many of the special
projects he directed led to the development of new agrochemical screening techniques
including solid phase extractions, GCMS-SIM methods, and most recently, LCMS and
LCMS/MS procedures. Dr. Cornacchia has in-depth experience regarding USEPA-GLP
Standards and the management of laboratory personnel.
SELECTED PUBLICATIONS & PRESENTATIONS
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"Quantitative Analysis of Pesticides by Thermospray LCMS and MS/MS," Bethem, R. A.,
Comacchia, J. W., Presented at the 38th ASMS Conference on Mass Spectrometry and Allied
Topics, June 5-10, 1990, Tucson, AZ.
"Determination of Triazine Pesticides and Degradation Products in Groundwater by
Thermospray Liquid Chromatography Mass Spectrometry," Bethem, R. A., Comacchia, J.
W., Presented at 10th Annual SETAC Meeting, Toronto, Canada (1989).
"Method Validation for Pesticide Determinatiqn in Water and Soil Using Quantitative
Thermospray Liquid Chromatography/Mass Spectrometry," Bethem, R. A., Comacchia, J. W.,
Kornfeld, R., Matusak, K., Presented at the Pittsburgh Conference, New York, New York
(1990).
Rice Herbicides: Molinate (Ordram) and Thiobencarb (Bolero), A Water Quality Assessment,"
Cornacchia, J.W., D.B Cohen, G.W. Bowes, R.J. Schnagl and B.L. Montoya. Special Projects
Report No. 84-4sp, California Water Resources Control Board.
PROFESSIONAL AFFILIATIONS
American Chemical Society
EDUCATION
B.S.
EXPERIENCE
Present
1986 -1990
1979 -1986
1974 -1979
'William J. Luksemburg
Director of HRMS Services
Chemistry, California State University, Fresno, CA (1974)
• Director of HRMS Services, ALTA Analytical Laboratory
Mr. Luksemburg, a co-founder, directs the routine analysis and method
development work in the High Resolution Mass Spectrometry department.
He is responsible for marketing HRMS dioxin services to environmental
engineering firms, the pulp and paper industry, government agencies and
other industrial clients. Mr. Luksemburg is also responsible for the
development of new markets using HRMS instrumentation. In addition,
Mr. Luksemburg directs routine and special projects, review and interpret
data, and interface with clients.
Principal Scientist/HRMS Manager, Enseco-Cal Lab
As Principal Scientist in the Special Services department at Enseco-Cal Lab
Mr. Luksemburg coordinated the operation and maintenance of five high
resolution magnetic sector instruments. He was responsible for developing
a business that now is one of the major suppliers of HRMS PCDD/PCDF
analysis to the pulp and paper industry in the U.S. Mr. Luksemburg also
coordinated the training and development of the staff in the operation and
maintenance of HRMS instruments.
Senior Chemist, Radian Corporation
.In Radian's Sacramento laboratory, Mr. Luksemburg was GC/MS
supervisor for ABN and VOA analysis. He coordinated the activities of
five chemists in the operation and maintenance of four quadrupole mass
spectrometers.
Chemist, Carnation Company
As a staff chemist, Mr. Luksemburg was involved in the analysis of
products and ingredients used in Carnation's animal feed division.
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QUALIFICATIONS
Mr. Luksemburg has over 14 years experience in production analytical laboratories including
IO years experience in the field of environmental mass spectrometry. Much of this
experience has involved PCDD/PCDF analysis of environmental samples and for the last four
years has concentrated on High Resolution Mass Spectrometry analysis of PCDD's/PCDF's in
a variety of matrices. Mr. Luksemburg is recognized through-out the pulp and paper industry
for his research and production work on dioxins and furans. He recently was recognized on
the international level when his chapter on dioxin analysis of pulp and paper (Rappe, 1990),
was published by the World Health Organization. He is one of the few individuals in the
world to successfully adapt the high resolution magnetic sector instruments to "production"
analysis of environmental samples at the picograrn and femtograrn levels.
RECENT PRESENTATIONS
"Determination of Method Detection Limits in Pulp and Pulp Mill Effluents," in Rotorua,
New Zealand, at the ISWPC Post Symposium Workshop, May 1991.
PUBLICATIONS
NCASI Technical Bulletin No. 551, "NCASI Procedures for the Preparation and Isomer
Specific Analysis of Pulp and Paper Industry Samples for 2,3,7,8,-TCDD and 2,3,7,8-TCDF,"
LaF!eur, L., Ramage, K., Bousquet, T., Brunck, R., Luksemburg, W., Miille, M., Peterson, R.,
and Valrnores, S., (1989).
"Optimization of Extraction Procedures for the Analysis of TCDDffCDF in Pulp, Paper Base
Stocks, and Pulp Industry Solid Wastes," Lafleur, L., Ramage, K., Gillespie, W.,
Luksemburg, L., Miille, M., and Valrnores, S., Chemosphere, Vol. 19, pp 643-648, 1989.
"Analytical Procedures for the Analysis of TCDD and TCDF in Food Sources," LaF!eur, L.,
Bousquet, T., Ramage, K., Davis, T., Luksemburg, W ., and Peterson, R., Presented by L.
Lafleur at Dioxin '89, Toronto, Canada. Waiting publication in Chemosphere.
"Determination of Polychlorinated Dibenzo-p-Dioxins and Polychlorinated Dibenzofurans in
Pulp and Paper Industry Wastewaters, Solid Wastes, Ashes and Bleached Pulps,"
Luksemburg, W., Environmental Carcinogens-Methods of Analysis and Exposure
Measurement-Volume II. Christopher Rappe, Editor, 1991.
PROFESSIONAL AFFILIATIONS
American Society for Mass Spectrometry
American Chemical Society
Technical Association of the Pulp and Paper Industry
EDUCATION
Robert A. Bethem
Director of LCMS Services
B.S. Chemistry, Antioch College, Yellow Springs, OH (1978)
EXPERIENCE
Present Director of LCMS Services, ALTA Analytical Laboratory
Mr. Bethem is a co-founder and member of the Board of Directors of
ALTA. He initiates and manages all method development and routine work
by Liquid Chromatography Mass Spectrometry (LC/MS), and tandem mass
spectrometry, (MS/MS).· He is responsible for the development of novel
methods for the trace analysis of pesticides in water and soil by LCMS. In
addition to his role in LCMS analysis, he is responsible for the application
of GC/MS/MS techniques for the trace analysis of organic compounds in
complex matrices.
1987 -1990 Principal Scientist/LCMS Manager, Enseco-Cal Lab
Created and managed the LCMS Services Department and provided
pesticide analysis services for industry and government Developed and
marketed several trace methods by GC/MS/MS. Supervised extraction and
instrument personnel and was responsible for the final review and
processing of all data. Coordinated and maintained two Finnigan MAT
TSQ-70' s and developed software for automated analysis.
1984 -1987 International Field Engineer, Finnigan MAT
Performed mass spectrometer applications and engineering support for the
Pacific Operations Centers in China and South America. Provided
applications and technical support to several large USEPA contract
laboratories.
1982 -1984 Manager of Mass Spectrometry, Cambridge Analytical Assoc.
Organized and maintained the GC and GCMS laboratories for EPA and
NIOSH protocol analysis. Supervised GC and GCMS personnel and was
responsible for final data review and report generation.
1978 -1982 Research Assistant, Massachusetts Institute of Technology
Provided low and high resolution analyses on several instruments using a
variety of ionization techniques at the N.I.H. facility for Mass Spectrometry.
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QUALIFICATIONS
Mr. Bethem has accumulated over 12 years of experience in mass spectrometry at a variety of
research and production environments. He has recently pioneered the application of
Thennospray LCMS to the quantitative analysis of pesticides and has demonstrated its ability
to produce superior data quality in actual field studies. Recent work and publications have
established him as one of the leaders in this field .. He is a current member of the Joint Task
Group of "Standard Methods for the Examination of Water and Wastewater" for the
development of new LCMS methods. Mr Bethem has an extensive background in biological
and environmental analysis. As a result of his work with an instrument manufacturer, he has
also developed a high degree of proficiency with software, electronic, and electro-mechanical
devices.
PUBLICATIONS
"Thennospray MS and MS/MS of Polar, Urinary Metabolites and Metabolic Conjugates,"
Draper, W. M., Brown, F. R., Bethem, R. A., Miille, M.J., Biomed Environ. Mass Spectrom.
1989, 18, 767.
"Anion Exchange Thennospray Tandem Mass Spectrometry of Polar Urinary Metabolites and
Metabolic Conjugates," Draper, W. M., Brown, F. R., Bethem, R. A., Miille, M.J., Liquid
Chromatog./Mass Spectrom.: Applications in Agricult, Pharm., and Environ. Chem., Mark A.
Brown, Editor, 1990.
"The Application of Tandem Mass Spectrometry to Environmental Measurements," Finnigan,
R., Poppeti, J., and Bethem, R., (In Press).
"Quantitative Analysis of Pesticides by Thennospray LCMS and MS/MS," Bethem, R. A.,
Comacchia, J. W., Presented at the 38th. ASMS Conference on Mass Spectrometry and Allied
Topics, June 5-10, 1990, Tucson, AZ.
"Determination of Triazine Pesticides and Degradation Products in Groundwater by
Thennospray Liquid Chromatography Mass Spectrometry," Bethem, R. A., Comacchia, J.
W., Presented at 10th Annual SETAC Meeting, Toronto, Canada (1989).
"Method Validation for Pesticide Determination in Water and Soil Using Quantitative
Thermospray Liquid Chromatography/Mass Spectrometry," Bethem, R. A., Comacchia, J. W.,
Kornfeld, R., Matusak, K., Presented at the Pittsburgh Conference, New York, New York
(1990).
PROFESSIONAL AFFILIATIONS
American Society for Mass Spectrometry
American Chemical Society
Joint Task Group -"Standard Methods for the Examination of Water and Wastewater"
EDUCATION
B.A.
B.A.
EXPERIENCE
Present
1989 -1990
1988 -1989
1986 -1988
Robert S. Mitzel
Director of Air Toxics
Chemistry, Chico State University, Chico, CA (1982)
Biology, Chico State University, Chico, CA (1982)
Director of Air Toxics, ALTA Analytical Laboratory
Mr. Mitzel, a co-founder, manages production scheduling and client
managing for the Air Toxics group. He is also responsible for the final
review and interpretation of analytical data and final reports. In addition,
he serves as a marketing-agent for Air Toxic Services and development of
new Air Toxic markets.
