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APPENDIX E
ANALYTICAL METHODS
- EPA Contract Laboratory Protocol for GC/MS Analysis
of Purgeable Organics in Water, Soils, and Sediments
- EPA Protocol for the Analysis of Volatile Principle
Organic Hazardous Constituents Using VOST
- National Institute for Occupational Safety
and Health Method
No. P & CAM 127
- Standard Method 209 G
6060A
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EPA CONTRACT LABORATORY PROTOCOL FOR GC/MS ANALYSIS
PURGEABLE ORGANICS IN WATER, SOILS, AND SEDIMENTS
6060A
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IV.
1. CC/MS Analytic of Purgeable Organic*
1.1 Summary of Method*
1.1.1 Water samples
An inert gas is bubbled through a 5 mL sample contained in a
specifically designed purging chamber at ambient temperature.
The purgeables are efficiently transferred from the aqueous
phase to the vapor phase. The vapor is swept through a torbent
column vhere the purgeables are trapped. After purging is com-
pleted, the sorbent column is heated and backflushed with the
inert gas to desorb the purgeables onto a gas chromatographic
column. The gas chromatograph is temperature programmed to
separate the purgeables which are then detected with a mass
spectrometer.
An aliquot of the sample is diluted with reagent water when
dilution is necessary. A 5 mL aliquot of the dilution is
taken for purging.
1.1.2 Sediment/Soil Samples
1.1.2.1 Low Level. An inert gas is bubbled through a mixture
of a 5 gm sample and reagent water contained in a sug-
gested specially designed purging chamber (illustrated
on page I>-95) at elevated temperatures. The purgeables
are efficiently transferred from the aqueous phase to
the vapor phase. The vapor is swept through a sorbent
column where the purgeables are trapped. After purging
is completed, the sorbent column is heated and back-
flushed with the inert gas to desorb the purgeables
onto a gas chromatographic column. The gas chromato-
graph is temperature programmed to separate the purge-
ables which are then detected with a Bass spectrometer.
r- ]_
Rev: 9/8-
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IV.
1.1.2.2 Medium Level. A measured amount of soil is extracted
with methanol. A portion of the methanol extract is
diluted to 5 ml. with reagent water* An inert gas
is bubbled through this solution in a specifically
designed purging chamber at ambient temperature.
The purgeables are effectively transferred from the
aqueous phase to the vapor phase. The vapor is swept
through a sorbent column where the purbeables are
trapped. After purging is completed, the sorbent
column ia heated and backflushed with the inert gas
to desorb the purgeables onto a gas chromatographic
column* The gaa chromatograph is temperature pro-
grammed to separate the purgeables which are then
detected with a mass spectrometer.
1.2 Interferences
1.2.1 Impurities in the purge gas, organic compounds out-gassing
from the plumbing ahead of the trap, and solvent vapors in the
laboratory account for the majority of contamination problems.
The analytical system must be demonstrated to be free from
contamination under the conditions of the analysis by running
laboratory reagent blanks aa described in Exhibit E. The use
of non-TFE tubing, non-TFE thread sealants, or flow controllers
with rubber components in the purging device should be avoided.
1.2.2 Samples can be contaminated by diffusion of volatile organlcs
(particularly fluoroearbona and methylene chloride) through
the septum seal into the sample during storage and handling.
A holding blank prepared from reagent water and carried through
the holding period and the analysis protocol serves as a check
on such contamination. One holding blank per case must be
analysed.
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1.2.3 Contamination by carry ever can occur whenever high level end
low level aamplet are sequentially analysed. To reduce carry
over, the purging device and sampling syringe must be rinsed
with reagent water between sample analyses. .Whenever an
unusually concentrated sample is encountered, it should be
followed by an analysis of reagent water to check for cross
contamination. For samples containing large amounts of 'water-
soluble materials, suspended solids, high boiling compounds
or high purgeable levels, it may be necessary to wash cut
the purging device with a detergent solution, rinse it with
distilled water, and than dry it in a 105'C oven between
analyses. The trap and other parts of the systea are also
subject to contamination; therefore, frequent bakeout and
purging of the entire systea may be required.
1.3 apparatus and Materials
1.3.1 Micro syringes - 25 uL and larger, 0.006 inch ID needle.
1.3.2 Syringe valve - two-way, with Luer ends (three each), if
applicable to the purging device.
1.3.3 Syringe - 5 ml., gas tight with shut-off valve.
1.3.4 Balance-Analytical, capable of accurately weighing 0.0001 g.
and a top-loading balance capable of weighing O.lg.
1.3.5 Glassware
1.3.5.1 o Bottle - 15 mL, screw cap, with Teflon cap liner.
o Volumetric flasks - class A with ground-glass stoppers
o Vials - 2 mL for CC autosampler.
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1.3.6 Purge and trap device - The purge aad trap device consists of
three aeparate pieces of equipment; the sample purger, trap
and Che desorber. Several complete devices are now commercially
available.
1.3.6.1 The sample purger muse be designed to accept 5 mL
samples with a water column at least 3 cm deep. The
gaseous head apace between the water column and the
trap must have a total volume of less than 15 mL. The
purge gas must pass through the water column as finely
divided bubbles with a diameter of less than 3 ma at
the origin. The purge gas must be introduced no more
than 5 ma from the base of the water column. The
•ample purger, Illustrated in Figure 1, meets these
design criteria. Alternate sample purge devices may
be utilized provided equivalent performance is
demonstrated.
1.3.6.2 The trap must be at least 25 cm long and have an inside
diameter of at least 0.105 inch. The trap must be
packed to contain the following minimum lengths of
absorbents: 1.0 cm of methyl silicone coated packing
(31 OV-1 on Chromosorb W or equivalent), 15 cm of 2,6-
dlphenylene oxide polymer (Tenax-GC 60/80 mesh) and 8
cm of silica gel (Davison Chemical, 35/60 mesh, grade
15, or equivalent). .The minimum specifications for the
trap are illustrated in Figure 2.
1.3.6.3 The desorber should be capable of rapidly heating
the trap to 160*C. The polymer section of the
trap should not be heated higher than 180*C and
the remaining sections should not exceed 220*C.
The desorber design, Illustrated in Figure 2, meets
these criteria.
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1.3.6.A The purge and trap device Bay be assembled as a
separate unit or be coupled to a gas chroaatograph
as Illustrated in Figures 3 and 4.
1.3.6.5 A heater or heated bath capable of maintaining the
purge device at 40*C + 1'C.
1.3.7 GC/MS system
1.3.7.1 Gas chroaatograph - An analytical system coaplete with
• temperature programmable gas chromatograph suitable
for on-coluon Injection and all required accessories
including syringes, analytical columns, and gases.
1.3.7.2 Column - 6 ft long x 0.1 in ID glass, packed with 12
SP-1000 on Carbopack B (60/80 mesh) or equivalent.
1.3.7.3 Mass spectrometer - Capable of scanning from 35
to 260 amu every seven seconds or less, utilizing
70 volts (nominal) electron energy in the electron
impact ionization mode and producing a mass spectruc
which meets all the criteria in table 2 when 50 ng
of 4-bromofluorobenzene (BFB) is injected through
the gas chroaatograph inlet.
1.3.7.4 GC/MS interface - Any gas chromatograph to mass
spectrometer interface that gives acceptable cali-
bration points at 50 ng or less per injection for
each of the parameters of interest and achieves all
acceptable performance criteria (Exhibit £) may
be used. Gas chroaatograph to mass spectrometer
interfaces constructed of all-glass or glass-lined
materials are recommended. Glass can be deactivated
by silanizlng vith dichlorodimethylsilane.
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1.3.7.5 Data system - A computer system must be interfaced
to the mass spectrometer that allows the continuous
acquisition and storage on machine readable media
of all mass spectra obtained throughout the duration
of the chromatographic program. The computer must
have software that allows searching any CC/HS data
file for ions of a specified mass and plotting such
ion abundances versus time or scan number. This
type of plot is defined as an Extracted Ion Current
Profile (E1CP). Software muse alto be available that
allows integrating the abundance in any ECIP between
specified time or scan number limits.
1.4 Reagents
V
1.4.1 Reagent water - Regent water is defined as water in which an
intefferent is not observed at the HDL of the parameters of
interest.
1.4.1.1 Reagent water may be generated by passing tap water
through a carbon filter bed containing about 453 g of
activated carbon (Calgon Corp., Filtrasorb-300 or
equivalent).
1.4.1.2 A water purification system (Hillipore Super-Q or
equivalent) may be used to generate reagent water.
1.4.1.3 Reagent water may also be prepared by boiling water
for 15 minutes. Subsequently, while maintaining the
temperature at 90*C, bubble a contaminant-free inert
gas through the water for one hour. While still hot,
transfer the water to a narrow-iaouth screw-cap bottle
and seal with a Teflon-lined septum and cap.
1.4.2 Sodium thiosulfate - (ACS) Granular.
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1.4.3 Methanol - Pesticide quality or cqvuivalent.
1.4.4 Stock standard solutions - Stock standard solutions may be
prepared from pure standard Materials or purchased and must
be traceable to EMLS/LV- supplied standards. Prepare stock.
standard solutions in methanol using assayed liquids or gases
as appropriate.
1.4.4.1 Place about 9.8 mL of methanol into a 10. 0 mL tared
ground glass stoppered volumetric flask. Allow the
flask to stand, unstoppered, for about 10 minutes or
until all alcohol wetted surfaces have dried. Weigh
the flask to the nearest 0.1 Kg.
1.4.4.2 Add the assayed reference Material as described below.
1.4.4.2.1 Liquids - Using a 100 uL syringe,
immediately add two or more drops of
assayed reference material to the flask
then reweigh. The liquid must fall
directly into the alcohol without
contacting the neck of the flask.
1.4.4.2.2 Gases - To prepare standards for any of
the four halocarbons that boil below 3CeC
(bromomethane, chloroethane, chloromethane,
and vinyl chloride), fill a 5 ml valved
gas-tight syringe with the reference
standard to the 5.0 mL mark. Lower the
needle to 5 ma above the methanol meniscus.
Slowly Introduce the reference standard
above the surface of the liquid. The
heavy gas rapidly dissolves in the
methanol.
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1.4.4.3 Reweigh, dilute to volume, stopper, then mix by
inverting the flask sever*! times. Calculate the
concentration in micrograms per microliter from the
net gain in weight. When compound purity is assayed
to be 962 or greater, the weight may be used without
correction to calculate the concentration of the stock
standards may be used at any concentration if they are
certified by the manufacturer. Commercial standards
Bust be traceable to EMSL/LV supplied standards.
1.4.4.4 Transfer the stock standard solution into a Teflon-
sealed screw-cap bottle. Store, with minimal head-
space at -10*C to -20*C and protect from light.
1.4.4.5 Prepare fresh standards weekly for the four gases and
2-chloroethyl-vinyl ether. All other standards must
be replaced after one month, or sooner if comparison
with check standards indicate a problem.
1.4.5 Secondary dilution standards - Using stock standard solutions,
prepare secondary dilution standards in methanol that contain
the compounds of interest, either singly or mixed together.
(See GC/MS Calibration in Exhibit E). Secondary dilution
standards should be stored with minimal headspace and should
be checked frequently for signs of degradation or evaporation,
especially just prior to preparing calibration standards from
them.
1.4.6 Surrogate standard spiking solution. Prepare stock standard
solutions for toluene-d8, p-bromofluorobenzene, and 1,2-
dichloroethane-d4 in methanol as described in Paragraph 1.4.4.
Prepare a surrogate standard spiking solution'from these stock
standards at a concentration of 250 ug/10 mL in methanol.
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1.4.7 Purge*ble Organic Matrix Standard Spiking Solution
1.4.7.1 Prepare a spiking solution in methancl that contains
the following compounds at a concentration of 250
ug/10. 0 ml:
Purgeable Organ!cs
1,1-dichloroethene
trichloroethene
chlorobenzene
toluene
benzene
1.4.7.2 Matrix spikes also serve as duplicates; therfore, add
an aliquot of this solution to each of two portions
from one sample chosen for spiking.
1.4.8 BFB Standard - Prepare a 25 ng/uL solution of BFB in methanol.
1.4.9 Great care must be taken to maintain the integrity of all stan-
dard solutions. It is recommended that all standard solutions
be stored at -10*C to -20*C in screw cap amber bottles with
teflon liners.
1.5 Calibration
1.5.1 Assemble a purge and trap device that meets the specification
in paragraph 1.3.6. Condition the trap overnight at JBO'C in
the purge mode with an inert gas flow of at least 20 mL/cin.
Prior to use, daily condition traps 10 minutes while back-
flushing at 180*C with the column at 22C*C.
1.5.2 Connect the purge and trap device to a gas chromatograph.
The gas chromatograph must be operated using temperature and
flow rate parameters equivalent to those in paragraph 1.7.1.2
Calibrate the purge and trap-CC/MS system using the Internal
standard technique (paragraph 1.5.3).
5/8,
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IV.
1.5.3 Internal standard calibration procedure. The three Internal
standards are bro»ochloro«ethane, 1,4-difluorobenrene, and
chlorobenzene-d5.
1.5.3.1 Prepare calibration standards at a miniaua of five
concentration levels for each HSL parameter. The
concentration levels are specified in Exhibit E.
Aqueous standards Bay be stored up to 24 hours, if
held in sealed vials with rero headspace as described
In paragraph 1*7. If not to stored, they mist be
discarded after an hour*
1.5*3.2 Prepare a spiking solution containing each of the
Internal standards using the procedures described in
paragraphs 1.4.4 and 1.4.5. It is recosnended that
the secondary dilution standard be prepared at a
concentration of 23 ug/mL of each internal standard
compound. The addition of 10 uL of this standard
to 5.0 aL of sample or calibration standard would
be equivalent of 50 ug/L.
1.5.3.3 Analyze each calibration standard, according to
paragraph 1.7 adding 10 uL of internal standard
spiking solution directly to the syringe. Tabulate
the area response of the characteristic ions against
concentration for each compound and internal standard
and calculate response factors (KJ) for each compound
using equation 1.
A* C<«
EQ. 1 RF - —£_ X —i£-
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Where:
Ax • Area of the characteristic ion for the coapound
to be Measured.
Ait • Area of the characteristic ion for the
specific internal standard from Exhibit E.
ci« * Concentration of the internal standard.
C, • Concentration of the coapound to be measured.
1.5.3.4 The average response factor (RJ) must be calculated
for all compound*. A system performance check must
be made before this calibration curve is used. Five
compounds (the system performance check compounds)
are checked for a minimus average response factor.
These compounds (the SPCC) are chloromethane, 1,1-
dichloroethane, bromoform, 1,1,2,2-tetrachloroethane,
and chlorobenzene. Five compounds (the calibration
check compounds, CCC) are useJ to evaluate the curve.
Calculate the Z Relative Standard Deviation (IRSD)
of BJ values over the working range of the curve.
A minimum IRSD for each CCC must be met before the
curve is valid.
XRSD • Standard deviation x 100
mean
See instructions for Form VI, Initial Calibration
Data for more details.
1.5.3.5 Check of the calibration curve should be perforate
once every 12 hours. These criteria are describe- :-
detail in the instructions for Fora VII, Cor.: ir.u:~.;
Calibration Check. The mlnimuo response factor fcr
the systea performance check compounds must be cr.ecke;
If this criteria is aet . the response facto: o: all
E-1I
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IV.
compounds are calculated and reported. A percent
difference of the daily response factor (12 hour)
compared to the average response factor from the
initial curve is calculated. The maximum percent
difference allowed for each compound flagged as
'CCC' in Form VII is checked. Only after both
these criteria are met can sample analysis begin.
1.5.3.6 Internal standard responses and retention times in
all samples must be evaluated immediately after or
during data acquisition. If the retention time for
any internal standard changes by more than 30 seconds
from the latest daily (12 hour) calibration standard.,
the chroma tographic system must be Inspected for mal-
functions and corrections mad* as required. If the
extracted ion current profile (E1CP) area for any
internal standard changes by more than a factor of
two (-50Z to +100Z), the mass apectrometric system
must be inspected for malfunction and corrections
made as appropriate. When corrections are made,
re-analysis of samples analyzed while the system
vas malfunctioning is necessary. Retention time and
, E1CP area records shall be maintained in appropriate
form by the laboratory as a part of its internal
quality control (Exhibit E).
1.6 CC/MS Operating Conditions
1.6.1 These performance tests require the following instrumental
parameters:
Electron Energy: 70 Volts (nominal)
Mass Range: 35 - 260
Scan Time: to give at least 5 scans per peak
but not to exceed 7 seconds per scan.
Mtf be
'
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1.7 Sample Analytic
1.7.1 Water Staple*
1.7.1.1 All samples and standard solutions must be allowed to
warm to ambient temperature before analysis.
1.7.1.2 Recommended operating conditions for the gas chromato-
graph - Column conditions: Carhop*k B (60/80 mesh with
1Z SP-1000 pakced in a 6 foot by 2 am ID glass column
with helium carrier gas at a flow rate of 30 aL/aln.
Column tcaperature is isothermal at *5*C for 3 minutes,
then programmed at 8*C per minute to 220*C and held
for 15 minutes.
1.7.1.3 After achieving the key ion abundance criteria, cali-
brate the system daily as described in Exhibit £.
1.7.1.4 Adjust the purge gas (helium) flow rate to 40 + 3 mL/
min. Variations from this flow rate may be necessary to
achieve better purging and collection efficiencies for
some compounds, particularly chloromethane and bromoform
1.7.1.5 Remove the plunger from a 5 ml syringe and attach a
closed syringe valve. Open the aample or standard
bottle which has been allowed to come to ambient temper-
ature, and carefully pour the aample into the syringe
barrel to just short of overflowing. Replace the
syringe plunger and compress the sample. Open the
syringe valve and vent any residual air while adjusting
the sample volume to 5.0 mL. This process of taking an
aliquot destroys the validity of the aample for future
analysis so if there is only one VOA vial, the analyst
should fill a aecond syringe at this time to protect
against possible loss of aample integrity. This second
aample is maintained only until such a time when the
E-13
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IV.
analyst ha* determined that the first sample has been
analyzed properly. Filling on* 20 ml syringe would
allow the use of only one syringe. If a second
analysis is needed from the 20 mL syringe, it must be
analyzed within 24 hours. Care sjust also be taken to
prevent air from leaking into the syringe.
1.7.1.6 The purgeable organlcs screening procedure (Section
III, paragraph 1.0), if used, will have shown the
approximate; concentrations of major sample componenta.
If a dilution of the sample was indicated, this
dilution shall be made just prior to GC/HS analysis
of the sample.
1.7.1.6.1 The following procedure will allow for
dilutions near the calculated dilution
factor from the screening procedure:
o All dilutions are made in volumetric
flasks (10 mL to 100 mL).
o Select the volumetric flask that will
allow for the necessary dilution. Inter-
mediate dilutions may be necessary for
extremely large dilutions.
o Calculate the approximate volume of
reagent water which will be added to
the volumetric flask selected and add
slightly less than this quantity of
reagent water to the flask.
o Inject the proper aliquot from the
ayringe prepared in paragraph 1.7.1.5
into the volumetric flask. Aliquotc
of less than 1 mL Increments are pro-
hibited. Dilute the flask to the mark
with reagent water. Cap the flask,
invert, and shake three times.
o Fill a 5 mL syringe with the diluted
sample as in paragraph 1.7.1.5.
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o If this is an intermediate dilution,
use it and repeat above procedure to
achieve larger dilutions.
1.7.1.7 Add 10.0 uL of the surrogate spiking solution (1.4.6)
and 10.0 uL of the internal standard spiking solution
(1.5.3.2) through the valve bore of Che syringe, then
close the valve. The surrogate and internal standards
stay be nixed and added as a single spiking solution.
The addition of 10 uL of the surrogate spiking solution
to 5mL of sample is equivalent to a concentration of
50 ug/L of each surrogate standard.
1.7.1.8 Attach the syringe-syringe valve assembly to the
syringe valve on the purging device. Open the syringe
valves and inject the sample into Che purging chamber.
1.7.1.9 Close both valves and purge the sample for 12.0+ 0.1
minutes at ambient temperature.
1.7.1.10 At the conclusion of the purge time, attach the trap
to the chromatograph, adjust Che device to the desorb
•ode, and begin the gas chromatographic temperature
rogran. Concurrently, introduce Che crapped materials
to the gas chrommatographic column by rapidly heating
Che trap to 180*C while backf lushing Che crap with an
inert gas between 20 and 60 mL/mln for four minutes.
If this rapid beating requirement cannot be met, the
gas chromatographic column must be used as a secondary
trap by cooling it Co 30*C (or subambientj if problems
persist) instead of the recommended initial temperature
of A5*C.
1.7.1.11 While Che crap is being desorbed into the gas chroma-
tograph, empty the purging chamber. Hash the chamber
with a minimum of two 5 mi. flushes of reagent water
to avoid carry-over of pollutant compounds.
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1.7.1.12 After desorbing the Maple for four minutes, recondi-
tion the trap by returning the purge and trap device
to th* purge mode. Uait 15 seconds then dote the
•yringe valve on the purging device to begin gas flow
through the trap. The trap temperature should be
maintained at 180*C. Trap temperatures up to 230*C
may be employed, however the higher temperature will
shorten the useful life of the trap. After approxi-
mately seven minutes turn off the trap heater and
open the syringe valve to stop the gas flov through
the trap. When cool, the trap is ready for the next
sample.
1.7.1.13 If the initial analysis of a sample or a dilution of
a sample indicates saturated ions of HSL compounds,
the sample must be reanalyzed at a higher dilution.
When a sample is analyzed that has saturated ions
from a compound, this analysis must be followed by a
blank reagent water analysis. If the blank analysis
is not free of interferences, the system must be
decontaminated. Sample analysis may not resume until
a blank can be analyzed that is free of interferences.
1.7.1.14 For low and medium level water samples, add 10 uL
of the matrix spike solution (1.4.7) to the 5aL of
sample purged. Disregarding any dilutions, this is
equivalent to a concentration of 50 ug/L of each
matrix spike standard.
1.7.1.15 All dilutions must keep the response of the major
constituents (previously saturated peaks) in the
upper half of the linear range of the curve.
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1.7.2 Sediment/Soil Saaples
Two approaches may be taken to determine whether the low level
or medium level method may be followed.
o Assume the sample is low level and analyze a 5 gram sample
o Use the X factor calculated from the optional Hexadecane
screen (Section III), paragraph 1.7.2.1.3
If/fpeaks are saturated from the analysis of a 5 gram sample.
a smaller sample «ize must be analyzed to prevent saturation.
However, the smallest sample size permitted is 1 ga. If smaller
than 1 gram sample size is needed to prevent saturation, the
medium level method must be used.
1.7.2.1 Low Level Method
The low level method is based on purging a heated
sediment/soil sample mixed with reagent water
containing the surrogate and internal standards.
Use 5 grams of sample or use the X Factor to decenaine
the sample size for purging.
o If the X Factor is 0 (no peaks noted on the
hexadecane screen), analyze a 5 gm sample.
o If the X Factor is between 0 and 1,0, analyze
a 1 gn sample.
1.7.2.1.1 The GC/MS systett should be set up as lr.
1.7.1.2 - 1.7.1. A. This should be done
prior to the preparation of the sample
to avoid lose of volatiles fron standards
and sample.
E-17
Rev: 9,!
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1.7.2.1.2 Leaove Che plunger fros a 5 ml "Luerlock"
type syringe equipped with a syringe valve
and fill until overflowing with reagent
water. Replace the plunger and compress
Che water to vent trapped air. Adjust the
voluoe to 5.0 ml. Add 10 uL. each of the
surrogate spiking solution (1.4.6) and the
internal standard solution to the syringe
through the valve. (Surrogate spiting
solution and internal standard solution may
be mixed together). The addition of 10 ul
of the surrogate spiking solution to 5 gv
.of sediment/ soil is equivalent to 30 ug/kg
of each surrogate standard.
1.7.2.1.3 The sample (for volatile organic*) consists
of the entire contents of the sample con-
tainer* Do not discard any supernatant
liquids. Mix the contents of the sample
container vlth a narrow metal spatula.
Weigh the amount determined in 1.7.2.1 into
a tared purge device. Use a top loading
• balance. Note and record the actual weight
to the nearest 0.1 gu.
1.7.2.1.3.1 Immediately after weighing the
sample weigh 5-10 g of the
sediment into a tared crucible.
Determine the percent moisture
by drying overnight at 105*C.
allow to cool in a desiccator
before weighing. Concentrations
of individual analytes will be
reported relative to the dry
weight of sediment.
