r/EPA
United States
Environmental Protection
Agency
Dynamic Field Activity Case Study:
Treatment System Optimization,
Umatilla Chemical Depot
      Plant Influent

lead



EAST

Mid-GAC
Sampling
Point
BANh




r
pol



                                   Effluent „.
                                   Sampling Plant Effluent
                                    Point
                  WEST
                lead
                   Mid-GAC
                   Sampling
                    Point
                BAN
                     polish

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                                Office of Solid Waste and
                            Emergency Response (5201G)
                                    EPA/540/R-02/007
                                 OSWERNo. 9200.1-45
                                      December 2002
Dynamic Field Activity Case Study:
 Treatment System Optimization,
     Umatilla Chemical Depot

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                                      Notice

This document has been funded by the United States Environmental Protection Agency (EPA)
under Contract 68-W-02-033. The document was subjected to the Agency's administrative and
expert review and was approved for publication as an EPA document. Mention of trade names
or commercial products does not constitute endorsement or recommendation for use.

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                              Acknowledgments

The Office of Emergency and Remedial Response would like to acknowledge and thank the
individuals who reviewed and provided comments on draft documents.  The reviewers include
EPA Headquarters and regional offices, state environmental programs, United States Department
of Defense, United States Department of Energy, and representatives from the private sector.

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                                 Contents
Exhibits	iv

Abbreviations 	  v

Abstract  	  1

Background  	  1

Original Treatment System Design	  2
      Analytical Method Selection	  3
      Initial Year of Operation	  4

Dynamic Optimization Study	  4

Cost Savings Analysis  	  5
      Optimized Treatment System Savings	  7
      Cost Savings of Using Field-Based Analytical Method  	  9
            Cost of RDX/TNT Colorimetric Method	  9
            Cost of SW-846 Method 8330	  9
            Total Savings  	  10

Lessons Learned 	  10
      Method Requirements Must Be Clearly Provided to the Contractor	  11
      Site-Specific Matrices May Require Method Modifications  	  11
      FAM Data Were Essential for the Optimization Process	  11
      Undocumented Analytical Issues May Exist for a Well-Researched Method . .  11

References	  13

Appendix A
      Treatment System Analytical Costs	  A-1

Appendix B
      Standard Operating Procedures for Analysis of TNT and RDX in Groundwater
      Using  Colorimetric Method	  B-1
                                     MI

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                                 Exhibits
Number                            Title                               Page

1     Groundwater Remediation Requirements	 2
2     Schematic Drawing of Umatilla Chemical Depot
      Groundwater Treatment Plant System	 3
3     Comparison of Dynamic Optimization Study Scenarios 2, 4, and 6	 6
4     Comparison of Dynamic Optimization Study Scenarios 1, 3, and 5	 7
5     Comparison of Water Treatment Cost for Each Scenario Tested	 8
                                    IV

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                                  Abbreviations
1,3-DNB     1,3-dinitrobenzene
1,3,5-TNB    1,3,5-trinitrobenzene
2,4-DNT     2,4-dinitrotoluene
2,6-DNT     2,6-dinitrotoluene
Ce           concentration of effluent
C;           concentration of influent
DEQ         Department of Environmental Quality
EPA         U.S. Environmental Protection Agency
FAM        field-based analytical methods
GAC         granular activated carbon
GPM        gallons per minute
HMX        high melting explosive
HPLC        high performance liquid chromatography
mg/L        micrograms per liter
NB          nitrobenzene
O&M        operation & maintenance
OU          operable unit
QC          quality control
RDX        Royal Demolition Explosive
RI           remedial investigation
ROD         record of decision
TNT         trinitrotoluene
UMCD       Umatilla Chemical Depot

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                          Operation and Maintenance
               Umatilla Chemical Depot, Hermiston, Oregon
Abstract

       The Army used a dynamic field activity (i.e., a project that combines on-site data
generation with on-site decision making) to optimize the treatment system at the Umatilla
Chemical Depot in 1999.  The use of field-based analytical methods (FAMs) allowed them to
maximize the usefulness of granular activated carbon and minimize the number of samples sent
to a fixed laboratory for confirmation.  The data provided by the FAMs met project requirements
and improved the overall project quality control by providing rapid feedback on treatment
problems as they occurred. Since its implementation, the optimized treatment system has been
providing the Army with an annual savings of at least 45 percent.
Background

       The Umatilla Chemical Depot (UMCD) was established as an Army ordnance depot in
1941 for the purpose of storing and handling munitions. It covers nearly 20,000 acres in
northeastern Oregon in Morrow and Umatilla Counties, approximately five miles west of
Hermiston, Oregon, and six miles south of the Columbia River. In 1988, UMCD was included in
the Department of Defense's Base Realignment and Closure (BRAC) Program, which required
its conventional  ordnance storage mission to be transferred to another installation.

       Beginning in the 1950s, UMCD operated an explosives washout plant on site. Munitions
were opened and washed with hot water to remove and recover explosives. The plant was
cleaned weekly,  and the wash water, which contained high concentrations of explosives, was
disposed of in two nearby unlined lagoons. The lagoons received a total of about 85 million
gallons of wash water during plant operations. Although lagoon sludges were removed regularly
during operation, explosives contained in the wash water percolated through the soil and into the
groundwater below the lagoons.

       A CERCLA remedial investigation (RI) of the explosives washout lagoons was initiated
in 1988 to determine the nature and extent of contamination.  Investigators discovered a 330-acre
groundwater plume  in an unconfmed sandy aquifer made up primarily of Royal Demolition
Explosive (RDX) with concentrations ranging up to 6,816 |_ig/L.  Trinitrotoluene (TNT) was also
in the groundwater at elevated concentrations (3,900 |ig/L), but the TNT was generally confined
to the area under and near the lagoons. In 1994, the Record of Decision (ROD) for the
groundwater operable unit (OU) selected groundwater extraction and granular activated carbon
(GAC) treatment as the remedy.  Exhibit 1 lists the chemicals of concern and their associated
cleanup levels.