Director of Mass Spectrometry, Enseco-Cal Lab
Directed five supervisors and 42 chemists in the GC/MS group. He was
responsible for extractions, analyses, final review and processing of all data
generated by the group. Served as project manager for selected accounts
focusing on priority pollutants and dioxin/furans. His accomplishments
included generating and managing a $7 million dollar production group in
1989. Mr Mitzel served as the focal person for the Air Toxic program at
Enseco-Cal Labs for mass spectrometry methods on Modified Method 5
(MM5) sampling trains.
Mass Spectrometry Lab Manager, Enseco-Cal Lab
Managed the mass spectrometry group through four supervisors and assisted
daily operations for the VOA, BNA, Dioxin, and extraction groups. He
also assisted development efforts for new GC/MS methods including
isotope dilution techniques for the analysis of polynuclear aromatic
hydrocarbons from the Exxon-Valdez oil spill.
GC/MS Dioxin Lab Manager, Enseco-Cal Lab
Initiated and managed the method development and routine analysis of
dioxin/furan samples. Collaborated with the USEPA for the development
of EPA Method 8280, and developed isotope dilution methods for
polychlorinated biphenyls, polynuclear aromatic hydrocarbons,
chlorobenzenes, and chlorophenols. He collaborated with the California Air
Resource Board with the development of Method 428 and 429, which are
now part of AB 2588 (Air Toxics "Hot Spots" Information Assessment Act
of 1987).
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1983 -1985
1982 -1983
GC/MS Supervisor, Enseco-Cal Lab
Managed the production night shift for the VOA, BNA, and Dioxin GCMS
groups.
Staff Chemist, California Analytical Laboratory
Conducted specialized and routine analyses for volatiles, semi-volatiles, and
dioxins. He operated several Finnigan MAT mass spectrometers including
the: OW A, 1020, 5100, 3200, 4500, TSQ-4500, TSQ-4600, and Incos 50.
Staff Chemist, California Analytical Laboratory
Mr. Mitzel conducted specialized and routine extraction and clean-up
methods for volatiles, semi-volatiles, and dioxins.
QUALIFICATIONS
Mr. Mitzel has over 11 years of experience in the environmental services business. ·He ' participated in the early development of novel techniques for the extraction and analysis of
2,3,7,8-TCDD and was instrumental in developing a multi-million dollar dioxin program for
Enseco, Cal Labs. He has since expanded the use of isotope dilution techniques for several
other compounds in a variety of complex environmental matrices. Mr. Mitzel has extensive
experience managing a large production groups in an environmental laboratory .
PUBLICATIONS
"Photolysis of Octachlorodibenzo-P-Dioxins on Soils: Production of 2,3,7,8-TCDD," Miller,
G., Herbert, V.R., Miille, M.J., Mitzel, R., Zepp, R.G., Chernosphere, 18, 1265-1274, 1989.
AWARDS
Graduated Cum Laude with honors in Biological Sciences
Botanical Society Award
PROFESSIONAL AFFILIATIONS
American Chemical Society
EDUCATION
M.S.
B.S.
EXPERIENCE
Present
1988 -1990
1987 -1988
Robert G. Peterson
Director of Technical Services
Chemistry, California State University, Sacramento, CA (1982)
Chemistry, California State University, Sacramento, CA (1975)
Director of Technical Services, ALTA Analytical Laboratory
Mr. Peterson is a co-founder and responsible for assisting in the resolution
of technical problems and development of solutions to new sample
preparation obstacles. Focuses on existing and future analytical methods.
Additionally, he functions as a focal point for Research & Development
efforts whether they are client or scientifically oriented.
Principal Scientist, Manager, Dioxins/Furans, Enseco-Cal Lab
As a Principal Scientist, Mr. Peterson was involved in developing new
methods, refining and troubleshooting existing methods, and aiding in
problem solving within the Special Services Group (Dioxins and Furans
analysis). Because of his unique cross-disciplined experience and
education, Mr. Peterson was frequently called upon as a primary scientific
resource for other organic and inorganic projects. He also served as Client
Manager for selected major accounts.
As a Manager, Mr. Peterson was responsible for the staff, production, and
resource allocations for the two Dioxin Preparations Laboratories. One lab
was devoted to prep for High Resolution dioxin/furan analyses and the
other was devoted to Low Resolution dioxin/furan analyses. His staff
consisted of 2 supervisors and 15 chemists/analysts.
Director of Inorganic Services, Enseco-Cal Lab
Directed all aspects of the lnorganics Department, including guiding the
Department to meet existing and projected business and technical goals. He
also served as Client Manager for selected major accounts.
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1980 -1982
1979 -1980
1976 -1979
' Organics Preparation Manager, Enseco-Cal Lab
Mr. Peterson not only managed the Organic Preparation Group, he was
directly involved in the creation and subsequent management of the Dioxin
Preparation Lab and the S!3-Ildards Preparation Group, which resulted in
upgraded laboratory QA/QC traceability and verification of standards. In
this capacity, he was responsible for the mobilization of resources to meet
test requests and time constraints, and was the liaison between the groups
and Client Managers for efficient coordination of work flow. He also
served as Client Manager to clients with organic analysis requests.
Senior Staff Chemist, California Analytical Laboratory
In this position, Mr. Peterson performed extractions, concentrations and
clean-ups on environmental samples of a diverse nature for organic
analytes.
Chemist, Sacramento County Water Quality Control Laboratory
Conducted inorganic and organic analysis of waters, sludges and sediments
pertinent to wastewater treattnent.
Chemist, Morse Laboratories
' Mr. Peterson conducted inorganic analysis of waters, sediments and crop
samples. He also served as Organics Lab Supervisor of satellite extractions
and clean-up laboratory.
QUALIFICATIONS
Mr. Peterson has a wide range of technical and management experience. His knowledge of
analytical chemistry covers a spectrum of cross-disciplines and he can provide expert
assistance in special organic and inorganic proj~ts. He is also an experienced teacher and
trainer. He presently coordinates and conducts an ongoing class, which is part of the
Hazardous Materials Certification Program at the University of California Extension, Davis
campus.
RECENT PRESENTATIONS
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(2)
"Quantitative Analysis and Practical Laboratory Techniques," University of California
Extension, Davis (1983 to present). Currently being taught Spring, Summer, Fall &
Winter quarters.
Hazardous Waste Analysis Seminar for J.H. Kleinfelder (1986).
(3) Hazardous Waste Analysis Seminar for Dames & Moore (1987).
(4)
(5)
(6)
(7)
"Training Program on Pesticide Residue Analysis" in Bangkok, Thailand for The
World Bank/UNIDO/UNDP/DOA, November 1987.
"Overview of Analytical Techniques for Pesticide Studies" as part of "Pesticides in
Soil and Groundwater," University of California Extension, Davis (1988).
"Analytical Techniques" as part of "Principles of Hazardous Materials Management,"
University of California Extension, Davis (1989, 1990, 1991, 1992).
"The Environment: Air and Water Quality, Land, Safety, Health and Proposition 65"
as part of "Advanced Executive Program," University of California Extension, Davis
(1990).
PUB LI CA TIO NS
"Cl5-Cl8 Isomers Synthesized from [13C]-2,3,7,8-Tetrachlorodibenzofuran via Surface
Chlorination," Bulletin of Environmental Contamination and Toxicoloe:y (1987).
NCASI Technical Bulletin No. 551, "NCASI Procedures for the Preparation and Isomer
Specific Analysis of Pulp and Paper Industry Samples for 2,3,7,8-TCDD and 2,3,7,8-TCDF,"
LaFleur, L., Ramage, K., Bousquet, T., Brunck, R., Miille, M., Luksemburg, W., Peterson, R.,
Valmores, S. (1989).
"Analytical Procedures for the Analysis of TCDD and TCDF in Food Sources," LaFleur, L.,
Bousquet, T., Ramage, K., Davis, T., Luksemburg, W., and Peterson, R.. Presented by L.
LaFleur at Dioxin '89, Toronto, Canada. Waiting publication in Chemosphere.
"Supercritical Fluid Extraction and Solid Phase Extraction Techniques Applied to the Analysis
of Pulp and Paper Mill Effluents for 2,3,7,8-Tetrachlorodibenzo-p-dioxin and 1,2,7,8/2,3,7,8-
Tetrachlorodibenzofuran," Peterson, R.G., Luksemburg, W.J., Hedin, J., Silverbush, B., Werst,
M., Maloney, N. Presented at the Research and Technology Transfer Conference, Toronto,
Ontario (1992).
PROFESSIONAL AFFILIATIONS
American Chemical Society
AWARDS
"Excellence in Teaching and Outstanding Service Award," University of California, Davis
(1989).
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EDUCATION
B.S.
EXPERIENCE
Present
1987-1990
1984-1987
Scott N. Jimison, CPA
Chief Financial Officer
Accounting/MIS, California State University, Sacramento, CA (1984)
Chief Financial Officer, AL TA Analytical Laboratory
Mr. Jimison is a co-founder and director of ALTA. In conjunction with the
CEO he is responsible for business planning, venture funding, and strategic
management His daily financial activities include preparation and analysis
of all financial data, forecasting, cash flow, instrument financing, inventory
control, client cost tracking, and risk management In addition to Mr.
Jimison's financial responsibilities, he manages the sample control
department and management information systems group.
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Director of Finance and Administrative Services, Enseco-Cal Lab
Mr. Jimison was responsible for all key financial activities including:
financial reporting, client project analysis, budgeting, asset financing,
purchasing, receiving and facility expansion. Mr. Jimison's
accomplishments include the installation, development, and maintenance of
the current financial system. In addition, Mr. Jimison managed the
construction of a 1,000 foot Chromatography prep lab, installation of
HV AC systems and completion of safety related building improvements.
Senior Auditor and Tax Accountant, Tonche Ross & Co.
Performed all aspects of audit services including audit planning, audit
supervision, client advisory services, and financial reporting. Tax services
included preparation of corporate, partnership, and personal tax returns
including tax planning and small business development In addition, Mr.
Jimison performed SEC reporting including !OK's, IOQ's, & 8K's.
QUALIFICATIONS
Mr. Jimison has accumulated knowledge in many phases of the environmental laboratory
business. His background enables him to provide services to develop the financial strength of
Alta, manage support groups to provide the best possible client service, and provide risk
management services to ensure Alta and its clients are properly insured against unforseen
loses. In addition, Mr. Jimison has the capability to provide a great deal of client financial
management services. With his experience as a CPA he has developed the understanding of
many business structures and the necessity for detailed financial data a client demands.