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Eev: 9/8*
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Percent moisture
gin of sample-gin of dry sample
gffl of sample * ltKJ " * moisture
1.7.2.1.4 Add the spiked reagent water to the purge
device and connect the device to the purge
and trap system. NOTL: Steps 1.7.2.1.2 -
1.7.2.1.3, prior to the attachment of the
purge device, must be performed rapidly to
•void loss of volatile organ!cs. These
steps Bust be performed in a laboratory free
of solvent fumes.
1.7.2.1.5 Heat the sample to 40*C + 1"C and purge the
sample for 12 + 0.1 minutes.
i
1.7.2.1.6 Proceed with the analysis as outlined in
1.7.1.10 - 1.7.1.13. Use 5 mL of the
same reagent water as the reagent blank.
1.7.2.1.7 For low level sediment/soils add 1U uL of
the matrix spike solution (1.4.7) to the 5
ml of water (1.7.2.1.2). The concentration
for a 5 gram sample would be equivalent to
50 ug/kg of each matrix spike standard.
1.7.2.2 Medium Level Method
The medium level method is based on extracting the sedi-
ment ''soil sample with metHanoi. An aliquot of the metr-
anol extract is added to reagent water containing the
surrogate and internal standards. This is purged at
ambient temperature. All samples with an X Factor >1.C
should be analyzed by the medium level method. If sat-
urated peaks occurred or would occur when a 1 gran: sac-
ple was analyzed, the median: level method oust be used.
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IV.
1.7.2.2.1 The sample (for volatile organic*)
consists of Che entire content* of the
aample container. Do not discard any
•upernatenc liquids. Mix the contents
of the sample container vith a narrow
metal spatula. Weigh 4 gn (wet weight)
into a tared 15 mL vial. Use a top
loading balance. Note a nd record the
actual %reight to the nearest 0.1 gm.
Determine the percent moisture as in
1.7.2.1.3.1.
1.7.2.2.2 Quickly add 9.0 mL of methanol, then
1.0 mL of the surrogate spiking solution
to the vial. Cap and shake for 2 minutes.
NOTE: Steps 1.7.2.2.1 and 1.7.2.2.2 must
be performed rapidly to avoid loss of
volatile organlcs. These steps must be
performed in a laboratory free of solvent
fumes.
1.7.2.2.3 Pipette for storage approximately 1 mL of
extract to a GC vial using a disposable
pipet. The remainder may be disposed of.
Transfer approximately 1 mL of the
reagent methanol to a GC vial for use
as the method blank for each case or
set of 20 samples, whichever is greater.
These extracts may be scored in the dark
at 4°C prior to analysis.
E-20
Rev: 9/84
-------
IV.
The addition of • 100 uL aliquot of each
of these extracts in paragraph 1.7.2.2.6
will give a concentration equivalent to
6,200 ug/kg of each surrogate standard.
1.7.2.2.4 The CC/MS system should be set up as in
1.7.1.2 - 1.7.1.4. This should be done
prior to Che addition of the aethanol
extract to reagent water.
1.7.2.2.5 The following table can be used to deter-
mine the volume of Bethanol extract to
add to the 5 mL of reagent water for
analysis. If the Hexadecane screen
procedure was followed use the X factor
(Option B) or the estimated concentration
(Option A) to determine the appropriate
volume. Otherwise, estimate the concen-
tration range of the sample from the low-
level analysis to determine the appropriate
volume. If the sample was submitted as a
medium level sample, start with 100 uL.
All dilutions must keep the response of
the major constituents (previously saturated
peaks) in the upper half of linear range
of the curve.
E-21
Rev: 9/84
-------
IV.
X Factor
Estimated
Concentration Range
Take this Volume of
Methanol Extract^/
ug/kg
uL
0.25 - 5.0
0.5 - 10.0
2.5 - 50.0
12.5 - 250
500 - 10,000
1000 - 20,000
5000 - 100,000
25,000 - 500,000
100
50
10
100 of 1/50 dilution37
Calculate appropriate dilution factor for concentrations exceeding the table.
I/ Actual concentration ranges could be 10 to 20 times higher than this if
the compounds are halogenated and the estimates are from CC/FID.
2J The volume of nethanol added to the 5 mL of water being purged should be
kept constant. Therefore, add to the 5 mL syringe whatever volume of
methanol is necessary to maintain a volume of 100 uL added to the syringe
2/ Dilute an aliquot of the methanol extract and then take 100 uL for
analysis.
E-22
Rev: 9/84
-------
IV.
1.7.2.2.6 Remove the plunger fron a 5 mL "Luerlock"
type syringe equipped with a syringe valve
•nd fill until overflowing with reagent
water. Replace the plunger and compress
the water to vent trapped air. Adjust the
volume to 4.9 mL. Pull the plunger back
to 5 mL to allow volume for the addition
of sample and standards. Add 10 uL of the
internal standard solution. Also add the
volume of methanol extract determined in
1.7.2.2.5 and a volume of methanol solvent
to total 100 uL (excluding methanol in
standards).
1.7.2.2.7 Attach the syringe-syringe valve assembly
to the syringe valve or the purging device.
Open the syringe valve and inject the water/
methanol sample into the purging chamber.
1.7.2.2.8 Proceed with the analysis as outlined in
1.7.1.9 - 1.7.1.13. Analyze all reagent
blanks on the same Instrument as the sac-
pies. The standards should also contain
100 uL of methanol to simulate the sample
conditions.
1.7.2.2.9 For a matrix spike in the medium level sed-
iment/soil samples, add 8.0 mL of methanol,
1.0 mL^of surrogate spike solution (1.4.6),
and 1.0 mL of matrix spike solution (1.^.7)
in paragraph 1.7.2.2.2. This results in a
6,200 ug/kg concentration of each matrix
spike standard when added to a 4 go sample.
Add a 100 uL aliquot of this extract to 5 m'.
of water for purging (as per paragraph
1.7.2.2.6).
Rev: 9/6-
E-23
-------
IV.
'.8 Qualitative Analytic
1.8.1 The target compounds listed in the Hazardous Substances List
(HSL), Exhibit C, shall be identified by an analyst competent in
the Interpretation of Bass spectra (see Bidder Pre-Award Labora-
tory Evaluation Criteria) by comparison of the sample mass spec-
trum to the mass spectrum of a standard of the suspected compound.
Two criteria must be satisfied to verify the identifications: (1)
elutlon of the sample component at the same CC relative retention
time as the standard component, and (2) correspondence of the
sample component and standard component mass spectra.
1.8.1.1 For establishing correspondence of the CC relative
retention time (RRT), the saaple component RRT must com-
pare within + 0.06 RRT units of the RRT of the standard
component. For reference, the standard must be run on
the same shift as the sample. If coelution of interfer-
ing components prohibits accurate assignment of the sam-
ple component RRT from the total ion chromatogram, the
RRT should be assigned by using extracted ion current
profiles for ions unique to the component of interest.
1.8.1.2 For comparison of standard and sample component mass
spectra, mass spectra obtained on the contractor's CC/
MS are required. Once obtained, these standard spectra
may be used for identification purposes, only if the
contractor's GC/MS meets the daily turning requirements
for BFB or DFTPP. These standard spectra may be
obtained from the run used to obtain reference RRTs.
1.8.1.3 The requirements for qualitative verification by
comparison of mass spectra are as follows:
(1) All ions present in the standard mass spectra at
a relative intensity greater than 10 Z (most abundant
ion in the spectrum equals 100!) must be present In
the sample spectrum.
E-24
Rev: 9/84
-------
IV.
(2) The relative intensities of ions specified In (1)
•use agree within plus or minus 20Z between the stan-
dard and sample spectra. (Example: For an ion with
an abundance of 50Z in the standard spectra, the
corresponding sample abundance must be between 30
and 70 percent).
(3) Ions greater than 10X in the sample spectrum but
not present in the standard spectrum must be consid-
ered and accounted for by Che analyst making the
comparison. In Task III, the verification process
should favor false negatives.
1.8.2 A library search shall be executed for Non-HSL sample components
for the purpose of tentative identification. For this purpose,
the most recent available version of the EPA/NIH Mass Spectral
Library shall be used. Computer generated library search rou-
tines should not use normalization routines that would misrepre-
sent the library or unknown spectra when compared to each other.
1.6.2.1 Up to 10 substances of greatest apparent concentra-
tion not listed in Exhibit C for the purgeable organic
fraction shall be tentatively identified via a forward
search of the EPA/NIH mass spectral library. (Sub-
stances with responses less than 102 of the internal
standard are not required to be searched in this
fashion). Only after visual comparison of sample
spectra with the nearest library searches will the mass
spectral interpretation specialist assign a tentative
identification.
1.8.2.2 Guidelines for making tentative identification: (1)
Relative intensities of major ions in the reference
spectrum (ions greater than 10Z of the most abundant
ion) should be present in the sample spectrum.
Rev: 98-
E-25
-------
IV.
(2) The relative intensities of the major ions should
agree within + 20Z. (Example: For an ion with an
abundance of SO percent of the standard spectra, the
corresponding sample ion abundance must be between 30
and 70 percent.)
(3) Molecular ions present in reference spectrum
should be present in sample spectrum.
(4) Ions present in the Maple spectrum but not in
the reference spectrum should be reviewed for possible
background contamination or presence of co-eluting
compounds.
(3) Ions present in the reference spectrum but not in
the sample spectrum should be reviewed for possible
subtraction from the sample spectrum because of back-
ground contamination or co-«luting compounds. Data
system library reduction programs can sometimes
create these discrepancies.
X
1.8.2.3 If in the opinion of the mass spectral specialise,
no valid tentative identification can be made, the
compound should be reported as unknown. The mass
spectral specialist should give additional classif-
ication of the unknown compound, if possible (i.e.
unknown aromatic, unknown hydrocarbon, unknown acid
type, unknown chlorinated compound). If probable
molecular weights can be distinguished, include them.
1.9 Quantitative Analysis
1.9.1 HSL components identified shall be quantified by the internal
standard method. The internal standard used shall be the one
nearest the retention time to that of a given analyte. The
E-26
5/84
-------
IV.
EICP area of the characteristic ions of analytes listed in
Tables 2 and 3 are used. The response factor (RF) fron the
daily standard analysis is used to calculate the concentration
in the sample. Use the response factor as determined in para-
graph 1.3.3.3 and the following equations:
Water (lov and medium level)
(AX)(IS)
Concentration ug/L - (Ais)(RF)(V0)
Where:
A, - Area of the characteristic ion for the compound to be
•easured
Ais - Area of the characteristic ion for the specific internal
standard from Exhibit E.
16 » Amount of internal standard added in nanograms (ng)
V0 - Volume of water purged in milliliters (ml) (take into
account any dilutions)
Sediment/Soil (medium level)
Concentration ug/kg • (Ax)(Ig)(Vt)
(Als)(Rf)(V1)(Ws)(D)
Sediment/Soil (low level)
Concentration ug/kg - '^x^^s^
(Als)(RF)(WBXD)
(Dry weight basis)
Where:
AX, 1B, Ais - same as for water, above
Vt - Volume of total extract (uL) (use 10,000 uL
or a factor of this when dilutions are made)
Vi - Volume of extract added (uL) for purging
D « 100 - 1 moisture
100
W6 - Weight of sample extracted (gm) or purged
E~2~ Rev: 9/6-
-------
IV.
1.9.2 An estimated concentration for Non-HSL components tentatively
identified shall be quantified by the internal standard Method.
For quantification, the nearest internal standard free of inter-
fereces shall be used.
1.9.2.1 The formula for calculating concentrations is the
same as in paragraph 1.9.1. Total area counts from
the total ion chroma tograms are to be used for both
the compound to be measured and the internal standard.
A response factor (RF) of one (1) is to be assumed.
The value from this quantltation shall be qualified
as estimated. This estimated concentration should be
calculated for all tentatively identified compounds
as well as those identified as unknowns.
1.9.2.2 Xylenes (o,m, & p - isomers) are to be reported as
total Xylenes. Since o- and p-Xylene overlap, the
Xylenes must be quantltated versus m-Xylene. Tne
concentration of all Xylene isomers must be added
together to give the total.
1.9.3 Calculate surrogate standard recovery on all samples, blanks
and spikes. Determine if recovery is within limits and report
on appropriate form.
1.9.3.1 Calculation for surrogate recovery.
Percent Surrogate Recovery • £d_ X 1002
where: Q^ - quantity determined by analysis
Qa • quantity added Co sample
E-28
Rev: 9/8*
-------
IV,
1.9.3.2 If recovery i»-not within limits, the following is
required:
o Check, to be sure there are no errors in calcula-
tions, surrogate solutions and internal standards.
Also, check instrument performance.
o Recalculate the sample data if any of the above
checks reveal a problem.
o Reanalyze the sample if none of Che above are a
problem.
o Report the data from both analyses along with
the surrogate data from both.
Table 2
Characteristic Ions for Surrogate and
Internal Standards for Volatile Organic Compounds
Compound Primary Ion Secondary Ion(s)
SURROGATE STANDARDS
4-Bromofluorobenzene 95 174, 176
1,2-Dlchioroethane d-4 65 102
Toluene d-B 98 70, IOC
INTERNAL STANDARDS
Bromochloromethane 128 49, 130, 51
1,4-Difluorobenrene 114 63, 88
Chlorobenzene d-5 117 82, 119
E-29
Rev: 9/84
-------
u.
Table 3
Characteristic Ions for Volatile HSL Compounds
Paraaeter
Primary Ion*
Secondary lon(s)
Chi or one thane
Broaotne thane
Vinyl chloride
Chloroethane
Methylene chloride
Acetone
Carbon dlsulfide
1 , 1-Dichl or oethene
1 , 1-Di Chloroethane
t rans-1 , 2-Dlchlor oethene
Chloroform
1 , 2- Di Chloroethane
2-Butanone
1,1, 1-Tri Chloroethane
Carbon tetrachloride
Vinyl acetate
Bromodichlorooe thane
1,1,2, 2-Tetrachlor oethane
1 ,2-Dichloropropane
trans-1 , 3-Dichloropropene
Trichlor oethene
Dibromochlorome thane
1 , 1 ,2-Tri Chloroethane
Benzene
cis-1 , 3-Dichloropropene
2-Chloro«thyl vinyl ether
Bromoform ~~
2-Hexanone
4-^tethyl-2-pentanone
Tetrachl or oethene
Toluene
Chlorobenzene
Ethyl benzene
Styrene
Total xylenes
50
94
62
64
84
43
76
96
63
96
83
62
72
97
117
43
83
83
63
75
130
129
97
78
75
63
173
43
43
164
92
112
106
104
106
52
96
64
66
49, 51, 86
58
78
61. 98
65, 83, 85, 98, 100
61, 98
85
64, 100, 98
57
99, 117, 119
119, 121
86
85, 129
85, 131, 133, 16t>
65, 114
77
95, 97, 132
208, 206
83, 85, 99, 132, 134
-
77
65, 106
171, 175, 250, 252, 254, 256
58, 57, 100
58, 100
129, 131, 166
91
114
91
78, 103
91
* The primary ion should be used unless interferences are present, in which
case, a secondary ion may be used.
E-30
Rev: 9/84
-------
«
f o ?
O* ^
a *
*«U ^
? s* ?
5ODEEZII
•
!
I
t
I
rs
o.vo
030
-------
IV.
Corrior out flow control
Prooouro rogvtoior
pont
Purgo got
flow control XT"
13X motocuJor
fiHor
Column o*on
column
\ opiionol 4-pon column
loloctton vor*o
tniot
wiro
f ^^
_ Trie (OH)
control
Purging
Hoto:
AH linot
trap ind GC
tnouU bo ho
3 Stnomot* of purgo on* trop
Corrior omt ftow control^
*ro**uro ro^ulotor
*urgo got
How control
13X moioculor
tttlor
V^L^JL- -i-,p- ConfirmotOTY
-AJ =| T-T-X, I > r» ootocior
\^"^. £T' » U J "**~-Anon/ticol column
optionol 4-port column
tolocvon votvo
6 •pen Trop miot
»•'*• J P.o»igtonco wiro
^3L2
Hootor control
170*C
on
*oto
All Itnoi
trop tnd GC
thouM ft* hooto*
to WC
«. Sehornotic of purgo on* trop Of**o — ootoro
E-32
5/84
-------
PURGE INLET FITTING
SAMPLE OUTLET FITTING
3- » 6mm 0 D GLASS TUBING
SEPTUM
CAP
Figure S. Low Soil* Inpinger
E-3:
5/8*.
-------
IV.
2. CC/MS Analysis of Extractables (Base/Neutrals and Acids)
2.1 Summary of Method
This method is to be used for the CC/MS analysis of extractable extracts
screened by Section III protocols and for confirmation of pesticides/PCBs
identified by GC/EC, if concentrations permit.
2.2 Apparatus and Materials
2.2.1 Gas chromatograph/mass spectrometer system.
2.2.1.1 Gas chromatograph - An analytical system complete with
a temperature programmable gas chromatograph suitable
for splitless injection and all required accessories
including syringes, analytical columns, and gases.
2.2.1.2 Column - 30 m x 0.25 mm ID (or 0.32 ma) bonded-phase
silicone coated fused silica capillary column (J&W
Scientific DB-5 or equivalent). A film thickness
of 1.0 micron is recommended because of its larger
capacity. A film thickness of 0.25 micron may be used.
2.2.1.3 Mass Spectrometer - Capable of scanning from 35 to 500
amu every 1 second or less, utilizing 70 volts (nominal)
electron energy in th electron impact ionization mode
and producing a mass spectrum which meets all required
criteria vhen 50 ng of decafluorotriphenylphosphine
(DFTPP) is injected through the GC inlet.
NOTE: DFTPP criteria must be met before any sample
extracts are analyzed. Any samples analyzed when
DFTPP criteria have act been met will require
reanalysis at no cost to the Government.
E-34
5/8..
-------
EPA PROTOCOL FOR THE ANALYSIS OF
VOLATILE PRINCIPLE ORGANIC HAZARDOUS CONSTITUENTS
USING VOST
6060A
-------
&EPA
Environmental Protection
Agency
c.r-.-1'Oou o
March 1984
Research and
Development
PROTOCOL FOR THE
COLLECTION AND ANALYSIS OF
VOLATILE POHCs USING VCST
Prepared for
Office of Solid Waste and Emergency Response
Prepared by
industrial Environmental Research
Laboratory /
Research Triangle Park NIC 27711
E-35
-------
RESEARCH REPORTING SERIES
Research reports of the Office of Research and Development. U.S. Environmental
Protection Agency, have been grouped into nine series. These nine broad cate-
gories were established to facilitate further development and application of
environmental technology. Elimination of traditional grouping was consciously
planned to foster technology transfer and a maximum interface m related fields.
The nine series are:
1. Environmental Health Effects Research
2. Environmental Protection Technology
3. Ecological Research
4. Environmental Monitoring
5. Socioeconomic Environmental Studies
6. Scientific and Technical Assessment Reports (STAR)
7. Interagency Energy-Environment Research and Development
8. "Special" Reports
9. Miscellaneous Reports
This report has been assigned to the SPECIAL REPORTS senes This ser.es is
reserved 'or reports which are intended to meet the technical information needs
of specifically targeted user groups. Reports m this series include Problem Orient-
ed Reports. Research Application Reports, and Executive Summary Documents.
Typical of these reports include state-of-the-art analyses, technology assess-
ments, reports on the results of major research and development efforts, design
manuals, and user manuals.
EPA REVIEW NOTICE
This report has been reviewed by the U S Environmental Protection Agency, and
approved for publication Approval does not signify that the contents necessarily
reflect the views and policy of the Agency, nor does mention of trade names or
commercial products constitute endorsement or recommendation for use.
This document >s available to the public through the National Technical informa-
tion Service. Springfield. Virginia 22161
E-36
-------
EPA-600/8- 84-007
March 1984
PROTOCOL
FOR THE
COLLECTION AND ANALYSIS OF
VOLATILE POHCs USING VOST
By
Earl M. Hansen
Envirodyne Engineers, Inc.
12161 Lackland Road
St. Louis, Missouri 63146
EPA Contract No. 68-02-3697
Technical Directive 003
EPA Project Officer: Robin M. Anderson
Technical Support Office
U. S. Environmental Protection Agency
Industrial Environmental Research Laboratory
Research Triangle Park, NC 27711
Prepared For
Office of Research and Development
U.S. Environmental Protection Agency
Washington, DC 2046U
-------
FOREWORD
This report has been produced by EPA's Office of Research and Development
as part of ongoing studies 1n support of engineering research and regulatory
programs Including EPA's Office of Solid Waste, EPA Regional Offices, and
appropriate State Agencies. The document contains state-of-the-art
operating protocols for sampling and analysis of volatile organic
constituents of flue gases from hazardous waste incinerators or other
similar combustor systems. It is Intended as a reference to be used for
guidance by personnel of the regulatory groups, personnel associated wirh
engineering RAD, and the regulated community.
Publication of this report does not constitute official designation as an
EPA method. Official test methods for hazardous waste related programs
are published in SW-846 "Tests Methods for Evaluating Solid Waste," as
well as in the Federal Register.
Frank T. Princiotta
Director
Industrial Environmental Research Laboratory
-------
CONTENTS
Foreword
Figures v
Acknowledgements vi
Introduction vii
Abstract viii
PART A: SAMPLE COLLECTION FOR THE DETERMINATION OF
EMISSIONS OF VOLATILE ORGANIC COMPOUNDS FROM
HAZARDOUS WASTE INCINERATORS A-1
1. Scope of Applicability A-l
2. Summary of Method A-3
3. Precision and Accuracy A-5
4. Interferences A-6
5. Apparatus A-7
5.1 Volatile Organic Sampling Train A-7
5.2 Probe A-7
5.3 Isolation Valve A-10
5.4 Condensers A-10
5.5 Sorbent Cartrides A-10
5.6 Impinger A-15
5.7 Metering Systems A-15
5.8 Sample Transfer Lines " A-16
6. Reagents and Materials A-16
6.1 2.6-Diphenyline Oxide Polymer Tenax (35/60 Mesh) A-16
6.2 Charcoal (SKC Lot 104 Petroleum Base or equivalent) A-l7
6.3 Viton 0-Ring A-13
6.4 Glass Tubes/Condensers - A-1S
6.5 Metal Parts A-18
6.6 Silica Gel A-18
6.7 Crushed Ice A-i*
6.8 Water A-19
6.9 Glass Wool A-19
6.10 Nitrogen A-19
7. Assembly and Conditioning of VOST Sorbent Cartridges A-iy
7.1 Introduction A-19
7.2 Assembly of Tenax Cartridges A-20
7.3 Assembly of Tenax/Charcoal Cartridges A-21
7.4 Sorbent Cartridge Quality Assurance A-22
8. Sample Collection Procedure A-2?
8.1 Pretest Preparation A-23
8.2 VOST Assembly A-24
8.3 Leak Checking A-24
8.4 Sample Collection A-26
8.5 Field, Trip, and Laboratory Blanks/Aqueous Field Blank A-2fi
E-39
-------
CONTENTS
'. Continued)
PART B: PROTOCOL FOR ANALYSIS OF SORBENT CARTRIDGES
FROM VOLATILE ORGANIC SAMPLING TRAIN B-1
1. Scope and Applicability B-l
2. Summary of Method B-2
3. Precision and Accuracy B-4
4. Apparatus B-4
4.1 Thermal Desorption Unit B-4
4.2 Purge and Trap Unit B-5
4.3 GC/MS Systen B-5
5. Reagents *-6
5.1 Reagent Water B-6
5.2 Analytical Trap Reagents B-7
5.3 Stock Standard Solution B-8
5.4 Secondary Dilution Standards 3-8
5.5 Brcmofluorobenzene (BFB) Standard 3-8
5.6 Deuterated (d$) Benzene Standard B-8
6. Calibration B-9
6.1 Assembly of P-T-D Device B-9
6.2 Internal Standard Calibration Procedure 3-9
7. Quality Control B-12
8. Sample Collection, Preservation, and Handling B-15
9. Daily GC/MS Performance Tests B-15
10. Sample Desorption and Gas Chromatography B-16
11. Aqueous Condensate B-17
12. Qualitative Identification B-17
13. Calculations B-18
14. Method Performance B-21
REFERENCES (For A and B) 3-22
E-40
-------
FIGURES
No. Page
1 Schematic of Volatile Organic Sampling Train A-8
2 Volatile Organic Sampling Train (I/O
Cartridge Design) A-9
3 I/O Sorbent Trap Assembly, Volatile Organic
Sampling Train (VOST) A-12
4 Inside/Inside VOST Cartridge A-13
5 VOST Field Data Sheet A-25
6 Schematic Diagram of Trap Desorption/
Analysis System B-3
E-41
-------
ACKNOWLEDGEMENT
The author wishes to acknowledge the assistance and technical
input of several people whose efforts led to the successful
completion of this document.
