DSHW-2006-000906 - 0901a06880134ade

DEPARTMENT OF THE ARMY
US ARMY CHEMICAL MATERIALS AGENCY
TOOELE CHEMICAL AGENT DISPOSAL FACILITY
11620 STARK ROAD
STOCKTON, UTAH 84071
REPLYTO
ATTENTION OF:
May 16, 2006
Tooele Chemical Agent Disposal Facility
UTAH DIVISION OF
SOLID & HAZARDOUS WASTE
PM-60288
SUBJECT: Tesl Plan for Mustard (H/HT/HD) Decontamination Verification, Revision 0,
May 9, 2006
Mr. Dennis Downs, Director
Utah Department ofEnvironmental Quality
Division of Solid and Hazardous Wasle
288 North 1460 West
Salt Lake Cily, Ulah 84116-0690
Dear Mr. Downs:
The subject documenl is attached for your review and approval. The purpose ofthe lest
plan is to demonstrate that HT 4.2-inch mortars and HD ton containers, following thermal
treatment in accordance wilh TOCDF's RCRA (Part B) Permii, are below the Waste Control
Limil (WCL). Approval of this test plan will provide TOCDF the ability to recycle the Ireated
metal components, thus supporting our Environmental Management System initiatives. In order
to implement this tesl plan to support recycling in the early stages of musiard processing,
approval in early June is appreciated. This will ensure that TOCDF personnel are fully apprised
of all lest plan requirements well in advance of implementation.
If you have any queslions regarding this issue, please contact Ms. Elizabeth A. Lowes at
[phone] or Mr. Trace Salmon al [phone].
Sincerely,
/JosephR. Majestic^r.
//EG&G Defense Materials, Inc.
// •CERTIFICATION STATEMENT
hn K. Donnelly rh
OCDF Govemment Facilily Representative
•CERTIFICATION STATEMENT
Enclosure
Copies Fumished:
CMA Risk Management Directorate (Mr. Slang)
DCD Risk Management Directorate (Mr. Levi)
TOCDF FO Represeniative (Ms. Snow)
File
• I CERTIFY UNDER PENALTY OF LAW THAT THIS DOCUMENT AND ALL ATTACHMENTS WERE PREPARED UNDER MY DIRECTION OR SLIPERVISION IN ACCORDANCE WITH A SYSTEM DESIGNED TO
ASSURE THAT QUALIFIED PERSONNEL PROPERLY GATHER AND EVALUATE THE INFORMATION SUBMITTED. BASED ON MY INQUIRY OF THE PERSON OR PERSONS WHO MANAGE THI; SYSTEM. OR
THOSE PERSONS DIRECTLY RESPONSIBLE FOR GATHERING THE INFORMATION. THE INFORMATION SUBMITTED IS. TO THE BEST OF MY KNOWLEDGE AND BELIEF. TRUE. ACCURATE AND
COMPLETE. I AM AWARE THAT THERE ARE SlC.VIf ICANT PENALTIES FOR SUBMITTING FALSE INFORMATION. INCLUDING THE POSSIBILITY OF FINE AND I.WPRISO.NMENT FOR KNOWING
VIOLATIONS
HAND DELIVERED
MAY 1 9 2006
UTAH DIVISION OF
SOLID & HAZARDOUS WASTE
Tooele Chemical Agent Disposal Facility
(TOCDF)
Test Plan for Mustard (H/HT/HD)
Decontamination Verification
May 9, 2006
Revision 0
TABLE OF CONTENTS
1. [NTRODUCTION '
l.h Background
1.2, Objectives ;
1.3, Organization
1.4, Changes to the Plan
2. SAFETY CRITERIA 3
3. SAMPLING STRATEGY '. 3
3.1. Sampling Objective 3
3.1.1. Statistical Objective 3
3.1.2. Sampling Accuracy/Representativeness 3
3.1.3. Statistical Design for Determination of Sample Size 3
3.1.4. Sampling Precision 4
3.2. Test Item Selection Considerations 4
3.2.1. Preparation and Movement of Test Items : 4
3.2.2. Thermal Treatment of Test Items , 5
3.2.3. Operational Parameter Record Keeping Requirements 5
3.2.4. Preparation of Thermally Processed Test Items for Sampling : 5
3.2.5. Collection of Metal Samples...., 5
3.2.6. Sample Transport 6
3.2.7. Sample Receipt and Storage 6
3.2.8. Disposal 6
3.2.9. Logbook 6
3.3. Analytical Procedures - 7
3.3.1. Applicable Quality Assurance Program Plans 7
3.3.2. Laboratory Operating Procedures 7
3.3.3. Analytical Sample Numbers 7
3.3.4. Metal Samples 8
3.3.5. DAAMS Samples 8
3.3.6. Practical Quantitation Limits (PQL) 8
3.4. Instrument Calibration ,. 8
4. QUALITY ASSURANCE AND REPORTPNG 8
4.1. Quality Control Objective 8
4.2. QC Samples ' 9
4.3. QC Requirements 9
4.3.1. Method Detection Limit (MDL) Study 9
4.3.2. Precision ' 10
4.3.3. Accuracy 10
4.3.4. Completeness 11
4.3.5. Representativeness and Comparability 12
4.3.6. Data Review, Validation, and Verification Requirements 12
4.3.7. Identification and Treatment of Outliers 13
4.3.8. Waste Control Limit (WCL) Calculations......,, 13
4.3.9. Documentation and Records , 13
4.3.10. Reports to Management 13
4.3.11. Final Report 13
Test Plan for Musiard (H/HD/HT) Deconlamination VcFillcalion May 9, 2006
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APPENDICES
Appendix I, Glossary of Terms 15
Appendix 2. List of Acronyms and Units 16
FIGURES
Figure 1. Project Organization Chart 2