Sharon K. Pierson
Quality Assurance Officer and Safety (QAO)
EDUCATION
B.S. Biological Sciences, University of the Pacific, Stockton, CA (1978)
EXPERIENCE
Present Quality Assurance Officer and Safety, ALTA Analytical Laboratory
As Quality Assurance Officer (QAO) oversees the laboratory's compliance with
ALTA's Quality Assurance Program Plan (QAPP), Standard Operating
Procedures (SOPs), USEPA Good Laboratory Practices (OLP) and any client
specific QA programs.
As Safety Officer, is responsible for the laboratory and facility safety program
and the management of hazardous materials and their disposition.
3/91 -10/91 Laboratory Manager, Roy F. Weston (Formerly Canonie Environmental
Services)
Upon sale of the Canonie Stockton laboratory to Weston, became Laboratory
Manager being responsible for the entire laboratory. Responsibilities included
management of analytical production, data validation of in-house and outside
client data, quality assurance, LIMS implementation, development of fiscal
budget and equipment expenditures, and professional staffing. Major clients
included several in the federal sector and other environmental consulting firms.
6/90 -3/91 Operations Manager, Canonie Environmental Services
Managed 40 chemists and technicians in a full service analytical laboratory.
Responsibilities included management of analytical production, projects, data
validation, finances, and hiring and reviewing personnel. Primary client base
was Canonie Environmental Services projects.·
3/89 -6/90 Client Service Coordinator, Radian Corporation, Radian Analytical
Services
Liaison between the laboratory and several large environmental clients.
Relayed information regarding laboratory capabilities, turnaround-times, price
quotations, preliminary data reports, data interpretation, and addressed any data
quality issues. Clients' base was both in-house and local environmental firms.
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9/88 -3/89 Project Administrator, Canonie Environmental Services
Established Project Administration program at Canonie. Responsibilities
included responding to inquiries regarding the laboratory's analytical
capabilities, turnaround-time, and pricing analytical analyses. Assisted
Operations Manager with workload projections for large engineering projects
requiring analytical services, helping in the preparation of site-specific Quality
Assurance Project Plans (QAPPs) and data review.
7/87 -8/88 Quality Assurance Officer, Canonie Environmental Services
Developed and maintained a fully integrated computerized database for tracing
quality control data, generated in all analytical departments of the laboratory.
Assisted the engineering staff during the preparation of site-specific QAPPs and
Data Quality Objectives.
10/83 - 7 /87 Staff Scientist, Canonie Environmental Services
As part of the GC/MS department was responsible for the operation and
maintenance of a Hewlett Packard 5970 GC/MSD with RTE-A data system for
the analysis of volatile organic' in various matrices according to EPA
methodology and the Contract Laboratory Program. Other areas of experience
and responsibilities at Canonie ,included supervising three chemists and two
technicians for analysis of volatile organic chemicals by automated purge and
trap gas chromatography in all matrices as per EPA, CA DOHS, and RWQCB
methodologies, conducting inorganic analysis by gravimetric and titrametric
methods and the use and application of safety equipment for workers during
hazardous waste site remediation.
2/82 -3/83 Field Investigator, California Department of Health Services
Compiled an inventory of hazardous waste sites in both San Joaquin and
Stanislaus counties for the California Department of Health Services
Abandoned Site Program.
QUALIFICATIONS
Ms. Pierson has over 9 years of experience in environmental analysis of both organic and
inorganic parameters in a variety of matrices. While at Canonie Environmental she help
implement a computerized database for monitoring quality control data in a full service
analytical laboratory and assisted in the development of Quality Assurance Project Plans. As
a Project Administrator and Client Services Coordinator Ms. Pierson has experience acting as
a liaison between the laboratory and client to allow the efficient coordination and
communication of project needs and data quality objectives. Ms. Pierson management
experience include the development of a fiscal budget for a full service analytical laboratory,
instrumentation purchase, and staff review and hires.
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TABLE OF CONTENTS
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Section I. Introduction
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I Section II. Analytical Services
I Section III. Facility
I Section IV. Equipment
I Section V. Quality Assurance -Section VI. Project Experience
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I Section VII. Appendix
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ft SECTION I.
Introduction
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INTRODUCTION
Alta Analytical Laboratory (ALTA) was formed in 1990 and is a privately held California
corporation employing a staff of over 20 scientists. AL TA' s primary mission is to provide
state-of-the-art mass spectrometry services to various industrial, consulting and governmental
clients. ALTA operates with the intent of providing data of highest quality, responsive service
and short turnaround time.
ALTA has within three years grown to a company with an expanding national and
international client base of over 400. This tremendous growth is attributable to the reputation
AL TA has gained in performing difficult trace level analyses reliably for the pulp and paper,
air toxics consulting and the agrichemical industries. ALTA's expertise lies in the analysis of
semivolatile organic compounds such as Dioxin/Furans (PCDD/Fs), Polynuclear Aromatic
Hydrocarbons (PAHs), Poly Chlorinated Biphenyls (PCBs), Chlorobenzenes, Chlorophenols,
other semivolatile compounds (8270 list) and select pesticides and herbicides.
ALTA's founders and technical staff represent a unique and highly experienced group of mass
spectrometry specialists. This strength in experience has enabled AL TA to provide
project/client specific method development and technical consulting unsurpassed in the
industry. AL TA staff have provided guidance to the government agencies responsible in the
development of USEPA Methods 8290, 1613A and California Air Resources Board (CARE)
Methods 428 and 429.
AL TA has actively participated in interlaboratory round robin studies and certification
programs such as the USEPA (ITD) study of PCDD/PCDFs in effluents; Radian Corporation
study of PCDD/PCDFs in soils; Environment Canada studies on Dioxin precursors DBD &
DBF, PCDD/PCDFs in air, PCDD/PCDFs in pulp and paper; Cambridge Isotopes Lab (CIL)
study on Coplanar PCBs and PCDD/PCDFs in fish; the National Council for Air and Stream
Improvement (NCASI) lab certification program study and the NCASI\USEP A variability
study on PCDD/PCDFs in pulp and paper. .
ALTA participates in the USEPA Special Analytical Services Program (SAS) on a regular
basis primarily in the area of PCDD/PCDFs analysis in difficult matrices. ALTA currently
holds two CARE contracts for the analysis of PCDD/PCDFs, PAHs, PCBs and other
semivolatile compounds in air samples.
ALTA is also committed to internally funded research and new method development. ALTA
has recently developed and presented papers on Solid Phase Extraction and Supercritical Fluid
Extraction of Dioxins in effluents.
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Oualitv is of paramount concern in the analytical industry today. In light of this, ALTA has
• implemented three company standards:
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ALTA will maintain a laboratory Quality Assurance Program
compliant with USEPA Good Laboratory Practice Standards
( 40 CFR sec. 160)
Laboratory Quality Control samples will be analyzed at a
frequency in excess of 15%. Internal standard and laboratory
control spike recoveries will meet or exceed method recovery
criteria or sample batches will be rerun at no additional charge
to our clients.
The routine turnaround time from sample delivery to generation
of a final written report will be 21 days.
In order to give an overview of Alta Analytical Laboratory, this Statement of Qualifications is
organized into sections on Analytical Services, Facility, Equipment, Quality Assurance and
Project Experience. Resumes for key technical staff can be found in the Appendix.
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SECTION II.
Analytical Services
ANALYTICAL SERVICES
ALTA analytical services can be divided into two groups -HRMS/LRMS and LCMSIMS.
HRMS/LRMS SERVICES -
The trend in environmental legislation and regulation over the last decade has been
increasingly driven by attempts to measure the impact of any exposure to the population via
risk assessments. For these studies to have meaning, it has been necessary in many cases to
be able to detect hazardous compounds at significantly lower levels. In the area of
Dioxins/Furans, Coplanar PCB' s and Polynuclear Aromatics, the necessary detection levels
have resulted in the need for superior instrumentation. High Resolution Mass Spectrometry
has become the most suitable analytical technique to fill this need.
ALTA's HRMS/LRMS group uses 3 magnetic sector double focusing VG High Resolution
Mass Spectrometers. The two model VG70SE's and the more recently acquired VG Autospec
typically enable ALTA to provide the lowest detection limits in the industry. ALTA has
experience in analyzing a wide variety sample types and matrices for Dioxins/Furans, PAH's,
PCB' s, Coplanar PCB' s, and selected other semi volatile organic compounds. Some typical
sample sources and types analyzed at AL TA are listed below:
Biological samples (fish, tissue, birds, clams, mussels, crayfish)
Environmental samples such as waters, soils
Foodstuffs and food packaging
Fuel oils
Human blood and tissue
Industrial waste samples (sludges, effluents, fly ash, still bottom)
Pulp and paper industry products, byproducts and wastes
Stack source emmisions (MMS train) from the following sources:
· · • cement kilns
• diesel fired boilers
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hazardous waste incinerators
medical waste incinerators
municipal waste incinerators
oil fired boilers
waste to energy plants
wood fired boilers
Ambient air studies (PUF, PUF/XAD2 sandwich)
• investigations
• remediation sites
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ALTA has the capability to perform all existing USEPA, CARE and NCASI methods for the
determination of dioxins/furans, PCB' s, P AH' s, chlorobenzenes and chlorophenols and other
selected organic contaminants by High or Low Resolution Mass Spectrometry. ALTA also
specializes in the development of new sample preparation techniques which enable ultra-low
level detection of semivolatile organics in complex sample matrices. The following tables list
methods performed routinely by the ALTA HRMS/LRMS group.