The following people provided valuable comments and
recommendations of the draft version of this protocol: Bob
DeRosier of Accurex Corporation, Paul Gorman of Midwest Research
Institute, Marvin R. Branscome and Charles Sparacino of Research
Triangle Institute, Denny Wagoner and Alston Sykes of TRW, and
Afaf K. Wensky of Battelle Columbus Laboratories. I would also
like to recognize the development work conducted by TRW which
provided valuable data for quality assurance monitoring of VOST
scrbent cartridges. I am especially grateful for the guidance and
constructive criticism received from Larry Johnson and Robin
Anderson of the Technical Support Office, USEPA-IERL, Research
Triangle Park, NC.
E-42
-------
INTRODUCTION
The Resource Conservation and Recovery Act (RCRA) requires
that owners/operators of facilities which treat hazardous waste
by incineration ensure that the incinerators are operated in a
manner which does not endanger human health or the environment
(1,2). The Code of Federal Regulation, Title 40, Part 264,
requires that a destruction and removal efficiency (DRC) of 99.99
percent be achieved for each principal organic hazardous constit-
uent (POHC) designated in the Trial Burn Permit (3). The DRE
standard implicitly requires sampling and analysis to quantify
POHCs in the waste feed material and stack gas effluent. The
"Sampling and Analysis Methods for Hazardous Waste Combustion"
manual (method manual) provides information on methods that are
applicable for collection and analyses of POHCs in process streams
of hazardous waste incinerator units (4).
The methods manual identifies three possible methods for
the collection of volatile organics (those with boiling points
<100°C). The methods include bag, glass bulb, and the Volatile
Organic Sampling Train (VOST). Evaluation of the bags and bulbs
indicates that these sampling systems are subject to a numoer of
technical problems. The most important of these problems is the
inadequate sensitivity for detection of POHCs present in low
concentrations.
The VOST provides increased sensitivity to low level concen-
tration of volatile POHCs due to the ability to concentrate the
gaseous effluent. The results of laboratory evaluation and field
application of the VOST have shown that it provides sufficient
sensitivity to permit calculation of a DRE equal to or greater
than 99.99 percent for volatile POHCs which are present in the
waste feed at 100 ug/g (5).
The metnods manual identifies the VOST as a suitable sampling
system for volatile organics and includes a paper describing the
VOST (5). A detailed protocol was not included in the methods
manual due to the fact that this is outside the scope of the docu-
ment. Since the VOST is new technology, it is felt a protocol
should be made available.
The purpose of this protocol is to provide a standard operat-
ing procedure to users of the VOST in the collection and analysis
of samples for volatile POHCs in the gaseous effluents of hazard-
ous waste incinerators or gaseous effluents of hazardous waste
co-fired combustion processes. The protocol is presented in two
parts. Part A describes the key components of the VOST train, and
the procedure for sample collection using VOST. Part B describes
the procedures for analysis of VOST sorbent cartridges for vola-
tile POKCs using purge-trap-desorb gas chromatography/nass
spectrometry (P-T-D GC/MS).
E-43
-------
ABSTRACT
This document provides a state-of-the-art operating protocol
for sampling and analysis of volati.le organic constituents of flue
gas from hazardous waste incinerators or other similar combustion
systems using the Volatile Organic Sampling Train (VOST). It is
intended to be used for guidance by personnel -of the regulatory
groups, personnel associated with engineering Research and
Development, an dthe regulated community.
The VOST is designed to extract and concentrate volatile
organic compounds (boiling $100°C) from stack gas effluents. The
concentrated organics are analyzed by procedures chosen to be
compatible with the VOST in order to obtain flue gas concentration
levels. This information is necessary to perform destruction and
removal efficiency (ORE) calculations for incinerator operations.
The results of laboratory evaluation and field use of the VOST
have shown that the VOST provides sufficient sensitivity to permit
calculation of a ORE equal to or greater than 99.99 percent for
volatile organics present in the waste feed at 100 ug/g.
The VOST is directly applicable to organic compounds with
boiling points of 30° to 100°C. Many organic compounds with boil-
ing points less than 30°C, or with boiling points in the 100° to
150°C range, may also be collected and analyzed by this method.
Field application of the VOST for compounds with boiling points
outside the 30° to 100°C range should be attempted only after
laboratory evaluation of the collection and recovery efficiencies
of the specific compounds.
The document is presented in two parts. Part A describes the
key components of the train, the procedures for preparation of the
sorbent materials, and procedures for sample collection using the
VOST. Part B describes the procedures for analysis of VOST
sorbent cartridges for volatile principal organic hazardous
constituents (POHCs) using purge-trap-desorb gas chromatography/
mass spectrometry (P-T-D GC/MS). Quality control procedures are
presented in both Sections A and B.
E-44
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PART A
SAMPLE COLLECTION FOR THE DETERMINATION OF THE EMISSIONS Ot
VOLATILE ORGANIC COMPOUNDS FROM
HAZARDOUS WASTE INCINERATORS
1. SCOPE AND APPLICABILITY
1.1 This protocol describes the method of collection of volatile
principal organic hazardous constituents (POHCs) from the stack
gas effluents of hazardous waste incinerators. This method is
applicable to compounds with boiling points in the range of 30° to
100°C. If the boiling point of a POHC of interest is less than
30°C. the POHC may breakthrough the sorbent under the conditions
of the sample collection procedure. Field application for POHCs
of this type should be supported by laboratory data which demon-
strates the efficiency of a volatile organic sampling train (VCST)
to collect POHCs with boiling points less than 30°C (Part B,
Section 7). The collection of organic compounds with low boiling
points may require using reduced sample volumes collected at flew
rates between 250 and 500 milliliters per minute (ml/min). Mary
compounds which boil in the range of 100° to 150°C (e.g., cnloro-
benzene, ethylbenzene, tetrachloroethane, bromoform) may be effi-
ciently collected and analyzed using this method. VOST recovery
efficiencies for these compounds should also be demonstrated,
where necessary, by laboratory data of the type described above
(Part B, Section 7).
E-45
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1.2 This method is applicable to the determination of volatile
POHCs in the stack gas effluent of hazardous waste incinerators
and other similar combustion systems. This method is designed for
use in calculating the destruction and removal efficiency (ORE)
for the volatile POHCs. The method provides sufficient precision
and accuracy to enable the calculation of ORE values equal to or
greater than 99.99 percent (5).
1.3 The sensitivity of this method is dependent upon the level of
interferences in the sample and the presence of detectable levels
of volatile POHCs in blanks. The target detection limit of this
method is 0.1 micrograms per cubic meter (ug/m^) [0.1 nanograms
per liter (ng/1)] of flue gas which permit calculation of a ORE
equal to or greater than 99.99 percent for those volatile POHCs
which may be present in the waste feed stream at 100 parts per
million (ppm). Laboratory development data (5) have demonstrated
a range of 0.1 to 100 ug/m3 (o.l to 100 ng/1) for selected
volatile POHCs.
1.4 The range of applicability for this method is limited by
breakthrough of volatile POHCs on the sorbent cartridges used tc
collect the sample, caution should be exercised in using the VOST
to collect samples from a stack gas stream in which one or more of
the volatile POHCs are present in concentrations greater than 5UO
ug/m3 (500 ng/1). If, for example, an incinerator uses a waste
fuel containing volatile POHCs at a concentration of 50,000 to
100,OOU wg/g, and the incinerator achieves a ORE of 99.99%, chen
E-46
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the concentration in the effluent would be 500 to 1000 yg/m3 (500
to 1,000 ng/1), respectively. Analysis using the procedures des-
cribed in Part B of this method would probably result in overload-
i
I ing the analytical instrumentation and therefore would not provide
valid data for that particular POHC. Where the waste contains
volatile POHCs at high concentrations, consideration should be
' given to collecting gaseous effluent samples using SLOW-VOST tech-
niques, gas bags or evacuated glass bulbs. Further, if the waste
i
1 contains volatile POHCs at high (50,000 ug/g) and low (10U ug/g)
( concentrations, these POHCs might not be quantifiable using only
' VOST. In this case, consideration should be given to either
1 collecting gaseous effluent samples using two VOST trains ,(one of
these trains should be operated under conditions of SLOW-VOST), or
i
, using one VOST train (SLOW-VOST) and gas bags or glass bulbs. The
examples cited above may result in chromatoyraphic interferences
or instrument overloading which will invalidate the results. If
i
1 this situation is anticipated, laboratory evaluation should be
i conducted prior to field use of the VOST (Part B, Section 7).
1.5 This method is recommended for use only by experienced sam-
pling personnel and analytical chemists, or under close super-
I
i vision by such qualified persons.
2. SUMMARY OF METHOD
I 2.1 A 2-hour sample of gaseous effluent is collected on car-
tridges using six pairs of cartridges, each pair sampling a maxi-
' murr. of 20 liters of gaseous effluent. The samples are collected
I
E-47
I
-------
at a sampling flow rate of 1 liter per minute, using temperature
controlled quartz or glass lined probe and a VOST. The gas stream
is cooled to 20°C by passage through a water-cooled condenser
and volatile POHCs are collected on a pair of sorbent cartridges.
Liquid condensate is collected in an impinger placed between the
two sorbent cartridges. The first sorbent cartridge (front
cartridge) contains approximately 1.6 grams Tenax, and the second
cartridge (back cartridge) contains approximately 1 gram each of
Tenax and petroleum based charcoal (SKC Lot 104 petroleum base or
equivalent, see Section 6.2.1), 3:1 by volume.
2.2 An alternative set of conditions for sample collection has
been used. This method involves collecting a sample volume of 20
liters or less at a reduced flow rate. Operation of the VOST
under these conditions has been referred to as SLOW-VOST. This
method has been used to collect 5 liters of sample (0.25 liters/
min for 20 minutes) or 20 liters of sample (0.5 liters/min for 40
minutes) on each pair of sorbent cartridges. Smaller sample
volumes collected at lower flow rates should be considered wnen
the boiling points of the POHCs of interest are below 30°C or for
volatile POHCs present in high concentrations in the stack gas.
2.3 The gaseous effluent shall be sampled over a 2-hour period.
This is accomplished using six pairs of Tenax and Tenax/charcoa 1
cartridges sampling a maximum of 20 liters of gaseous effluent on
each pair of cartridges. Fewer pairs of cartridges may be
E-48
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required using SLOW-VOST (Section 2.2). A minimum of three pairs
of Tenax and Tenax/charcoal cartridges shall be collected for
SLOW-VOST sampling.
2.4 Analysis of the cartridges (described in Part B) for volatile
POHCs using purge-trap-desorb gas chromatograph/mass spectrometer
(P-T-D GC/MS) which is carried out by thermally desorbing each
cartridge with the gas passing through a water filled purge column
onto an analytical trap. The analytical trap is subsequently
heated and the effluent gas passes into the GC/MS.
3. PRECISION AND ACCURACY
3.1 The results of laboratory evaluations of the VOST for
selected volatile POHCs showed that the recovery of the analytes
from three pairs of replicate cartridges ranged from ±50 percent
of the expected value (5).
3.2 Prior to field operation of the VOST at a hazardous waste
incinerator, a laboratory trial should be conducted using either
selected volatile POHCs of interest or two or more of the volatile
POHCs for which data are available (5). The user shall demon-
strate proficiency which is within the precision and accuracy cf
the method (Part B, Section 7). Experienced users of VOST who
have demonstrated proficiency with the VOST and can provide data
which supports the applicability of the VOST for the POHCs may be
exempt from this requirement. Before the VOST shall be used to
E-49
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sample compounds below 30*C, the user must demonstrate throuyh
laboratory evaluations of the collection and recovery efficiencies
that the accuracy and precision requirements are met (Part B,
Section 7).
4. INTERFERENCES
4.1 Interferences arise primarily from background contamination
of sorbent cartridges prior to or after use in sample collection.
Many potential interferences can be due to exposure of the sorbent
materials to solvent vapors prior to assembly and exposure to sig-
nificant concentrations of volatile POHCs in the ambient air at
hazardous waste incinerator sites. Benzene and toluene appear to
be inherent contaminants on Tenax. This may present problems in
the analysis of these compounds using VOST due to high background
concentrations. To minimize this problem, the use of additional
field blanks is recommended (see Section 8.5).
i
4.2 To avoid or minimize the low level contamination of train
components with volatile POHCs, care should be taken to avoid con-
tact of all interior surfaces or train components with synthetic
organic materials (e.g. organic solvents, lubricating and sealing
greases), and train components should be carefully cleaned and
conditioned according to the procedures described in Sections 5, 6
and 7 of this protocol. The sorbent cartridges should be condi-
tioned and stored in an environment free of volatile organic
compounds.
E-50
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5. APPARATUS
5.1 Volatile Organic Sampling Train
5.1.1 A schematic diagram of the principal components of the
VOST is shown in Figure 1. A diagram of the assembled components
of one version of the VOST is shown in Figure 2. The VOST
consists of: a quartz or glass lined probe with a glass wool
particulate plug, an isolation valve, a water cooled glass
condenser with thermocouple placed at the outlet to monitor gas
stream temperature (see Section 5.6.2), a sorbent cartridge
containing Tenax (1.6 grams), an empty impinger for condensate
removal, a second water cooled glass condenser, a second sorbent
cartridge containing Tenax and petroleum based charcoal (3:1 by
volume; approximately 1 gram of each), a silica gel drying tube, a
calibrated rotameter, a sampling pump, and a dry gas meter.
5.1.2 The gas pressure during sampling and for leak checking is
monitored by vacuum gauges which are in line with and downstream
of the silica gel drying tube.
5.2 Probe
5.2.1 The probe shall be maintained at a temperature of at
least 130°C in the gas stream prior to the first condenser. If
one or more of the volatile POHCs boil between 130* to 150°C, the
probe shall be maintained at a temperature equivalent to the
boiling point of the least volatile POHC. The probe w*y require
heating to achieve this temperature. If stack temperatures are
excessively high, an air or water cooled probe may be required to
E-51
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I
Ui
Heated Probe
Glass Wool
Particulate
Filler
STACK
(or test System)
Isolation Valves
Carbon Filler
Thermocouple
Sorbent
Cartridge
Condensole
Trap Impinger
Condenser
Backup
Sorbent
Cartridge
Silica Gel
Vacuum
Indicator
fHTff*
Exhaust
Pump
Rotameter
Dry Gas
Meter
FIGURE I
SCHEMATIC OF
VOLATILE ORGANIC SAMPLING TRAIN
(VOST)
-------
.TEFLON PLUG VALVE
"/SOCKET JOINT
CONDENSERS
TUBING
TEFLON TUBING
TENAX
CARTRIDGE
TENAX/CHARCOAL
CARTRIDGE
IMPINGER
SILICA £EL
HOLDE
VACUUM GAGES
WATER BATH
CASE
FIGURE 2
VOLATILE ORGANIC SAMPLING TRAIN
(1/0 CARTRIDGE DESIGN)
E-53
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avoid damage to the probe and to achieve a temperature of 20°C at
inlet to first sorbent cartridge (see Section 5.4). Isokinetic
sample collection is not a requirement for the use of VOST since
the compounds of interest are in the vapor phase at the point of
sample collection.
5.3 Isolation Valve
5.3.1 The isolation valves must be a greaseless stopcock with a
glass bore and sliding Teflon plug with Teflon wipers (Ace 8193 or
equivalent). These valves are used to permit ambient air to be
admitted after leak checking (Section 8.3) and for purging the
probe prior to sample collection (Section 8.4).
5.4 Condensers
5.4.1 The condensers (Ace 5979-14 or equivalent) shall be of
sufficient capacity to cool the gas stream to 20°C or less prior
to passage through the first sorbent cartridge. The cop connec-
tion of the condenser shall be able to form a leak-free, vacuum-
tight seal without usiny vacuum sealing greases.
5.5 Soroent Cartridges
5.5.1 The sorbent cartridges for the VOST are available and
acceptable in either of two configurations: the inside/outside
(I/O) or inside/inside (I/I) configuration. The terms I/O or I/I
pertain to the instrument configuration for thermal desorption of
the sorbent tubes. For the I/O design, the carrier gas contacts
the inside and outside of the sorbent tubes during the desorpt. icr..
E-54
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while for the I/I design, the carrier gas is directed only through
the inside of the cartridge. For the I/O configuration, the
cartridge is held in the VOST within an outer glass tube and in a
metal carrier (Figure 3). For the I/I configuration, a single
glass tube is used, with or without a metal carrier (Figure 4).
In either case, the sorbent packing will be the same. The first
pair of sorbent cartridges shall be packed with approximately 1.6
grams Tenax GC resin, and the second cartridge of a pair shall be
packed with Tenax GC and petroleum based charcoal (3:1 by volume;
approximately 1 gram of each).
5.5.2 The second sorbent cartridge shall be packed so that the
sample gas stream passes through the Tenax layer first and then
through the charcoal layer. Note that when sorbent cartridges are
analyzed using the P-T-D GC/MS procedure described in Part B,
Section 10.2, the gas flow through the sorbent cartridges during
desorption is in the opposite direction from the gas flow througn
the sorbent cartridges during sample collection. The inlet side
of each cartridge during sample collection shall be clearly iden-
tified so that it becomes the outlet side duriny the desorption
step of the analytical procedure.
5.5.3 The sorbent cartridges shall be glass tubes with approxi-
mate dimensions of 10 centimeters by 1.6 centimeters (cm) I.D.
The two acceptable designs (I/O, I/I) for the sorbent cartridge
are described in further detail below.
E-55
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i
Ul
TOP
BOTTOM
Section cut throuqh qlaaa tubes
(showing screen. C-clip and O-rinq in place)
LEGL'ND
A - Stainless Steel Carrier
B - Glass Tube (103 mm x 20 mm ID)
C - Small Glass Tube (10 cm x 1.6 cm ID)
D - Fine Mesh Stainless Steel Screen
E - Stainless Steel C-Clip
F - O-Rinq (Viton)
G - Nuts (3)
II - End Cap with Viton O-Rinq
I - Netal Hod with Threaded End (3)
J - Tenax/Charcoat Sorbents
K - Cajon Fitting '
FIGURE 3
I/O SORBENT CARTRIDGE ASSEMBLY
VOLATILE ORGANIC SAMPLING TRAIN (VOST)
Assembled Trd|>
NTS
-------
39aididVO ISOA 3QISNI-3QISNI
3HO9U
lOOMSSVlO
>OOOOOOOOOOOOOO OOOOOOOOOOOOOO
oooooooooooooooooooooooooooo
oooooooooooo oooooooooooooo oc]
oooooooooooooooooooooooooooo
OOOOOOOOOOOOOOOOOOOOOOOOOOO(
OOOOOOOOOOO' VWIJTI OOOOOOOOOOOO
oooooooooooooooooooooooooooo
)OOOOOOOOOOOOOOOOOOOOOOOOOOO(
oooooooooooooooooooooooooooo
|)OOOOOOOOOOOOOOOOOOOOOOOOOOO(
OOOOOOOOOOOOOOOOOQQQQQOQQQQQ
in
I
w
0*
n
3
UJ3QI
-------
5.5.3.1 Inside/Outside Type Sorbent Cartridge - A diagram of an
I/O type sorbent cartridge is shown in Figure 3. In this design,
the sorbent materials are held in the glass tube with a fine mesh
stainless steel screen and a C-clip. The glass tube is then
placed within a larger diameter glass tube, and held in place
using Viton 0-rings. The purpose of the outer glass tube is to
protect the exterior of the resin-containing tube from contamina-
tion. The two glass tubes are held in a stainless steel cartridge
holder. The ends of the glass tubes are held in place by Viton
O-rings placed in machine grooves in each metal end piece. The '
three cylindrical rods are secured in one of the netal end pieces
and fastened to the other end piece by appropriately sized nuts,
thus sealing the glass tubes into the cartridge holder. The end
pieces are fitted with a threaded nut onto which a threaded end
cap, fitted with a Viton 0-ring seal, is placed to protect the
resin from contamination during transport and storage.
5.5.3.2 Inside/Inside Type Sorbent Cartridge - A diagram of an
I/I type sorbent cartridge is shown in Figure 4. This cartridge
is a single glass tube (10 cm by 1.6 cm I.D.) which has the ends
reduced in size to accommodate a 1/4 or 3/8-inch Swagelok or Cajon
gas fitting. The resin is held in place by glass wool at each end
of the resin layer. The amounts of each type of sorbent material
used in the I/I design are the same as for the I/O design.
Threaded end caps are placed on the sorbent cartridge after pack-
ing with sorbent to protect the sorbent from contamination during
E-53
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storage and transport. Care should be exercised in the placement
of the threaded end cap; the male threaded fitting should be
backed about 1 mm from the end of the tube prior to tightening to
prevent crushing or chipping of the end of the tube.
5.6 Impinger
5.6.1 The impinger which is used to collect aqueous condensate
shall have a liquid volume of 125 ml and shall be capable of
providing a leak-free seal to the outlet of the Tenax sorbent
cartridge. The silica gel drying tube should have sufficient
capacity for at least 20 to 30 grams of silica gel.
5.7 Metering System
5.7.1 The metering system for VOST shall consist of: vacuum
gauges, a leak-free pump (Thomas Model 107 or equivalent), a cali-
brated rotameter (Linde Model 150 or equivalent) for monitoring
the gas flow rate, a dry gas meter with 2 percent accuracy (7) at
the required sampling rate, and related valves and equipment. The
dry gas meter shall indicate 1 liter of gas volume for each revo-
lution of the dial. Users of VOST have suggested that the rota-
meter does not need to be calibrated, but a calibrated rotameter
serves as a useful verification of the volume measurement from the
dry gas meter.
5.7.2 Provisions will be made for monitorinn the temperature of
the sample gas stream between the first condenser and first sor-
bent cartridge. This can be done by placing a thermocouple or. the
E-59
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exterior glass surface of the outlet from the first condenser.
The temperature at that point shall be less than 20°C. If it is
not, an alternative system, providing increased cooling capacity,
must be used.
5.8 Sample Transfer Lines
5.8.1 All sample transfer lines connecting the probe to VOST
shall be less than 5 feet in length, if possible, and shall be
heat-traced Teflon (to maintain a temperature of at least 13UeC in
the gas stream) with connecting fittings which are capable of
forming leak-free, vacuum-tight connections without the use of
sealing grease. All other sample transfer lines used with the
VOST (e.g., to connect impinger with second condenser) will oe
Teflon with connecting fittings that are capable of forming leak-
free, vacuum-tight connections without the use of sealing grease.
6.' REAGENTS AND MATERIALS
6.1 Tenax, 35/60 Mesh (2,6-Diphenylene Oxide Polymer)
6.1.1 The new Tenax is Soxhlet extracted for 24 hours with
methanol (Burdick & Jackson, pesticide grade or equivalent). The
Tenax is dried for 6 hours in a vacuum oven at 50°C before use.
Users of I/O and I/I sorbent cartridges have used slightly differ-
ent thermal conditioning procedures. Although strict equivalence
of the procedure has not been demonstrated, these methods have
produced results that meet method quality assurance requirements
(Part B, Section 7.4). I/O sorbent cartridges packed with Tenax
are thermally conditioned by flowing organic-free nitrogen
E-60
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30 ml/min through the resin while heating to 250°C for 8 hours.
Sorbent cartridges of the I/I design packed with Tenax are
thermally conditioned for 12 to 16 hours by flowing organic-free
nitrogen (30 ml/min) through the resin while heating to 190°C.
After thermal conditioning, the sorbent cartridges shall be stored
for 24 hours At room temperature prior to monitoring the car-
tridges for residual organic contamination (see Section 7.4). The
use of pentane to extract new Tenax and charcoal to remove non-
polar impurities is not recommended. (Users have experienced
problems with residual pentane in the sorbents during analysis,
and therefore, this procedure is not recommended.)
6.1.2 If very high concentrations of organic compounds have
been collected on the resin (e.g., micrograms of analytes), the
sorbent may require Soxhlet extraction as described above. Pre-
viously used Tenax cartridges are thermally reconditioned by the
method described above.
6.2 Charcoal (SKC Lot 104 Petroleum Base or Equivalent)
6.2.1 New charcoal is prepared as described in 6.1.1 above.
Due to possible problems with charcoal contamination, new charcoal
should be used. Users of VOST have restricted the types of char-
coal used in sorbent cartridges to only petroleum-based types.
Criteria for other types of charcoal are currently under develop-
ment. Other types of charcoal are acceptable if recovery of POHC
in laboratory evaluations meet the criteria (*50 percent) of the
method (Part B, Section 7).
E-61
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6.3 Viton O-Ring
6.3.1 All 0-rings used in VOST shall be Viton. Prior to use,
these 0-rings shall be thermally conditioned in a vacuum oven at
200°C for 48 hours. O-rings will be stored in clean, screw capped
glass containers prior to use.