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                                      Exhibit 1
                     Groundwater Remediation Requirements
Chemicals of Concern
Hexahydro-1,3,5-trinitro-1,3,5-triazine(RDX)
2,4,6-trinitrotoluene (TNT)
1 ,3,5-trinitrobenzene (1 ,3,5-TNB)
1,3-dinitrobenzene (1,3,-DNB)
2,4-dinitrotoluene (2,4-DNT)
2,6-dinitrotoluene (2,6-DNT)
Octahydro-1 ,3,5,7-tetranitro-1 ,3,5,7-tetrazine (HMX)
Cleanup
Criteria
2.1 |jg/L
2.8 |jg/L
1.8|jg/L
4.0 |jg/L
0.6 |jg/L
1.2|jg/L
350 |jg/L
Highest
Concentration
6,816 |jg/L
3,900 |jg/L
441 |jg/L
24.4 |jg/L
497 |jg/L
5.3 |jg/L
1,448|jg/L
       The Army Corps of Engineers (the Corps), in coordination with EPA, took responsibility
for the design and operation of the treatment system. By using FAMs in the operation of the
treatment plant and by undertaking a dynamic optimization process, the BRAC Cleanup Team,
which included the Corps, the Corps' contractor, Oregon Department of Environmental Quality
(DEQ), and EPA, demonstrated a quantifiable savings in the plant's annual operational expenses
of greater than 45 percent, which represents a cost reduction of approximately $180,000 per year.
In addition, unquantifiable savings were achieved through better treatment plant quality control
(QC).
Original Treatment System Design

       Startup of the treatment system occurred in January 1997. Three extraction wells pumped
approximately 1,300 gallons per minute (gpm) of contaminated groundwater to two parallel
treatment lines, each containing two tanks with 20,000 pounds of GAC. Exhibit 2 presents a
schematic drawing of the treatment system. Water entered the treatment area in a single pipe that
split to feed two parallel systems that each contained a lead tank and a polishing tank. Water
exiting the polishing tanks of each system was recombined before it was piped into three aquifer
recharge areas. Twenty-seven groundwater monitoring wells and the three extraction wells were
used to evaluate the progress and effectiveness of the cleanup. These wells were sampled on a
regular schedule. The sample analysis was performed by an off-site laboratory to get a complete
evaluation of all the contaminant levels.

The original  operating procedure for each of the tank systems included sampling the water at a
port in the piping between the lead and polishing tank (i.e., mid-GAC) on a weekly basis and
analyzing the samples using an on-site colorimetric method. Based on FAM results, when
concentrations of RDX exceeded 5 pg/L at a mid-GAC port, the system was shut down.  Water

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                                     Exhibit 2
                 Schematic Drawing of Umatilla Chemical Depot
                      Groundwater Treatment Plant System
       Plant Influent,
                       lead
                            EAST
                              Mid-GAC
                             Sampling
                               Point
BANf-
         polish
                 Effluent  _,   ,_„,
                 Sampling Plant Effluent
                  Point
samples were then collected for off-site analysis from each mid-GAC port and from the effluent
sampling point to confirm that breakthrough had occurred in at least one of the lead tanks and
that no breakthrough had occurred in the polishing tanks. Because the reliability of the FAM
data had already been demonstrated prior to designing the procedure, the contents of both lead
tanks were changed out for off-site regeneration before confirmatory data were received.  The
minimally contaminated polishing tank then became the lead tank. RDX was chosen as the
primary chemical to monitor because it was the contaminant with the highest concentration and
the lowest affinity for the GAC, therefore, it would be the first chemical exhibiting breakthrough.
Analytical Method Selection

      Before designing the treatment system, the Corps and EPA conducted a study of all the
available commercial and emerging FAMs to determine if any could be used for RDX and TNT.
Their search uncovered three methods for RDX and five methods for TNT, all of which were
classified as either immunoassay, colorimetric, continuous flow immunosensor, or fiber optic
biosensor.  All were tested and compared with SW-846 Method 8330, which utilizes high
performance liquid chromatography (FIPLC). Method 8330 has documented quantitation limits
of 0.84 |_ig/L for RDX and 0.11 |_ig/L for TNT.
      Based on the results of these tests, the colorimetric method was selected. It demonstrated
detection limits of 3.8 |_ig/L for RDX and 0.9 |_ig/L for TNT (Craig et al., 1996), which was

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acceptable because the action level set at the mid-GAC sampling port was 5 pg/L for RDX (the
team has since shown that the site specific detection limit for RDX is 2.0 pg/L).  The Standard
Operating Procedures for FAMs used at UMCD can be viewed at:
http://www.epa.gov/superfund/programs/dfa/casestudies.
Initial Year of Operation

      During the initial year of operation, the BRAC Cleanup Team encountered two incidents
that demonstrated the FAM was providing an added layer of QC protection. The first occurred
after one routine change out.  The FAM results indicated that the treatment system effluent
contained 16 |_ig/L RDX so the system was immediately shut down.  A subsequent investigation
indicated that not all of the spent GAC had been removed from the tank when the GAC was
replenished. If off-site analysis with the normal turnaround time of three weeks had been used to
minimize analytical costs, the contaminated discharge would have continued during that period.
In the second incident, FAM data allowed the team to correct a problem with a corroded butterfly
valve that was allowing contaminated influent water to bypass the lead carbon unit.  Again, the
use of off-site analysis as the sole source of analytical data would have resulted in contaminated
groundwater bypassing the lead GAC unit for several weeks before the problem was caught and
corrected.

      Although the startup period indicated that the FAM was providing significant benefits for
the project by providing a high level of QC and by meeting the project requirements, other
aspects of the treatment system seemed to be inadequate. The primary problem that the system
operator noticed was that breakthrough was occurring on the lead tanks much sooner than
expected, resulting in a very high expenditure on GAC.  After some discussion, the BRAC
Cleanup Team decided to perform an optimization study that would seek to reduce the systems
operating costs.
Dynamic Optimization Study

       To determine areas where efficiencies could be gained, the Corps reviewed the entire
treatment system design. Initially, the study examined the system design parameters (e.g., size of
the unit, flow rate, type of charcoal, and regeneration and charcoal make-up process). One
problem they found and fixed immediately was that the type of GAC they were using did not
contain an adequate pore size to effectively remove RDX from groundwater.  By changing the
GAC specification they were able to significantly improve the treatment system.

       Another problem they discovered involved the system flow rate, which was providing too
little contact time for the RDX.  Because changing the system to provide an adequate dwell time
involved expensive redesign and construction, the BRAC Cleanup Team set out to improve the
system's efficiency and lower operating costs with the existing design.  The team decided that the

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best method of optimizing the system was to determine the most cost effective use of GAC and
treatment monitoring analysis for the project as a whole, rather than as individual components.
As a result, they developed and tested five sampling and analysis scenarios over four test cycles
of carbon change-out starting in December 1997.  After the first two test cycles, the team added a
sixth scenario that would accommodate changes in contaminant concentrations over time.  A
summary and comparison of all six scenarios is presented in Exhibits 3 and 4.

       The exhibits show the conditions for sampling and analysis for each scenario.  The start-
up conditions are the same for each, with RDX and TNT being tested with FAMs at the mid-
GAC and effluent points. Each of the subsequent rows describes the sampling protocol that was
used for each phase of the different scenarios.  They describe where samples are collected (e.g.,
mid-GAC), the conditions for their collection (e.g., on a weekly basis), the analytical method
used (e.g., FAM for RDX), and the conditions for ending or changing the sampling and analysis
strategy (e.g., RDX values exceed 5 jig/L at mid-GAC).