TABLES
Table 1. Number and Types of Samples 7
Table 2. Instrument Calibrations 8
Table 3. Summary of QA/QC Criteria for Metal Coupon Analyses 11
Table 4. Summary of QA/QC Criteria for DAAMS Tube Analyses 11
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L INTRODUCTION
1.1. Background
The U.S. Army has designed and built a hazardous waste disposal facility for the destruction ofthe
chemical agent munition stockpile stored at the Deseret Chemical Depot (DCD) located 20 miles south of
Tooele, Utah. This facility, called the Tooele Chemical Agent Disposal Facility (TOCDF), was designed
and-built to dispose of chemical agents GB (Sarin), VX, and mustard (H-series), drained munitions,
contaminated refuse, bulk containers, liquid wastes, explosives, and propellant components. Metal
components associated with the disposal process are thermally treated in the Metal Parts Furnace (MPF)
to ensure that the metal components meet, as a minimum, the Army criteria for the 5X level of
decontamination (1000 °F for at least 15 minutes). By Army definition, at the 5X level of
decontamination, the agent molecules have been completely degraded, Iteins that meet the 5X criteria
can be released for general use or sold to the general public. However, in accordance with the Utah
Administrative Code, Environmental Quality R315 Solid and Hazardous Waste requirement, any residue
from the chemical agent and munitions treatment is a listed hazardous waste and is classified and
manifested as F999. This F999 classification severely limits the opportunities for disposal.
This test plan applies to the following mustard-filled inetal components: HT 4.2-inch mortars and HD ton
containers (TCs). Due to the limited number of HD 4,2-inch mortars and the processing-related
deformation ofthe H 155nim projectiles, these items are not addressed. This test plan is designed to
demonstrate that residual agent in the metal components, after thermal treatment in the TOCDF MPF, is
below the Waste Control Limit (WCL).
Appendices 1 and 2 contain a glossary of terms and a list of acronyms and units used in this test plan,
1.2. Objectives
The objectives are twofold. First, to deinonstrate to the State of Utah, Department ofEnvironmental
Quality, Division ofSolid and Hazardous Waste (DSHW) that meta) components from mustard-filled
munitions thermally decontaminated in the MPF have no residual agent above the WCL. Second, if
successful, this project will demonstrate that metal components can safely be released from govemment
control and, results of this test program will support a petition for the removal ofthe Utah F999 hazardous
waste code if TOCDF elects to file such a petition.
1.3. Organization
As co-permittees of TOCDF, the Chemical Materials Agency (CMA) and EG&G have shared interest and
responsibilities for this test activity. EG&G/Battelle will perform all actions in completing these tests.
Actions include, but are not limited to, Test Planning, Test Performance, Test Validation, and Report
Generation. The project organization chart is depicted in Figure 1.
1.4. Changes to the Plan
To ensure that all test objectives and quality standards are met, this plan will be implemented as written.
Only the Test Director or his designee may approve deviations or changes to this test plan. If changes and
deviations are necessary, the Test Director will obtain DSHW concurrence before implementation.
Test Plan for Musiard (H/HD/HT) Decontaminaiion Verification M.Ty 9, 2006
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Figure L
Project Organization Chart
TOCDF
Sampling Team
TOCDF Maintenance
TOCDF Monitoring Branch
TOCDF
Test Director
TOCDF
Risk Management
QA/QC
Environmental Compliance
Safety
TOCDF
Chemical Assessment
Laboratory
• Laboratory Support (Extractions)
• DAAMS Support (DAAMS)
Battelle
• Data Evaluation & Reponin;
Tesl Plan for Mustard (H/HD/HT) Decontaminaiion Verification
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May 9, 2006
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2. SAFETY CRITERIA
All work will be performed in accordance with U.S. Army regulations, TOCDF site safety requirements
and applicable work planning and work control requirements. In addition, samples will be obtained and
analyzed in accordance with all applicable TOCDF Standard Operating Procedures (SOPs), Laboratory
Operating Procedures (LOPs), and Work Orders (WOs).