6.4 Glass Tubes/Condensers
6.4.1 The glass resin tubes and condensers shall be cleaned
with a non-ionic detergent in an ultrasonic bath, rinsed well with
organic-free water and dried at 1108C. Resin tubes of the I/O
design should be assembled as described in Section 7 prior to
storage. Resin tubes of the I/I design shall be stored in glass
containers with Teflon lined screw caps. Condensers shall be
capped with appropriate end caps prior to use.
6.5 Metal Parts
6.5.1 The metal parts (e.g. , stainless steel carriers, C-clips,
end plugs), used in either the I/O or I/I cartridge design, are
cleaned by ultrasonication in a warn non-ionic detergent solution,
rinsed with reagent water, air dried and heated in a muffle
furnace for 2 hours at 400°C.
r
6.6 Silica Gel - - Indicating Type. 6-16 Mesh
6.6.1 New silica gel may be used as received. Silica gel which
has been previously used shall be dried for 2 hours at 175°C.
E-62
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6.7 Crushed Ice
6.7.1 Crushed ice from any source may be added to the coolant
in the reservoir.
6.8 Water
6.6.1 Water used for leak checking resin cartridges and rinsing
glassware shall be reagent (see Part 6, Section 5.1); water used
for cooling train components in the field may be tap water.
6.9 Glass Wool
6.9.1 Glass wool shall be Soxhlet extracted for 8 to 16 hours
using pentane, and oven dried at 110°C before use. The glass wool
shall be checked prior to use to ensure that it does not contain
residual pentane. If all pentane cannot be removed, an alternate
solvent such as methanol may be used.
6.10 Nitrogen
6.10.1 Nitrogen gas will be organic-free (Linde-Union Carbide,
99.999% pure, hydrocarbon-free, or equivalent). In-line moisture
traps, 5A° molecular sieve adsorbent tubes, or cryogenic traps r.ay
be used to ensure purity.
7. ASSEMBLY AND CONDITIONING OF VQST 50RBENT CARTRIDGES
7.1 Introduction
7.1.1 This section describes assembly of the sorbent cartridges
and procedures for storage and transport of assembled cartridges.
E-63
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The assembly and packing of the sorbent cartridges should be
carried out in an area free of volatile organic material. This is
preferably done in a laboratory in which no organic solvents are
handled or stored, and in which th« laboratory air is charcoal
filtered. Alternatively, the assembly procedure can be conducted
in a glove box or glove bag which can be purged with organic-free
nitrogen.
7.2 Assembly of Tenax Cartridges
7.2.1 The Tenax, glass tubes and metal cartridge parts are
cleaned and stored according to the procedures described in Sec-
tion 6. Approximately 1.6 grams of Tenax is weighed and packed
into the sorbent tube which has a stainless steel screen and
C-clips (I/O design) or by glass wool (I/I design) in the down-
stream end. The Tenax is held in place by inserting a stainless
steel screen and C-clips in the upstream end (I/O design) or glass
wool (I/I design). The cartridges are assembled in the metal
holders (Section 5.5) and leak checked by putting on one of the
end caps and pressurizing the cartridge to 30 psi with organic-
free nitrogen and immersing the cartridge in distilled water tc
check for the appearance of bubbles. Cartridges which are
determined to be leak-free are then conditioned as described in
Section 7.4.
7.2.2 Assembled and conditioned resin tubes of the I/O design
are placed in ice water for storage and transport. Conditioned
resin tubes of the I/I design are capped and placed in ice water
E-64
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for storage and transport. Limited experience by VOST users for
storing and transporting resin tubes of the I/I design indicates
that these tubes may be stored and transported in screw capped
culture tubes placed in a clean glass or metal container which
contains clean charcoal. The storage container is kept cold using
ice or cold pack storage. Storage containers shall be kept in an
area free from sources of organic contamination. The need for
these precautions is dependent upon the user's ability to maintain
blank cartridges free from contamination during storage and
transport.
7.3 Assembly of Tenax/Charcoal Cartridges
7.3.1 The Tenax, charcoal and metal cartridge parts are cleaned
and stored according to the procedures described in Section '6.
The tubes are packed with approximately a 3:1 volume ratio of
Tenax and charcoal (approximately 1 gram of each). The cartridge
is assembled such that the inlet side during sampling collection
is Tenax, followed by a layer of charcoal at the outlet side of
the sorbent cartridge. The Tenax and charcoal are held in place
by the stainless steel screens and C-clips (I/O design) or by
glass wool (I/I design). The glass tubes of the I/O design con-
taining the Tenax and charcoal are then leak checked as described
in Section 7.2, checked for quality assurance as described in
Section 7.4, and placed in the metal carriers according to the
procedures outlined in Section 5.5. The end caps are placed on
the assembled cartridges, and the assembled cartridges are placed
E-65
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in ice water for storage and transport as described in Section
7.2. Glass tubes of the I/I design are leak checked as described
in Section 7.2, and conditioned as described in Section 7.4. The
end caps are placed on the assembled cartridges, and they are
placed in a suitable container for storage and transport as
described in Section 7.2.
7.4 Sorbent Cartridge Quality Assurance
7.4.1 This section describes two methods which can be used to
verify that the sorbent cartridges (Tenax and Tenax/charcoal) are
free from background contamination prior to sample collection.
7.4.2 The gas chromatograph with flame ionization detector is
calibrated using direct injection of propane standards at the
appropriate concentrations. The chromatographic column shall De
1.8 m x 0.25 cm I.D., stainless steel or glass packed with 1%
SP-1000 on Carbopack (60/80 mesh) or equivalent. Following
assembly and leak checking of the sorbent cartridges, they are
connected to a source of organic-free nitrogen. Nitrogen is
passed through each trap at a flow rate of at least 30 ml/min,
while the traps are heated to 200°C. The effluent from the trap
is monitored with a flame ionization detector to check for emis-
sion of volatile organic compounds from the cartridge. The condi-
tioning is continued until the amount of total chromatographable
organics is below 0.2 ny as propane.
E-66
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7.4.3 The gas chromatograph with flame ionization detector is
calibrated by analyzing a Tenax cartridge which has been spiked
with 1*75 ng benzene, 175 ng toluene and 150 ng bromofluorobenzene
(BFB). The cartridge is spiked using the solvent-flush technique
(see Part B, Section 6.2.3). The chromatographic conditions
shall be the same as those described in Part B, or shall demon-
strate the capability of identifying background levels of volatile
POHCs with the required sensitivity. Following assembly and leak
checking, the sorbent cartridge(s) is placed in the desorption
heater for 10 minutes with a helium flow of 50 ml/min. The efflu-
ent from the cartridge is passed through a trap filled with glass
beads which is cooled in liquid nitrogen. (If a pair of Tenax and
Tenax/charcoal cartridges are monitored in a single desorption
run, the Tenax/charcoal cartridge should be upstream ofthe Tenax
cartridge.) At the end of the 10-minute desorption period, the
glass bead filled trap is heated, the carrier gas flow directed to
a gas chromatograph equipped with flame ionization detector and
chromatographic column suitable for volatile organic analysis (see
Part B, Section 4.3.2). Blank sorbent cartridges which are moni-
tored using this technique shall contain less than 2 ny total
chromatographable organics (as benzene or toluene). If in using
this procedure the background exceeds 10 ng (as benzene or
toluene), the cartridges must be recleaned and reanalyzed.
8. SAMPLE COLLECTION PROCEDURE
8.1 Pretest Preparation
8.1.1 All train components shall be cleaned and assembled as
described in Sections 5, 6, and 7. The dry gas meter shall have
E-6"
-------
been calibrated within 30 days prior to use. All field data
shall be recorded on a Field Data Sheet (or field notebook). An
example of a Field Data Sheet for VOST is shown in Figure 5.
8.2 VOST Assembly
8.2.1 The VOST is assembled according to the schematic diagram
in Figure 2. Cooling water is circulated to the condensers and
the temperature of the cooling water shall be maintained near
O°C. The end caps of the sorbent cartridges will be placed in a
clean screw capped glass container during sample collection. The
condensate pot shall not be immersed in ice water.
8.3 Leak Checking
8.3.1 The train is leak checked by closing the valve at the
inlet to the first condenser and pulling a vacuum equivalent to
10 inches Hg (250 mm Hg) above the system's operating pressure.
The traps and condensers are isolated from the pump and the leak
rate noted. The system shall hold at 10 inches Hg above the
system operating pressure with no discernible leakage (pressure
increase of less than 0.1 inches Hg/min). If the leak check does
not meet specifications, the cause of the problem must be identi-
fied and corrected and leak check repeated. After leak checking,
the train should be returned to atmospheric pressure by attaching
a charcoal filled tube to the isolation valves above the first
condenser and opening the valve to admit air to the train through
the charcoal filter. These procedures will minimize contamination
of VOST train components by excessive .exposure to the fugitive
emissions at hazardous waste incinerator sites.
E-68
-------
riant
Date
Location^
Operator^
field Blank I.O.i *ana«
•tack No.
•robe Mo.
Von No.
NotMater Ha.
Dry Gaa Motor Mo.
Mir
Mo>
Leak
Chock
CertrK
T*na«
lae 1.0.
*•!>••/
Oi«rco*l
MDUiaotvr
towlliif
I l/»ln)
TU
Initial
•
final
•••pi Ing
Duration
(•Inl
rroba
1*M|>.
<*C)
taroBotrlo
rr*Mura
(in of N?)
Oonlnuto* thoraaftar.
to aaapla collection on ono pair of Tana* and Tana*/char coal trapa.
IJRF 5. VOST FIELD DATA SHEET"
-------
8.3.2 After leak checking but before the initiation of sample
collection, the probe shall be purged with stack gas. This can be
accomplished by attaching a pump to the isolation valve above the
first condenser and drawing stacH "gas through the probe via the
isolation valve, so that at the initiation of sample collection
the probe is purged of ambient air.
8.4 Sample Collection
8.4.1 Prior to the initiation of sample collection, the probe
shall be located in the stack at a point of average stack gas
velocity and temperature. (These values can be determined using
the procedures described in References 6 and 7.) Care should be
exercised in the location of the probe in the stack to minimize
effects of dilution air which may enter the stack through the sam-
pling port and thereby impair the collection of a representative
sample of the stack gas.
8.4».2 After leak checking (see Section 8.3.1), sample collec-
tion is accomplished by opening the valve at the inlet to the
first condenser, turning on the pump, a"nd sampling at a rate of
1 liter/minute for 20 minutes. The volume of sample for any pair
of traps shall not exceed 20 liters. The temperature of the gas
stream at the inlet to the first sorbent cartridge must be main-
tained at or below 20°C during sample collection (see Section
5.6.2) .
E-70
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8.4.3 After the collection of 20 liters of sample, the train is
leak tested using the procedures described in Section 8.3. if
this post leak test criterion is not met, the samples shall not be
analyzed. If leak check criterion is met, the train is returned
to atmospheric pressure as described in Section 8.3.1, the two
sorbent cartridges removed, the end caps replaced, and the car-
tridges returned to a suitable container for storage and transport
until analysis (see also Section 7.2.2).
8.4.4 In some cases, there may be a requirement to analyze the
aqueous condensate. This situation may arise for water soluble
volatile organic compounds. For these situations, preliminary
laboratory evaluation of the sampling and recovery efficiency
(including the purging efficiencies of the compounds) must be
performed (Part B, Sections 7 and 11). Sampling and analysis pro-
cedures for water soluble volatile organics are currently being
developed. In this case, when a pair of sorbent cartridges is
changed, duplicate samples of the aqueous condensate should be
poured into 40 ml glass vials equipped with plastic screw caps
(Pierce 13075 or equivalent), and Teflon-faced silicon septa
(Pierce 12722 or equivalent). If insufficient condensate is
available, the vials shall be topped off with reagent water. The
vials shall be carefully filled just to overflowing so that no air
bubbles pass through the sample as the vial is being filled. The
vial shall be sealed so that no air bubbles are entrapped in it.
Vials shall be stored and transported at ice or cold pack
temperature.
-------
8.4.5 A new pair of cartridges is placed in the VOST. The VOST
leak checked as described in Section 8.3 and the sample collection
process repeated as described above. Sample collection continues
until six pairs of cartridges have 'been taken (see Section 2.3).
A maximum of six pairs of cartridges may be taken over a 2-hour
sampling period (see Section 2.3).
8.4.6 All sample cartridges shall be stored on cold packs or
ice until ready for analysis.
8.5 Field, Trip and Laboratory Blanks/Aqueous Field Blanks
8.5.1 Field Blanks - Blank Tenax and Tenax/charcoal cartridges
are taken to the sampling site and the end caps removed for tne
period of time required (approximately 5 minutes) to exchange two
pairs of cartridges on VOST. After the two VOST cartridges have
been exchanged, the end caps are replaced on the blank Tenax and
Tenax/charcoal tubes. These are returned to appropriate storage
(see Section 7.2.2) and analyzed with the sample cartridges. At
least one pair of field blanks (one Tenax, one Tenax/charcoal)
shall be included with each six pairs of sample cartridges col-
lected (or for each field trial using VOST to collect volatile
POHCs). It is advisable to use two pairs of field blanks for each
six pairs of cartridges collected.
8.5.2 Trip Blanks - At least one pair of blank cartridges (one
Tenax, one Tenax/charcoal) shall be included with the shipment of
cartridges to a hazardous waste incinerator site. These trip
E-72
-------
blanks will be treated as any other cartridges except that the end
caps will not be removed during storage at the site. This pair of
cartridges will be analyzed to monitor potential contamination
which may occur during storage and shipment. One user (5) recom-
mended including one pair of trip blanks for each VOST run con-
ducted during a trial burn to obtain a more meaningful basis for
blank correction of sample cartridges (Part B, Section 12.1.2).
8.5.3 Laboratory Blanks - One pair of blank cartridges (one
Tenax, one Tenax/charcoal) will remain in the laboratory using the
method of storage for field samples. If the field and trip blanks
contain high concentrations of contaminants (e.g., greater than
i
2 ng of a particular POHC), the laboratory blank shall be analyzed
in order to identify the source of contamination.
8.5.4 Aqueous Field Blanks - If the aqueous condensate is to be
analyzed for volatile POHCs, an aqueous field blank is required.
This consists of duplicate samples of reagent water placed in
vials described in Section 8.4.3. These vials shall be stored
and shipped in the same way as empty vials/aqueous condensate
samples, and should be analyzed at the same time as the aqueous
condensate samples. Additionally, a reagent water sample (pre-
pared as above) will be retained in storage in the laboratory. If
the analysis of aqueous field blanks shows the presence of POHCs,
the corresponding laboratory blank shall be analyzed to verify
that the residual contamination is not due to contamination of the
aqueous field blanks at the time of preparation or during storage
in the laboratory.
E-T3
-------
PART B
PROTOCOL FOR ANALYSIS OF SORBENT CARTRIDGES
FROM VOLATILE ORGANIC SAMPLING TRAIN
1. SCOPE AND APPLICABILITY
1.1 This method covers the analysis of volatile POHCs collected
on Tenax and Tenax/charcoal sorbent cartridges using a VOST. Mucn
of the description for purge-trap-desorb (P-T-D) GC/MS analysis is
included in References 8 and 9. Since the majority of gas streams
sampled using VOST will contain a high concentration of water, the
analytical method is based on the quantitative thermal desorption
of volatile POHCs from the Tenax and Tenax/charcoal cartridges and
analysis by P-T-D GC/MS in order to minimize the effects .of water
on the analysis. This method is applicable to organic compounds
with boiling points between 30° and 100°C. Many compounds with
boiling points below 30°C and between 100° and 150°C, may be
efficiently collected and analyzed using this method. However,
laboratory evaluation of the collection and recovery efficiency
for compounds with boiling points outside the range of 30° to
100°C (or those for which no VOST data are available) shall be
performed (see Section 7).
1.2 This method is applicable to the analysis of Tenax and
Tenax/charcoal cartridges used to collect volatile POHCs from wet
stack gas effluents from hazardous waste incinerators.
E-74
-------
1.3 The sensitivity of the analytical method for a particular
volatile POHC depends on the level of interferences, the presence
of detectable levels of volatile POHCs in blanks, and the ability
to purge the volatile POHCs from -water. The target detection
limit for the method is 0.1 jjg/m3 (o.l ng/1) in the stack gas.
This corresponds to 2.0 ng adsorbed on a single pair of Tenax and
Tenax/charcoal cartridges. Since 2 ng of a POHC may not be
detectable by P-T-D GC/MS analysis, the method is designed to
permit thermal desorption of up to five pairs of Tenax and Tenax/
charcoal cartridges onto a single pair for analysis in order to
achieve the target detection limit of the method. For a POHC
present in the gaseous effluent at a concentration of 0.1 wy/m^
(0.1 ng/1), the desorption of multiple pairs of cartridges onto a
single pair for analysis can provide a total of 10 ng for analysis
by P-T-D GC/MS.
1.4 This method is recommended for use only by experienced ana-
lytical chemists or under the close supervision of such qualified
persons.
2. SUMMARY OF METHOD
2.1 A schematic diagram of the analytical system is shown in
Figure 6. Pairs of the sorbent cartridges are spiked with an
internal standard and thermally desorbed for 10 minutes at 180°C
with organic-free nitrogen gas (at a flow rate of 100 ml/min),
bubbled through 5 ml of organic-free water, and trapped on an
analytical sorbent trap. After the 10-minute desorption, the
E-75
-------
I
Flow to
GC/MS
Flow During
Oetorption
F|ow
| Adtorplion
D-K
O-K
N
CD
•A.
fr-lJ''
Frit
Aoolylicol Trop
with Heating Coll
(0.3 cm diameter
by 25cm long)
; rO
MjO
Pu»g«
Thermo!
Detorplion
Chomber
Healed
Lin*
Vent
(T) 3% Sf-JlOO (I cm)
TenoM (7.7cm)
3 ) Silica Gel (7.7cm)
hM^
0 CHotcool (7.7cm)
FIGURE 6
SCHEMATIC DIAGRAM OF TRAP DESORPTION
/ANALYSIS SYSTEM
-------
analytical sorbent trap is rapidly heated to 180°C with the
carrier gas flow reversed so that the effluent flow from the
analytical trap is directed into the GC/MS. The volatile POHCs
are separated by temperature programmed gas chromatography and
detected by low resolution mass spectrometry. The concentrations
of volatile POHCs are calculated using the internal standard
technique. To achieve increased sensitivity, multiple pairs of
cartridges (up to five pairs) may be desorbed onto a single pair
of Tenax and Tenax/charcoal cartridges. The resulting pair is
analyzed by P-T-D GC/MS.
3. PRECISION AND ACCURACY
3.1 The overall accuracy of sample collection and analysis usinj
VOST has been determined in laboratory evaluations to average *50
percent for analysis of three replicate cartridges (5). These
values may be revised as further evaluation of VOST performance is
conducted.
3.2 The precision for the internal standard response (area)
should t>e 20 percent during any given analysis period at a
particular multiplier voltage of the mass spectrometer.
4. APPARATUS
4.1 Thermal Desorption Unit
4.1.1 The thermal desorption unit (Nutech Corporation Model 32'J
or equivalent) shall be capable of thermally desorbing the sorbent
E-77
-------
resin tubes. It shall be capable of rapidly heating the tubes to
180°C*10°C with flow of organic-free nitrogen through the tubes.
4.2 Purge and Trap Unit
4.2.1 The purge and trap unit consists of three separate pieces
of equipment: the sample purger, analytical sorbent trap and the
desorber. It should be capable of meeting all requirements of
Sections 5.2 thru 5.2.4 of EPA Method 624 for analysis of purge-
able organic compounds from water (8, 9). The analytical trap as
specified in EPA Method 624 consists of 3% SP-2100, Tenax, silica
gel, charcoal. Some users have found that improved performance
can be achieved using only Tenax and charcoal in the analytical
sorbent trap (5).
4.3 GC/MS System
4.3.1 Gas Chromatograph - An analytical system complete with a
temperature programmable GC suitable for on-column injection, and
all required accessories including syringes, analytical columns,
and gases.
4.3.2 Co1umn - Column dimensions shall be 1.8 m long by 0.25 cm
I.D. , stainless steel or glass, packed with 1% SP-1000 on Carbo-
pack 3 (60/80 mesh) or equivalent.
4.3.3 Mass Spectrometer - Capable of scanning from 20 to 260
amu every 7 seconds or less, utilizing 70 volts (nominal) electron
energy in the electron impact ionization mode and producing a mass
E-78
-------
spectrum which meets all criteria described in Method 624 when 5C
ng of 4-bromofluorobenzene (BFB) is injected through the GC inlet
4.3.4 GC/MS Interface - Any- GC to mass spectrometer interface
that gives acceptable calibration points at 50 ng or less per
injection for each of the parameters of interest and achieves all
performance criteria of Method 624 may be used. GC to mass
spectrometer interfaces constructed of all-glass or glass-lined
materials are recommended. Glass can be deactivated by silanizin
with dichloro-dimethylsilane.
4.3.5 Data System - A computer system must be interfaced to
the mass spectrometer that allows the continuous acquisition and
storage on machine readable media of all mass spectra obtained
throughout the duration of the chromatographic program. The com-
puter must have software that allows searching any GC/MS data fil<
for ions of a specified mass and plotting such ion abundances
versus time or scan number. This type of plot is defined as an
Extracted Ion Current Profile (EICP). Software must also be
available that allows integrating the abundance in any EICP
between specified time or scan number limits.
5. REAGENTS
5.1 Reagent Water
5.1.1 Reagent water is defined as water in which an interferent
is not observed at the detection limit of the parameters of
interest.
E-79
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5.1.2 Reagent water may be generated by passing tap water
through a carbon filter bed containing about 450 grams of acti-
vated carbon (Calgon Corporation, Piltrasorb-300 or equivalent).
*
5.1.3 Reagent water may also be prepared by boiling distilled
water for 15 minutes. Subsequently, while maintaining the temper-
ature at 90°C, bubble a contaminant-free, inert gas through the
water for one hour. While still hot, the water should be trans-
ferred to a narrow mouth, screw cap bottle and sealed with a
Teflon lined septum and cap.
5.1.4 Other methods which can be shown to produce reagent water
can be used.
5.2 Analytical Trap Reagents
a) Tenax (60/80 mesh) - Chromatographic grade or equivalent
b) Methyl silicone packing - 3% OV-1 on Chromosorb w (60/80
mesh) or equivalent
c) Silica gel, Davison Chemical (35/00 mesh), Grade 15 or
equivalent •
d) Charcoal, petroleum based (SKC Lot 104 or equivalent) (see
Section 6.2 in Part A)
E-80
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5.3 Stock Standard Solution
5.3.1 Stock standard solutions will be prepared from pure
standard materials or purchased certified solutions. The stock
standards should be prepared in me-Chanol using assayed liquids or
gases as appropriate. Because of the toxicity of some of the
organohalides, primary dilutions of these materials should be
prepared in a hood. A NIOSH/MESA approved toxic gas respirator
should be used when the analyst handles high concentrations of
such materials.
5.3.2 Fresh standards should be prepared weekly for volatile
POHCs with boiling points of <30°C. All other standards must be
replaced monthly, or sooner if comparison with check standards
indicates a problem.
5.4 Secondary Dilution Standards
5.4.1 Using stock standard solutions, prepare secondary dilu-
tion standards in methanol which contain the compounds of interest
either singly or mixed together, and at concentrations such that
the desorbed calibration standards will bracket the working range
of the analytical system.
5.5 Bromofluorobenzene (BFB) Standard
5.5.1 Prepare a 25 ug/ml solution of BFE in methanol.
*
5.6 Deuterated (dft) Benzene Standard
5.6.1 Prepare a 25 ug/ml solution in methanol.
E— 0 "1
OX
-------
6. CALIBRATION
6.1 Assembly of P-T-D Device
6.1.1 Assemble a purge and trap desorption device (P-T-D) which
meets all the requirements of Section 10.2 of this protocol and
Section 5.2 of USEPA Method 624 (3).
6.1.2 Connect the thermal desorption device to the purge and
trap device. Calibrate the P-T-D GC/MS system using the internal
standard technique (Section 6.2).
6.2 Internal Standard Calibration Procedure
6.2.1 This approach requires the use of deuterated benzene as
the internal standard for these analyses. Other internal stand-
ards may be proposed for use in certain situations. The important
criteria for choosing a particular compound as an internal stand-
ard are that it be similar in analytical behavior to the compounds
of interest, and it can be demonstrated that the measurement of
the internal standard is not affected by method or matrix inter-
ferences. Other internal standards which have been used are
dio-ethylbenzene and d4~l ,2-dichloroethane. Several users add 50
r.g of BFB to all sorbent cartridges (in addition to one or more
internal standards) to provide continuous monitoring of the GC/MS
performance relative to BFB.