       Scenario 2 represents  the initial, or baseline, treatment design in which the system was
shut down and the GAC of the first tank was replaced as soon as concentrations at the point
between the two tanks (i.e., mid-GAC) exceeded 5 pg/L RDX. The new scenarios allowed RDX
concentrations at the mid-GAC to substantially exceed 5 pg/L because the GAC in the lead tank
had not been optimally loaded, and the polishing tank, with careful observation, prevented the
plant's effluent from exceeding the cleanup criteria.

       The BRAC Cleanup Team took a dynamic approach to improve efficiency based on
evaluations of the data being generated. For instance, the sixth scenario involved sampling
decisions based upon an innovative approach of using the ratio of the RDX concentrations
between the effluent at the mid-GAC point (Ce) and the influent to the treatment system (C;).
When the ratio was less than 0.25, they would collect samples once  every two weeks. As
concentrations at the mid-GAC increased, and the ratio of Ce/C; was between 0.25 and 0.50,
samples would be collected once a week. Once the ratio of concentrations rose above 0.50,
samples would be collected daily until break through in the lead tank was detected. These
sampling protocols would allow the lead tank GAC to be fully utilized.

       The results of the first three test cycles were used to select the two most cost effective
scenarios for comparison during the fourth test cycle.  These were scenarios 4 and 6. Based on
the findings of the fourth test cycle, scenario 6 was selected  as the most cost effective option.
Exhibit 5 presents a summary of treatment  cost data for each scenario through the four test
cycles.
Cost Savings Analysis

       There are two useful ways of calculating cost savings for this case study: to compare the
cost of the optimized treatment design with the cost of the original treatment design; and to
compare the cost of using the FAM as part of the system design with using the off-site analysis

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                                          Exhibit 3
         Comparison of Dynamic Optimization Study Scenarios 2, 4, and 61
Activity
Start-up
1st
Sampling
Protocol
ond
Sampling
Protocol
3rd
Sampling
Protocol
4*
Sampling
Protocol
Sample Location
FAM
8330
Sample Location
FAM
Rate
Condition
8330
Sample Location
FAM
Rate
Condition
8330
Sample Location
FAM
Rate
Condition
8330
Sample Location
FAM
Rate
Condition
8330
Scenario 2
(original design)
Mid-GAC and Effluent
RDX and TNT
None
Mid-GAC
RDX Weekly
< 5 ppb
None
Mid-GAC and Effluent
RDX Not Applicable
> 5 ppb = shutdown
(Mid-GAC)
Mid-GAC and effluent
confirmation @ shutdown
Scenario 4
Mid-GAC and Effluent
RDX and TNT
None
Mid-GAC
RDX Weekly
< 150 ppb
None
Effluent
RDX Every other day
> 150 ppb, until
breakthrough at effluent
Mid-GAC and effluent
confirmation @ shutdown

Scenario 6
Mid-GAC and Effluent
RDX and TNT
None
Mid-GAC and Effluent
RDX
Not Applicable
Begin on week 5
None
Mid-GAC andEffluent
RDX
0<
Every other
week
Ce/Ci) < 0.25
None
Mid-GAC and Effluent
RDX
Every week
0.25 < (Ce/Ci) < 0.50
None
Mid-GAC and Effluent
RDX
3 per week
(Ce/Ci) > 0.50, until RDX
breakthrough
Mid-GAC and effluent
confirmation @ shutdown
alone.  The following discussion provides an estimate of the quantifiable benefits of using FAMs
in the optimized treatment system.
              1 Each of the six scenarios used different sampling protocols that dictated the type and
       frequency of analyses.  For scenario 2, the original sampling design, there were only two protocols
       used after startup. As long as RDX concentrations at the mid-GAC were below 5 ppb, samples
       were collected weekly. Once mid-GAC concentrations exceeded 5 ppb, the system would be
       shutdown and samples would be collected at the mid-GAC and effluent for analysis with SW-864
       Method 8330.

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                                         Exhibit 4
         Comparison of Dynamic Optimization Study Scenarios 1, 3, and 5
Activitv
Start-up
1st
Sampling
Protocol
ond
Sampling
Protocol
3rd
Sampling
Protocol
Sample
Location
FAM
8330
Sample Location
FAM Rate
Condition
8330
Sample Location
FAM Rate
Condition
8330
Sample Location
FAM Rate
Condition
8330
Scenario 1
Mid-GAC and Effluent
RDX and TNT
None
Mid-GAC
RDX Weekly
< 50 ppb
None
Mid-GAC
RDX 3 per week
100 ppb
Mid-GAC during
sampling scheme
Mid-GAC and Effluent
RDX Every other day
>100 ppb mid-GAC, until
breakthrough @ effluent
Mid-GAC and effluent
confirmation ©shutdown
Scenario 3
Mid-GAC and Effluent
RDX and TNT
None
Mid-GAC
RDX Weekly
< 100 ppb
None
Mid-GAC
RDX Bi-weekly
< 200 ppb
None
Mid-GAC and Effluent
RDX Every other day
>200 ppb mid-GAC, until
breakthrough @ effluent
Mid-GAC and effluent
confirmation @ shutdown
Scenario 5
Mid-GAC and Effluent
RDX and TNT
None
Mid-GAC
RDX Weekly
< 150 ppb
None
Mid-GAC and
Effluent
RDX Not Applicable
>150 ppb =shutdown
(Mid-GAC)
Mid-GAC and effluent
confirmation @ shutdown

Optimized Treatment System Savings

       Although the optimization study cannot be used to directly compare scenario 2 (the
original treatment design) with scenario 6 (the optimized treatment design),2 a minimum cost
savings can be extrapolated from the study by first comparing the cost difference between
scenarios 2 and 4 in cycle I, then by comparing the cost difference between scenarios 4 and 6 in
cycles HI and IV. In cycle 1, scenario 4 ($0.344/1,000 gallons) is about 30 percent less expensive
than scenario 2 ($0.486/1,000 gallons).  In cycles IE and IV, scenario 6 ($0.344 and
$0.371/1,000 gallons) is 5 to 18 percent less expensive than scenario 4 ($0.360 and $0.449/1,000
               Treatment costs for scenario 2 in cycles II, III, and IV were not representative because
       the treatment system protocols for scenario 2 called for a completely new lead tank to be installed
       as soon as breakthrough occurred at the mid-GAC, whereas during the optimization study the lead
       tank was partially loaded with RDX to accommodate the other five scenarios. Direct comparison
       is further complicated by the fact that RDX influent concentrations fell from 700 \igfL in cycle I to
       300 ng/L in cycle IV.