TABLE 1. -Methods Performed by ALTA HRMS/LRMS Group
USEPA 1613A S,E,Sl,T,W X
USEPA 8290 P,Sl,E,S,T,W,Fo,Sb X
USEPA 8280 S,W,Fa,Fo,Sb ' X
USEPA 613 w X
USEPA 513 w X
NCASI 551 P,Sl,E,S,W ,Fa X
NCASIPCDD P,S1,E,S,W ,Fa ' X
WHO P,Sl,E,S,W ,Fa X
USEPA 23 MM5 X
USEPA TO9 PUF X
USEPA TO13 PUF or MM5 X
CARB 428 MM5 X X
CARB 429 MM5 X
ALTA Custom Methods All X X X X
Sample Matrix key:
E = Effluent S Soil
Fa Fly Asb Sb Still Bottom
Fo Fuel Oils SI = Sludge
p = Pulp/paper T = Tissue
MM5 JvlM.5 Train air sample PUF Polyurethane foam plug air sample
TABLE 2. -Typical Dioxin/Foran Detection Limits using HRMS and LRMS
EPA Method 23 HRMS MM5 1-5 2-20 50
pg/smpl pg/smpl pg/smpl
CARB Method 428 HRMS MM5 1-5 2-20 50
pg/smpl pg/smpl pg/smpl
CARB Method 428 LRMS MM5 100 500 1000
pg/smpl pg/smpl pg/smpl
EPA Method TO-9 HRMS PUF 1-5 2-20 50
pg/smpl pg/smpl pg/smpl
EPA Method 8290 HRMS SOLIDS 0.2-0.5 PPT 1-5 10
PPT PPT
EPA Method 1613A HRMS EFFLUENTS 5 25 50
/WATERS PPQ PPQ PPQ
EPA Method 1613A HRMS PULP 0.5 2.5 5
PPT PPT PPT
TABLE 3. -Typical Reporting Limits for PAHs and PCBs
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EPA Method TO-13 HRMS MM5 orPUF 5-10
(for PAHs)
EPA Method TO-13 LRMS MM5 or PUF 100-200
(for PAHs)
CARB Method 429 HRMS MM5 5-10
(for PAHs)
CARB Method 429 LRMS MM5 100-200
(for PAHs)
CARB Method 428 HRMS MM5 1-5
(for PCBs)
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LCMS & LCMS/MS SERVICES -
AL TA offers both routine analyses and method development services for pesticide residue and
pharmaceutical studies utilizing Liquid Chromatography Mass Spectrometry (LCMS) with
Thermospray (TSP), Electrospray (ESI) and Atmospheric Chemical Ionization (APCI)
interfaces. ALTA also offers Tandem Mass Spectrometry in conjunction with liquid
chromatography (LC/MS/MS) using TPS, ESI, and APCI.
The development of new LCMS instrumentation has moved this technique from the research
environment into field monitoring programs: In addition to the advantages of LCMS when
analyzing non-volatile or thermally labile compounds, the increased sensitivity and selectivity
derived from LCMS is useful when low detection limits are required and sample amounts are
limited.
The application of MS/MS to the soft ionization characteristics of any of these liquid
chromatography interfaces results in a powerful analytical tool. LC/MS/MS techniques
provide the pesticide residue chemist with streamlined sample preparation, structural
confirmation and excellent detection limits.
The sensitivity and selectivity of LC/MS/MS methods produce sample preparation procedures
requiring limited clean-up. Costs for multi-analyte screens using LC/MS/MS are similar to
those involving conventional LC or GC methods due to the resulting high sample throughput.
This is particularly true if the equivalent conventional method requires more than one
instrument type or involves lengthy clean-up procedures.
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SECTION III.
Facility
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FACILITY
ALTA's operations are housed in an 11,000 square foot custom designed laboratory located in
El Dorado Hills California, 25 miles east of downtown Sacramento. ALTA's laboratory was
initially completed in December 1990 and a 2,500 sq. ft. expansion completed in April 1993.
The facility features:
• Large sample log-in and sample storage areas including a walk-in
freezer and walk-in refrigerator. Sample Control freezers and
refrigerators are continuously monitored for temperature by an Omega
5000 data logger. The data logger has a local alarm and is remotely
monitored during non business hours ensuring that laboratory personnel
will be notified in the event of a refrigerator or freezer failure.
• 5 separate sample preparation laboratories are designed to maximize
throughput and minimize sample cross contamination. Each lab is
windowed and spacious to provide chemists with a safe and high
capacity work environment. Sample preparation capabilities include
sample grinding and drying, MM5 air train preparation, supercritical
fluid extraction, biological tissue processing and soil core subsampling .
• An open floor plan, 2,000 square foot instrument operations room.
Accommodating 3 magnetic sector instruments and 3 triple stage
quadrupole instruments, this design facilitates communication between
instrument analysts. Instrument coolers are remotely located and pump
emissions are evacuated to minim\ze noise and maintain safe working
conditions.
• Separate Data Review carols and offices. Areas adjacent or proximal
to the instrument operations room allow analysts to access and review
instrument generated data in quiet; spacious conditions.
• Separate Quality Assurance data review office and separate Data
Archive Room designed to meet USEPA Good Laboratory Practices
standards regarding data security.
In August 1992 ALTA opened an East Coast satellite office in Newburyport, MA. Its
function is to provide ALTA a regional presence to better develop ties and improve service to
existing and potential Eastern U.S clients.
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SECTION IV.
Equipment
EQUIPMENT
ALTA utilizes state-of the-art magnetic sector or triple stage quadrupole mass spectrometers.
Each instrument is fully automated for 24 hour operations. Data can be off-loaded to stand-
alone computers for data processing and review or directly uploaded into the laboratory
information management system (LIMS).
Sample preparation capacity is large with over 60 soxhlet extractor positions and 15 rotary
evaporators. 17 fume hoods each surrounded by open bench space are positioned throughout
the preparatory labs.
Below is listed a description of the laboratory equipment:
HRMS Analytical Instrumentation -
CTC Autosampler Model A200S (3)
DEC Vaxstation 3100 w/Opus Data System (3)
DEC Vaxstation 4000 w/ Opus Data System (2)
Neslab HX200 Water Cooler (2)
Neslab HX500 Water Cooler (1)
VG 70SE High Resolution Double Focusing Mass Spectrometer (2)
VG Autospec High Resolution Mass Spectrometer (1)
LRMS Analytical Instrumentation -
CTC Autosampler Model A200S (2)
DEC Vaxstation 2100 w/ Utrix-32 Operating System (2)
DEC Vaxstation 5000 (1)
Finnigan MAT APCI/ESI Electrospray LCMS interface (1)
Finnigan MAT TSP-2 Thermospray LCMS interface (2)
Finnigan MAT TSQ-700 (3)
Waters Model 510 HPLC Pump (1)
Waters Model 590 MS Liquid Chromatograph (1)
Waters Model 600 MS Liquid Chromatograph (3)
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Sample Preparation Equipment -
4 ft. fume hoods (I)
6 ft. fume hoods (3)
8 ft. fume hoods (13)
Berke! Scharfen Food Slicer (1)
Buchler Rotary Evaporator (15)
Electrothermal Electromantle 6 sample capacity (10)
Electrothermal Electromantle 3000 mL capacity (6)
Fischer Scientific Model A-160 Analytical Balance (1)
Fischer Scientific Model XL-3000 Top Loader Balance (I)
IEC Centra - 8 Centrifuge (1)
Lab Line Model 3590 Orbit Shaker (I)
Neslab Coolflow CFT-33 Cooler (5)
Organomation 24 Station N-EV APorators (4)
Supercritical Fluid Extractor -Isco-2300 (1)
Thomas Grinder ( 1)
Thermolyne 1400 Furnace Kiln
VWR 1320 Oven (3)
Zymark Turbo Evaporator (I)
Data Management and Report Production Equipment -
ALTA uses Netware 386 and a Paradox based PC LIMS system
Canon Fax-L770 Facsimile
Concentrator (1)
HP Laser Jet II Printer (1)
HP Laser Jet IID Printer (1)
HP Laser Jet IDP Printer (1)
HP Laser Jet IV Printer (2)
Kodak Ektaprint 90E Photocopier
Modem Server (1)
Network Server (1)
Personal Computer 386/16 (2)
Personal Computer 386/20 (3)
Personal Computer 386/33 (2)
Personal Computer 486/33 (7)
Sample Storage Equipment -
Freezer 2-door 50 sq.ft. capacity (1)
Freezer 3-door 68 sq. ft. capacity (1)
Freezer Walk-in 1150 sq. ft. capacity (1)
Omega 5000 Temperature Logger (1)
Refrigerator 1-door 20 sq. ft. capacity (3)
Refrigerator 2-door 50 sq. ft. capacity (3)
Refrigerator Walk-in 430 sq. ft. capacity (1)
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SECTIONV.
Quality Assurance
QUALITY ASSURANCE
The AL TA Quality Assurance Program has been designed to ensure that our laboratory
reports meet or exceed the minimum data quality objectives stipulated in our client's project
plans or the applicable method.
. Basic laboratory systems, including personnel training, analytical standards management, and
equipment operation are documented by Standard Operating Procedures (SOP's) in strict
accordance with USEPA Good Laboratory Practices. Additional project or study specific QC
options are available upon request Based on the three tier approach described below, AL TA
conducts a comprehensive QA Program that goes well beyond that typically available from
other commercial laboratories.
TIER 1.-USEPA Good Laboratory Practices Standards
AL TA' s standard operating procedures cover all operations and were written in
accordance to USEPA GLP Standards required under 40 CFR Part 58 and Part 160.
1n particular, ALTA has taken the approach to adhere to GLP standards throughout
the laboratory whenever possible including work not conducted in support of
FIFRNFDA registration requirements (e.g., NPDES, RCRA and SARA). This
approach, although more stringent, ensures maximum uniformity in laboratory
operations, particularly data collection and record keeping.
TIER 2.-Method Performance Evaluation
ALTA routinely analyzes the following QC samples to monitor HRMS/LRMS method
performance:
• one method blank per set (batch) of samples extracted,
• a pair of laboratory control samples (LCS l/LCS2) for every 20 or less
samples of similar matrix and analysis, or every 2 weeks whichever is
less,
• periodically, a pair of matrix spikes (MS/MSD).
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TIER 3.-Study/Project Specific QC Options
AL TA offers study/project ·specific quality control options on an as-needed basis
including:
• Matrix Spike, Duplicate Spike samples,
• Duplicate samples
• Resin, Filter QC' s,
• Raw data package (chromatograms, data sum sheets,.calibrations)
• USEPA Method Detection Lim.it (MDL) Studies,
• Method Development and Validation Studies,
• Storage Stability Studies,
• Multiple column or MS/MS Confirmations.
Project Management
As a client of ALTA, your analytical work will be overseen by an experienced environmental
chemist with "hands-on" involvement in your project Studies are assigned by matching
expertise with analytical program requirements. This ensures that clients receive expert
consultation beginning with project definition and ending with the discussion of the final
report. The resumes of key technical personnel are provided in the Appendix.