6.2.2 Prepare calibration standards at a minimum of three con-
centration levels for each analyte of interest. The calibration
standards are -prepared by spiking a blank.Tenax or Tenax/charcoal
E-82
-------
cartridge with a methanolic solution of the calibration standards
(including 50 ng of the internal standard, such as deuterated
benzene) using the flash evaporation technique.
6.2.3 The cartridge shall be mounted in the gas chromatograph
so that the carrier gas enters the cartridge in the same direction
as during sample collection (which is opposite to the direction of
gas flow during P-T-D GC/MS analysis). The glass cartridge should
be attached to the injection port of a gas chromatograph. The
injector temperature is maintained at 160°C, and the carrier gas
flow through the cartridges should be maintained at about 50
ml/min.
<
6.2.4 The flash evaporation technique requires filling the
needle of a 5.0 (ul) syringe with clean methanol and drawing air
into the syringe until the tip of the plunger reaches the 1.0 ul
mark. This is followed by drawing a methanolic solution of the
calibration standards (containing 25 ug/ul of the internal
standard) until the tip of the plunger reaches the 3.0 AJ! mark.
The contents of the syringe should be slowly expelled through the
gas chromatograph injection port over about 15 seconds. After 25
seconds have elapsed, the gas flow through the cartridge should be
shut off, the syringe removed, and the cartridge analyzed by the
P-T-D GC/MS procedure outlined in Section 10.2. The total flow of
gas through the cartridges during addition of calibration standard
to blank cartridges, or internal standards to sample cartridges,
should be 25 ml or less to avoid breakthrough of volatile sample
components.
E-33
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6.2.5 Analyze each calibration standard on both Tenax and
Tenax/charcoal cartridges according to Section 10. The calibra-
tion procedures shall be identical to those used for analysis of
sample cartridges. If cartridges are analyzed separately, then
the Tenax and Tenax/charcoal cartridges must be calibrated sepa-
rately. The direction of carrier gas flow through the cartridges
during the desorption step should be opposite from the gas flow
through the cartridge during sample collection so the inlet side
of the cartridge during sample collection becomes the outlet side
during P-T-D analysis. Tabulate the area response of the charac-
teristic ions of each analyte against the concentration of the
internal standard and calculate response factor (RF) for each
compound using Equation 1.
RF = Ascis/AisCs [1]
where As « Area of the characteristic ion for the analyte
to be measured
Ais * Area of the characteristic ion for the internal
standard
Cis * Amount (ng) of the internal standard
Cs * Amount (ng) of the volatile POHC in calibration
standard
If the RF value over the working range is a constant «10% RSD) ,
the RF can be assumed to be invariant and the average RF can be
used for calculations. Alternatively, the results can be used to
plot a calibration curve of response ratios, As/Ais versus RF.
E-84
-------
6.2.6 The working calibration curve or RF must be verified on
each working day by the measurement of one or more of the cali-
bration standards. If the response varies by more than *25%, new
calibration standards must be prepared and analyzed.
7. QUALITY CONTROL
7.1 Each laboratory that uses this method is required to operate
a formal quality control program. The minimum requirements of
this program consist of an initial demonstration of laboratory
capability and the analysis of blank Tenax and Tenax/charcoal
cartridges spiked with the analytes of interest. The laboratory
shall demonstrate collection and/or recovery efficiencies for
compounds with boiling points outside the 30° to 100°C range,
which meet the method criteria, prior to field use of the VOST
(Part A, Section 3.2). The laboratory is required to maintain
performance records to define the quality of data which are
generated. Ongoing performance checks must be compared with
established performance criteria to determine if results are
within the expected precision and accuracy limits of the method.
(Note: NBS traceable audit cylinders are beiny developed by
Research Triangle Institute under the direction of USEPA-EMSL,
Research Triangle Park, NC. The cylinders may be used for
performance trials and evaluation of collection and recovery
efficiencies in lieu of the methods specified in this section.)
E-Si
-------
7.1.1 Before performing any analyses, the analyst must demon-
strate the ability to generate acceptable precision and accuracy
with this method. This ability is established as described in
Section 7.2.
7.1.2 Recovery data for compounds boiling between 100° and
150*C must be provided which meets the method criteria (see
Section 7.2.2). Laboratory evaluation is required in lieu of that
data. The method of evaluation is that specified in Section 7.2
with the exception that it is not required to pull 20 liters of
organic-free nitrogen through the sorbent cartridges.
7.1.3 Laboratory evaluation of collection and recovery effi-
ciencies shall be performed for compounds with boiling points
below 30°C. Due to the possibility of sample breakthrough and
poor recovery of the sample from the charcoal, the evaluation
shall be comparable to that described in Reference 5. A gas
stream containing the POHC shall be generated and sampled using
the VOST. The sampling rate for the laboratory evaluation shall
be the same as that proposed for field application. The
laboratory evaluation must meet the precision and accuracy
criteria described in Section 7.2.2.
7.1.4 The laboratory must spike all Tenax and Tenax/charcoal
cartridges with the internal standard(s) to monitor continuing
laboratory performance. This procedure is described in
1 Section 6.2.
E-86
-------
7.2 To establish the ability to generate acceptable accuracy and
precision, the analyst must spike blank Tenax and Tenax/charcoal
with the analytes of interest at two concentrations in the working
range by the flash vaporization technique discussed in Sections
6.2.3 and 6.2.4. The cartridges are removed from the gas chroma-
tograph and connected to a source of organic-free nitrogen. The
cartridges sample 20 liters of nitrogen at a flow rate equivalent
to that proposed for field use of VOST.
7.2.1 The average response factor (RF) and the standard devia-
tion (S) for each must be calculated.
7.2.2 The average recovery and standard deviation must fall
within the expected range for determination of volatile POHCs
using this method. The expected range for recovery (indicative of
accuracy) of volatile POHCs using this method is *50 percent. The
expected standard deviation is 25 percent.
7.3 The analyst must calculate method performance criteria for
the internal standard .
7.3.1 Calculate upper and lower control limits for method
performances using the average area response (A) and standard
deviation (S) for internal standard:
Upper Control Limit (UCL) « A + 3S
Lower Control Limit (LCD = A - 3S
r-87
-------
The UCL and LCL can be used to construct control charts which are
useful in observing trends in performance. The control limits
must be replaced by method performance criteria as they become
available from the USEPA.
7.4 Each day, the analyst must demonstrate through analysis of
blank Tenax and Tenax/charcoal cartridges and reagent water that
interferences from the analytical system are under control.
i
8. SAMPLE COLLECTION, PRESERVATION AND HANDLING
j 8.1 The requirements for sample collection, preservation, and
; handling are described in Part A of this protocol.
9. DAILY GC/MS PERFORMANCE TESTS
9.1 The daily GC/MS performance tests required for this method
are described in Section 10 of EPA Method 624 (9). The key
abundance criteria for BFB which must be met before any samples
are analyzed are listed below. This can be done by injecting 50
ng of BFB directly on the column or by adding 50 ng of BFB to a
blank Tenax sorbent cartridge (see Sections 6.2.3 and 6.2.4) and
desorbing this cartridge according to the procedures described in
Section 10. The latter procedure is preferred when all sample
sorbent cartridges are spiked with BFB in addition to one or more
of the internal standards discussed in Section 6.2.1.
E-88
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BFB KEY ION ABUNDANCE CRITERIA
Mass Ion Abundance Criteria
50 15 to 40% of mass 95
75 30 to 60% of mass 95
95 Base Peak, 1UO% Relative Abundance
96 5 to 9% of mass 95
173 <2% of mass 174
174 >50% of mass 95
175 5 to 9% of mass 174
176 >95% but <101% of mass 174
177 5 to 9% of mass 176
10. SAMPLE DESURPTION AND GAS CHROMATOGRAPHY
10.1 The P-T-D GC/MS procedures are those described in Section 11
of Method 624 (9) with the addition of the procedure described in
Section 10.2 for desorption of Tenax and Tenax/charcoal
cartridges.
10.2 The schematic of the P-T-D GC/MS system is shown in Figure
6. The sample cartridge is placed in the thermal desorption
apparatus (Nutech 320 or equivalent) and desorbed in the P-T-D
system by heating to 180°C for 10 minutes. Sample cartridges may
be desorbed in pairs. However, if the analyte concentrations are
anticipated to be sufficiently high to saturate the GC/MS when
desorbed in pairs, consideration should be given to individual
analysis of cartridges. The desorbed components pass into the
bottom of the water column, are purged from the water and
E-89
-------
collected on the analytical sorbent trap. After the 10-minute
desorption period, the compounds are desorbed from the analytical
sorbent trap into the GC/MS system according to the procedures
described in Section 11 of Method 624.
11. AQUEOUS COMPENSATE
11.1 Analysis of aqueous condensate samples should be performed
t
according to the procedures described in References 8 and 9. If
t
. the volatile POHCs of interest are water soluble, it is necessary
!
to demonstrate that this method is capable of recovery of the
volatile POHCs of interest using Method 624. This can be accom-
j plished by P-T-D GC/MS analysis of reagent water which has been
, fortified with the analytes of interest.
• 11.2 If adequate recovery of water soluble volatile POHCs cannot
I be achieved using the procedures described in References 8 and 9,
I
alternative methods for analysis, such as direct aqueous inject-
ion, may be required. If an alternative analytical method is
used, method performance must be documented by analysis of labora-
tory reagent water which has been fortified with the volatile
POHCs of interest.
11.3 Methods for analysis of water soluble volatile POHCs in
aqueous condensate are currently under development.
12. QUALITATIVE IDENTIFICATION
12.1 The qualitative identification procedure of volatile POHCs
using this protocol is described in Section 12 of Method 624 (9),
E-90
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13. CALCULATIONS
13.1 When an analyte has been qualitatively identified, quantifi-
cation should be based on the integrated abundance from the EICP
of the primary characteristic ion chosen for that analyte. If the
sample produces an interference for the primary characteristic
ion, a secondary characteristic ion should be used.
13.1.1 Using the internal standard calibration procedure, the
amount of analyte in the sample cartridge is calculated using the
response factor (RF) determined in Section 6.2.5 and Equation 2.
Amount of POHC « AsCis/AisRF [2]
where AS * Area of the characteristic ion for the analyte
to be measured
Ais = Are* for tne characteristic ion of the internal
standard
Cj_s « Amount (ng) of internal standard
13.1.2 The choice of methods for evaluating data collected using
VOST for incinerator trial burns is a regulatory decision. The
procedures used extensively by one user are outlined below (10).
13.1.3 The total amount of the POHCs of interest collected on a
pair of traps should be summed. These values should then be blank
corrected. Guidelines for blank correction of sample cartridges
are outlined below.
E-91
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13.1.3.1 After all blanks (field and trip) are analyzed, a
paired t-test should be used to determine whether trip blanks are
significantly different from field, blanks. If no difference is
found, then the mean and standard deviation of the combined field
and trip blanks for each POHC of interest is calculated, and that
value is used as the blank.
13.1.3.2 If, using the paired t-test, the field and trip blanks
are determined to be different, then the field blank (or the mean
of multiple field blanks) associated with a particular run should
be used as the blank value for that particular run.
13.1.3.3 If an individual field blank is used as the blank value
for a particular run, the VOST user must evaluate whether this
blank is different from sample cartridges associated with this
blank. Although no specific criteria are offered here for guid-
ance in this case, specific criteria for use of individual field
blanks for blank correction will be developed as more data for use
of VOST becomes available. This situation can be alleviated by
including two field blanks (i.e., two blank Tenax and two blank
Tenax/charcoal cartridges) per run.
13.1.4 Next, for each sample/POHC combination, a determination
must be made as to whether a particular sample is significantly
different from the associated blank. If the mean of the trip and
field blanks is used, then a sample is different from the blank if
E-92
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(measured sample value)-(mean blank value) £3
x blank standard deviation
If the sample is determined to be different from the blank accord-
ing to the above criteria, then .the emission value of a particular
POHC is blank corrected by subtracting the mean blank value (as
defined in Section 12.1.3) from the measured sample value. (If an
individual field blank is used as the blank value, the above
criteria do not apply.)
13.1.5 If, according to the above procedures, the sample cannot
be distinguished from the blank (i.e., for a given POHC there is a
high sample value and high blank value or there is a low sample
(
value and low blank value), the measured sample value is not blank
corrected. In this case, the measured sample value is used to
calculate a maximum emission value (and therefore a minimum DRE
value) for that particular run.
13.1.6 The observation of high concentrations of POHCs of inter-
est in blank cartridges indicates possible residual contamination
of the sorbent cartridges during shipment and use at the site.
Data which fall in this category (especially data indicating high
concentrations of POHCs in blank sorbent cartridges) should be
qualified with regard to validity, and blank data should be re-
ported separately. The applicability of data of this type to the
determination of DRE is a regulatory decision. Continued observa-
tion of hign concentrations of POHCs in blank sorbent cartridges
E-92
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indicates that procedures for cleanup, monitoring, shipment and
storage of sorbent cartridges by a particular user, be investi-
gated to eliminate this problem.
13.1.7 After blank corrections have been made, the amounts of
individual. POHCs on each sorbent cartridge used for a given run is
summed and divided by the volume of gas sampled to obtain the
concentration of each POHC in the stack gas.
13.1.8 If any internal standard recoveries fall outside the con-
trol limits established in Section 7.3.1, data for all analytes
determined for that cartridge(s) must be qualified with the
observation.
14. METHOD PERFORMANCE
14.1 The method detection limit, average recoveries and standard
deviation of the average recoveries of the analytes determined
using this method have not yet been established. The method
performance will be documented as more data become available.
E-94
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REFERENCES
(For A and B)
1) Resource Conservation and Recovery Act, Subtitle
{3001-3013,42 USC 6921-6934 (1976) and Supplement IV (I960)].
2) Vogel, G., et al. "Guidance M,anual for Hazardous Waste
Incineration Permits," EPA-68-01-0092, SW-966, NTIS
PB-84/100577, July 1982.
3) Code of Federal Regulations, Title 40, Part 60, Appendix A,
1980.
4) Harris, J. C., et al. "Sampling and Analysis Methods for
Hazardous Waste Combustion," EPA 600/8-84-002, February 1984.
5) Jungclaus, G., et al. "Development of a Volatile Organic
Sampling Train (VOST)," Presented at 9th Annual Research
Symposium, Land Disposal, Incineration and Treatment of
Hazardous Wastes, Ft. Mitchell, KY, May 2-4, 1983.
6) Federal Register, 42, 41758-41768, August 18, 1977.
7) USEPA. Quality Assurance Handbook for Air Pollution
Measurement Systems, Vol. Ill, Office of Research and
Development,Environmental Monitoring and Support Laboratory,
Research Triangle Park, NC.
8) Federal Register, 44, 69464, December 3, 1979.
9) Longbottom, J. and J. Lichtenberg, eds. , "Methods for Organic
Chemical Analysis of Municipal and Industrial Wastewater;
Test Methods," Method 624, EPA-600/4-82-057, 1982.
10) Trenholm, A. Midwest Research Institute, Personal
Communication, August 5, 1983.
E-95
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TECHNICAL REPORT DATA
ffleatt rtud Ifurucnon* on tHt rtvtne be fort comptennfj
i HEPORTNO 2.
EPA-600/3-84-007
4 TlTLt AND SUiTITLE
Protocol for the Collection and Analyses of Volatile
POHCs Using VOST
7 AuTMORtSl
Earl M. Hansen
9 PERFORMING ORGANIZATION NAME AND ADDRESS
Envirodyne Engineers, Inc.
121C1 Lackland Road
St. Louis, Missouri 63416
12 SPONSORING AGENCY NAME AND ADDRESS
EPA, Office of Research and Development
Industrial Environmental Research Laboratory
Research Triangle Park, NC 27711
3. RECIPIENT'S ACCESSION- NO.
•. REPORT OATE
March 1984
•. PERFORMING ORGANIZATION CODE
•. PERFORMING ORGANIZATION REPORT is
10. PROGRAM ELEMENT NO.
11. CONTRACT/GRANT NO
68-02-3697, Task 3
13. TYPE Of REPORT ANO PERIOD COVERI
Task Final: 4/83-2/84
14. SPONSORING AGENCY CODE
EPA/600/13
is. SUPPLEMENTARY NOTES IERL-RTP project officer is Robin M. Anderson, Mail Drop
919/541-7607.
62
16. ABSTRACT
The document is a state-of-the-art operating protocol for sampling and
analysis of volatile organic constituents of flue gas from hazardous waste inciner-
ators or other similar combustor systems using the Volatile Organic Sampling Tra
(VOST). It is intended to be used for guidance by personnel of the regulatory grou-
personnel associated with engineering research and development, and the regula
community. The document is in two parts. Part A describes the key components „
the train, the procedures for preparing the sorbent materials, and procedures for
sample collection using the VOST. Part B describes the procedures for analyzing
VOST sorbent cartridges for volatile principal organic hazardous constituents
(POHCs) using purge-trap-desorb gas chromatography/mass spectrometry (P-T-I
GC/MS). Quality control procedures are presented in both parts.
•7. . IDENTIFIERS/OPES ENDED TERMS
Pollution Control
Stationary Sources
VOST
19 ScCUR'TY CLASS ,THu Report/
Unclassified
20. SICUR'TY CLASS /Thu pag*l
Unclassified
c. COSATi Fieid/Croui
13 B
21B 11G
07C 06T
14B
14G
n NQ o* PAGES
60
22 PRICE
EPA Porm 2320-1 U-73)
E-96
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f'i
I '
f 1
NATIONAL INSTITUTE
FOR OCCUPATIONAL SAFETY AND HEALTH
METHOD NO. P & CAM 127
6060A
-------
ORGANIC SOLVENTS IN AIR
Physical and Chemical An.-.lypis Branch
Analytical Method
Analyte:
Matrix:
Procedure:
Date Issued:
Date Revised:
Organic Solvents
(See Table 1)
Air
Adsorption on charcoal
desorption with carbon
disulfide, GC
9/15/72
7/15/74
Method No:
Range:
Precision:
Classification :
PiCAM 1^7
For the specific j
compound, refer :
to Tables I&II
10.5:: RSD
i
i
See Table 1
i
Principle of the Method
1.1 A known volume of air is drawn through a charcoal tube to trap the
organic vapors present.
1.2 The charcoal in the tube is transferred to a snail, graduated test
tube end desorbed with carbon disulfide.
1.3 An aliquot of the desorbed sample is injected into a gas chronato-
graph.
1.4 The area of the resulting peak is determined and compared with areas
obtained from the injection of standards.
Range and Sensitivity
The lower limit in mg/sample for the specific compound at 16 x 1
attenuation on a gas chromatograph fitted with a 10:1 splitter is
shown in Table 1. This value can be lowered by reducing the
attenuation or by eliminating the 10:1 splitter.
Interferences
3.1 When the amount of water ir the air is so great that condensation
actually occurs in the tube, organic vapors will not be trapped.
Preliminary experiments indicate that high humidity severely
decreases the breakthrough volume.
3.2 V*hen two or more solvents are knr'.T or suspected to be prese-;: in
ci'e c i.-, suc'.i inrurr'.jLion iin.luci;i.' -hs-ii fUSpecccU
should be transmitted with the sarpi-?; since vith dif
polarity, one may displace another fr-'~ the charcoal.
E-9-
-------
3.3 It must be enphasized that any compound which has the same
retention time as the specific compound under study at the
operating conditions described in this method is an inter-
ference. Hence, retention tine data on a single column, or
even on a number of columns, cannot be considered as proof
of chemical identity. For this reason it is important that
a sample of the bulk solvent(s) be submitted at the sane time
so that identity(ies) can be established by other means.
3.A If the possibility of interference exists, separation conditions
(column packing, temperatures, etc.) must be changed to circum-
vent the problem.
4. Precision and Accuracy
A.I The mean relative standard deviation of the analytical method is
8%. (Ref. 11.4).
4.2 The mean relative standard deviation of the analytical method
plus field sampling using an approved personal sampling pump is
10% (Ref. 11.4). Part of the error associated with the method
is related to uncertainties in thfe sample volume collected. If
a more powerful vacuum pump with associated gas-volume integrating
equipment is used, sampling precision can be improved.
4.3 The accuracy of the overall sampling and analytical method is 1C%
(NIOSH's unpublished data) when the personal sanpling punp is
calibrated with a charcoal tube in the line.
5. Advantages and Disadvantages of the Method
5.1 The sanpling device is small, portable, and involves no liquids.
Interferences are minimal, and most of those which do occur can be
eliminated by altering chromatographic conditions. The tubes are
analyzed by means of a quick, instrumental method. The method can
also be used for the simultaneous analysis of two or more solvents
suspected to be present in the sane sample by sir.ply changing gas
chromatographic conditions from isothermal to a teaperature-
programned mode of operation.
5.2 One disadvantage of the method is that the amount of sample which
can be taken is limited by the number of milligrams that the tube
will hold before overloading. When the sample value obtained for
the backup section of the charcoal trap exceeds 25^ of that found
on the front section, the possibility of sample loss exists.
During sample storage the more volatile cor.pounds will migrate
jhro-jghout che _ube -.MCil aquilibrlur. is> rsacheJ (jj'-' oi c?.t
sar.ple on the backup section) .
E-98
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5.3 Furthermore, the precision of the method is limited by the
reproducibility of the pressure drop across the tubes. This
, drop will affect the flow rate and cause the volune to be
}' imprecise, because the punp is usually calibrated for one
tube only.
;" " 6. Apparatus
6,1 An approved and calibrated personal-sampling pump for personal
|i samples. For an area sample any vacuum pump whose flow can be
' • determined accurately at 1 liter per minute or less.
.. 6.2 Charcoal tubes: glass tube with both ends flame sealed, 7 cm
I long with a 6-mm O.D. and a 4 -mm I.D., containing 2 sections of
20/40 mesh activated charcoal separated by a 2-mm portion of
urethane foam. The activated charcoal is prepared from coconut
j' shells and is fired at 600DC prior to packing. The absorbing
' section contains 100 mg of charcoal, the backup section 50 rig.
; A 3-rrtm portion of urethane foam is placed between the outlet
i. end of the tube and the backup section. A plug of silylated
glass wool is placed in frontof the absorbing section. The
press-re drop across the tuLe n-sc be less than one inch of
mercury at a flow rate ot 1 £pm.
/
6.3 Gas chroma to graph equipped with a flame ionization detector.
; 6.4 Column (20 ft x 1/8 in) with 10% FFAP stationary phase on 80/100
mesh, acid-washed DMCS Chromosorb U solid support. Other colunr.s
capable of performing the required separations may be used.
| 6.5 A mechanical or electronic integrator or a recorder and some
method for determining peak area.
6.6 Glass stoppered micro tubes. The 2.5-nt graduated microcentrifuge
tubes are recommended.
6.7 Hamilton syringes: 10 '.1, and convenient sizes for making
standards .
6.8 Pipets: 0.5 ml delivery pipets or 1.0 ri. type graduated in
0.1 ni increments.
i 6.9 Volumetric flasks: 10 ml or convenient sizes for making standard
solution?.
7.1 Spectrocuality carbon disulfice O'sthesor. Colerar and Bell)
E-99
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7.2 Sr.rple of the specific compound 'jndrT stuc'v, nrcfer.iblv
chromatoquality grade.
7.3 Bureau of Mines Grade A helium.
7.4 Prer>urified hydrogen.
7.5 Filtered compressed air.
8. Procedure
8.1 Cleaning of Equipment. All glassware used for the laboratory
analysis should be detergent washed and thoroughly rinsed with
tap water and distilled water.
8.2 Calibration of Personal Purps. Each personal pump must be
calibrated with a representative charcoal tube in the line. This
will minimize errors associated with uncertainties in the sample
volume collected.
8.3 Collection and Shipping of Samples
?.?.! Irradiate]y before S2T.plir.~, the errl^ of the tube should
be broken to provide an oceninp at least one-half the
internal diameter of the tube (2mm) .
8.3.2 The smaller section of charcoal is used as a back-up and
should be positioned nearest the sampling pump.
8-3.3 The charcoal tube should be vertical during sampling.
8.3.A Air being sampled should rot be passed through any hose
or tubing before entering the charcoal tube.
8.3.5 The flow, time, and/or volume must be measured as accurately
as possible. The sample should be taken at a flow rate of
1 Upm or less to attain the total sarnie volume required.
The minimum, and maximum ssr.ple volumes that should ba
collected for each solvent are shown in Table 1. The
minimum volume quoted must be collected if the desired
sensitivity is to be achieved.
E.3.6 The temperature and pressure of the atmosphere beina sampled
should be measured and recorded.
The charcoal tubes shoul: be cached '..'i-th the supplied plasti
caps- immediately after sarolinc. Vnder no circurst^rces
should rubber ccps be useJ.
E-100
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8.3.8 One tube should be bandied in the same manner as the
sample tube (break, seal, and transport), except that
no air is sampled through this tube. This tube should
be labeled as a blank.