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                                          Exhibit 5
           Comparison of Water Treatment Cost for Each Scenario Tested
Test
Cycle
Number


1





II





III





IV



Scenario
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
Carbon
Cost3
$0.162
$0.280
$0.163
$0.162
$0.169
N/A
$0.275
$0.856
$0.275
$0.280
$0.350
N/A
$0.123
$0.343
$0.123
$0.123
$0.183
$0.123
N/A
N/A
N/A
$0.152
N/A
$0.152
Analytical
Cost3
$0.143
$0.117
$0.097
$0.097
$0.114
N/A
$0.196
$0.198
$0.157
$0.160
$0.200
N/A
$0.199
$0.128
$0.158
$0.154
$0.106
$0.138
N/A
N/A
N/A
$0.213
N/A
$0.135
Other O&M
Cost3
$0.085
$0.089
$0.085
$0.085
$0.085
N/A
$0.089
$0.109
$0.089
$0.089
$0.091
N/A
$0.083
$0.091
$0.083
$0.083
$0.085
$0.083
N/A
N/A
N/A
$0.084
N/A
$0.084
Total Cost3
$0.390
$0.486
$0.345
$0.344
$0.368
N/A
$0.560
$1.16
$0.521
$0.529
$0.641
N/A
$0.405
$0.562
$0.364
$0.360
$0.374
$0.344
N/A
N/A
N/A
$0.449
N/A
$0.371
         'Costs are calculated per 1,000 gallons.
gallons).  Therefore, scenario 6 should be at least 30 percent less expensive than scenario 2. The
treatment system currently treats approximately 600,000,000 gallons per year.  An extrapolation
of this estimate indicates that the optimized system is saving approximately $95,000 in operating
expenses per year.4
              4 The yearly operating cost for scenario 2 based on cycle I would have been $291,600;
       the yearly operating cost for scenario 4 based on cycle I would have been $206,400; since scenario
       6 was 5 to 18 percent less expensive than scenario 4 in cycles III and IV, a conservative
       extrapolation results in a yearly operating cost of $196,080 ($206,400 minus 5 percent) for
       scenario 6 in cycle I. The estimated savings are therefore $95,520.
                                              8

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       Another check on this estimate is to examine the number of days the GAC lasted before
and after the optimization system was initiated.  Previously, the GAC required removal after 40
to 60 days, even after the more appropriate GAC was used. The new system, however, allowed
the GAC to last between 125 and 170 days over the first four cycles of its use. While this
comparison provides only a rough indication of the impact of the new treatment design and does
not attempt to estimate the affect of decreasing concentrations over time, it does provide
corroborating evidence that the new protocols are more efficient in their use of GAC than the
original system.
Cost Savings of Using Field-Based Analytical Method

       Although the previous calculation provides ample evidence for the financial benefits of
optimizing a groundwater treatment system using FAMs, it does not measure the full impact of
this approach because many project managers use only off-site analysis for treatment system
monitoring.  Consequently, it is useful to determine the cost savings of this project compared
with what it might have cost if FAMs were not considered at all.
Cost of RDX/TNT Colorimetric Method

       The cost of the FAM from the manufacturer was $24 per analysis.  Since RDX and TNT
require two separate analyses, the two together cost $48.  However, when the cost of labor,
expendables, data validation, and data management are also considered, the FAM cost the project
$237.70 for analysis of RDX and $289.99 for both RDX and TNT.  A detailed breakdown of
how these costs were derived is provided in Appendix A.
Cost of SW-846 Method 8330

       The off-site laboratory contracted to run Method 8330 charged $275 for regular
turnaround (3 weeks, providing results on all nitroaromatics and nitroamines).  The fully loaded
cost (labor, shipping, data validation, and data management) of an analysis for the project was
$466.26 (see Appendix A for detailed costing information). However, if Method 8330,
conducted at an off-site laboratory, were the only source of analytical data, 36-hour turnaround
would be required at an additional cost of $400. Because a 36-hour turnaround was very rarely
used by the project, the fully loaded cost is not available, however, it would likely be
approximately $600 per sample based on the fully loaded cost of the regular turnaround off-site
samples.

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Total Savings

       The first step in calculating the additional project savings from using FAMs is to estimate
the cost increase of using quick turnaround off-site analysis in place of the analytical procedures
used in the original treatment system design.  Although the exact figure is difficult to calculate
because both off- and on-site analyses were used in these protocols (i.e., scenario 2), this
calculation can be simplified by observing that at each sampling event, the analytical cost would
have, at a minimum, doubled if off-site analysis were the only method (see Exhibits 3 and 4).
For example, during startup, RDX and TNT were analyzed with FAMs at an analytical cost of
$290. Had off-site analysis been used, the cost would have been $600. Therefore, the analytical
cost of the original treatment design would have been at least twice the amount found in the
optimization study's scenario 2 of cycle I. These analytical protocols would result in a total
project cost of $0.603 per 1,000 gallons5. The same logic used to estimate the savings from
scenario 6 may be used to derive the total project savings.  Consequently, because scenario 4 is
45 percent less expensive than  scenario 2 (in cycle I) would have been if it had used only off-site
analysis, scenario 6 must be at  least 45 percent less expensive as well. Therefore, total project
savings  are approximately $180,000 per year (i.e., approximately twice the savings of $95,000
calculated for the optimized system versus the original system).

      Moreover, additional, unquantifiable, savings have been demonstrated by having the data
available in the field to make site operating decisions.  As mentioned earlier, rapid sample
analysis enabled a timely resolution to  a leaking valve problem and a carbon change-out mistake.
Consequently, these data have resulted in better project QC and more effective site remediation.
Likewise, it was this increased  confidence in the project's QC procedures that provided
regulators with the security  to allow a plant operating strategy that completely utilizes the GAC
until breakthrough  is documented at the final effluent point.
Lessons Learned

       Although the capabilities and limitations of the FAM for this groundwater pump-and-
treat system were thoroughly researched before it was selected, a number of problems were
discovered during the initial stages of its integration into the project. The lessons learned from
this experience include:

•      Method requirements must be clearly provided to the contractor;
•      Site-specific matrices may require method modifications;
•      FAM data were essential for the optimization process; and
•      Undocumented analytical issues may exist for well researched methods.
              5 FromExhibit 5: analytical cost of $0.117 X 2 = $0.234 + $0.369 (GAC and O&M) =
       $0.603

                                           10

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Method Requirements Must Be Clearly Provided to the Contractor