3. SAMPLING STRATEGY
3.1. Sampling Objective
The objective of these studies is to demonstrate that the thermally treated metal components associated
with mustard processing through the MPF have no residual agent above the WCL. The populations of
interest are the HT 4.2-inch mortars, HD ton containers, and their associated components. Two discrete
sampling/analytical events are plamied - one each for the HT 4.2-inch mortars and the HD ton containers.
These studies will statistically prove with a high level of confidence that no detectable agent above the
WCL remains in the metal components after the thermal decontamination process.
3.1.1. Statistical Objective
The statistical objective of this study is to determine with 99% confidence that mustard concentration
levels in the thermally treated metal (mustard-filled munitions) are less than the WCL.
3.1.2. Sampling Accuracy/Representativeness
Sampling accuracy/representativeness is achieved by random sampling ofthe population. Due to the
random nature of munitions in storage, any thermally decontaminated ton container processed through the
MPF is considered representative ofthe entire population of similar mustard-filled metal components.
3.1.3. Statistical Design for Determination of Sample Size
To meet the study statistical objective, the specific nurnber of HT 4.2-inch mortars and HD ton containers
required for sampling must be established. Statistical design for the determination of sample size was
completed through the use of EPA QA/G-4, "Guidance for the Data Quality Objectives Process," The
formula to be used for the sample size determination for each munition type was obtained from this
document and is as follows:
(z,.„+Z,_J'o' 1
"^ A^ ^2^-
Where: n = number of samples
Z = Standard nonnal values (from standard normal curve distribution tables)
A = U-AL
U = lower bound of the "gray region" = 40 ng/g (ppb) for H/HD/HT
AL= action level = WCL-200 ng/g (ppb) for H/HD/HT
Test Plan for Mustard (H/HD/HT) Decontamination Verification May 9, 2006
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The following values can be assigned to the equation for the determination of sample size:
a = sigma or standard deviation value to be obtained from the method detection
limit (MDL) studies at the WCL (1 Z) value (ppb)
a = 0,01 (Type 1 error, required to detect false positive error 99% ofthe time)
(3 =0.01 (Type II error, required lo detect false negative error 99% ofthe time)
Z|.a= Z up = Z] .0.01 = 2.33 (derived for one-tailed test for a Gaussian curve)
By substituting in the provided values the equation above reduces to:
(2.33 +2.33)'o' I ..,
n^- '-— +-2.33
(40-200)^ 2
or
« = (0.000848a-)+ 2.714
Using the values listed above, the number of samples («) required will be determined from MDL studies.
A sample standard deviation (estimate of a) of 40 ppb will yield a required sample size of five. Similarly
a sample standard deviation of 80 ppb would require a sample size of nine (all results are rounded up to
the next whole number).
3.1.4. Sampling Precision
Sampling precision is achieved by taking an appropriate number of samples from each population. The
calculations and statistical techniques used to determine the appropriate number of samples are shown
above.
3.2. Test Item Selection Considerations
For this project, two discrete sampling/analytical events are planned - one each during processing of HT
4.2-inch mortars and HD ton containers at normal conditions during their respective shakedown periods,
"n" samples, as defined in Section 3.1.3, from HT 4.2-inch mortars and HD ton containers will be
collected for testing. Due to the random nature ofthe munitions in storage, no extra measures will be
taken to define which items are selected and delivered by DCD for processing through the MPF.
Once the number of samples required ("«") is determined from the MDL studies, EG&G will collect these
samples from the trays currently being processed during the shakedown period.
HT 4.2-inch Mortars: Samples will be collected from "«" trays of mortars processed during the
shakedown period. One mortar, randotnly selected, will represent each ofthe "M" trays,
HD Ton Containers: Samples will be collected from "«" ton containers processed during the shakedown
period.
3.2.1. Preparation and Movement of Test Items
No special measures are required for either the HT 4.2-inch mortars or the HD ton containers.
Test Plan for Mustard (H/HD/HT) Deconlaminaiion Verification May 9. 2006
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3.2.2. Thermal Treatment of Test Items
The mustard test items will be processed and theimally decontaminated in the MPF using standard
operating parameters, which assure aminimum of 1000 °F for at least 15 minutes. Once the TCs have
been punched, the punched holes will then serve as the orientation to the top ofthe item.