Sample Tracking
Clients conducting long term field studies or other monitoring studies often require that
sample batches be analyzed according to a study or project specific analytical program. In
order to provide this level of tracking and routine handling, AL TA assigns a Study ID and a
sample Batch ID to all sample batches as they are logged into the AL TA Laboratory
Information Management System (LIMS). This enables the Sample Control personnel to use
a study template which reduces errors during i'og-in, and facilitates the assignment of
appropriate analytical tests.
Study Audits
ALTA's QA Program has been designed to comply with USEPA Good Laboratory Practice.
As part of GLP compliance, those studies conducted under a formal protocol will be routinely
audited during the critical phases of sample preparation and analysis. In addition, study
protocols specify unique ongoing QC requirements, including study specific precision and
accuracy control limits.
Cost Accounting
ALTA's in-house accounting program routinely tracks invoices by Study ID (as well as Client
ID). Upon request, project reports can be generated monthly, quarterly or year-to-date to
document laboratory costs associated with a particular study or project. This service is
valuable for project managers working under a fixed budget, or those that have multiple
projects running concurrently with ALTA In addition, it allows ALTA to verify the volume
of revenue generated by an account and award volume discounts (if applicable) on a real time
basis.
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SECTION VI.
Selected Project Experience
SELECTED PROJECT EXPERIENCE
Air Toxics Monitoring Projects:
1. Performed PCDD/PCDF, PAR and semi-volatile analyses for the WTI Hazardous
Waste Incinerator Trial Bum on over 50 samples (1992).
2. Stack emission monitoring of a hazardous waste incinerator test burn for P AH' s and
PCDD/PCDF using California Air Resources Board (CARB) Methods 428 and 429
(LRMS & HRMS).
3.
4.
5.
6.
7.
8.
9.
10.
Stack emission tests of hospital infectious waste incinerators for PCDD/PCDF and
P AH' s by CARB Methods 428 and 429 (LRMS & HRMS).
Sugar plant stack emission test and process water analysis for PCDD/PCDF by CARB
Method 428 and EPA Method 1613A (HRMS).
Refinery stack emission monitoring of PAH's by CARB Method 429 (HRMS).
Diesel/natural gas boiler stack testing for P AH' s by CARB Method 429
(LRMS & HRMS).
Ambient Air Analysis by Modified EPA Method TO-9 for PCDD/PCDF's (USEPA
SAS #5710-D-01).
PCDD/PCDF Ambient Air Round Robin Study conducted for Environment Ontario
[Contact: R.E. Clement (Environment Ontario), 416-235-5906].
Ambient Air Analysis by Modified EPA Method TO-9 for PCDD/PCDF, PAR, and
Coplanar PCB's (USEPA SAS #1226).
ALTA holds 1-year contracts for California Air Resources Board for CARB 428 and
429 for 1993.
Pulp and Paper Industrial Monitoring Projects:
1.
2.
USEPA Industrial Technology Division Method 1613A interlaboratory method
performance evaluation study involving pulp mill effluent analysis for PCDD/PCDF
[Contact: William Telliard (USEPA-ITD), 202-383-7120].
NCASI Certification performance check sample analysis of standard reference pulps,
sludges and effluents for TCDD/TCDF using NCASI Method 551
[Contact: Larry LaFleur (NCASI), 503-752-8801].
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Pulp and Paper Industrial Monitoring Projects (continued):
3.
4.
5.
6.
NPDES compliance pennit monitoring of PCDD/PCDF in fish by the Stalling's
Method.
Detennination of TCDD/TCDF in finished paper products by NCASI Method 551.
Interlaboratory study (DF-1) for the detennination of dibenzo-p-dioxin and
dibenzofuran in defoamers for Environment Canada.
NPDES compliance pennit monitoring of PCDD/PCDF in pulp and paper industry
effluents using EPA Method 1613A and NCASI Method 551.
7. NCASI/USEPA joint variability study involving analysis of pulp, sludge & pulp mill
effluent for PCDD/PCDF. [Contact: Larry LaF!eur]
Municipal and Industrial Monitoring Projects:
' 1. Detennination of PCDD/PCDF in soil samples by EPA Method 8290
2.
3.
(SAS #5674-S-0l).
Measurement of of PCDD/PCDF in power plant ash samples by EPA Method 8290.
Analysis of still bottom waste for PCDD/PCDF by EPA Method 8280.
4. NPDES compliance monitoring of POTW effluent by EPA Method 1613A.
5.
6.
7.
8.
Determination of PCDD/PCDF in refinery waste effluent by EPA Methods 8280 and
1613A.
Analysis of Drinking Water for 2,3,7,8-TCDD using EPA Method 1613A.
Fish Round Robin Study. [CIL Contact: Joel Bradley]
Soil Round Robin Study. [Radian Contact: Larry Keith]
Agrochemical Studies:
1.
2.
3.
Development of TSP-LCMS methods for the determination of hydroxy triazines in soil
and water.
Broad scale terrestrial field soil dissipation study involving the measurement of a
dihydroxy triazine by TSP-LCMS.
Development of several TSP-MS/MS methods for the determination of a sulfonyl urea
and its degredates in soil.
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SECTION VII.
Appendix
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AL TA Organizational Flowchart
Key Technical Staff Resumes
Certifications
APPENDIX
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ALT A Organizational Flowchart
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ALTA ANALYTICAL LABORATORY
WllliamJ.
Luksemburg
Director of
HRMS Services
James Hedin
Associate Scientist
Martha Maier
Associate Scientist
Nial Maloney
Associate Scientist
Brad Silverbush
Associate Scientist
Michael Werst
Associate Scientist
Version: July 21, 1993
NON-GLP
Robert S. Mitzel
Director of
Air Taxies
Phil Hartwick
Associate Scientist
Melanee Schuld
Associate Scientist
Richard Spas
lab Technician
Dr. John W. Cornacchia
President
Scott N. Jimison
Director of
Financial
'Services
Ken Flatt
Sample Custodian
De Rutz
Receptionist
Cathi Stovall
Admin. Assistant
Sharon Pierson
guality Assurance Officer
Shelly Weagraff
QA Associate/Archivist
GLP
Bob Peterson
Director of
Technical
Services
BobBethem
Director of
LCMS Services
Kay Brown
Associate Scien!i
Shannon Bryant
Associate Scienti
Jeri Frier
Associate Scienti
Jim Lehman
Associate Scienti..
Scott Serl
Associate Scienri.
Paul Woolley
Associate Scienti.,
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EDUCATION
Ph.D.
B.S.
EXPERIENCE
Present
1989 -1990
1987 -1989
1986 -1987
John W. Cornacchia, Ph.D.
President
Ecology, University of California, Davis, CA (1982)
Animal Science, University of California, Davis, CA (1975)
President, AL TA Analytical Laboratory
Dr. Cornacchia is co-founder, CEO, and a member of the Board of
Directors of ALT A. He is responsible for the management of business
planning including venture funding, sales and marketing and the review of
laboratory operations. He participates in the planning of agrochemical
studies, particularly field dissipation studies and groundwater monitoring
projects.
Senior Program Administrator, Enseco-Cal Lab
Responsible for managing USEPA-FIFRA Environmental Fate Studies
conducted for Fortune 500 chemical companies and government agencies.
Also was responsible for all sales and marketing of LCMS and LCMS/MS
services for the USEPA-FIFRA pesticide residue testing market.
Director of Production Planning & Control/Director of Information
Services, Enseco-Cal Lab
Coordinated the scheduling and planning of laboratory production capacity
and managed the Information Services Group (ISG) for the largest
commercial laboratory in California. His ISG functions included the
operation of the Sample Control Department, Data Control Group and the
Computer Group. In addition, he managed analytical services programs
supporting large-scale terrestrial field dissipation studies, groundwater
monitoring investigations, and surface water surveys.
Technical Manager, Enseco-Cal Lab
Provided consultative services to agrochemical clients responding to the
California Groundwater Contamination Prevention Act (AB2021) including
the preparation of terrestrial field dissipation study reports. Managed
analytical programs in support of aquatic field dissipation studies.
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1981 -1986 Senior/Associate Environmental Specialist, Division of Water Quality,
California Water Resources Control Board.
As a member of the Pollutant Investigations Branch Special Studies Unit,
Dr. Comacchia designed, implemented and managed large-scale pesticide
and water quality monitoring projects and aquatic bioassay studies. As pan
of the Pesticide Registration and Evaluation Unit/Priority Chemicals Unit,
he performed statewide chemical risk assessments of agrochemicals
including malathion, molinate, and_ thiobencarb.
QUALIFICATIONS
Dr. Comacchia has over nine years of experience in environmental research examining the
fate and effects of agrochemicals in aquatic and terrestrial systems. He spent the first five
years as a regulator performing aquatic risk assessments regarding pesticide usage in
California, and the last four years developing analytical programs in support USEPA FIFRA
Environmental Fate Studies and governmental water quality assessments. Many of the special
projects he directed led to the development of new agrochemical screening techniques
including solid phase extractions, GCMS-SIM methods, and most recently, LCMS and
LCMS/MS procedures .. Dr. Comacchia has in-depth experience regarding USEPA-GLP
Standards and the management of laboratory personnel.
SELECTED PUBLICATIONS & PRESENTATIONS
"Quantitative Analysis of Pesticides by Thermospray LCMS and MS/MS," Bethem, R. A.,
Cornacchia, J. W., Presented at the 38th AS~S Conference on Mass Spectrometry and Allied
Topics, June 5-10, 1990, Tucson, AZ.
"Determination of Triazine Pesticides and Degradation Products in Groundwater by
Thermospray Liquid Chromatography Mass Spectrometry," Bethem, R. A., Cornacchia, J.
W., Presented at 10th Annual SETAC Meeting, Toronto, Canada (1989). , .
"Method Validation for Pesticide Determination in Water and Soil Using Quantitative
Thermospray Liquid Chromatography/Mass Spectrometry," Bethem, R. A., Cornacchia, J. W.,
Kornfeld, R., Matusak, K., Presented at the Pittsburgh Conference, New York, New York
(1990).
Rice Herbicides: Molinate (Ordram) and Thiobencarb (Bolero), A Water Quality Assessment,"
Cornacchia, J.W., D.B Cohen, G.W. Bowes, R.J. Schnagl and B.L. Montoya. Special Projects
Report No. 84-4sp, California Water Resources Control Board.
PROFESSIONAL AFFILIATIONS
American Chemical Society
William J. Luksemburg
Director of HRMS Services
EDUCATION
B.S. Chemistry, California State University, Fresno, CA (1974)
EXPERIENCE
Present Director of HRMS Services, ALTA Analytical Laboratory
Mr. Luksemburg, a co-founder, directs the routine analysis and method
development work in the High Resolution Mass Spectrometry department.