       During the project start-up period, the on-site laboratory was unable to produce the
detection limits that a Corps researcher had documented. By investigating the problem, the
BRAC Cleanup Team discovered a number of problems that had been caused by the contractor's
misunderstanding of the method requirements. First, the FAM operator was neither a chemist
nor had she been  properly trained because the contractor did not understand the level  of expertise
that was needed to perform the work.  Second, the laboratory facilities were inadequate because
there was no running water within the trailer where the analyses were taking place. Third, cross-
contamination was a problem because both the trailer used for analysis and the path for accessing
water was dirty.  Finally, some of the equipment selected was inadequate, such as pumps that did
not provide enough suction for filtration.  Consequently, it is critical that the project manager
write a statement of work in such a way that contracting firms understand the level of training
and qualifications necessary to perform and interpret the analysis and the conditions required for
setting up the field laboratory.
Site-Specific Matrices May Require Method Modifications

       The BRAC Cleanup Team initially was unable to obtain the required level of perfor-
mance from the FAM due to the high levels of nitrates in the groundwater. By working with the
method developers, the team was able to make modifications to improve performance for the
site-specific matrix.  To ensure that the modifications were properly documented, the site-
specific SOPs for RDX and TNT analyses were also modified.
FAM Data Were Essential for the Optimization Process

       The BRAC Cleanup Team found that their ability to analyze RDX and TNT within hours
enabled them to proceed with the treatment plant optimization process. If the team had not been
able to assess and report contaminant concentrations in the effluent water quickly, regulators
would not have allowed the treatment plant to completely use the GAC units before they were
replaced.
Undocumented Analytical Issues May Exist for a Well-Researched Method

       The BRAC Cleanup Team discovered a number of significant issues affecting the results
during the project start-up period as well as once the project was fully implemented even though
the reliability of the FAM had been thoroughly tested in a laboratory. Their findings  included:

•      Method blanks should be run with each batch to identify contamination problems.
                                          11

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Analyst-specific response curves should be developed because several steps in the
method are very sensitive to analyst technique.
Blank spikes developed with a second source standard and run through the extraction and
analysis procedure provide valuable information on data quality.
It is critical that the analyst note the color of the colorimetric response because an
elevated absorbance reading, due to particulate matter, can be misinterpreted.
Dinitroaromatic  compounds will cause a false positive response.
The method is very sensitive to the brand of acetone, deionized water, and reagents used.
The method is heat and possibly light sensitive, consequently, the work station requires a
constant temperature.
                                     12

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                                    References
Craig, H., G. Ferguson, A. Markos, A. Kusterbeck, L. Shriver-Lake, T. Jenkins, and P. Thorne.
1996. Field demonstration of on-site analytical methods for TNT and RDX in groundwater.
Proceedings of the Great Plains-Rocky Mountain Hazardous Substance Research Center
(HSRC)AVaste Education and Research Consortium (WERC) Joint Conference on the
Environment, Albuquerque, NM, May 21-23, 1996. http://www.engg.ksu.edu/HSRC/96Proceed/
craig.pdf

Crockett, A.B., H.G. Craig, and T. Jenkins.  1999.  Field Sampling and Selecting On-site
Analytical Methods for Explosives in Water. Federal Facilities Forum Issue, EPA/600/S-99/002,
U.S. Environmental Protection Agency,  http://www.epa.gov/tio/tsp/download/water.pdf

EnSys.  1997. TNT Soil Test System, Strategic Diagnostics Inc. Newark, DE.
http://www.sdix.com/PDF/Products/nsystnt.pdf

EnSys.  1998. RDX Soil Test System, Strategic Diagnostics Inc., Newark, DE.
http ://www. sdix. com/PDF/Products/nsy srdxpp. pdf

Jenkins, T.F., P.G. Thorne, M.E. Walsh. 1994. Field Screening Method for TNTandRDXin
Groundwater, CRREL Special  Report 94-14, U.S. Army Corps of Engineers.

Remtech, Inc. 2000. Field Sampling Plan for Treatment System Operation and Maintenance
Services, Contaminated Groundwater Remediation, Explosives Washout Lagoons, Umatilla
Chemical Depot Hermiston, Oregon, Revision 1. West Richland, Washington.

Remtech, Inc. 2000. Quality Assurance Project Plan for Treatment System Operation and
Maintenance Services, Contaminated Groundwater Remediation, Explosives Washout Lagoons,
Umatilla Chemical Depot Hermiston, Oregon, Revision 1.  West Richland, Washington.

Remtech, Inc. 2000. Standard Operating Procedures for Analysis of TNT and RDX in
Groundwater Using Colorimetric Method.  West Richland, Washington.

USAGE. 1998.  Remedial Action Report: Contaminated Groundwater Remediation Project,
Explosives  Washout Lagoons, Groundwater Operable Unit, Umatilla Chemical Depot. Seattle
District, U.S. Army Corps of Engineers.

USAGE. 1999.  Breakthrough Study and Plant Optimization Report, Umatilla Chemical Depot.
Seattle District, U.S. Army Corps of Engineers.
                                         13

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USEPA.  1994c. Method 8330: Nitroaromatics and nitroamines by high performance liquid
chromatography (HPLC). Test Methods for Evaluating Solid Waste, Physical/Chemical Methods,
SW-846.  Office of Solid Waste, Washington, DC.
http://www.epa.gov/epaoswer/hazwaste/test/main.htm

USEPA.  1996.  Explosives in Water Field Screening Technologies UMDA and SUBASE Bangor
(draft). Prepared by Black & Veatch Special Projects Corp., Tacoma, WA, for U.S.
Environmental Protection Agency Region 10, Project Number 71370.

USEPA.  1997.  Test Methods for Evaluating Solid Waste, SW-846. Office of Solid Waste,
Washington, DC. http://www.epa.gov/epaoswer/hazwaste/test/main.htm
                                         14

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                            Appendix A
                 Treatment System Analytical Costs
             Field Sampling and Analysis Costs (RDX and TNT)
Description
Labor
Sampling Labor
Extraction and Analysis
QA Review/Reporting
Database and Statistics
Administration and Other
Direct Labor Subtotal
Fringe® 33. 75%
Labor and Fringe Subtotal
Test Kits
EnSys Kit
Subtotal
Supplies
Empore Filters w/10% loss
Glass fiber filter
Test tubes
Alumina-A Cartridge
Acetone
Syringe and 0.45 filter
Sample Bottles
Misc. foil, DI water, vials
Subtotal
Equipment
Vacuum Flasks
Vacuum Pump
Filter Apparatus
Photometer
Misc. Bottles, Tubing, etc.
Subtotal
ODCs and Labor/Fringe Subtotal
G&A@ 18.27%
Total Estimated Cost
Fixed Fee @ 10%
Grand Total
Quantity
Units
Unit Rate (S)
Cost/Sample (S)

0.25
2.00
1.00
0.50
1.00
Lh*
Lh
Lh
Lh
Lh
31.70
16.83
27.79
27.79
27.79
7.93
33.66
27.79
13.90
27.79
111.06
37.48
148.55