3.2.3. Operational Parameter Record Keeping Requirements
Copies of selected MPF-related Process Data Acquisition and Recording System (PDARS) data will be
included in the final test report. This data will verify that the furnace operating conditions and process
time requirements were met for each test item processed.
3.2.4. Preparation of Thermally Processed Test Items for Sampling
After cooling on the MPF discharge conveyor, the processed 4,2-inch mortars and TCs will first be
vacuumed of any residual metal flakes, and then be transported to the Residue Handling Area (RHA).
Prior to sampling, Monitoring Branch personnel will posifion a portable Depot Area Air Monitoring
System (D/VAMS) apparatus in the RHA in the area of sample acquisition. The DAAMS apparatus will
be set up, and operated in accordance with TE-LOP-522.
3.2.5. Collection of Metal Samples
Sample coupons will be collected as described in this section for the MDL studies as well as the discrete
sampling events.
Sample coupons will be obtained by removing a circular sample with a 1.75" outside diameter hole saw
(or similar) from the lower portion ofthe mortars and from the low side (opposite the punched side) ofthe
TCs to ensure sampling from an area which had agent exposure during storage. "No cutting oil or
lubrication will be used while cutting the samples. The circular sample size will be approximately 1.7"
diameter. The thickness vvill be dependent on the exact sample location, but may range from
approximately 0.2" for mortars and will be approximately 0:5" for TCs,
Field duplicates will be taken in accordance with Section 4 of this plan. The Test Director will provide
the sampling schedule to DSHW to allow them the opportunity to witness the operation.
The TOCDF Control Room will initiate a sample/analysis request in accordance with PRP-OP-021 for
each set of samples. TOCDF monitoring personnel will then prepare sample/analysis forms, sample
containers, and sample labels in accordance with TE-LOP-534 for coupon samples. The location of
sampling will be recorded as the MPF burn tray number and the specific location on the bum tray for the
mortar being cut for samples. The location of sampling will be recorded as the specific serial number
assigned to the TC being cut for samples.
Work orders and a job hazard analysis will be generated in accordance with PRP-MG-015 for collection
ofthe coupons. Trained personnel will collect the coupons in the RHA. The Test Director wiil provide
technical oversight during the sampling process. During the drilling process, personnel will wear
appropriate Personal Piotective Equipment (PPE), Personnel will measure the surface temperature ofthe
area to be cut for the sample just before and immediately after the drilling using an infrared thermometer
(or, similar). The results will be recorded in the field logbook.
During sampling, the DAAMS apparatus will sample approximately two feet above the cutting area for
the sole purpose ofsupporting the metal analysis results. The results will not be related to worker health
Test Plan for Musiard (H/HD/HT) Decontaminaiion Verification May 9, 2006
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and safety monitoring conducted at DAAMS locations throughout the plant. Three DAAMS tubes will bc
aspirated during the process to provide an "A" and "B" tube. The third tube will serve as the QP (to be
spiked in the lab). The single set of three DAAMS tubes will be used throughout the sample collection
process for each mortar or ton container sampled.
One sample will be collected from each ofthe mortars and TCs identified for sampling. Multiple samples
may be collected from a single TC or mortar for use in the MDL studies. Four additional coupons will be
collected from one mortar and TC. One ofthe extra coupons will be used as the sample duplicate, the
second will be used for a matrix spike (MS), the third will be used as a matrix spike duplicate (MSD), and
the fourth will be used as a lab control sample (LCS). Additional quality control (QC) samples will be
collected in accordance with Tables 1, 3, and 4.
The coupons will be placed in the open sampling containers provided by Monitoring Branch personnel.
Monitoring Branch personnel will seal the samples, and complete sample chain-of-custody documentation
for the samples collected in accordance with TE-LOP-534.
Personnel performing the work shall ensure that hazardous waste that is expected to be generated will be
handled in accordance with PRP-SA-046 and PRP-OP-022. Personnel performing the work shall also
ensure that the work area is clean and tools are returned to proper locations when the work is complete.
3.2.6. Sample Transport
Monitoring Branch personnel will deliver the samples to the laboratory in accordance with TE-LOP-534.
3.2.7. Sample Receipt and Storage
At (he Chemical Assessment Laboratory (CAL), an individual trained and authorized will receive and
store the samples in accordance with TE-LOP-597.
3.2.8. Disposal
Sample and analytical residues will be properly managed in accordance with TE-LOP-553. Since the
sample and analytical residues are similar in nature to other wastes generated at TOCDF, they will be
disposed of in consonance with waste management and disposal protocols already in place.