He is responsible for marketing HRMS dioxin services to environmental
engineering firms, the pulp and paper industry, government agencies and
other industrial clients. Mr. Luksemburg is also responsible for the
development of new markets using HRMS instrumentation. In addition Mr.
Luksemburg directs routine and special projects, review and interpret data,
and interface with clients.
1986 -1990 Principal Scientist/HRMS Manager, Enseco-Cal Lab
As Principal Scientist in the Special Services department at Enseco-Cal Lab
Mr. Luksemburg coordinated the operation and maintenance of five high
resolution magnetic sector instruments. · He was responsible for developing
a business that now is one of the major suppliers of HRMS PCDD/PCDF
analysis to the pulp and paper industry in the U.S. Mr. Luksemburg also
coordinated the training and development of the staff in the operation and
maintenance of HRMS instruments.
1979 -1986 Senior Chemist, Radian Corporation
In Radian's Sacramento laboratory, Mr. Luksemburg was GC/MS
,,, supervisor for ABN and VOA analysis. He coordinated the activities of
five chemists in the operation and maintenance of four quadrupole mass
spectrometers.
1974 -1979 Chemist, Carnation Company
As a staff chemist, Mr. Luksemburg was involved in the analysis of
products and ingredients used in Carnation's animal feed division.
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QUALIFICATIONS
Mr. Luksemburg has over 14 years experience in production analytical laboratories including
10 years experience in the field of environmental mass spectrometry. Much of this
experience has involved PCDD/PCDF analysis of environmental samples and for the last four
years has concentrated on High Resolution Mass Spectrometry analysis of PCDD's/PCDF's in
a variety of matrices. Mr. Luksemburg is recognized through-out the pulp and paper industry
for his research and production work on dioxins and furans. He recently was recognized on
the international level when his chapter on dioxin analysis of pulp and paper (Rappe, 1991),
was published by the World Health Organization. He is one of the few individuals in the
world to successfully adapt the high resolution magnetic sector instruments to "production"
analysis of environmental samples at the picogram and femtogram levels.
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RECENT PRESENTATIONS
"Determination of Method Detection Limits in Pulp and Pulp Mill Effluents," in Rotorua,
New Zealand, at the ISWPC l;'ost Symposium Workshop, May 1991.
"Comparison of NCASI Method 551, EPA Method 1613A, and the Proposed FDA Method for
the Analysis of 2,3,7,8-TCDD and 2,3,7,8-TCDF in Food Packaging Material," in Boston,
MA, at the 1993 TAPPI Environmental Conference, March 1993.
PUBLICATIONS
NCASI Technical Bulletin No. 551, "NCASI Procedures for the Preparation and Isomer
Specific Analysis of Pulp and Paper Industry Samples for 2,3,7,8,·TCDD and 2,3,7,8-TCDF,"
Lafleur, L., Ramage, K,, Bousquet, T., Brunck, R., Luksemburg, W., Miille, M., Peterson, R.,
and Valmores, S., (1989).
"Optimization of Extraction Procedures for the Analysis of TCDD/TCDF in Pulp, Paper Base
Stocks, and Pulp Industry Solid Wastes," .Lafleur, L., Ramage, K., Gillespie, W.,
Luksemburg, L., Miille, M., and Valmores, S., Chemosphere, Vol. 19, pp 643-648, 1989.
"Analytical Procedures for the Analysis of TCDD and TCDF in Food Sources," Lafleur, L.,
Bousquet, T., Ramage, K., Davis, T., Luksemburg, W., and Peterson, R., Presented by L.
Lafleur at Dioxin '89, Toronto, Canada. Waiting publication in Chemosphere.
"Determination of Polychlorinated Dibenzo-p-Dioxins and Polychlorinated Dibenzofurans in
Pulp and Paper Industry Wastewaters, Solid Wastes, Ashes and Bleached Pulps,"
Luksemburg, W., Environmental Carcinogens-Methods of Analysis and Exposure
Measurement-Volume 11, World Health Organization, Christopher Rappe, Editor, 1991.
PROFESSIONAL AFFILIATIONS
American Chemical Society
American Society for Mass Spectrometry
Technical Association of the Pulp and Paper Industry
EDUCATION
B.S.
EXPERIENCE
Robert A. Bethem
Director of LCMS Services
Chemistry, Antioch College, Yellow Springs, OH (1978)
Present Director of LCMS Services, AL TA Analytical Laboratory
Mr. Bethem is a co-founder and member of the Board of Directors of
ALTA. He initiates and manages all method development and routine work
by Liquid Chromatography Mass Spectrometry (LC/MS), and tandem mass
spectrometry, (MS/MS). He is responsible for the development of novel
methods for the trace analysis of pesticides in water and soil by LCMS. In
addition to his role in LCMS analysis, he is responsible for the application
of GC/MS/MS techniques for the trace analysis of organic compounds in
complex matrices.
1987 -1990 Principal Scientist/LCMS Manager, Enseco-Cal Lab
Created and managed the LCMS Services Department and provided
· pesticide analysis services for industry and government. • Developed and
marketed several trace methods by GC/MS/MS. Supervised extraction and
instrument personnel and was responsible for the final review and
processing of all data. Coordinated and maintained two Finnigan MAT
TSQ-70' s and developed software for automated analysis.
1984 -1987 International Field Engineer, Finnigan MAT
Performed mass spectrometer applications and engineering support for the
Pacific Operations Centers in China and South America. Provided
···,:: applications and technical support to several large USEP A contract
· laboratories.
1982 -1984 Manager of Mass Spectrometry, Cambridge Analytical Assoc.
Organized and maintained the GC and GCMS laboratories for EPA and
NIOSH protocol analysis. Supervised GC and GCMS personnel and was
responsible for final data review and report generation.
1978 -1982 Research Assistant, Massachusetts Institute of Technology
Provided low and high resolution analyses on several instruments using a
variety of ionization techniques at the N.I.H. facility for Mass Spectrometry.
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QUALIFICATIONS
Mr. Bethem has accumulated over 12 years ,of experience in mass spectrometry at a variety of
research and production environments. He has recently pioneered the application of
Thermospray LCMS to the quantitative analysis of pesticides and has demonstrated its ability
to produce superior data quality in actual field studies. Recent work and publications have
established him as one of the leaders in this field. He is a current member of the Joint Task
Group of "Standard Methods for the Examination of Water and Wastewater" for the
development of new LCMS methods. Mr Bethem has an extensive background in biological
and environmental analysis. As a result of his work with an instrument manufacturer, he has
also developed a high degree of proficiency with software, electronic, and electro-mechanical
devices.
PUBLICATIONS
"Thermospray MS and MS/MS of Polar, Urinary Metabolites and Metabolic Conjugates,"
Draper, W. M., Brown, F. R., Bethem, R. A., Miille, M.J., Biomed Environ. Mass Spectrom.
1989, 18, 767.
"Anion Exchange Thermospray Tandem Mass Spectrometry of Polar Urinary Metabolites and
Metabolic Conjugates," Draper, W. M., Brown, F. R., Bethem, R. A., Miille, M.J., Liquid
Chromatog./Mass Spectrom.: Applications in Agricult, Pharm .. and Environ. Chem., Mark A.
Brown, Editor,-1990.
"The Application-of Tandem Mass Spectrometry to Environmental Measurements," Finnigan,
R., Poppeti, J., and Bethem, R., (In Press).
"Quantitative Analysis of Pesticides by Thermospray LCMS and MS/MS," Bethem, R. A.,
Comacchia, J. W., Presented at the 38th. ASMS Conference on Mass Spectrometry and Allied
Topics, June 5-10, 1990, Tucson, AZ.
"Determination of Triazine Pesticides and Degradation Products in Groundwater by
Thermospray Liquid Chromatography Mass Spectrometry," Bethem, R. A., Comacchia, J.
W., Presented at 10th Annual SETAC Meeting, Toronto, Canada (1989).
"Method Validation for Pesticide Determination in Water and Soil Using Quantitative
Thermospray Liquid Chromatography/Mass Spectrometry," Bethem, R. A., Comacchia, J. W.,
Kornfeld, R., Matusak, K., Presented at the Pittsburgh Conference, New York, New York
(1990).
PROFESSIONAL AFFILIATIONS
American Chemical Society
American Society for Mass Spectrometry
Joint Task Group -"Standard Methods for the Examination of Water and Wastewater"
EDUCATION
B.A.
B.A.
EXPERIENCE
Present
1989 -1990
1988 -1989
1986 -1988
Robert S. Mitzel
Director of Air Toxics
Chemistry, Chico State University, Chico, CA (1982)
Biology, Chico State University, Chico, CA (1982)
Director of Air Toxics, ALTA Analytical Laboratory
Mr. Mitzel, a co-founder, manages production scheduling and client
management for the Air Toxics group. He is also responsible for the final
review and interpretation of analytical data and final reports. 1n addition,
he serves as a marketing agent for Air Toxic service and development of
new Air Toxic markets.
Director of Mass Spectrometry, Enseco-Cal Lab
Directed five supervisors and 42 chemists in the GC/MS group. He was
responsible for extractions, analyses, final review and processing of all data
generated by the group. Served as project manager for selected accounts
focusing on priority pollutants and dioxin/furans. His accomplishments
included generating and managing a $7 million dollar production group in
1989. Mr. Mitzel served as the focal person for the Air Toxic program at
Enseco-Cal Labs for mass spectrometry methods on Modified Method 5
(MMS) sampling trains.
Mass Spectrometry Lab Manager, Enseco-Cal Lab
Managed the mass spectrometry group through four supervisors and assisted
daily operations for the VOA, BNA, Dioxin, and extraction groups .. He
also assisted development efforts for new GC/MS methods.including
isotope dilution techniques for the analysis of polynuclear aromatic
hydrocarbons from the Exxon-Valdez oil spill.
GC/MS Dioxin Lab Manager, Enseco-Cal Lab
Initiated and managed the method development and routine analysis of
dioxin/furan samples. Collaborated with the USEPA for the development
of EPA Method 8280, and developed isotope dilution methods for
polychlorinated biphenyls, polynuclear aromatic hydrocarbons,
chlorobenzenes, and chlorophenols. He collaborated with the California Air
Resource Board with the development of Method 428 and 429, which are
now part of AB 2588 (Air Toxics "Hot Spots" Information Assessment Act
of 1987).