8.3.9 Capped tubes should be packed tightly before they are
shipped to minimize tube breakage during shipping.
8-3.10 Samples of the suspected solvent(s) should be submitted
to the laboratory in containers furnished by NIOSH for
such purpose. These liquid bulk samples should not be
transported in the same container as the samples or blank
tube. If possible, a bulk air sample (at least 50£ air
drawn through tube) should be shipped for qualitative
identification purposes.
8.4 Analysis of Samples
8.4.1 Preparation of Samples. In prepration for analysis, each
charcoal tube is scored with a file in front of the first
section of charcoal and broken open. The glass wool is
removed and discarded. The charcoal in the first (larger)
section is trans f^-.-ed to a small stoppered test tube. The
i>eparatinp, section of foam is renoved and discarded; the
second section is transferred to another test tube. These
two sections are analyzed separately.
8.4.2 Desorption of Samples. Prior to analysis, one-half ml of
carbor. disulfide is pipetted into each test tube. (All work
with carbon disulfide should be performed in a hood because
of its high toxicity.) Tests indicate that desorptior. is
complete in 30 minutes if the sample is stirred occasionally
during this period. The use of graduated glass-stoppered,
microcentrifuge tubes is recommended so that one can observe
any apparent change ir. volume during the desorption process.
Carbon disulfide is a very volatile solvent, so volume
changes can occur during the desorption process depending or.
the surrounding ter.perature. The initial volume occupied by
the charcoal plus the 0.5 mi CS0 should be noted and corres-
ponding volune adjustments should be made whenever necessary
just before GC analysis.
8.4.3 GC Conditions. The typical operating conditions for the gas
chromatograph are:
1. 85 cc/r.in. (70 p?ig) heliur?, carrier gas flow.
2. 65 cc/r.in. (24 psig) hydrogen gas flow to detector.
-> _ c.o^ cc/-ir.. •'5C ~wi~/ Jw.r j'^ov
4. 200°C injector tcrr?erature.
E-101
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5. 200°C manifold temperature (detector)
6. Isothermal oven or column temperature - refer to Table 1
for specific compounds.
8.4.4 Injection. The first step in the analysis is the injection
of the sample into the gas chromatograph. To eliminate
difficulties arising from blowback or distillation vithin
the syringe needle, one should employ the solvent flush
injection technique. The 10 \ti syringe is first flushed
with solvent several times to wet the barrel and plunger.
Three microliters of solvent are drawn into the syringe
to increase the accuracy and reproducibility of the
injected sample volume. The needle is removed from the
solvent, and the plunger is pulled back about 0.2 u£ to
separate the solvent flush frop the sample with a pocket
of air to be used as a marker. The needle is then immersed
in the sample, and a 5-uJ. aliquot is withdrawn, taking into
consideration the volume of the needle, since the sample in
the needle will be completely injected. After the needle
is removed from the sample and prior to injection, the
plunger is pulled back a short distance to minimize evap-
oration of the sanple from the tip of the needle. Duplicate
injections of each sample and standard should be nade. No
more than a 3% difference in area is to be expected.
8.4.5 >feasurement of area. The area of the sample peak is r.easured
by an electronic integrator or some other suitable fora of
area measurement, and preliminary results are read from a
standard curve prepared as discussed below.
7B.5 Determination of Desorption Efficiency
8.5.1 Importance of determination. The desorption efficiency of a
particular compound can vary fron one laboratory to another
and also from one batch of charcoal to another. Thus, it is
necessary to determine at least once the percentage of the
specific compound that is removed in the desorption process
for a given rtor.pound, provided the same batch of charcoal is
used. The Physical and Chemical Analysis Branch of NIOSH
has found that the desorption efficiencies for the cocpour.ds
in Table 1 are between 81* and 100" and vary with each batch
of charcoal.
8.5.2 Procedure for determining desorption efficiency. Activated
charcoal equivalent to the amount in the first section of the
sampling tube (100 rg) is measured into a 5cn, 4-n=r. I.D.
glass tube, flar:e-sealed at one end (similar to co—.ercially
available culture tubes). This charcoal T.ust be frcr the
same batch as that used in obtaining the samples and can be
E-102
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with Parafiln. A known anount of the compound is injected
directly into the activated charcoal with a microliter
syringe, and the tube is capped with more Parafilm. The
amount injected is usually equivalent to that present in
a 10-liter sample at a concentration equal to the federal
standard.
At least five tubes are prepared in this manner and allowed
to stand for at least overnight to assure complete abosrption
of the specific compound onto the charcoal. These five tubes
are referred to as the samples. A parallel blank tube should
be treated in the same manner except that no sample is added
to it. The sample and blank tubes are desorbed and analyzed
in exactly the same manner as the sampling tube described in
Section 8.3.
Two or three standards are prepared by injecting the sane
volume of compound into 0.5 mi of C$2 with the same syringe
used in the preparation of the sample. These are analyzed
with the sarnies.
The desorption efficiency equals the difference between the
average peak area of the sasples and the peak area of the
blank divided by the average peak area of the standards, cr
Area sasple - Area blank
desorption efficiencv = '""
Area standard
9. Calibration and Standards
It is convenient to express cone ntration of standards in terns of
mg/0.5 mx CS- because samples are desorbed in this amount of CS->. To
minimize error due to the volatility of carbon disulfide, one can inject
20 times the weight into 10 n- of CS->. For exar.ple, to prepare a 0.3 -g/
0.5 r.l standard, one vculd inject 6.0 rg into exactly 10 r.l c: CH^ i- a
plass-stcppered flask. The density of the specific cor.pour.d is used to
convert 6.0 rig into micrcliters for easy measurement with a micreliter
syringe. A series of standards, varying in concentration over the rar.ge
of interest, is prepared and analyzed under the sar.e GC conditions ar.d
during the same time pericd as the unknown samples. Curves arc estab-
lished by plotting concentration in r.g/0.5rv versus peak area.
•^ X
NOTI: Since no ir.t-arr.ai itaru.-.rd is use." in the method, standard sciatic-:
rust be analyzed at the sare t-'.re t'1?.: tl-e sample ar.alysis is ccr.5 . This
durinc the sare dav of the TID res-onse.
E-103
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10. Calculation:*
10.1 The weight, in mg, correspond ins to each peak area is read from
the standard curve for the pirt i rul ".'r cor.po'jnd. '>> volune
corrections are needed, because the standard curve is based on
ng/0.5 m£ C$2 and the volume of sample injected is identical to
the volune of the standards injected.
10.2 Corrections for the blank must he nade for each sample.
Correct mg = mgg - mp.,
where:
n8s * m? found in front section of sample tube
ngjj « mg found in front section of blank tube
A similar procedure is followed for the backup sections.
10.3 The corrected amounts present in the front and backup sections of
the same sample tube are added to determine the total measured amount
in the sample.
10.4 This total weight is'divided by the determined desorption efficiency
to obtain the total mg per sample. _ _
10.5 The volume of aJr sampled is converted to standard cor.d^cio.-.s of
of 25°C and 760 inn Hg.
s
where:
P 293
Vs = V * 760 T+273
V = volume of air in liters at 25°C and 760 r.= Hg
V = volume of air in liters as measured
P = Baronetric pressure ir. ca Hg
T = Temperature of air in degree centigrade
10.6 The concentration of the organic solvent in the air sampled can be
e:-:pressed in r.g per rP, which is numerically equal to ug per liter
of air
, 3 ,. total zi2 ("Section 10.4) x 1COC (,?/-;)
r.g/mj = ug/i = • —
10.7 Another method of expressing concentration is pp~, defined as -.of
compounds per liter cf air
ppm = 1.1 of compound/Vs
*»•,;• of co-pound 24.45
ppn = ' :<
Vs :r';
where:
JJ«.t5'- r.dijr »-oiu .e ec ^.^'L and 760 rrr. H;.
\": = nolecuiar weight of the co-scur.d (Table i)
E-104
— — -- -**•*-* •
-------
11. References
11.1 White, L.D., D.G. Taylor, P. A. Mauer , and R.E. Kupel , "A
Convenient Optimized Method -for the Analysis of Selected Solvent
Vapors in the Industrial Atmosphere," Amer. Ind. Hyg. Assoc . J.,
(1970).
11.2 Young, D.M. and A.D. Crowe 11, Physical Adsorption of Gases,
Buttervorths, London, 196?, pp. 137-146.
11.3 Federal Register. _37_ (/'202), 22139-221-42 (October 18, 1972).
11.4 NIOSH Contract HSM-99-72-98, Scott Research Laboratories, Inc.,
"Collaborative Testing of Activated Charcoal Sampling Tubes for
Seven Organic Solvents," pp. 4-22, 4-27 (1973).
E-105
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W
I
M
O
CT\
TAIJLE i
PARAMETERS ASSOCIATED WITH PtCAB ANALYTICAL METHOD NO. 127
Solvent
Method
Classification
Detection IJinit
(mg/sample)
Acetone
Beiueno
Carton trtrachlor ide •• I
Chlurof orm
Dic'iloromothane
p-f) [oxalic
Eth fli-ne d Ichlor Ide
Methyl i-thyl ketone
S'ty i ene
Tut i achloroethylene
1,1 2-1 1 Ichloroc'thane
1,1 i -t r Ichlovouthane
(: 'ethyl Chloroform)
Tr i . h lomet hy lone
Tol i ---nr |,( ..«
.Kyi- MI-
(a) Minimum volume, in liters,
(b) I'lii-KC arc breakthrough vol
D
A
A
A
D
A
I)
B
U
B
B
B
A
B
A
required to me
umes calculated
_
0.01
0.20
0.10
0.05
0.05
0.05
0.01
0.10
0.06
0.03
0.05
0.05
0.01
0.02
asure 0.
with d<-i
Sample
mit ., .
) Minimum13'
0.5
0.5
10
0.5
0.5
1
1
0.5
1.5
1
10
0.5
1
0.5
0.5
Volume (£)
(b)
Maximum
7.7
55
60
13
3.8
18
12
13
34
25
97
13
17
22
31
GC Column
Temperature(°C)
60
90
60
80
85
100
90
80
150
1JO
150
150
90
120
100
Molecular
Weight
58.1
78.1
154.0
119
84.9
88.1
99.0
72.1
104
166
133
133
131
92.1
U»6
net ivatotl coconut charcoal. Concentrations of vapor in air at 5 times the OSHA standard (reference 11.3)
-jr ')!!() ppm, whichever is lower, 25°C, and 760 torr were assumed. These values will be as much as 50% lower
for aln'osplu-rc-s of high humidity. The effects of multiple contaminants have not been investigated, but It
is suspected that Iff.s volatile compounds may displr.ee more volatile compounds (See 3.1 and 3.2)
-------
TABLE II
CHEMICALS WHICH HAVE GREATER THAN 80%
DCSCP.PTIO:: EFFICIENCY BUT HAVE NOT BEEN
THOROUGHLY TESTED 3Y NIOSH
Class E (Proposed)
Acrylonitrile
Allyl glycidyl ether
n-Amyl acetate
2-Butoxyethanol
n-Butyl acetate
n-Butyl alcohol
n-Butylglycidyl ether
Chlorobenzene
Cyclohexane
Cyclohexanone
o-Dichlorobenzene
p-Dichlorobenzene
Diethyl ether
N.N-Dimethyl aniline
Epichlorohydrin
2-Ethoxylethyl acetate
Ethyl acetate
Ethylbenzer.e
Ethyl butyl ketone
Fufural
Heptane
Hexane
Isoa-vl acetate
Isobutyl acetate
Isobutyl alcohol
Isoctane
Isophorone
Isopropyl acetate
Isopropyl glycidyl ether
2,6-Lutidine
Methyl acetate
Methyl acrylate
Methyl n-butyl ketone
Methyl ethyl ketore
Methyl isobutyl ketone
Methyl nethacrylate
i-Methyl styrene
p-M«jthyl styrene
n-Octane
3-Octar.one
Pentane
2-Per. tnnone
a-pinene
r.-Propyl acetate
1,1,2,2-Tetrachloroethane
Tetrahydrcfurar.
Trichlorotrifluoroethane (Freon 113)
Recorrr.ended Sample Size
E-107
-------
I '
STANDARD METHOD 209 G
6060A
-------
209 G. -Volatile and Fixed Matter in Nonfiltrable Residue and in
Solid and Semisolid Samples
1. General Discussion
This method is applicable to the deter-
mination of total residue on evaporation
and us fixed and volatile fractions in such
solid and semisohd samples as river and
lake sediments, sludges separated from
water and wastewater treatment process-
es, and sludge cakes from vacuum filtra-
tion, cenmfugauon. or other sludge dewa-
jcrmg processes.
The determination of both total and vol-
atile residue in these materials is subject to
negative error due to loss of ammonium
carbonate [(NH4):.CO,] and volatile organ-
ic matter while drying. Although this is
true also for wastewater. the effect tends
to be more pronounced with sediments.
and especially with sludges and sludge
cakes.
The mass of organic matter recovered
from sludge and sediment requires a long-
er ignition time than that specified for resi-
due from wastewaters. effluents, or pol-
luted waters. Carefully observe specified
ignition time and temperature to control
losses of volatile inorganic salts.
Make all weighings quickly because wet
samples tend to lose weight by evapora-
tion After drying or ignition, residues of-
ten are very hygroscopic and rapidls ab-
sorb moisture from the air.
2 Apparatus
See Sections 209A.2 and 209B.2.
3 Procedure
a. Solid and setnisoltJ stinipln:
I) Total residue and moisture —
a) Preparation of evaporating dish—Ig-
nite a clean evaporating dish at 550 = 50 C
for 1 hr in a muffle furnace. Cool in a des-
iccator, weigh, and store in a desiccator
until ready for use.
bl Fluid samples —If the sample con-
tains enough moisture to flow more or less
readily, stir to homogenize, place 25 to
50 g in a prepared evaporating dish, and
weigh to the nearest 10 mg. Evaporate to
dry ness on a water bath, dry at 103 C for I
hr. cool in an individual desiccator con-
taining fresh desiccant. and weigh
c) Solid samples— If the sample con-
sists of discrete pieces of solid material
(dewatered sludge, for example), take
cores from each piece with a No. 7 cork
borer or pulverize the entire sample
coarsely on a clean surface by hand, using
rubber gloves. Place 25 to 50 g in a pre-
pared evaporating dish and weigh to the
nearest 10 mg Place in an oven at 10? C
overnight. Cool in an individual desiccator
containing fresh desiccant and weigh Pro-
longed heating may result in a loss of vola-
tile organic matter and (NH..I..CO,. bui
it usually is necessary to dry samples
thoroughly.
2) Volatile residue —Determine volatile
residue, including organic matter and vol-
atile inorganic salts, on the total residue
E-108
-------
obtained in I) above. Avoid loss of solids
by decrepitation by placing dish in a cool
muffle furnace, heating furnace to 550 C,
and igniting for 60 mm. (First ignite sam-
ples containing large amounts of organic
matter over a gas burner and under an ex-
haust hood in the presence of adequate air
to lessen losses due to reducing conditions
and to avoid odors in the laboratory.) Cool
m a desiccator and re weigh. Report results
as fixed residue (percent ash) and volatile
residue.
h. Sonfiltrable residue (suspended
matter):
1) Preparation of glass-fiber filter-
Place a glass-fiber niter in a membrane ni-
ter holder. Hirsch funnel, or Buchner fun-
nel, with wrinkled surface of filter facing
upward. Apply vacuum to the assembled
apparatus to seat filter. With vacuum ap-
plied, wash filter with three successive 20-
mL portions of distilled water. After the
water has filtered through, disconnect vac-
uum, remove filter, transfer to an alumi-
num or stainless steel planchet as a sup-
port, and dry in an oven at 103 C for 1 hr
(30 mm in a mechanical convection oven).
If volatile matter is not to be determined,
cool filter in a desiccator to balance tem-
perature and weigh. If volatile matter is to
be determined, transfer filter to a muffle
furnace and ignite at 550 C for 15 min. Re-
move filter from furnace, place in a desic-
cator until cooled to balance temperature.
and weigh.
2) Treatment of sample—Except for
samples that contain high concentrations
of filtrable matter, or that filter very slow-
ly, select a sample volume £14 mL/cm*
titter area.
Place prepared filter in membrane filter
holder. Hirsch funnel, or Buchner funnel.
with wrinkled surface upward. With vacu-
um applied, wet filter with distilled water
to seat it against holder or funnel. Measure
well-mixed sample with a wide-tip pipet
or graduated cylinder. Filter sample
through filter using suction. Leaving suc-
tion on, wash apparatus three times
10-mL portions of distilled water, allowing
complete drainage between washings. Di$.
continue suction, remove filter and dry to
constant weight (see 209B.3c) at 103 C for
I hr in an oven (30 min in a mechanical
convection oven). After drying, cool filter
in a desiccator to balance temperature and
weigh.
3) Filtration with Gooch crucibles—Al.
tematively, use glass-fiber filters of 2.2 or
2.4 cm diam with Gooch crucibles and fol-
low the procedure in Section 209D.36.
4) Ignition—Ignite filter with its non-
filtrable residue (total suspended matter)
for 15 min at 550 ± 50 C, transfer to a des-
iccator, cool to balance temperature, and
weigh.
4. Calculation
a. Solid and semisolid samples:
total residue
A x IQO
B
volatile residue
fixed residue
b. Sonfiltrable residue (suspended mat-
ter):
mg nondurable volatile residue L
. (D ~ & * ' -000
sample volume. mL
mg nondurable fixed residue L
C x i.OQO
3g _M«HM_^_«_~^~^H^^
sample volume. mL
where:
A " weight of dried solids, mg.
B « weight of wet sample, mg.
C * weight of ash. mg.
D « weight of residue before ignition, mg,
and
E » weight of residue after ignition, mg.
5. Precision and Accuracy
See Section 209D.5.
E-109
-------
Methods for Chemical Analysis of Water 2 SOKOLOFF. V.P 1933. Water of crystalliza
' a Wastes 1974 U.S EPA. Technology lion in total solids of water analysis Ind
*" r. 625-'6-74-003. pp 266-267 Eng. Chem.. Anal Ed 5.336
209 I. Bibliography
E.J 4 H H WAGENHALS 1923 medium in the suspended solids determma-
'studies of representative sewage plants tion Sewage Ind. Wastes 30-1062
Pub Health Bull. Ho 132. NUSBAUM. I 1958 New method for determma-
MOWARD C.S 1933. Determination of total tion of suspended solids. Sewage Ind
dissolved solids in water analysis Ind Wastes 30:1066.
Ing Chem.. Anal Ed 5.4 SMITH. A.L 4 A.E GREENBERG 1963 Evalu-
HONS G.E 4B MORE> 1941. The effect of ation of methods for determining sus-
drymg time on the determination of solids pended solids in wastewater. J Water Pol-
in sewage and sewage sludges Sewage lui. Control Fed 35'940.
Works J 13-936. GOODMAN. B.L. 1964. Processing thickened
FncHER. A.J 4 G.E. SYMONS 1944 The de- sludge with chemical conditioners. Pages
termination of settleable sewage solids by 78 et seq in Sludge Concentration. Filtra-
weight Woier Works Sewage 91:37. tion and Incineration Univ. Michigan Con-
DIGEN. J 4 F E. NUSSBERGER. 1956 Notes on tinued Education Ser. No. 113. Ann Arbor.
the determination of suspended solids WYCKOFF. B.M. 1964 Rapid solids determma-
Sewage Ind Wastes 28:237 tion using glass fiber filters. Water Sewage
CMANIN G.. E.H. CHOW. R B ALEXANDER 4 Works 111:277
j POWERS 1958. Use of glass fiber filter
E-110
-------
APPENDIX F
FIELD/ANALYTICAL DATA
6060A
-------
PARAMETER
CONTROL PARAMETERS
1. TARGET SOIL RESIDENCE TIME
a. TARGET SCREW SPEED
2. TARGET SOIL DISCHARGE TEMP
3. TARGET AIR INLET TENP
4. TARGET AIR FLU RATE
SOIL SYSTEM PARAMETERS
1. TEMPERATURE
a. FEED SOIL (C)
b. PROCESSED SOIL (C)
2. VOCs
a. FEED SOIL
1. D1CHLORDETHYLEN!
COI
2. TRICHLOROETHYLEI
C(
3. TETRACHLOROETHYi
4. IYLENE-LAB (ug/kg)
CORRESP (ug/kg)
(I/HR)
5. OTHER VOCs-LAB (ug/kg)
CORRESP
6. TOTAL VOCs-LAB (ug/kg)
CORRESP
b. PROCESSED SOIL
1. DICHLOROETHYLE
2. TRICHLQROETHYL
3. TETRACHLOROETH
4. XYLENE lug/kg)
(I/HR)
5. OTHER VOCs (ug/kg)
(I/HR)
6. TOTAL VOCs (ug/kg)
(I/HR)
c. REMOVAL EFFICIENCY
1. DICHLOROETHYLENE (I)
2. TRICHLOROETHYLENE (Z)
3. TETRACHLOROETHYLENE (Z)
4. IYLEHE (1)
5. OTHER VOCs (I)
6. MAJOR 4 CONTAMINANTS
7. TOTAL VDCs (I)
flHE («IN>
(SEC/REV)
rEHP 1C)
1C!
ISCFH)
•LAB lug/kg)
1ESP (ug/kg)
(I/HR)
HAS (ug/kg)
RESP (ug/kg)
(I/HR)
NE-LAB (ug/kg)
:ORRESP (ug/kg)
(I/HR)
)
)
)
g/kg)
g/kg)
I/HR)
g/kg)
g/kg)
I/HR)
(ug/kg)
(I/HR)
(ug/kg)
(I/HR)
NE (ug/kg)
(I/HR)
)
)
(I)
(I)
NE (Z)
NTS (I)
RUN 1
60.00
128.57
50.00
25.00
100.00
24.57
51.72
550.00
IDL
BDL
«210.00
BDL
BDL
•32,00
BDL
BDL
BDL
BDL
BDL
760.00
BDL
BDL
1552.00
BDL
BDL
BDL
BDL
BDL
BDL
BDL
BDL
BDL
BDL
BDL
BDL
BDL
BDL
-
-
-
-
-
-
-
RUN 2
60.00
128.57
50.00
90.00
100.00
24.57
60.79
63000.00
560699.29
1.111E-01
1600000.00
3306351.19
6.553E-OI
1500000.00
2907049. B4
5.761E-01
18000.00
23483.09
4.654E-03
•6200.00
10091.62
2.000E-03
3187200.00
6807675.03
1.349E+00
«670.00
1.217E-04
40000.00
7.266E-03
320000.00
5.813E-02
•3600.00
6.540E-04
BDL
BDL
364270.00
6.617E-02
99.89
98.89
89.91
85.95
100.00
95.09
95.10
RUN 3
45.00
96.43
50.00
25.00
100.00
24.57
49.72
t77.00
BDL
BDL
1400.00
24240.01
4.002E-03
3900.00
54553.76
9.006E-03
*66.00
36344.01
6.000E-03
120.00
BDL
BDL
5463.00
115137.78
1.901E-02
BDL
BDL
«13.00
1.761E-06
•46.00
6.231E-06
BDL
BDL
8DL
BDL
59.00
7.992E-06
.
99.96
99.93
100.00
-
99.96
99.96
RUN 4
45.00
96.43
100.00
90.00
100.00
24.57
113.72
«31.00
BDL
BDL
•41.00
51.12
1.588E-05
180.00
6468.28
2.009E-03
BDL
28.86
8.965E-06
BDL
56.89
1.767E-05
252.00
6605.14
2.052E-03
BDL
BDL
•62.00
1.SB8E-05
•37.00
9.477E-06
•35.00
8.965E-06
•69.00
1.767E-05
203.00
5.200E-05
.
-
99.53
-
-
98.31
97.47
RUN 5
60.00
128.57
100.00
90.00
100.00
24.57
97.52
330000.00
939856.95
2.080E-01
19000000.00
3475593.37
7.692E-01
950000.00
596447.68
1.320E-01
320000.00
298223.84
6.600E-02
•70000.00
144593.38
3.200E-02
20670000.00
W54715.22
1.207E+00
BDL
BDL
•6900.00
1.1B5E-03
BDL
BDL
BDL
BDL
BDL
BDL
6900.00
1.1BSE-03
100.00
19.85
100.00
100.00
100.00
99.90
99.90
RUN 6
45.00
96.43
100.00
25.00
100.00
24.57
89.32
210000.00
529398.11
2.026E-01
11000000.00
2907304.09
1.113E*00
•70000.00
50501.13
1.933E-02
380000.00
291577.20
1.116E-01
•88000.00
89691.54
3.433E-02
11748000.00
3868472.08
1.4BIE+00
•1900.00
6.254E-04
57000.00
1.876E-02
•1000.00
3.291E-04
•7900.00
2.600E-03
• 1000.00
3.291E-04
68800.00
2.264E-02
99.69
98.31
98.30
97.67
99.04
98.46
98.47
F-l
-------
PARAMETER
RUN 1
RUN 2
RUN 3
RUN 4
RUN 3
RUN 6
3.