3.2.9. Logbook
Monitoring personnel will record sampling information pertinent to sampling in a sampling log. The log
will be bound and have consecutively numbered pages. All entries will be made in indelible ink and all
corrections will follow the prescribed error correction protocols of one line through the eiTor and initial
with date of correction also annotated. Sampling personnel will also record all information on the
appropriate sampling forms.
At a minimum, entries in the logbook will include the following:
• Purpose of sampling
• Location and description ofthe sampling
• Documentation of procedures for preparation of reagents or supplies which become an integral part of
the sample (e.g., DAAMS tubes)
• Idenfification of sampling crew members
Test Plan for Musiard (H/HD/HT) Decontaminaiion Verification May 9, 2006
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Type of sample
Number of samples taken
Sampling methodology
Surface temperatures measured before and after cutting of metal coupons
Date and time of collection
Collector's sample identification number(s)
Sample transportation method
General observations
Sample containers, preservative
Deviation from the sampling methods (and approval initials)
3.3. Analytical Procedures
3.3.1. Applicable Quality Assurance Program Plans
The TOCDF Participant Quality Assurance Plan (PQAP) (CDRL 22) and the TOCDF Laboratory Quality
Control Plan (LQCP) will be followed for this project. The revisions of these plans current at the time of
the test will apply.
3.3.2. Laboratory Operating Procedures
Where applicable, the approved Laboratory Operating Procedures already in place will be used and
followed. As required, work orders will be generated in accordance with PRP-MG-015.
3.3.3. Analytical Sample Numbers
The CAL will be responsible for the preparation ofthe QC samples and analysis ofthe samples.
Laboratory QC samples include preparation blanks, quality control plant samples (QPs), and quality
control laboratory samples (QLs). Table 1 lists the expected number of samples for analysis.
Table 1.
Number and Types of Samples
.....Samples^ ^;.:J
1 DAAMS A tube
I DAAMS B tube
I Metal Sample
%• "i."' QC;SainplS-" j:
IDAAMSQP
1 Metal Sample Duplicate
1 Metal Matrix Spike (MS)
1 Metal Matrix Spike Duplicate (MSD)
1 Metal Lab Control Sample (LCS)
1 Preparation Blank
';;f-SamplingJE"requencj^'
Per TC or mortar
Per 20 TCs or mortars'
If less than 20 TCs or mortars are sampled, then one complete sel ofthe QC samples lisied will be
collecled.
Test Plan for Mustard (H/HD/HT) Decontamination Verification
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3.3.4. Metal Samples
Metal samples and QC samples will be extracted and analyzed in accordance with this plan using a
Laboratory work order that will be developed and approved after completion ofthe MDL studies. The
total number of samples to be collected and analyzed for each 5X study will be determined from the
standard deviation ofthe WCL (1 Z) results from the MDL studies.
3.3.5. DAAMS Samples
DAAMS samples will be analyzed in accordance with TE-LOP-562. QPs spiked at the 1 Z Single Cycle
Vapor Screening Limit (VSL) equivalent will be analyzed along with the samples.
3.3.6. Practical Quantitation Limits (PQL)
The PQL for mustard is 200 ng/g (ppb) for extraction analysis and 15 ng for DAAMS. The PQL
corresponds to 1 WCL for extraction analysis and 0.5 VSL for a five-minute aspiration at 1.00 L/min.
This, according to chemical stockpile disposal programmatic guidelines, is defmed as the reportable limit
(RL).
3.4. Instrument Calibration
Prior to analysis, instrument calibration status will be verified by QLs, as required by TE-LOP-562
(DAAMS) or TE-LOP-572 (Extracts). If necessary, instruments will be calibrated (or recalibrated) in
accordance with Table 2.
Table 2.
Instrument Calibrations
|., Method
i
DAAMS
Extraction
.., .Ahaiytical a
EquipmenL '
GC
GC
|> Calibration
Three Point
Calibration
Three Point
Calibration
Calibrjation
V ...^Q0:ks •••••
QLper
TE-LOP-562
QLper
TE-LOP-572
..^Talet'- 1
• ..Criteria
• t%>.:. ;.. .
Correlation
Coefficient
> 0.995
Correlation
Coefficient
> 0.995
4. QUALITY ASSURANCE AND REPORTING
4.1. Quality Control Objective
The overall objective ofthe measurement data is to demonstrate that thermally decontaminated metal
components associated with mustard munitions have no residual agent above the WCL.
Test Plan for Musiard (H/HD/HT) Decontamination Verification
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4.2. QC Samples
The types of QC samples that will be used to document the validity ofthe generated data are described
below:
• Preparation Blank - A preparation blank is chloroform, hexane, or methylene chloride analyzed
in the same proportion and by the same method as samples. The preparation blank is prepared
from the same lot of solvents used to extract agent from the samples. It is analyzed on the same
sequence as the extracted samples. The preparation blank also serves as the reagent blank,
• Lab Control Standard (LCS) - A sanded., clean metal coupon spiked with 1 WCL equivalent of
mustard prior to extraction. The LCS determines the accuracy ofthe laboratory results.