1
each
24.00
24.00
24.00

2
1
2
1
100
1
2
2
each
each
each
each
ml
each
each
each
9.35
0.30
0.80
1.75
0.01
3.00
4.00
2.50
18.70
0.30
1.60
1.75
1.00
3.00
8.00
5.00
39.35

1
1
1
1
1
each
each
each
each
each
100.00
448.00
173.00
1700.00
100.00
2.00
1.00
4.00
3.00
1.00
11.00
222.90
40.72
263.62
26.36
289.98
* Labor hours
                                A-1

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           Field Sampling and Analysis Cost (RDX only) per Sample
Description
Labor
Sampling Labor
Extraction and Analysis
QA Review/Reporting
Database and Statistics
Administration and Other
Direct Labor Subtotal
Fringe® 33. 75%
Labor and Fringe Subtotal
Test Kits
EnSys Kit
Subtotal
Supplies
Empore Filters w/10% loss
Glass fiber filter
Test tubes
Alumina-A Cartridge
Acetone
Syringe and 0.45 filter
Sample Bottles
Misc. foil, DI water, vials
Subtotal
Equipment
Vacuum Flasks
Vacuum Pump
Filter Apparatus
Photometer
Misc. Bottles, Tubing, etc.
Subtotal
ODCs and Labor/Fringe Subtotal
G&A@ 18.27%
Total Estimated Cost
Fixed Fee @ 10%
Grand Total
Quantity
Units
Unit Rate (S)
Cost/Sample (S)

0.25
1.50
0.50
0.25
1.00
Lh*
Lh
Lh
Lh
Lh
31.70
16.83
27.79
27.79
27.79
7.93
25.25
13.90
6.95
27.79
81.80
27.61
109.41

1
each
24.00
24.00
24.00

2
1
1
1
75
1
2
2
each
each
each
each
ml
each
each
each
9.35
0.30
0.80
1.75
0.01
3.00
4.00
2.50
18.70
0.30
0.80
1.75
0.75
3.00
8.00
5.00
38.30

1
1
1
1
1
each
each
each
each
each
100.00
448.00
173.00
1700.00
100.00
2.00
1.00
4.00
3.00
1.00
11.00
182.71
33.38
216.09
21.61
237.70
* Labor hours
                                   A-2

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        Fixed Laboratory 8330 Sampling and Analysis Cost per Sample
Description
Labor
Sampling Labor
Packaging and Shipping
QA Review/Reporting
Database and Statistics
Administration and Other
Direct Labor Subtotal
Fringe® 33. 75%
Labor and Fringe Subtotal
Other Direct Costs
Shipping Costs
Sample Bottles
Bubble Wrap, Ice, PPE, etc.
Cooler Replacement
Subtotal
Laboratory Costs
8330 Analysis
EOF
Subtotal
ODCs and Labor/Fringe Subtotal
G&A@ 18.27%
Total Estimated Cost
Fixed Fee @ 10%
Grand Total
Quantity
Units
Unit Rate (S)
Cost/Sample (S)

0.25
0.50
2.00
0.50
1.00
Lh*
Lh
Lh
Lh
Lh
31.70
31.70
27.79
27.79
27.79
7.93
15.85
55.58
13.90
27.79
121.04
40.85
161.89

1
1
1
1
each
each
each
shipment
15.00
4.00
2.00
0.50
15.00
4.00
2.00
0.50
21.50

1
0.25
each
package
150.00
100
150.00
25.00
175.00
358.39
65.48
423.87
42.39
466.26
* Labor hours
                                   A-3

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                                  Appendix B
             Standard Operating Procedures for Analysis of
	TNT and RDX in Groundwater Using Colorimetric Method	

      The following standard operating procedure (SOP) was developed by the Army Corps of
Engineers for use at the Umatilla Chemical Depot.  It is repeated below as it appeared in their site
specific Sampling and Analysis Plan. The procedure includes a modification to account for high
nitrate levels in the water.
Description

      This SOP describes a field analytical method for determining TNT and RDX
concentrations in water. The method uses solid phase extraction to remove and pre-concentrate
the analytes from water. In the method, a 2 L water sample is passed through a stack of two
membranes to pre-concentrate TNT on the top disk and RDX on the bottom disk. Acetone is
used to elute RDX from the bottom disk, and a chemical reaction is induced that causes a color
change indicative  of RDX in the solution. The RDX concentration is estimated from the
absorbence at 510 nm on a Hach DR2000 spectrophotometer. Next, the top disk is eluted with
acetone and a different chemical reaction is induced causing a color change indicative of TNT.
The TNT concentration is  estimated from the absorbence at 540 nm on the Hach DR2000.  The
contract required detection limit for TNT is 1.0 |_ig/L and for RDX is 5  pg/L.  Sample extraction
and analysis may take between 1.5 and 5 hours per sample depending on the number of parallel
extraction apparatus.
Safety Precautions

•     Extraction and analysis should be performed in a well ventilated area.

•     Laboratory technicians should wear chemical resistant gloves and safety glasses.


Extraction Procedure

Materials Needed (per sample)

      2 Empore extraction membranes
      aluminum  foil
      2 25x200 mm glass test tubes
      filter flask apparatus
      vacuum pump
      tweezers
      timer (minutes/seconds)

                                       B-1

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Reagents Needed (per sample)

       2 L of sample
       acetone, technical grade
       DI water
       tap water/DI water/acetone for cleaning
Pitfalls
       Never let the disks go dry. Throw the disks out and start over if they do. Keep the disks
       covered with at least 1A inch of fluid during the extraction phase.

       Apply the vacuum gradually so as not to damage the membranes. If you see particles in
       the acetone extracts at this point, vacuum was applied too suddenly.

       Do not shake the sample prior to filtering.
Procedure

1.      Use gloves during the entire procedure.

2.      Use tweezers to place two Empore extraction membranes centered on the lower portion
       of the filter apparatus; cover squarely with the upper portion of the filter apparatus and
       clamp securely. Do not touch the membranes with your hands. A glass fiber filter may
       also be used to remove particulate.

3.      Slowly add 30 ml acetone to the stack and allow it to soak for 10 minutes.

4.      Slowly apply vacuum to the filter flask apparatus until there is minimum dripping of
       acetone (evidence that both filters are completely saturated). Shut off vacuum; add 10 ml
       of D. I. water. Let set for 10 minutes or until about 1A inch of liquid remains, whichever
       occurs first. The next two steps go quickly, so have materials measured and in place
       before starting.

5.      Fill the reservoir with sample before the fluid level is reduced to 1A inch.  Reapply
       vacuum ever so slightly. The sample may be filtered through at a rate of 10 to 100
       ml/min.