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1985 -1986
1983 -1985
1982 -1983
GC/MS Supervisor, Enseco-Cal Lab
Managed the production night shift for the VOA, BNA, and Dioxin GCMS
groups.
Staff Chemist, California Analytical Laboratory
Conducted specialized and routine analyses for volatiles, semi-volatiles, and
dioxins. He operated several Finnigan MAT mass spectrometers including
the: OWA, 1020, 5100, 3200, 4500, TSQ-4500, TSQ-4600, and Incos 50.
Staff Chemist, California· Analytical Laboratory
Mr. Mitzel conducted specialized and routine extraction and clean-up
methods for volatiles, semi-volatiles, and dioxins.
QUALIFICATIONS
Mr. Mitzel has over 11 years of experience in the environmental services business. He
participated in the early development of novel techniques for the extraction and analysis of
2,3,7,8-TCDD and was instrumental in developing a multi-million dollar dioxin program for
Enseco, Cal Labs. He has since expanded the use of isotope· dilution techniques for several
other compounds in a variety of complex environmental matrices. Mr. Mitzel has extensive
experience managing large production groups in an environmental laboratory.
PUBLICATIONS
"Photolysis of Octachlorodibenzo-P-Dioxins on Soils: Production of 2,3,7,8-TCDD," Miller,
G., Herbert, V.R., Miille, M.J., Mitzel, R., Zepp, R.G., Chemosphere, 18, 1265-1274, 1989.
AWARDS
Graduated Cum Laude with honors in Biological Sciences
Botanical Society Award
PROFESSIONAL AFFILIATIONS
American Chemical Society
EDUCATION
M.S.
B.S.
EXPERIENCE
Present
Robert G. Peterson
Director of Technical Services
Chemistry, California State University, Sacramento, CA (1982)
Chemistry, California State University, Sacramento, CA (1975)
Director of Technical Services, AL TA Analytical Laboratory
Is responsible for assisting in the resolution of technical problems and
development of solutions to new sample preparation obstacles. Focuses on
existing and furure analytical methods. Additionally, he will function as a
focal point for R & D efforts whether they are client or scientifically
oriented.
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1988 ·-1990 ·· • Principal Scientist, Manager, Dioxins/Furans, Enseco-Cal Lab
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1987 -1988
1982 -1987
As a Principal Scientist, Mr. Peterson was involved in developing new
methods, refining and troubleshooting existing methods, and aiding in
problem solving within the Special Services Group (Dioxins and Furans
analysis). Because of his unique cross-disciplined experience and
education, Mr. Peterson was frequently called upon as a primary scientific
resource for other organic and inorganic projects. He also served as Client
Manager for selected major accounts.
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As a Manager, Mr. Peterson was responsible for the staff, production, and I
resource allocations for the two Dioxin Preparations Laboratories. One lab
was devoted to prep for High Resolution dioxin/furan analyses and the
other was devoted to Low Resolution dioxin/furan analyses. His staff I
consisted of 2 supervisors and 15 chemists/analysts.
Director of Inorganic Services, Enseco-Cal Lab
Directed all aspects of the Inorganics Department, including guiding the
Department to meet existing and projected business· and technical goals.
He also served as Client Manager for selected major accounts.
Organics Preparation Manager, Enseco-Cal Lab
Mr. Peterson not only managed the Organic Preparation Group, he was
directly involved in the creation and subsequent management of the Dioxin
Preparation Lab and the Standards Preparation Group, which resulted in
upgraded laboratory QNQC traceability and verification of standards. In
this capacity, he was responsible for the mobilization of resources to meet
test requests and time constraints, and was the liaison between the groups
and Client Managers for efficient coordination of work flow. He also
served as Client Manager to clients with organic analysis requests.
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1980 -1982
1979 -1980
1976 -1979
Senior Staff Chemist, California Analytical Laboratory
Performed extractions, concentrations and clean-ups on environmental
samples of a diverse nature for organic analytes.
Chemist, Sacramento County Water Quality Control Laboratory
Conducted inorganic and organic analysis of waters, sludges and sediments
pertinent to wastewater treatment.
Chemist, Morse Laboratories
Mr. Peterson conducted inorganic analysis of waters, sediments and crop
samples. He also served as Organics Lab Supervisor of satellite extractions
and clean-up laboratory.
QUALIFICATIONS
Mr. Peterson has a wide range of technical and management experience. His knowledge of
analytical chemistry covers a spectrum of cross-disciplines and he can provide expert
assistance in special organic and inorganic projects. He is also an experienced teacher and
trainer. He presently coordinates and conducts an ongoing class, which is part of the
Hazardous Materials Certification Program at the University of California Extension, Davis
campus .
RECENT PRESENTATIONS
(1) "Quantitative Analysis and Practical Laboratory Techniques," University of California
Extension, Davis (1983 to present). Currently being taught Spring, Summer, Fall &
Winter quarters.
(2) Hazardous Waste Analysis Seminar for J.H. Kleinfelder (1986).
(3) Hazardous Waste Analysis Seminar for Dames & Moore (1987).
(4) "Training Program on Pesticide Residue Analysis" in Bangkok, Thailand for The World
Bank/UNIDO/UNDP/DOA, November 1987.
(5) "Overview of Analytical Techniques for Pesticide Studies" as part of "Pesticides in Soil
and Groundwater," University of California Extension, Davis (1988).
' (6) "Analytical Techniques" as part of "Principles of Hazardous Materials Management,"
University of California Extension, Davis (1989, 1990, 1991, 1992.)
(7) "The Environment: Air and Water Quality, Land, Safety, Health and Proposition 65" as
part of "Advanced Executive Program," University of California Extension, Davis
(1990).
PUB LI CA TIO NS
"Cl5-Cl8 Isomers Synthesized from [13C]-2,3,7,8-Tetrachlorodibenzofuran via Surface
Chlorination," Bulletin of Environmental Contamination and Toxicology (1987).
NCASI Technical Bulletin No. 551, "NCASI Procedures for the Preparation and Isomer
Specific Analysis of Pulp and Paper Industry Samples for 2,3,7,8-TCDD and 2,3,7,8-TCDF,"
Lafleur, L., Ramage, K., Bousquet, T., Brunck, R., Miille, M., Luksemburg, W., Peterson, R.,
Valmores, S. (1989).
"Analytical Procedures for the Analysis of TCDD and TCDF in Food Sources," Lafleur, L..
Bousquet, T., Ramage, K., Davis, T., Luksemburg, W., and Peterson, R.. Presented by L.
Lafleur at Dioxin '89, Toronto, Canada. Waiting publication in Chemosphere.
"Supercritical Fluid Extraction and Solid Phase Extraction Techniques Applied to the Analysis
of Pulp and Paper Mill Effluents for 2,3,7,8-Tetrachlorodibenzo-p-dioxin and 1,2,7,8/2,3,7,8-
Tetrachlorodibenzofuran," Peterson, R.G., Luksemburg, W.J., Hedin, J., Silverbush, B., Werst,
M., Maloney, N. Presented at the Research and Technology Transfer Conference, Toronto,
Ontario (1992).
PROFESSIONAL AFFILIATIONS
American Chemical Society
American Society for Mass Spectrometry
Society of Quality Assurance
AWARDS
"Excellence in Teaching and Outstanding Service Award," University of California, Davis
(1989).
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James M. Hedin
Associate Scientist
EDUCATION
B.S. Chemistry, University of Minnesota, Duluth, MN (1986)
EXPERIENCE
Present Associate Scientist, ALTA Analytical Laboratory
Mr. Hedin performs routine analysis and method development work in the High
Resolution Mass Spectrometry department He is responsible for routine
maintenance of HR/MS instruments. Mr. Hedin also aides in the training of
new staff, reviews and interpre~ data, and interfaces with clients.
1988 -1990 GC/MS Chemist, Enseco-Cal Lab
As GC/MS Chemist at Enseco-Cal Lab Mr. Hedin was responsible for the
operation and maintenance of quadrapole GC/MS instruments. His duties
entailed sample analysis by EPA methods for volatiles and semi-volatiles. Mr.
Hedin also aided in the training of the staff in the department
1987 -1988 Extraction Chemist, Enseco-Cal Lab
Mr. Hedin's duties entailed sample extraction for Dioxin/Furan Analysis by
High Resolution Mass Spectrometry. He assisted in the training of new staff,
and the developement of new extraction techniques.
QUALIFICATIONS
Mr. Hedin has over 6 years experience in production analytical laboratories including 5 years
experience in the field of environmental mass spectrometry. Much of this experience has
involved PCDD/PCDF analysis of environmental samples and for the last three years has
concentrated on High Resolution Mass Spectrometry analysis of PCDD's/PCDF's in a variety
of matrices.
PROFESSIONAL AFFILIATIONS
American Society for Mass Spectrometry
EDUCATION
Philip T. Hartwick
Associate Scientist
B.S. Biology and Environmental Studies, Tulane University, New Orleans, LA (1981)
EXPERIENCE
Present Associate Scientist, AL TA Analytical Laboratory
Mr. Hartwick specializes in Air Toxics methods. Responsibilties include
project management, client liaison, Air Toxics marketing and the air sample
preparation laboratory.
1990 -1991 Director of Mass Spectrometry, Enseco-Cal Lab
Directed a group of five supervisors and 40 chemists using 17 low resolution
GC/MS systems with an annual revenue-of 7 million. Was reponsible for day
to day operations, method development, and quality and timeliness of GC/MS
projects. Served as a Program Administrator to select accounts including client
liason. Was involved in strategic planning for the entire laboratory.
1989 -1990 Manager of GC/MS, Enseco-Cal Lab
Was responsible for accepting work for and releasing all data from the GC/MS
Jab. Prioritized the use of lab instrumentation and personnel. Assisted the
Director and supervised problem solving associated with instrumentation,
personnel, methodologies and data.
1987 -1989 GC/MS Laboratory Supervisor, Enseco-Cal Lab
Mr. Hartwick is a specialist in Quadrupole Mass Spectrometry using both MID
and full scan capabilities. Supervised all phases of analyses for volatile organic
compounds by GC/MS. Responsibilities included scheduling analyses, data
review, spectral interpretation, instrument tuning and routing maintenance. He
is extensively involved in regulatory analysis, particularly for EPA-CLP, and
USATHAMA contract testing. of dioxin/furan samples.