• Matrix Spike (MS) - A mortar or TC sample spiked with 1 WCL equivalent of mustard prior to
extraction.
• Matrix Spike Duplicate (MSD) - A duplicate mortar or TC sample spiked with 1 WCL equivalent
df mustard prior to extraction.
• Quality Control Laboratoiy Sample (QL) - A QC standard prepared independently of calibration
standards to verify the accuracy ofthe analytical calibrafion standard solufions and to verify
instrument control status.
• Quality Control Plant Sample (QP) - DAAMS sample spiked with mustard and then analyzed to
determine a percent recovery, QPs demonstrate the analyfical sensitivity and matrix bias.
Extraction QPs also provide sample extraction efficiencies.
• Metal Sample Duplicate - Duplicate field samples that provide estimates of precision for sample
results greater than the MDL.
4.3. QC Requirements
4.3.1. Method Detection Limit (MDL) Study
One MDL study will be performed on HD TC coupons. The results will be used as the basis for both the
HD TC and HT mortar 5X tests since both munitions were manufactured from carbon steel. The MDL
study will be conducted in accordance with the requirements ofthe TOCDF LQCP and 40 CFR Part 136,
Appendix B to prove the extraction and analytical methodologies. The HD TCs selected for the cutting of
metal coupon samples for the MDL studies will have been previously processed through the MPF.
The coupons will be spiked with an appropriale amount of agent, detennined as outlined in Section 4.3.8,
and then immediately extracted with chloroform, hexane, or methylene chloride, concentrated, and
analyzed. The extraction methodology will be based on methods commonly used for extraction of
mustard from solid matrices (i.e., TE-LOP-572).
The metal coupon MDL study will be performed by analyzing a minimum of 7 spiked coupons. The
MDL will be calculated in accordance with 40 CFR Part 136, Appendix B,
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4.3.2. Precision
Precision is defined as the degree of mutual agreement among individual measurements made under
prescribed conditions. Duplicate samples will be collected for the metal coupons and a precision value
will be calculated. Precision goals for extractions have been included in Table 3.
Precision will be calculated for laboratory duplicate analysis using the following equation:
RPD = •x,+x,
/
xlOO
Where: RPD = Relative Percent Difference
Xl = Analytical Result of Sample
X2 = Analytical Result of Duplicate
4.3.3. Accuracy
Accuracy is the degree of agreement of a measurement to an accepted reference or true value. The
accuracy will be determined from analysis of samples spiked with a known concentration. Accuracy
objectives have been set and are presented in Tables 3 and 4. The formula which will be used to assess
the accuracy ofthe laboratory QA/QC data (e.g. matrix spike analysis) is as follows:
%R =
{QSS - Qus) xlOO
Where: %R = Percent recovery
Qss = Quantity of Analyte Found in the Spike Sample
Qus = Quantity of Analyte Found in the Unspiked Sample
Qs = Quanfity of Added Spike
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Table 3.
Summary of QA/QC Criteria for Metal Coupon Analyses
iOiialitylEaraiiietef
Preparation Blank
QL
MS
MSD
LCS
Holding Time
^Method/Erequency ;
1 per 20 mortars or
TCs
Per TE-LOP-572
I per 20 mortars or
TCs
1 per 20 mortars or
TCs
1 per 20 mortars or
TCs
-
§%,... • •.Criteria^ti3;-4,/i,
<RL
100 ± 25%
Based on MDL Study
as approved by DSHW
Based on MDL Study
as approved by DSHW
Based on MDL Study
as approved by DSHW
30 Days
.:'S'.- 60rrect;ive^ctionj._ •^;-';
Per TE-LOP-572.
Per TE-LOP-572.
Per TE-LOP-572.
Per TE-LOP-572.
Reanalyze samples.
Resample
Table 4.
Summary of QA/QC Criteria for DAAMS Tube Analyses
1 •«-'• ^; •'; *-f.''-
Quality Parameter
Preparation Blank
QL
QP
Holding Time
Method/Frequency
Analyzed with
calibration standards
Per TE-LOP-562
Per TE-LOP-562
-
Criteria
<RL
100 ± 15%tf>0.3ng
100+ 35% if <0.3ng
IOO ±40%
72 hours
-^i. ' ^,''»:-5 ,••'»;?:•"•' ••> •:• ^-if: •• ^'.-l
; Corre1|Hve:Actiofc.; '-
Determine source of
contamination.
Reanalyze.
Assess impact on data.
Narrate.
Per TE-LOP-562.