4.
5.
6.
AIR
1.
2.
MOISTURE
i. EICAVATE9 SOIL (Zl
b. FEES SOIL ID
(t/HR)
1. ENTHALPY (BTU/D
c. PROCESSED SOIL
-------
PARAMETER
RUN 1
RUN 2
RIM 3
RUN 4
RUN 5
RUN 6
r
c. MANIFOLD 12
1. OICHLOROETHYLENE Ippi/voJ)
(I/HR)
2. TRICHLOROETHYLENE (pp»/vol)
(I/HR)
3. TETRACHLOROETHYLENE (ppi/vol)
(I/HR)
4. IVLENE (ppi/vol)
(I/HR)
5. OTHER VDCs (ppi/vol)
(I/HR)
6. TOTAL VOCs (ppi/vol)
(I/HR)
d. MANIFOLD 13
1. OICHLOROETHYLENE (ppi/vol)
(I/HR)
2. TRICHLORDETHYLENE (ppi/vol)
(I/HR)
3. TITRACHLOROETHYLENE (ppi/vol)
(I/HR)
4. XYLEXE (ppi/vol)
(I/HR)
5. OTHER VOCs (ppi/vol)
(I/HR)
6. TOTAi VOCs (ppi/vol)
(I/HR)
I. AFTERBURNER INLET
1. OICHLOROETHYLENE (ppi/vol)
(I/HR)
2. TRICHLOROETHYLENE (ppi/vol)
(I/HR)
3. TETRACHLOROETHYLENE (ppi/vol)
(I/HR)
4. XYLENE (ppi/vol)
(I/HR)
5. OTHER VOCs (ppi/vol)
(I/HR)
6. TOTAL VOCs (ppi/vol)
(I/HR)
f. STACK
1. DICHLOROETHYLENE (ppi/vol)
(I/HR)
2. TRICHLOROETHYLENE (ppi/vol)
(I/HR)
3. TETRACHLOROETHYLENE (ppi/vol)
(I/HR)
4. XYLENE (ppi/vol)
(I/HR)
5. OTHER VOCs (ppi/vol)
(I/HR)
6. TOTAL VOCs (ppi/vol)
(I/HR)
BDL
BDL
BDl
BDL
BDL
BDL
BDL
BDL
BDL
BDL
BDL
BDL
87.00
1.110E-01
375.00
6.4BOE-01
237.00
5.180E-01
3.00
4.000E-03
2.00
2.000E-03
704.00
1.283E+00
BDL
BDL
1.70
4.000E-03
3.00
9.000E-03
3.00
6.000E-03
BDL
BDL
7.70
1.900E-02
BDL
BDL
BDL
BDL
1.10
2.000E-03
BDL
BDL
BDL
BDL
1.10
2.000E-03
208.00
2.090E-OI
567.00
7.680E-01
76.70
1.320E-01
60.00
6.600E-02
24.70
3.200E-02
936.40
1.206E+00
196.00
2.020E-OI
785.00
1.094E+00
11.00
1.900E-02
97.00
1.090E-01
32. BO
3.400E-02
1121.80
1.458E+00
F-3
-------
PARAMETER
RUN 1
RUN 2
RUN 3
RUN 4
RUN 5
RUN 6
MOISTURE
l.
b.
PROCESS AIR (Z/vol)
(t/HR)
1. ENTHALPY (BTU/I)
INFILTRATION AIR (I/vol)
(I/HR)
1. ENTHALPY (BTU/I)
2.00
3.00
1097.90
2.00
2.24
1097.90
1.50
1.10
1122.80
1.50
2.56
1096.60
2.80
3.40
1098.80
2.80
2.99
1098.80
1.60
1.40
1134.20
1.60
2.08
1098.40
1.20
0.77
•1124.90
1.20
1.50
1095.40
2.10
1.60
1097.90
2.10
2.55
1097.90
C. MANIFOLD il (I/vol>
(I/HRI
d. MANIFOLD 12 (I/vol)
(t/HR)
c. MANIFOLD 13 (Z/vol)
(I/HR)
*. AFTERBURNER INLET (Z/vol)
(I/HR)
1. ENTHALPY (BTU/t)
9. STACK (I/vol)
(I/HR)
4. FLOWATE
i. PROCESSOR INLET (HACFM)
(OSCFH)
(t/HR)
b. INFILTRATION AIR (DSCFM).
(I/HR)
c. HAHIFOLl II INACFM)
(DSCFM)
(I/HR)
d. MANIFOLD 12 (HACFN)
(DSCFM)
(I/HR)
c. MANIFOLD 13 (HACFK)
(DSCFft>
(I/HR)
*. AFTERBURNER INLET (MCFH)
(DSCFM)
(I/HR)
9. STACK (UACFM)
(OSCFH)
(I/HR)
5. PARTICULAR EHISS-ABI/STACK (6R/HACFM)
(6R/DSCFM)
(I/HR)
6. HYDROGEN CHLORIDE EMISSIONS (I/DSCFM)
(I/HR)
7. CARBON DIOIIDE EMISSIONS (I/vol)
(I/HR)
B. OIY6EN EMISSIONS (Z/vol)
(I/HR)
9. CARBON MONOXIDE EMISSIONS (I/vol)
(I/HR)
8.18
22.70
1105.20
-
-
55.10
51.70
234.00
39.10
176.00
7.39
18.90
1102.60
-
-
29.10
24.70
112.00
59.90
270.00
14.00
36.00
1106.10
-
-
45.40
41.90
189.00
37.00
167.00
21.30
58.00
1122.00
-
-
38.30
30.90
140.00
45.50
205.00
21.40
50.70
1121.60
-
-
26.40
22.50
102.00
43.90
198.00
22.70
56.30
1126.10
30.90
63.70
27.70
25.90
117.00
42.40
191.00
113.00
90.80
410.00
104.00
84.60
382.00
106.00
78.90
356.00
119.00
76.40
345.00
104.00
66.40
300.00
110.00
68.30
308.00
283.00
50.80
234.00
F-4
-------
,...,
' I
PARAMETER
10. ENERGY - AIR/MOISTURE
i. PROCESS AIR INLET (BTU/HR)
1. SPECIFIC HEflT (BTU/IF)
2. HOISTURE (BTU/HR)
b. INFILTRATION AIR INLET (BTU/HR)
1. SPECIFIC HEAT (BTU/IF)
2. MOISTURE (BTU/HR)
c. AFTERBURNER INLET (BTU/HR)
1. SPECIFIC HEAT (BTU/IF)
2. MOISTURE (BTU/HR)
0. OIL SYSTEM PARAMETERS
1. TEMPERATURE
a. SCREH INLET 1C)
b. SCREH OUTLET/TROUGH INLET 1C)
' c. THOOBH OUTLET (C)
2. PRESSURE
a. SCREH INLET (PSI61
b. SCREM OUTLET/TROUGH INLET (PSIB)
, 3. FLOHRATE (6PH)
(I/HR)
4. HEAT RELEASED
*. INLET (BTU/HR)
1. SPECIFIC HEAT-INLET (BTU/IF)
fa. OUTLET (BTU/HR)
1. SPECIFIC HEAT-OUTLET (BTU/IF)
E. PROPANE SYSTEM PARAMETERS
1. PROPANE CONSUMPTION (SCFM)
(I/HR)
RUN 1
RUN 2
RUN 3
RUN 4
RUN 5
RUN 6
F. PROCESSOR PARAMETERS
1. SCREH SPEED (SEC/REV)
E. HEAT LOSS (BTU/HR)
1. PERCENT TOTAL HEAT (BTU/HR)
4625.66
2.399E-01
3293.70
) 3479.13
2.399E-01
2457.57
9879.36
2.400E-01
25086.04
129.05
123.20
121.11
28.00
B) 9.36
11.00
553B.16
687929.74
) 4.700E-01
641036.89
IF) 4.630E-01
3.78
0.43
125.63
24474.33
52.19
3816.35
2.403E-01
1235.08
5220.70
2.399E-01
2806.04
8544.58
2.400E-01
20839.14
103.30
97.74
96.59
32.00
11.00
11.70
5890.59
577707.83
4.500E-01
533565.40
4.400E-01
2.36
0.27
125.50
25484.58
57.73
3817.72
2.399E-01
3735.92
3373.33
2.399E-01
3285.30
8731.97
2.400E-01
39819.60
95.98
93.33
93.33
26.00
7.00
11.00
5538.16
498966.95
4.400E-01
487343.46
4.400E-01
4.17
0.48
95.20
-23322.13
-200.65
5748.88
2.407E-01
1587. B8
4140.91
2.399E-01
2279.61
11606.49
2.403E-01
65076.00
192.84
178.99
159.07
20.72
7.01
9.00
4531.22
901865.94
5.250E-01
713990.54
4.950E-01
2.66
0.30
97.70
118908.65
63.29
3609.46
2.404E-01
B66.17
3657.52
2.399E-01
1638.42
9962.84
2.403E-01
56865.12
174.09
162.93
144.81
26.96
7.75*
11.20
5638.85
983459.48
5.050E-01
800373.46
4.850E-01
1.86
0.21
125.00
123328.99
67.36
2312.63
2.399E-01
1756.64
3775.64
2.399E-01
2801.10
11165.71
2.404E-01
63399.43
270.32
97.30
203.75
22.68
6.95
9.80
4934.00
1509605.85
5.900E-01
1052576.39
5.350E-01
3.08
0.35
94.00
385469.11
84.34
F-5
-------
PARAMETER
CONTROL PARAMETERS
1. TARGET SOIL RESIDENCE TIME (HIN)
«. TARGET SCREH SPEEO (SEC/REV)
2. TARGET SOIL DISCHARGE TEMP (0
3. TARGET AIR INLET TEMP (C)
4. TARGET AIR FLN RATE (DSCFH)
SOIL SYSTEM PARAHETERS
1. TEMPERATURE
a. FEED SOIL (C)
b. PROCESSED SOIL (C)
2. VOCs
a. FEED SOIL
1. OICHLOROETHYLENE-LAI lug/kg)
CORRESP lug/kg)
(t/HR)
2. TRIQiOROETHYLEIE-LAI (ug/kg)
CORRESP (ug/kg)
(I/HR)
3. TETRACHLOROETHYLENE-LAB (ug/kg)
CORRESP (ug/kg)
(»/HR>
4. irLENE-LAB (ug/kg)
CORRESP (ug/kg)
(I/HR)
5. OTHER VDCt-LAB (ug/kg)
CORRESP (ug/kg)
(I/HR)
6. TOTAL VOCs-LAI (ug/kg)
CORRESP (uq/kq)
(I/HR)
ta. PROCESSED SOIL
1. 01CHLOROETHYLEME (ug/kg)
(I/HR)
2. TRICHLOROETHYLEME (ug/kg)
(I/HR)
3. TETRACHLOROETHYLENE (ug/kg)
(I/HR)
4. XYLENE (ug/kg)
(I/HR)
5. OTHER VOCs (ug/kg)
(I/HR)
6. TOTAL VOCs (ug/kg)
(4/HR)
c. REMOVAL EFFICIENCY
1. OICHLDROETHYLENE (I)
2. TRICHLOROETHYLENE (I)
3. TETRACHLQROETHYLENE (Z)
4. IYLENE (Z)
S. OTHER VOCs (Z)
6. MAJOR 4 CONTAMINANTS IZ)
7. TOTAL VOCs (Z)
RUN 7
30.00
64.29
50.00
90.00
100.00
26.26
56.68
« 300. 00
164.76
4.367E-OS
tWO. 00
30402.08
8.059E-03
1410.00
82.38
2.184E-03
IDL
7544.79
2.000E-03
BDL
BDL
BDL
1340.00
38194.01
1.012E-02
170.00
4.367E-05
230.00
5.909E-W
»85.00
2.1B4E-05
BDL
BDL
BDL
BDL
485.00
1.244E-04
-
99.27
-
100.00
-
98.77
98.77
RUN 8
30.00
64.29
50.00
25.00
100.00
28.33
53.16
220000.00
290840.89
7.278E-02
5900000.00
1955264.05
4.893E-01
930000.00
699130.61
1.750E-01
240000.00
85967.17
2.151E-02
tSOOOO.OO
12495.16
3.127E-03
7340000.00
3043697.89
7.617E-01
160000.00
3.878E-02
880000.00
2.133E-01
400000.00
9.696E-02
64000.00
1.551E-02
«12900.00
3.127E-03
1516900.00
3.677E-01
46.71
56.41
44.58
27.89
-
51.94
51.73
RUN 9
30.00
64.29
100.00
90.00
100.00
30.97
104.07
470000.00
889055.80
1.989E-01
930000.00
1997441.48
4.470E-01
«98000.00
346212.67
7.747E-02
• 20000. W
106904.95
2.392E-02
BDL
38923.73
8.710E-03
1518000.00
3378538.63
7.560E-01
15000.00
2.941E-03
61000.00
U196E-02
33000.00
6.471E-03
20000.00
3.922E-03
3620.00
7.098E-04
132620.00
2.601E-02
98.52
97.32
91.65
83.61
91.85
96.62
96.56
RUN 10
60.00
128.57
150.00
90.00
100.00
29.79
158.66
140000.00
586105.97
8.538E-02
1300000.00
2678536.44
3.902E-01
1500000.00
1422031.07
2.072E-01
120000.00
27197366.92
3.962E+00
§22000.00
39127.35
5.700E-03
3082000.00
31923167.75
4.6S1E+00
«730.00
8.2B4E-OS
1800.00
2.043E-04
1400.00
1.5B9E-04
4550.00
6.241E-05
BDL
BDL
4480.00
5.084E-04
99.90
99.95
99.92
100.00
100.00
99.99
99.99
RUN 11
45.00
96.43
150.00
90.00
100.00
30.94
137.34
73000.00
264041.00
6.632E-02
760000.00
2382812.77
6.165E-01
410000.00
727841.10
1.8B3E-01
*49000.00
65883.46
1.705E-02
*7100.00
20052.88
5.188E-03
1299100.00
3460631.21
8.954E-01
1300.00
3. 159E-04
2100.00
5.103E-04
1300.00
3.159E-04
190.00
4.617E-05
775.00
1.383E-04
5665.00
1.377E-03
99.54
99.92
99.83
99.73
96.37
99. H7
99.65
RUN 12
30.00
64.29
150.00
90.00
100.00
27.33
143.27
47000.00
472189.12
6.723E-02
220000.00
2390625.98
3.404E-01
230000.00
1257606.98
1.790E-01
50000.00
167493.06
2.3B5E-02
« 11 000. 00
65106.38
9.269E-03
558000.00
4353021.51
6.197E-01
2000.00
2.256E-04
12000.00
1.354E-03
27000.00
3.046E-03
7500.00
8.460E-04
§1500.00
1.692E-04
50000.00
5.640E-03
99.66
99.60
98.30
96.45
98.17
99.10
99.09
F-6
-------
PARAMETER
RUN 7
RUN
RUN 9
RUN 10
RUN 11
RUN 12
3. MOISTURE
a. EXCAVATED SOIL (II
b. FEED SOIL (I)
II/HR)
1. ENTHALPY IBTU/I)
c. PROCESSED SOIL (I)
(l/Hfi)
1. ENTHALPY (BTU/I)
""" 4. BASS FLWRAfE
1 a. FEED SOIL
1. NET BASIS (t/HR)
2. DRY BASIS (*/HR)
1 t. PROCESSED SOIL
1. NET BASIS (t/HR)
2. BRY BASIS (I/HR)
i 5. DENSITY
i . *. FEED SOIL (I/CU FT)
b. PROCESSED SOIL (t/CU FT)
fc. ENERGY - SOIL/HOISTURE
a. SOIL IN
1. INERT SOIL (BTU/HR)
2. MOISTURE (BTU/HR)
i b. SOIL OUT
l . 1. INERT SOIL (BTU/HR)
2. MOISTURE (BTU/HR)
«.. AIR SYSTEM PARAMETERS
', 1. TEMPERATURE
t. AMBIENT AIR (C)
b. HEATER EFFLUEKT/PROC IKLET (C)
1 , c. INFILTRATION AIR (C)
1 -' d. MANIFOLD 11 (C)
e. MANIFOLD 12 (C)
. 1 i. MANIFOLD 13 (C)
J . q. AFTERBURNER INLET (C)
h. STACK
2. VOCs
! a. AMBIENT AIR
' 1. TOTAL VOCs (ppi/vol)
(I/HR)
15.30
16.40
35.14
47.02
10.50
26.98
101.90
265. 08
229.93
256.91
229.93
62.58
78.32
3645.29
1652.23
6163.35
2748.80
27.00
97.00
27.00
48.00
47.00
49.00
42.00
968.00
IDL
BDL
21. 6Q
17.80
40.50
51.01
13.80
33.08
95.91
250.25
208.99
242.40
208.95
104.30
74.40
3468.98
2066.02
5336.05
3173.04
29.00
29.00
29.00
39.00
39.00
43.00
42.00
1009.00
IDL
BDL
30.90
26.40
38.27
56.00
5.80
11.35
187.12
223.77
184.74
196.09
184.72
76.78
62.89
3242.00
2143.30
8102.64
2123.29
•
33.00
98.00
33.00
102.00
113.00
131.00
102.00
923.00
BDL
BDL
MANIFOLD II
1. DICHLOROETHYLENE (ppi/vol.)
(I/HR)
2. TRICHLDRQETHYLENE (ppi/vol)
(I/HR)
3. TETRACHLOROETHYLENE (ppi/vol)
(I/HR)
4. IYLENE Ippi/vol)
(I/HR)
5. OTHER VOCs (ppi/vol)
(I/HRI
6. TOTAL VOCs (ppi/vol)
(I /HP. I
18.70
20.60
27.63
54.00
0.10
0.11
288.20
145.66
113.40
113.48
113.37
84.75
68.55
1941.88
1491.97
7200.77
32.56
33.00
89.00
33.00
80.00
91.00
109.00
91.00
979.00
BDL
BDL
18.30
17.30
15.57
56.00
0.30
0.73
248.04
258.73
242.27
243.00
242.27
91.27
~
4249.05
871.68
13528.99
180.48
26.00
98.00
26.00
93.00
114.00
122.00
101.00
897.00
BDL
IDL
13.30
18.70
31.21
49.02
2.00
2.25
259.31
142.37
110.54
m.'BC
110.54
95.61
69.37
1795.10
1529.73
6409.03
M3.54
27.00
95.00
27.00
112.00
126.00
136.00
118.00
876.00
BDL
BDL
F-7
-------
PARAHETER
RUN 7
RUN 8
RUN 9
RUN 10
RUN 11
RUN 12
c. MANIFOLD 12
1. OICHLOROETHYLENE (ppi/vol)
(t/HR)
2. TRICHLOROETHYLENE (ppi/vol)
(t/HR)
3. TETRACHLOROETHYLENE (ppi/vol)
(I/HR)
4. IYLEHE (ppi/vol>
(t/HR)
5. OTHER VOCs (ppi/vol)
It/HR)
6. TOTAL VOCs (ppi/vol)
(t/HR)
d. NANIFOLD 13
1. OICHLOROETHYLENE tppi/vol)
(t/HR)
2. TRICHLOROETHYLENE (ppi/vol)
(t/HR)
3. TETRACHLOROETHYLENE (ppi/vol)
(I/HR)
4. IYLENE (ppi/vol)
(t/HR)
5. OTHER VOCs (ppi/vol)
(t/HR)
6. TOTAL VOCs (ppi/vol)
(t/HR)
e. AFTERBURNER INLET
1. OICHLOROETHYLENE (ppi/vol)
(t/HR)
2. TRICHLOROETHYLENE (ppi/vol)
(t/HR)
3. TETRACHLOROETHYLENE (ppi/vol)
(t/HR)
4. IYLENE (ppi/vol)
(t/HR)
S. OTHER VOCs (ppi/vol)
(t/HR)
6. TOTAL VOCs (ppi/vol)
(t/HR)
*. STACK
1. OICHLORQETHYLENE (ppi/vol)
(t/HR)
2. TRICHLOROETHYLENE (ppi/vol)
(t/KR)
3. TETRACHLOROETHYLENE (ppi/volI
(t/HR)
4. IYLENE (ppi/vol)
(t/HR)
S. OTHER VOCs (ppi/vol)
(t/HR)
6. TOTAL VOCs (ppi/vol)
(t/HR)
BDL
BDL
4.40
8.000E-03
BOL
BOL
1.50
2.000E-03
BOL
BDL
3.90
l.OOOE-02
24.20
3.400E-02
145.00
2.760E-01
32.50
7.800E-02
3.60
6.000E-03
BOL
BDL
205.30
3.940E-01
173.00
1.960E-01
283.00
4.350E-01
36.60
7.100E-02
15.80
2.000E-0:
7.40
8.000E-03
515.80
7.300E-01
75.00
8.530E-02
254.00
3.900E-01
106.00
2.070E-01
3184.00
3.962E+00
4.70
5.700E-03
3623.70
4.650E+00
54.00
6.800E-02
362.00
6.160E-01
87.00
1.880E-01
12.00
1.700E-02
3.80
5.000E-03
518.80
8.940E-01
63.00
6.700E-02
238.00
3.390E-01
97.00
1.760E-01
20.00
2.300E-02
8.50
9.100E-03
426.50
6.141E-01
BDL
BDL
BDL
BDL
BDL
BDL
F-8
-------
PARAMETER
RUN 7
RUN
RUN 9
RUN 10
RUN 11
RUN 12
I
r •
r-
>. .t
\ •'
R (I/vol)
(t/HR)
Y (BTU/I)
ON AIR (Z/vol)
(I/HR)
Y (BTU/I)
2.00
2.50
1148.20
2.00
2.74
1096.60
2.20
2.60
1096.40
2.20
3.28
1098.40
3.00
2. BO
1148.90
3.00
3.77
1101.40
2.BO
2.90
1143.20
2. BO
3.18
1101.80
2.50
2.20
1148.90
2.50
3.76
1095.80
1.90
2.00
1147.00
1.90
1.74
1096.60
3. MOISTURE
«. PROCES
1. ENT
b. 1HFILT
1. ENT
c. HANIFOLD II (I/vol)
(I/HR)
d. MANIFOLD 12 (Z/vol)
(I/HR!
t. MANIFOLD 13 (Z/vol)
(I/HR)
4. AFTERBURNER INLET (Z/vol)
(I/HR)
1. ENTHALPY (BTU/I)
9. STACK (Z/vol)
(I/HR)
4. FLOWATE
«. PROCESSOR INLET (UACFH)
(DSCFR)
(t/HR)
t. INFILTRATION AIR (DSCFH)
(I/HR)
c. MANIFOLD II (HACFH)
(DSCFH)
(I/HR)
d. HANIFOLD 12 IHACFH)
(DSCFH)
(t/HR)
t. MANIFOLD 13 (HACFH)
(DSCFH)
(I/HR)
i, AFTERBURNER INLET (UACFH)
(DSCFH)
(I/HR)
9. STACK (HACFH)
(DSCFH)
(I/HR)
5. PARTICULATE EHISS-ABI/STACK (6R/KACFH)
(6R/DSCFH)
(I/HR)
6. HYDROGEN CHLORIDE EMISSIONS (I/DSCFH)
(I/HR)
7. CARBON DIOIIDE EMISSIONS (Z/vol)
(I/HR)
8. OXYGEN EMISSIONS (Z/vol)
(I/HR)
9. CARBON HQNOHDE EMISSIONS (Z/vol)
(I/HR)
4.94
13.40
1108.20
10.10
34.50
57.60
43.90
198.00
47.80
216.00
4.64
13.30
1108.20
13.70
50.85
44.20
41.10
186.00
52.00
234.00
13.70
33.50
1151.90
24.80
92.60
42.50
31.90
144.00
43.50
196.00
13.70
33.60
1144.40
17.60
60.75
46.90
36.00
163.00
39.40
177.00
11.30
20.80
1151.10
-
-
41.20
31.10
140.00
52.30
237.00
14.30
32.70
1161.90
-
-
49.20
37.80
171.00
32.10
145.00
114.00
91.70
414.00
541.00
113.00
522.00
-
-
-
-
-
-
-
-
-
-
-
113.00
93.10
420.00
602.00
116.00
524.00
B.OOOE-03
4.200E-02
4.100E-02
1.080E-04
7.520E-01
7.00
55.80
10.60
61.50
BDL
BDL
120.00
75.40
340.00
599.00
102.00
460.00
4.200E-03
2.400E-02
2.100E-02
2.940E-04
l.BOOE+00
7.40
51.90
9.40
48.00
BDL
•BDL
114.00
75.40
340.00
553.00
104.00
480.00
6.800E-03
3.600E-02
3.200E-02
2.4BOE-04
1.550E+00
7.70
54.90
9.00
46.70
IDL
BDL
129.00
83.40
377.00
513.00
103.00
475.00
-
-
-
-
-
-
-
-
-
-
-
116.00
69.90
316.00
392.00
77.60
357.00
-
-
-
-
-
-
-
-
-
-
-
F-9
-------
PARAMETER
RUN 7
RUN 8
RUN 9
RUN 10
RUN 11
RUN 12
10. ENERGY - AIR/WISTURE
4. PROCESS AIR INLET (BTU/Hft)
1. SPECIFIC HEAT (BTU/tf)
2. MOISTURE (BTU/HR)
b. INFILTRATION AIR INLET (BTU/HR)
1. SPECIFIC HEAT (BTU/tF)
2. MOISTURE (BTU/HR)
c. AFTERBURNER INLET (BTU/HR)
1. SPECIFIC HEAT (BTU/tF)
2. MOISTURE (BTU/HR)
OIL SYSTEM PARAMETERS
1. TEMPERATURE
t. SCREH INLET (C)
b. SCREH OUTLET/TROUGH INLET (C)
c. TROUGH OUTLET (C)
2. PRESSURE
a. SCREH INLET (PSI6)
b. SCREN OUTLET/TROUGH INLET (PSIG)
3. FLOHRATE (6PH)
(I/HR)
4. HEAT RELEASED
a. INLET (BTU/HR)
1. SPECIFIC HEAT-INLET (BTU/tF)
b. OUTLET (BTU/HR)
1. SPECIFIC HEAT-OUTLET (BTU/tF)
PROPANE SYSTEM PARAMETERS
1. PROPANE CONSUMPTION (SCFH)
(t/HR)
PROCESSOR PARAMETERS
1. SCREH SPEED (SEC/REV)
HEAT LOSS (BTU/HR)
1. PERCENT TOTAL HEAT (BTU/HR)
.