1982 -1986 Staff Chemist, California Analytical Laboratory
Conducted routine and non-routine GC/MS analyses for volatile and
semivolatile organic compounds and dioxins/furans. Operated and maintained
GC/MS instruments, trained personnel and analyzed EPA-CLP, RMA volatile
and semivolatile and commercial client samples.
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QUALIFICATIONS
Mr. Hartwick has over l O years of experience in the environmental analytical business. His
extensive experience includes VOA, BNA, dioxin/furan sample preparation and GC/MS
analytical techniques, project management, data review, and personnel management and
training. He was responsible for managing a multimillion dollar revenue mass production
GC/MS facility at Enseco Cal-Lab. There he spearheaded task groups focused on improving
the quality of the GC/MS product and shortening the delivery time to the client by
incorporating new team building management techniques. Mr. Hartwick has more recently
been involved in marketing for AL TA on the west coast of the United States and in the
international arena which included trips to Australia and New Zealand.
PROFESSIONAL AFFILIATIONS
Air & Waste Management Association
American Chemical Society
Clean Air Society of Australia and New Zealand
Martha M. Maier
Associate Scientist
EDUCATION
B.S.
B.S.
Chemistry, University of Wisconsin, Madison, WI (1983)
Philosophy, University of Wisconsin, Madison, WI (1983)
EXPERIENCE
Present Associate Scientist, AL TA Analytical Laboratory
Ms. Maier coordinates analytical work from ALT A's East Coast office. Assists
customers in setting up projects and coordinates sample shipping, analysis and
reporting. Also responsible for marketing in the eastern United States and
attends technical meetings and presents papers.
1990 -1992 Technical Sales, Enseco-Cal Lab
She coordinated the dioxin/furan marketing program. Responsibilities included
preparing bids, organizing exhibits, and overseeing the production of marketing
materials. Acted as a liaison between the salespeople and the dioxin/furan
laboratory.
1988-1990 HR GC/MS Operator, Enseco-Cal Lab
1987-1988
1986-1987
1984-1986
Dioxin/furan analysis of pulp, food, and low level environmental samples using
high resolution GC/MS. Promoted to scientist position in December 1989.
Involved in data review and project management.
GC/MS Operator, Enseco-Cal Lab
Dioxin/furan analysis using low resolution GC/MS systems. Promoted to lead
person in May 1988.
GC/MS Semivolatile Operations Supervisor,
Radian Corporation
Responsible for the scheduling and completion of all semivolatile analyses.
Trained other operators in Semivolatile and routine instrument maintenance.
GC/MS Operator, Radian Corporation
Analyzed environmental samples for volatile and semivolatile organic
pollutants suing EPA methods 624, 625, SW-8240, SW-8270, and by EPA
Contract Lab Protocol. Performed routine maintenance on all systems.
Responsible for interfacing the GC/MS Lab with the laboratory database
management system.
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1984-1984 Analytical Chemist, Wisconsin Dept of Agriculture, Madison, \VI
Assayed pesticide formulations using HPLC, GC, and TLC; researched,
developed and modified methods.
PROFESSIONAL AFFILIATIONS
Air & Waste Management Association
Technical Association of the Pulp and Ppaer .Industry
PRESENTATIONS
"Analysis of Coplanar PCBs using High Resolution Mass Spectrometry," in Long Beach, CA,
at the HazMat Conference, November 1992.
QUALIFICATIONS
Ms. Maier has over 9 years experience in environmental analytical laboratories, including 8
years in the field of GC/MS. Her extensive background in the analysis of PCDD/PCDF in
environmental samples is valuable in her present role as project manager.
Sharon K. Pierson
Quality Assurance Officer and Safety (QAO)
EDUCATION
B.S. Biological Sciences. University of the Pacific, Stockton, CA (1978)
EXPERIENCE
Present Quality Assurance Officer and Safety, ALTA Analytical Laboratory
As Quality Assurance Officer (QAO) oversees the laboratory's compliance with
ALTA's Quality Assurance Program Plan (QAPP), Standard Operating
Procedures (SOPs), USEPA Good Laboratory Practices (GLP) and any client
specific QA programs.
As Safety Officer, is responsible for the laboratory and facility safety program
and the management of hazardous materials and their disposition.
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1991 Laboratory Manager, Roy F. Weston (Formerly Canonie Environmental I
Services)
Upon sale of the Canonie Stockton laboratory to Weston, became Laboratory
Manager being responsible for the entire laboratory. Responsibilities included •
management of analytical production, data validation of in-house and outside
client data, quality assurance, LIMS implementation, development of fiscal
budget and equipment expenditures, and professional staffing. Major clients I
included several in the federal sector and other environmental consulting firms.
1990 -1991 Operations Manager, Canonie Environmental Services I
Managed 40 chemists and technicians in a full service analytical laboratory.
Responsibilities included management of analytical production, projects, data I
validation, finances, and hiring and reviewing personnel. Primary client base
was Canonie Environmental Services projects.
1989 -1990 Client Service Coordinator, Radian Corporation, Radian Analytical
Services
Liaison between the laboratory and several large environmental clients.
Relayed information regarding laboratory capabilities, turnaround-times, price
quotations, preliminary data reports, data interpretation, and addressed any data
quality issues. Clients' base was both in-house and local environmental firms.
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9/88 -3/89 Project Administrator, Canonie Environmental Services
Established Project Administration program at Canonie. Responsibilities
included responding to inquirif?S regarding the laboratory's analytical
capabilities, turnaround-time, and pricing analytical analyses. Assisted
Operations Manager with workload projections for large engineering projects
requiring analytical services, helping in the preparation of site-specific Quality
Assurance Project Plans (QAPPs) and data review.
7/87 -8/88 Quality Assurance Officer, Canonie Environmental Services
Developed and maintained a fully integrated computerized database for tracing
quality control data, generated ·in all analytical departments of the laboratory.
Assisted the engineering staff during the preparation of site-specific QAPPs and
Data Quality Objectives.
10/83 -7 /87 Staff Scientist, Canonie Environmental Services
As part of the GC/MS department was responsible for the operation and
maintenance of a Hewlett Packard 5970 GC/MSD with RTE-A data system for
the analysis of volatile organic in various matrices according to EPA
methodology and the Contract Laboratory Program. Other areas of experience
and responsibilities at Canonie included supervising three chemists and two
technicians for analysis of volatile organic chemicals by automated purge and
trap gas chromatography in all matrices as per EPA, CA DOHS, and RWQCB
methodologies, conducting inorganic analysis by gravimetric and titrametric
methods and the use and application of safety equipment for workers during
hazardous waste site remediation.
2/82 -3/83 Field Investigator, California Department of Health Services
Compiled an inventory of hazardous waste sites in both San Joaquin and
Stanislaus counties for the California Department of Health Services
Abandoned Site Program.
QUALIFICATIONS
Ms. Pierson has over 9 years of experience in environmental analysis of both organic and
inorganic parameters in a variety of matrices. While at Canonie Environmental she help
implement a computerized database for monitoring quality control data in a full service
analytical laboratory and assisted in the development of Quality Assurance Project Plans. As
a Project Administrator and Client Services Coordinator Ms. Pierson has experience acting as
a liaison between the laboratory and client to allow the efficient coordination and
communication of project needs and data quality objectives. Ms. Pierson management
experience include the development of a fiscal budget for a full service analytical laboratory,
instrumentation purchase, and staff review and hires.
EDUCATION
Bradley B. Silverbush
Associate Scientist
B.S. Biochemistry, University of California, Davis, CA (1988)
EXPERIENCE
Present Associate Scientist, ALTA Analytical Laboratory
Mr. Silverbush performs routine analysis and method development work in the
High Resolution Mass Spectrometry department. He is responsible for routine
maintenance of HR/MS instruments and for the preparation, QC, etc. of all
Standards. In addition, Mr. Silverbush assists in the training of new staff,
reviews and interprets data, and interfaces with clients.
1990 -1991 GC/MS Chemist, Enseco-Cal Lab
As GC/MS Chemist at Enseco-Cal Lab Mr. Silverbush was responsible for the
operation and maintenance of quadrapole GC/MS instruments. His duties
entailed sample analysis by EPA methods for volatiles. He was also
responsible for the training of the staff in the department.
1988 -1990 Extraction Chemist, Enseco-Cal Lab
Duties entailed sample extraction for Dioxin/Furan Analysis by High
Resolution Mass Spectrometry. Involved with the training of new staff, and
the development of new extraction techniques.
QUALIFICATIONS
Mr. Silverbush has over 5 years experience in production analytical laboratories including 4
years experience in the field of environmental mass spectrometry. Much of this experience
has involved PCDD/PCDF analysis of environmental samples and for the last two years has
concentrated on High Resolution Mass Spectrometry analysis of PCDD's/PCDF's in a variety
of matrices.
PROFESSIONAL AFFILIATIONS
American Society for Mass Spectrometry
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CURRENT CERTIFICATIONS
Arizona Department of Health Services -(Certificate No.: AZ0058)
Tetra-Octa dioxins and furans in wastewater and drinking water by
EPA Method 1613A
Exp: 1012819 3
Commonwealth of Kentucky -(Certificate No.: 90063)
Dioxin in drinking water by EPA Method 1613A
Exp:12/31/93
New York State Department of Health -(Certificate No.: I 1411)
2,3,7,8-TCDD in potable water by EPA Method 1613A
Tetra-Octa dioxins in non-potable water by EPA Method 613
Exp:411/94
State of California -(Certificate No.: 1640)
Dioxins in drinking water by EPA Methods 513 and 1613A
Hazardous waste by EPA Methods 8280 and 8290
Wastewater by EPA Method 1613A
Exp:10131193 (Renewal pending)
State of Florida
Dioxins in drinking water by EPA Method 613 & 1613A
(Pending)
State of Tennessee -(Certificate No.: 02996)
Dioxins in drinking water by EPA Method 1613A
Exp:4/29/96
State of Utah -(Certificate No.: E-201)
Dioxins in drinking water by EPA Method 1613A
Exp:5131195
State of Wisconsin -(Certificate No.: 998036160)
Dioxins in drinking water by EPA Method 1613A
Exp:6130194
Washington Department of Ecology -(Certification No.: C091)
Wastewater for dioxin by EPA Method 1613A
Exp:3/26/94
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CERTIFICATIONS IN PROGRESS
State of Michigan
Dioxins in drinking water by EPA Method J613A
State of North Carolina ' Awaiting PE results before application can be submitted for certification of dioxins in drinking water.
State of Pennsylvania
Dioxins in drinking water by EPA Method 1613A
7-14-93