Per TE-LOP-562.
Record and Report
4.3.4. Completeness
Completeness is defined as the amount of valid data from a measurement system compared to the amount
that was expected under optimal normal conditions. Completeness should be 100%.
Completeness will be reported as the percentage of all measurements judged to be valid. Every attempt
will be made to ensure that all data generated will be valid data. If data appears questionable based on
circumstances that occurred or were observed during either the field sampling or laboratory analyses (i.e.,
sampling or analytical methods were not followed, unreasonable results, or equipment), it will be flagged
and an explanation provided.
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4.3.5. Representativeness and Comparability
Representativeness is defined as the degree to which data accurately and precisely represent a
characteristic of a population, parameter variations at a sampling point, process condition, or an
environmental condition. Comparability is defined as expressing the confidence with which one data set
can be compared to another.
It is recognized that the usefulness ofthe data is also contingent upon meeting the criteria for
representativeness and comparability. The statistical design provided in Section 3.1.3 will insure that the
mortars and ton containers sampled represent the population of mustard items. Comparability will be
insured by using standard analytical methods and procedures, chemical agent standard analytical
reference materials (CASARMs), and QC and sample duplicates.
4.3.6. Data Review, Validation, and Verification Requirements
Data validation is the process of accepting or rejecting data on the basis of established criteria. The QC
persormel will use validation methods and criteria appropriate to the type of data, even those judged to be
an "outlying" or spurious value. The persons validating the data will have sufficient knowledge (i.e., at
least one year experience in data validation) ofthe sampling and analytical methods to identify
questionable values and deviations from criteria specified in the LOP, WO, or the TOCDF LQCP.
Field sampling data will be validated by TOCDF based on a judgment ofthe representativeness ofthe
sample, maintenance and cleanliness of sampling equipment, and the adherence to TOCDF approved
procedures or work orders. All field data will be recorded in the field sampling logbook. The field
sampling logbooks will be reviewed to ensure that each entry is properly completed. Any discrepancies
or errors will be noted and/or corrected.
QC personnel, using criteria outlined in this document, will validate analytical and sampling data. The
results from the field and laboratory QC samples will be used to further validate analytical results. The
QA/QC personnel will review all laboratory and sampling raw data to verify calculated results reflect
consistency, meet applicable QC criteria and do not contain transmittal errors.
The following criteria will be used to evaluate the field sampling data:
• Use of approved test procedures or work orders.
• Proper operation of the process being tested.
• Use of properly operating and calibrated equipment.
• Proper sample traceability maintained.
The criteria listed below will be used to evaluate analytical data:
• Use of approved analyfical procedures.
• Use of properly operating and calibrated instrumentation.
• Precision and accuracy achieved should be comparable to that achieved in previous analytical
programs and consistent with the objectives stated in the TOCDF LQCP.
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4.3.7. Identification and Treatment of Outliers
Any QC blanks or sample results yielding values above the RL analysis will be repeated in triplicate. In
these instances appropriate measures will be taken to identify and eliminate interferences and/or potential
contamination. Additional samples may be required for sample results above the RL. Out of control QP
or QL results will be handled in accordance with the applicable LOP.
4.3.8. Waste Control Limit (WCL) Calculations
Calculations used to determine the appropriate mustard spike concentrations that correspond to the WCL
(200 ng/g) curve are defined in this section. Methods will be developed during the MDL study to ensure
that the calibration range specified in TE-LOP-572 covers from 0.2 WCL to 1.5 WCL,
It is anticipated that the oxide layer characteristics for mustard items manufactured from carbon steel, i.e.,
4.2-inch mortars and ton containers, are similar to those determined during the GB 5X Decontamination
Study. The mustard spike will be determined based on the surface area ofthe test coupons and an oxide
density of 0.12 g/cm' (determined during the GB 5X Study). Based on the expected test coupon
dimensions, the mustard spike will be as follows:
• The drilled coupon dimensions will be approximately 1.7 inches (43 mm) in diameter with an
oxide layer surface area of approximately 2.27 in' (14.52 cm').
• The MDL study will be based on a 1.74 g sample (i.e., 0.12 g/cm' x 14.52 cm').
• From the previous calculation, the amount of mustard corresponding to the WCL would be 348
ng (i.e., 200 ng/g X 1.74 g).
4.3.9. Documentation and Records
Reports and documentation will be provided as identified in this test plan. They will be submitted to
DSHW through the TOCDF Field Office for final approval and will be filed by EG&G for any future
reference.
Personnel will use standardized forms and field notebooks to ensure completeness, traceability, and
comparability ofthe process information and samples collected. A second person will conduct field
checks ofthe standardized fonns and records to ensure accuracy and completeness. Verification will be
documented.