6.      Continue filling the reservoir until 2 L of sample has penetrated the membrane.  Do not
       allow the fluid level to fall below 1A inch until the entire sample has been passed through.
                                          B-2

-------
7.      Add 10 ml of DI water to the reservoir just before the last of the sample penetrates into
       the membrane. This will aid in washing out the nitrate interference.

8.      Continue to apply vacuum for about 2 minutes after the last of the sample has been
       extracted. This is to remove excess water.

9.      Remove the upper portion of the filter apparatus from the filter stack and discard the glass
       fiber filter, if used.

10.    Remove both the disks and set them face up on a clean piece of aluminum foil marked
       "T" for top disk and "B" for bottom disk, these will be  used later for your TNT and RDX
       extracts.

11.    Reassemble the filter apparatus and rinse first with DI water and second with acetone.

12.    Disassemble the filter apparatus and pour the water from the 2,000 ml Pyrex flask into a
       waste container.

13.    Wash a 25 x 200 mm tube with DI water, rinse with acetone, label the tube (RDX or
       TNT, sample number, date), place it in the flask, and replace the funnel.

14.    Place the RDX disk membrane (bottom) on top of the lower portion of the filter
       apparatus. Reassemble the filter stack.

15.    Add 7 ml of acetone to the reservoir and soak for exactly 3 minutes.

16.    Apply vacuum and aspirate acetone into the 25x200 mm tube until dripping stops.

17.    Remove the membrane and discard. Cap the 25 x 200 mm test tube. If possible, samples
       should be analyzed on the day of extraction.  Otherwise, the meniscus should be marked
       on the test tube and the tube refrigerated. If the fluid level falls below the meniscus line,
       the tube should be refilled with acetone to its original level.

18.    Reassemble the vacuum apparatus with the TNT (top) disk, which was set aside in Step
       10 and a fresh 25 x 200 mm test tube (washed as described in Step 13).

19.    Add 25 ml acetone to the reservoir and allow soaking for exactly 3 minutes.

20.    Apply vacuum and aspirate into the 25 x 200 mm tube. Cap the 25 x 200 mm  test tube. If
       possible, samples should be analyzed on the day of extraction. Otherwise, the  meniscus
       should be marked on the test tube and the tube refrigerated.  If the fluid level falls below
       the meniscus line, the tube should be refilled with acetone to its original level.
                                          B-3

-------
21.     Decontaminate the reservoir and filter holder by washing with tap water, rinsing with DI
       water, and final rinsing with acetone.

22.     Collect all liquids generated during the decontamination process for incorporation into
       the treatment plant process.
RDX Analysis

Materials Needed (per sample)

       10 ml syringe with 0.45 |_im filter
       2 13 ml holding vials
       30 ml syringe with 0.45 |_im filter
       desiccator and desiccants
       Alumina-A filter
       2 matched Hach cuvettes/stoppers
       Hach DR2000 set to 510 nm
       5 ml syringe with 0.45 |_im filter
       50 ml reaction vial
       analytical balance
       Kimwipes™
       spatula
       Miscellaneous glass volumetric pipettes, flasks, and graduated cylinders


Reagents Needed (per sample)

       5 ml acetone, technical grade
       Hach NitriVer 3 powder pillow
       20 ml DI water
       0.2 g of zinc dust, 100 to 325 mesh
       RDX Standards for laboratory control
       Miscellaneous amounts of tap water/DI water/acetone for cleaning
       0.75 ml of acetic acid solution (77 percent glacial acetic acid and 23 percent DI water)
Pitfalls
       The reaction of the acidified extract with zinc is the most crucial step in obtaining
       consistent and correct results. The step should be done as quickly as possible (10 seconds
       at the longest).  The reaction is also temperature dependent and should be performed in a
                                          B-4

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       cool setting. If the extract was refrigerated, make sure the extract is between 60-80 °F
       before beginning the analysis.

       The zinc syringe should be tapped gently so that the zinc is at the bottom of the syringe
       before removing the plunger.

•      Check the filters at the bottom of the syringes to make sure that they are securely fastened
       before adding extract.

       Some samples may display a milky or cloudy appearance even after being filtered into the
       sample cuvette. These samples should be re-filtered and the cuvette cleaned. If the
       extract is still cloudy, read and record the absorbence, make a note of the cloudiness in
       the laboratory log, and indicate that this is a false positive. If a pink color also is present,
       this should be taken as a positive reaction for RDX; however, the associated result will be
       biased high.

•      Make sure that the NitriVer pillow is completely dissolved in the reaction vessel
       containing 20 ml water.  Do not let this solution sit for more than 10 minutes before
       using.

•      Be sure to record the volumes used for all dilutions, not just the dilution factor.  This will
       aid in checking for any mathematical errors.

       Let the bubbles dissolve before reading the absorption.

       Store the zinc dust and prepared zinc syringes in the desiccator.

•      The test also will show a positive reaction for HMX.


Preparation Before Analysis

Using the spatula, place approximately 0.2 g of zinc dust into the barrel of a 5 ml syringe with a
0.45 jam filter attached.  Replace the plunger.  Store all zinc syringes in a desiccator with
desiccant for at least 24 hours before they are used.


Procedure

1.      Condition the alumina-A filter with 5 ml of acetone. Pour 5  ml of acetone into the 10 ml
       syringe with the alumina-A filter.  Let the acetone filter through at a rate of one ml per
       minute.
                                           B-5

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2.      Shake the 10 ml syringe dry and reuse for the next step.

3.      Pour 5 ml of extract into the 10 ml syringe with the alumina-A filter. Filter the extract
       into a labeled 13 ml holding vial. Filter at a rate of 1 ml per minute.

4.      Pour 5 ml of extract into the 10 ml syringe with attached filter. Filter the extract into a
       labeled 13 ml holding vial. Reserve the remaining 1 ml extract for possible dilutions.

5.      Add 0.75 ml of the acetic acid solution to each 13 ml holding vial.  Shake to mix and set
       aside for several minutes.

6.      Add 20 ml DI water to a 50 ml reaction vessel.  If the reaction vessel came supplied with
       DI water, remove the supplied water before adding fresh DI water.  Add the NitriVer
       pillow to the 50 ml reaction vessel.  Shake until completely dissolved.  If batching
       samples, be sure to label the reaction vessel. Let set for at least 5 minutes but no longer
       than 10 minutes.

7.      Slowly remove the plunger of the 5  ml zinc syringe, shaking the powder down. Holding
       the syringe over the reaction vessel, pour the extract into the 5 ml zinc syringe. Replace
       plunger, invert once and filter rapidly into the 50 ml reaction vessel containing 20 ml DI
       water.  This step must be done as quickly as possible, approximately within 10 seconds.

8.      Shake the reaction vessel to mix and wait at least 10 minutes, but no longer than 15
       minutes, for color to develop.