4.3.10. Reports to Management
If any corrective action is required during the program, these actions will be reported immediately to the
Test Director. If the Test Director determines that an event should be repeated, the decision will be made
at that point and will be communicated to those involved.
4.3.11. Final Report
The final Test Report will contain as a minimum the following items:
• Executive Summary
• Test Program Introduction
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Summary of Events
Analytical Results
Results of MPF Operating Parameters as recorded by PDARS
Quality Assurance/Quality Control Summary
Additional Documentation (e.g., calibration data)
Statistical Analysis (if applicable)
Copies of Signed Test Change Request Letters (if applicable)
Discussion of any results including anomalies
Conclusions
Analytical results in the final report will include the following:
Project Narrative, which includes a summary ofthe test, any quality problems found, and
corrective actions taken.
Sample results including sample identification numbers, sample description, sampling date and
time, mustard analysis result, and the reporting limit.
Chain of Custodies (COCs)
Copies of raw data, which includes analytical run sequence logs, chromatograms for the
calibration curve and standards, sample chromatograms, extraction analysis worksheets, QC
sample results, and QP analysis worksheets.
MDL study results and associated raw data
Compilation and evaluation of analytical calibration and QA/QC data, and identification of
problems encountered and the solutions implemented.
Summary of sampling and analytical methods used and any deviations from referenced methods.
Copies of log books and laboratory notebooks
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Appendix 1. Glossary of Terms
Limit of Quantification (LOQ): The lowest true (target) analyte concentration that 97.5 percent (l-a) of
the fime results in 97.5 percent (1-P) confidence the agent is detected by the method or monitoring
system. Here a is the risk that agent is present but not reportable by the method or monitor, and p is the
risk that agent is reportable by the method or monitor when no agent is present. This limit can be
determined graphically from the upper and lower limits ofthe 95 percent confidence interval around the
regression line. For the purposes of this test plan, the reportable limit (RL) will be used instead ofthe
LOQ: it should be noted that the RL must be greater than or equal to the LOQ. The true LOQ for Class 1
analysis methods will be established during the MDL study.
Reportable Limit (RL): Reporting level equivalent to 0.2 WCL or 0.5 VSL. The FIL must be greater than
or equal to the LOQ.
Wasle Control Limit (WCL): The WCL refers to a control standard for monitoring wastes, which is 200
ng/g for musiard (H/HD/HT).
5X (XXXXX): Indicates, as defined by Department ofthe Army (DA) Pamphlet 385-61, Toxic Chemical
Agent Standards, Paragraph 5.1(c)(3), that an item has been decontaminated completely ofthe indicated
agent and may be released for general use or sold to the general public in accordance with all applicable
federal,-state, and local regulations. An item is decontaminated completely when the item has been
subjected to procedures that are known to completely degrade the agent molecule. Or, when analyses,
submitted through Major Army Command (MACOM) and DA channels for approval by the Department
of Defense Explosives Safety Board, have shown that the total quantity of agent is less than the minimal
health effects dosage as determined by the United States Surgeon General. One approved
decontamination method is heating the item to 1000 °F for 15 minutes.
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Appendix 2. List of Acronyms and Units
CAL
cm'
CMA
DA
DAAMS
DCD
DSHW
EPA
op
g
g/cm'
LCS
LOQ
LOP
LQCP
MACOM
MDL
mm
MPF
MS
MSD
ng
ng/g
PDARS
ppb
PQAP
PQL
PPE
QA
QC
QL
QP
RHA
RL
RPD
SOP
TC
TOCDF
VSL
WCL
WO
Chemical Assessment Laboratory
square centimeters
Chemical Materials Agency
Department ofthe Army
Depot Area Air Monitoring System
Deseret Chemical Depot
State of Utah, Department ofEnvironmental Quality,
Waste
U.S. Environmental Proteciion Agency
Degrees Fahrenheit
grams
grams per square centimeter
Lab Control Sample
Limit of Quantificafion
Laboratory Operating Procedure
Laboratory Quality Control Plan
Major Army Command
Method Detecfion Limit
millimeter
Metal Parts Furnace
Matrix Spike
Matrix Spike Duplicate
nanogram
nanograms/gram
Process Data Acquisiiion and Recording Sysiem
Part per billion
Participant Quality Assurance Plan
Practical Quantitation Limit
Personal Protective Equipment
Quality Assurance
Qualily Control
Quality Control (Lab) Sample
Quality Control (Plant) Sample
Residue Handling Area
Reportable Limil
Relative Percent Difference
Standard Operating Procedures
Ton Container
Tooele Chemical Agent Disposal Facility
Vapor Screening Limit
Waste Control Liinil
Work Order
Division ofSolid and Hazardous
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