9.      Filter the sample into a clean DR2000 cuvette. Note in the laboratory logbook any
       obvious color.

10.    Zero the instrument and obtain a background absorbence. (see Operation of Hach
       DR2000)

11.    Read the absorbence of the sample and record along with any color changes.

12.    Between samples, clean the cuvettes with DI water and acetone (in that order)  using a
       stopper and shaking vigorously.

13.    Periodically check that the instrument is correctly reading zero with the reference cuvette.

14.    Calculate the concentration of the extract using the following equation:

                            RDX (|_ig/L) = Ai x DF x VCF x RF

       where
                                           B-6

-------
             Ai = (absorbence of sample - absorbence of blank)
             DF = dilution factor
             VCF = volume correction factor is equal to 1.4 when the extraction volume is 7
             ml
             RF = response factor is listed in the laboratory

For sample concentrations where the absorbance is greater than 0.800, the reserved sample
extract should be diluted with acetone, taken through the reaction steps, and the absorbance read
and recorded.
TNT Analysis

Materials Needed (per sample)

       30 ml syringe with 0.45 |_im filter attached
       Hach DR2000 set at 540 nm
       2 matched Hach cuvettes/stoppers
       Miscellaneous glass volumetric pipettes, flasks, and graduated cylinders


Reagents Needed (per sample)

       Developer solution
       DI water/acetone for rinsing
       TNT standard for laboratory control


Pitfalls

       The test will also react for TNB and DNT.

•      If the extract was refrigerated make sure the extract is between 60-80 °F before beginning
       the analysis.


Procedure

1.      Zero the instrument and obtain a background absorbence. (see Operation of Hach
       DR2000)

2.      Pour 25 ml of extract into a 30 ml syringe with attached filter. Filter the sample into the
       sample cuvette.


                                         B-7

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3.      Read and record the initial absorbence.

4.      Add one drop of EnSys TNT developer solution.

5.      Shake tube continuously for 3 seconds.

6.      Read the final absorbence and record. Also note any color present in the extract and how
       the color developed.

7.      Periodically check the instrument is correctly reading zero with the reference cuvette.

8.      Calculate the concentration using the following equation:

                      TNT (|_ig/L) = [Af - (2 x Ai)] x DF x VCF x RF
       where
             Ai = initial absorbence
             Af = final absorbence
             DF = Dilution factor
             VCF = volume  correction factor equal to 1.25 for 25 ml extraction volume
             RF = response factor listed in the laboratory

Samples with TNT final absorbencies grater than 0.800 require dilutions.  Use the reserved
sample extract, perform the analysis, and record the results.


Quality Control/Quality Assurance

       A laboratory control standard should be analyzed each day that an analysis is performed,
and is used to verify that the analysis portion of the procedure is performed acceptably. The
absorbence must be within 0.307 to 0.373 for RDX and 0.174 to 0.272 for TNT for the test to be
in control.  If the standard is not in control, try again, paying particular attention to the zinc step.

       A blank must  be extracted each day that samples are  extracted.  The method blank and its
associated samples should all be analyzed at the same time. The blank must be clean and
colorless. If any  contamination is noted, review the glassware cleaning procedures or possible
sources of cross contamination. Note problem and resolution in the logbook.

       A blank spike must be extracted each week that samples are extracted. This blank spike
is used to verify that the extraction portion of the procedure is being performed in an acceptable
manner. A 2 L portion of DI water should be spiked with RDX and/or TNT and carried through
the extraction procedure. Spike in 80 |_il of a standard solution in acetone containing RDX and/or
TNT at 500 mg/L each. The concentration of standard in the final extracts will be 20 |_ig/L.  The

                                          B-8

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blank spike and its associated samples should be analyzed at the same time. The acceptable range
for spike recovery is 60 to 140 percent.

       Field duplicates must be extracted and analyzed at a rate of 10 percent. The precision
goal is ±50 percent RPD. Select duplicates that represent various concentration levels.

       The reliability of the method is operator dependent. Each operator needs to do five
qualifying spike samples through the extraction and analysis procedures to produce their own
response factors for TNT and RDX analysis. The response factors need to be reevaluated
periodically or when a major change in the procedure occurs.

       All results and comments should be recorded in ink in a laboratory notebook with the
name of the analysis and date clearly entered.
Operation of Hach DR2000

1.      Turn on the Hach. The instrument will read "Selftest" followed by "Method?" Select
       "0" and press "read/enter".

2.      Rotate the wavelength dial to the desired setting: 510 for RDX and 540 for TNT.
       Approach the wavelength from the high side when adjusting.

3.      Fill both cuvettes to the line with acetone.

4.      Insert the "reference" cuvette into the cell holder with the side marked "25 ml" on the
       right.

5.      Close the light shield and press "Clear/Zero" to establish the reference.

6.      Remove the reference and place the "sample" cuvette in the holder with the side marked
       "25 ml" on the right.

7.      Press "Read/Enter" and record the absorbence in the laboratory logbook as ABS
       background.

8.      If the reading is greater than ±0.002, clean the cuvettes and repeat the procedure.

9.      Proceed with sample analysis.
                                          B-9

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Cleaning Cuvettes

1.      Fill the matched cuvettes with 5 ml of water.

2.      Cap each cuvette and shake vigorously for 3 seconds.

3.      Empty into a waste container.

4.      Fill the cuvettes with 5 ml of acetone.

5.      Cap and shake for 3  seconds.

6.      Empty into waste container.

7.      Repeat the acetone wash.

8.      Wipe the outside of the cuvettes with Kimwipes™.  Take care especially to clean the side
       labeled "25 ml" and  the side opposite.


General Interferences

1.      Do not use the reagents beyond the expiration date.

2.      TNT samples must be analyzed immediately after adding the Developer Solution.  RDX
       samples must be analyzed within 60 minutes of the color incubation step.

3.      Operate test kits at less than  39°C (100°F).  Store at less than 80°F and out of direct
       sunlight.

4.      Store all standards in the refrigerator.
                                         B-10

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References

Jenkins, T.F., P.O. Thorne, M.E. Walsh. Field Screening Method for TNT and RDX in
Groundwater. U.S. Army Corps of Engineers, CRREL Special Report 94-14, May 1994.

EnSys. 1997.  TNT Soil Test System, Strategic Diagnostics Inc., Newark, DE.

EnSys. 1998.  RDX Soil Test System, Strategic Diagnostics Inc., Newark, DE.

U.S. EPA, Explosives in Water Field Screening Technologies UMDA and SUBASE Bangor
(draft), prepared by Black and Veatch Special Projects Corp., Tacoma, WA, for U.S.
Environmental Protection Agency Region 10, Project Number 71370, March 1996.
                                       B-11

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