9866.72
2.412E-01
2870.50
4176.56
2.399E-01
3000.84
10691.14
2.400E-01
14849.88
85.40
82.16
82.16
23.17
7.08
10.00
5034.69
402068.33
4.300E-01
393970.94
4.350E-01
2.38
0.27
64.27
-1143.62
-14.12
.
3757.12
2.399E-01
2855.84
4726.70
2.399E-01
3604.22
10846.08
2.400E-01
14739.06
87.78
79.44
79.44
23.00
7.50
9.80
4934.00
407803.69
4.350E-01
368676.30
4.270E-01
2.64
0.30
63.65
25512.03
65.20
.
7238.32
2.412E-01
3216.92
4299.46
2.400E-01
4156.68
17688.26
2.413E-01
38588.65
252.08
242.09
239.79
24.85
7.13
10.50
5286.42
1476511.91
5.750E-01
1384758.85
5.650E-01
2.33
0.27
62.77
49546.90
54.00
.
7550.19
2.410E-01
3315.28
3882.67
2.400E-01
3507.95
16043.85
2.410E-01
38451.84
248.01
237.80
236.85
29.80
8.72
11.70
5890.59
1606353.64
5.700E-01
1511907.10
5.600E-01
2.13
0.24
126.77
54407.47
57.61
.
7037.25
2.412E-01
2527.58
4480.28
2.399E-01
4122.22
19449.41
2.413E-01
23942.88
f
262.08
251.32
242.99
21.63
6.88
9.60
4833.30
1424326.34
5.850E-01
1281795.17
5.650E-01
1.86
0.21
93.58
108717.46
76.28
.
8369.30
2.411E-01
2294.00
2803.71
2.399E-01
1912.50
18658.86
2.416E-01
37994.13
292.52
281.59
269.63
24.11
7.21
10.40
5236.08
1783968.90
6.100E-01
1598193.30
5.100E-01
2.14
0.24
62.00
140834.38
75.81
F-10
-------
n
PARAHETER
•••••
A. CONTROL PARAMETERS
1. TARBET SOIL RESIDENCE TIHE (KIN)
a. TAR6ET SCREV SPEED (SEC/REV)
2. TARBET SOIL DISCHARGE TEHP (C)
3. TARGET AIR INLET TEHP (C)
4. TARGET AIR FLOU RATE (DSCFH)
-£. SOIL SYSTEM PARAMETERS
1. TEMPERATURE
a. FEED SOIL (C)
b. PROCESSED SOIL (C)
2. VOCs
a. FEE) SOIL
1. D1CHLOROETHYLENE-LAB (ug/kg)
CORRESP (ug/kg)
(t/HR)
2. TRICHLOROETHYLENE-LAB (ug/kg)
CORRESP tug/kg)
(I/HR)
3. TCTRACHLOROETHrL£NE-LA6
-------
PARAMETER
RUN 13
RUN 14
RUN 15
RUN 16
RUN 17
RUN 18
3.
4.
5.
6.
AIR
1.
^
X.
NOISTURE
a. EICAVATED SOIL (I)
fa. FEE! SOIL (I)
ft/HR)
1. ENTHALPY (BTU/I)
c. PROCESSED SOIL (I)
(I/HR)
1. ENTHALPY (BTU/I)
MASS FLOHRATE
a. FEED SOIL
1. NET BASIS (t/HR)
2. DRY BASIS (I/HR)
ta. PROCESSED .SOIL
1. NET BASIS (I/HR)
2. BRY BASIS (i/HR)
DENSITY
a. FEED SOIL (t/CU FT)
b. PROCESSED SOIL (I/CU FT)
ENERGY - SOIL/HOISTURE
a. SOIL IN
1. INERT SOIL (BTU/HR)
2. NOISTURE IBTU/HR)
b. SOIL OUT
1. INERT SOIL (BTU/HR)
2. MOISTURE (BTU/HR)
SYSTEM PARAMETERS
TEMPERATURE
a. AMBIENT AIR (C)
b. HEATER EFFLUENT /FW INLET (C)
c. INFILTRATION AIR (Cl
d. MANIFOLD 11 (C)
c. MANIFOLD 12 (C)
4. MANIFOLD 13 (C)
q. AFTERBURNER INLET (C)
h. STACK
VOCs
a. AMBIENT AIR
1. TOTAL VOCs (ppi/vol)
(I/HR)
17.40
15.50
18.37
44.03
0.10
0.16
318.48
178.79
160.29
160.44
160.28
95.62
72.53
2437.15
808.83
11138.98
30.98
26.00
26.00
26.00
73.00
88.00
107.00
87.00
886.00
BDL
BDL
15.20
16.70
29.83
41.03
0.10
0.15
319.53
182.98
152.67
152.82
152.67
90.34
74.20
2234.56
1224.04
10613.24
48.73
25.00
25.00
25.00
63.00
84.00
122.00
84.00
886.00
BDL
BDL
16.60
20.60
34.00
43.03
1.00
1.47
254.18
181.34
146.41
147.89
146.41
109.38
72.06
2193.06
1463.11
8331.96
374.22
24.00
24.00
24.00
91.00
111.00
139.00
97.00
908.00
BDL
BDL
15.20
17.70
42.29
41.03
4.40
9.16
172.02
242.22
198.94
208.10
198.94
87.79
69.06
2893.28
1735.11
8102.89
1574.94
23.00
23.00
23.00
71.00
90.00
112.00
81.00
883.00
SDL
BDL
b. HANIFOU II
1. DICHOROETHYLENE (ppi/vol)
(I/HR)
2. TRICHLOROETHYLENE (pp«/vol)
(I/HR)
3. TETRACHLOROETHYLENE (ppt/vol)
(I/HR)
4. IYLENE (ppi/vol)
(t/HR)
5. OTHER VOCs (ppi/vol)
(I/HR)
6. TOTAL VOCs (ppi/vol)
(I/HR)
15.20
13.84
26.17
36.04
0.30
0.35
218.48
141.50
114.91
115.26
114.91
91.85
75.54
1571.11
943.02
5736.15
75.55
23.00
23.00
23.00
61.00
75.00
98.00
76.00
918.00
BDL
BDL
18.30
19.60
32.41
42.03
3.50
6.59
118.89
214.17
181.75
188.34
181.75
88.16
74.91
2683.11
1362.33
5502.46
783.69
27.00
99.00
27.00
57.00
62.00
72.00
62.00
919.00
BDL
BDL
F-12
-------
PARAHETEf?
RUN 13
RUN 14
RUN IS
RUN 16
RUN 17
RUN IB
n
c. MANIFOLD 42
1. OICHLOROETHYLENE (ppi/vol)
(I/HR)
2. TRICHLOROETHYLENE (ppi/vol)
(I/HR)
!. TETRACHLOROETHYLENE (ppi/vol)
(I/HR)
4. IYLENE (ppi/voi)
(I/HR)
5. OTHER VDCs (ppi/vol)
(I/HR)
6. TOTAL VOCs Ippi/vol)
(I/HR)
d. HANIFOU) 13
1. DICHLOROETHYLEME (ppi/vol)
(I/HR)
2. TRICHLOROETHYLENE (ppi/vol)
(I/HR)
3. TETRACHLOROETHYLENE (ppi/vol)
(I/HR)
4. irUME (ppi/vol)
(I/HR)
5. OTHER VOCs (ppi/vol)
(I/HR)
6. TOTAL VDCs (ppi/vol)
(I/HR)
e. AFTERBURNER INLET
1. OICHLOROETHYLENE (ppi/vol)
(I/HR)
2. TRICHLOROETHYLENE (ppi/vol)
(I/HR)
3. TETRACHLOROETHYLENE (ppi/vol)
(I/HR)
4. IYIEHE (ppi/vol)
(t/HR)
5. OTHER VOCs (ppi/vol)
(I/HR)
6. TOTAL VOCs (ppi/vol)
(I/HR)
f. STACK
1. DICHLOROETHYLENE (ppi/vol)
(I/HR)
2. TRICHLOROETHYLENE (ppi/vol)
(I/HR)
3. TETRACHLOROETHYLENE (ppi/vol)
(I/HR)
4. IYLENE (ppi/vol)
(I/HR)
S. OTHER VOCs (ppi/vol)
(I/HR)
6. TOTAL VOCs (ppi/vol)
(I/HR)
35.00
4.400E-02
37.00
4.200E-02
9.60
2. 100E-02
4.20
6.000E-03
1.60
2.000E-03
87.60
1.350E-01
52.00
7.500E-02
183.00
3.560E-01
9.20
2.300E-02
11.00
1.800E-02
2. BO
4.000E-03
258.00
4.760E-01
121.00
1.530E-01
281.00
4.800E-01
112.00
2.440E-01
24.00
3.300E-02
6.00
8.000E-03
544.00
9.180E-01
82.00
1.160E-01
270.00
5.150E-01
136.00
3.2BOE-01
11.00
1.800E-02
3.60
5.000E-03
502.60
9.820E-01
20.00
2.900E-02
90.00
1.790E-01
85.00
2.140E-01
1.10
2.000E-03
BDL
BDL
196.10
4.240E-01
1.70
2.000E-03
0.40
7.000E-04
1.00
2.000E-03
1.00
l.OOOE-03
1.20
2.000E-03
5.30
7.700E-03
F-13
-------
PARAMETER
RUN 13
RUN 14
RUN 15
RUN 16
RUN 17
RUN 18
3. MOISTURE
a. PROCESS AIR (Z/vol)
(f/HRt
1. ENTHALPY IBTU/I)
b. INFILTRATION AIR (Z/vol)
(t/HR)
1. ENTHALPY (BTU/t)
2.30
3.04
1096.20
2.30
2.49
1096.20
2.00
2.50
1095.40
2.00
2.92
1095.40
2.00
2.40
1094.90
2.00
2.37
1094.90
1.60
2.10
1093.60
1.60
2.17
1093.60
2.00
2.50
1094.10
2.00
3.08
1094.10
2.30
3.10
1149.70
2.30
2.98
1096.60
c. MANIFOLD II (I/vol)
(*/HR)
d. MANIFOLD 12 (Z/vol >
(I/HR)
e. MANIFOLD 13 (Z/vol)
(I/HR)
*. AFTERBURNER INLET (Z/vol)
(I/HR)
1. ENTHALPY (BTU/f)
g. STACK (Z/vol)
(I/HR)
4. FLQHRATE
a. PROCESSOR INLET (HACFH)
(DSCFH)
(I/HR)
b. INFILTRATION AIR (DSCFH)
c. HANIFOU II (HACFH)
(DSCFH)
(t/HR)
d. MANIFOLD 12 (HACFH)
(DSCFH)
(I/HR)
e. HANIFQLJ 13 (HACFH)
(DSCFH)
(t/HR)
1. AFTERBURNER INLET (HACFH)
(OSCFH)
(I/HR)
g. STACK (HACFH)
(OSCFH)
(I/HR)
5. PARTICULATE EHISS-ABI/STACK (6R/HACFH)
(6R/DSCFR)
(t/HR)
6. HYDR06EN CHLORIDE EMISSIONS (I/DSCFN)
(t/HR)
7. CARBON DIOHDE EMISSIONS (Z/vol)
(I/HR)
B. OXYGEN EHISSIONS (Z/vol)
(I/HR)
9. CARBON HONOIIDE EMISSIONS (Z/vol)
(I/HR)
9.28
23.70
1141.70
11.60
35.10
1139.70
13.70
37.30
1148.20
12.50
37.40
1137.40
10.30
31.40
1133.40
11.00
31.90
1123.60
48.10
45.00
203.00
37.70
170.00
47.00
44.30
200.00
51.00
230.00
44.90
42.40
192.00
41.40
186.00
47.90
45.90
207.00
47.50
215.00
46.00
43.70
197.00
53.80
243.00
62.20
46.90
212.00
45.10
203.00
120.00
82.70
373.00
507.00
106.00
486.00
141.00
95.30
430.00
510.00
103.00
472.00
131.00
83.80
378.00
472.00
90.90
418.00
138.00
93.40
422.00
484.00
96.70
445.00
139.00
97.50
440.00
561.00
113.00
518.00
127.00
92.00
415.00
629.00
125.00
574.00
F-14
-------
PARAMETER
RUN 13
RUN 14
RUN 15
RUN 16
RUN 17
RUN 18
1
f
1
'
'
T
f~*
fj
n
i •
10. ENERGY - AIR/MOISTURE
a. PROCESS AIR INLET (BTU/HR)
1. SPECIFIC HEAT D. OIL SYSTEM PARAMETERS
1. TEMPERATURE
a. SCREH INLET (C)
b. SCREH OUTLET/TROUGH INLET (C)
c. TROUGH OUTLET (C)
2. PRESSURE
a. SCREH INLET (PS 161
b. SCREH OUTLET/TROUGH INLET (PSI6)
3. FLOHRATE (6PH)
(i/HR)
4. HEAT RELEASED
a. INLET (BTU/HR)
i, SPECIFIC 'HEAT-INLET IBTU/IFJ
b. OUTLET (BTU/HR)
1. SPECIFIC HEAT-OUTLET (BTU/IF)
E. PROPANE SYSTEM PARAMETERS
1. PROPANE CONSUMPTION (SCFR)
(I/HR)
F. PROCESSOR PARAMETERS
1. SCREH SPEED (SEC/REV)
6. HEAT LOSS (BTU/HR)
' 1. PERCENT TOTAL HEAT (BTU/HR)
.
3837.54
2.399E-01
3288.60
3213.70
2.399E-01
2729.15
16946.79
2.409E-01
27058.29
235.45
226.84
226.84
19.59
7.50
8.40
4229.14
1079503.21
5.600E-01
1024177.60
5.500E-01
2.21
0.25
129.00
16445.56
29.73
.
3694.46
2.399E-01
2738.50
4248.63
2.399E-01
3198.23
18977.14
2.409E-01
40003.47
257.18
243.76
231.29
21.17
7.83
9.00
4531.22
1300713.53
5.800E-01
1137609.54
5.600E-01
2.21
0.25
96.00
110799.82
67.93
.
3462.33
2.398E-01
2627.76
3354.23
2.398E-01
2595.03
18836.47
2.412E-01
42B27.B6
301.29
286.05
265.74
18.08
7.76
7.50
3776.02
1333720.59
6.1SOE-01
1127308.95
5.850E-01
2.04
0.23
62.93
151736.55
73.51
.
3643.47
2.398E-01
2296.56
3784.28
2.39BE-01
2369.41
18067.61
2.408E-01
42538.76
219.06
210.86
206.14
32.63
7.96
12.90
6494.75
1508976.32
5.450E-01
1400461.26
5.350E-01
2.47
0.28
64.65
54932.98
50.63
.
3467.46
2.398E-01
2735.25
4277.12
2.398E-01
3369.82
17877.27
2.407E-01
35586.76
B
205.98
197.13
190.92
23.68
10.57'
8.90
4480.87
965532.22
5.350E-01
875298.16
5.200E-01
2.42
0.28
131.23
47320.10
52.44
.
10748.45
2.412E-01
3564.07
3925.20
2.399E-01
3266.04
14320.44
2.403E-01
35842.84
144.33
138.77
138.51
21.79
7.20
9.40
4732.61
662854.66
4.800E-01
432399.96
4.750E-01
2.76
0.32
99.33
-445.55
-1.46
F-15
-------
PARAMETER
CONTROL PARAMETERS
1. TAR6ET SOIL RESIDENCE TIME (HIM)
a. TARGET SCfiEV SPEED (SEC/REV)
2. TARGET SOIL DISCHARGE TEMP (C)
3. TARGET AIR INLET TEMP (C)
4. TARGET AIR RON RATE (DSCFM)
SOIL SYSTEM PARAMETERS
1. TEMPERATURE
a. FEED SOIL (C)
b. PROCESSED SOIL (C)
2. VOCs
a. FEED SOIL
1. OICHLOROETHrLENE-LAB lug/kg)
CQftRESP lug/kg)
(I/HR)
2. TRICHLOROETHYLENE-LAI (ug/kg)
CORRESP (ug/kg)
(i/HR)
3. TETRACHLOROETHYLENE-LAB (ug/kg 1
CORRESP (ug/kg)
(I/HR)
4. IYLEME-UIB (ug/kg)
CORRESP lug/kg)
(*/HR)
5. OTHER VOCt-LAB (ug/kg)
CORRESP (ug/kg)
(I/HR)
6. TOTAL VKs-LAB (ug/kg)
CORRESP (ug/kg)
(I/HR)
b. PROCESSED SOIL
1. DICHLOROETHYLENE (ug/kg)
(t/HR)
2. TRICHLOROETHYLENE (ug/kg)
(I/HR)
3. TETRACHLOROETHYLENE (ug/kg)
(I/HR)
4. XYLENE (ug/kg)
(I/HR)
5. OTHER VOCs (ug/kg)
(I/HR)
6. TOTAL VOCs (ug/kg)
(I/HR)
c. REMOVAL EFFICIENCY
1. DICHLOROETHYLENE (I)
2. TRICHLOROETHYLENE (I)
3. TETRACHLOROETHYLENE (Z)
4. IYLEHE (I)
5. OTHER VOCs (I)
6. MAJOR 4 CONTAMINANTS (Z)
7. TOTAL VOCs (Z)
RUN 19
60.00
128.57
210.00
90.00
100.00
25. a
223.89
*750.00
2793.49
6.472E-04
BOL
2560.31
5.928E-04
8DL
127.44
2.950E-05
3340.00
10869.69
2.517E-03
« 530. 00
7189.73
1.66SE-03
4580.00
23542.66
5.451E-03
240.00
4.721E-03
980.00
1.928E-04
150.00
2.950E-05
84.00
1.652E-05
1345.00
2.645E-04
2799.00
5.505E-04
92.71
67.48
-
99.34
84.11
92.45
89.90
RUN 20
90.00
192.86
210.00
90.00
100.00
25.93
218.07
•740.00
2591.13
4.000E-04
BOL
1301.54
2.009E-04
MOO. 00
BDL
BDL
13000.00
12976.19
2.003E-03
t2360.00
17939.50
2.769E-03
16500.00
34808.38
3.373E-03
BDL
BDL
7.00
9.212E-07
BDL
BDL
«24.00
3.158E-06
527.00
6.935E-05
558.00
7.343E-05
100.00
99.54
-
99.84
97.50
99.84
98.63
- RUN 21
75.00
160.71
210.00
90.00
100.00
25.19
232.67
»20.00
BDL
BDL
»70.00
9.47
1.850E-04
*30.00
BDL
BDL
160.00
11808.47
2.306E-03
H5.00
19682.16
3.843E-03
293.00
31500.10
6.150E-03
BDL
BDL
H2.00
1.850E-06
BDL
BDL
•36.00
5.549E-06
27B.OO
4.285E-05
326.00
5.025E-05
-
-
-
99.74
98.88
99.68
99.18
RUN 22
60.00
128.57
150.00
90.00
100.00
31.08
140.96
BDL
BOL
BDL
SDL
170.46
2.829E-05
SDL
22.16
3.677E-06
34000.00
40418.83
6.707E-03
5600.00
21719.74
3.604E-03
39600.00
62331.19
1.034E-02
BDL
BDL
200.00
2.829E-05
*26.00
3.677E-06
51.00
7.213E-06
737.00
1.042E-04
1014.00
1.434E-04
-
-
-
99.89
97.11
99.42
98.61
RUN 23
90.00
192.86
150.00
90.00
100.00
28.65
149.96
BDL
8.64
9.706E-07
BDL
138.28
1.553E-05
BDL
13.83
1.553E-06
1500.00
57999.59
6.514E-03
360.00
33292.60
3.739E-03
1880.00
91452.94
1.027E-02
HO.OO
9.706E-07
160.00
1.553E-03
Mb. 00
1.553E-06
140.00
1.359E-05
1431.00
1.3B9E-04
1757.00
1.705E-04
0.00
0.00
0.00
99.79
96.29
99.52
98.34
RUN 24
60.00
128.57
50.00
25.00
100.00
20.22
59.97
22000.00
22000.00
3.182E-03
180000.00
180000.00
2.603E-02
140000.00
140000.00
2.025E-02
18000.00
18000.00
2.603E-03
5520.00
5520.00
7.984E-04
365520.00
365520.00
5.287E-02
890.00
1.128E-04
5000.00
6.338E-04
1300.00
1.648E-04
130.00
1.648E-05
95.00
1.204E-03
7415.00
9.399E-04
96.45
97.57
99.19
99.37
98.49
98.22
98.22
F-16
-------
PARAMETER
RUN 1?
RUN 20
RUN 21
RUN.22
RUN 23
RUN 24
pic.
f]
n
3. MOISTURE
a. EXCAVATED SOIL (I)
b. FED SOIL (I)
(I/HR)
1. ENTHALPY (BTU/I)
c. PROCESSED SOIL (1)
(t/HR)
1. ENTHALPY (BTU/t)
4. MASS FLWRATE
a. FEED SOIL
1. NET BASIS (t/HR)
2. DRY BASIS
-------
PARAMETER
RUN 19
RUN 20
RUN 21
RUN 22
RUN 23
RUN 24
c. MANIFOLD 12
1. OICHLOflOETKYLENE (ppi/vol)
(I/HR)
2. TRICHLOROETHYLENE (ppi/vol)
(t/HR)
3. TETRACHLOROETHYLENE (ppi/vol)
(I/HR)
4. IYLENE (ppi/vol)
(I/HR)
5. OTHER VOCs (ppi/vol)
tl/HR)
6. TOTAL VOCs (ppi/vol)
(I/HR)
d. BANIFOLD 13
1. OICHLOftOETHriENE (ppi/vol)
(I/HR)
2. TRICHLOROETHYLENE (ppi/vol)
(I/HR)
3. TETRACHLOROETHYLENE (ppi/vol)
(I/HR)
4. XYLENE (ppi/vol)
(I/HR)
5. OTHER VOCs (ppi/vol)
(I/HR)
6. TOTAL VOCs Ippi/vol)
(I/HR)
e. AFTERBURNER INLET
1. OICHLOROETHYLENE (ppi/vol)
(I/HR)
2. TRICHLOROETHYLEME (ppi/vol)
(I/HR)
3. TETRACHLOROETHYLENE (ppi/vol)
(I/HR)
4. IYLENE (ppi/vol)
(I/HR)
5. OTHER VOCs (ppi/vol)
(I/KRI
6. TOTAL VOCs (ppi/vol)
(I/HR)
f. STACK
1. DICHLOROETHYLENE (ppi/vol)
(I/HR)
2. TRICHLOROETHYLENE (ppi/vol)
(I/HR)
3. TETRACHLQROETHYLENE (ppi/vol)
(I/HR)
4. ZYLENE (ppi/vol)
(t/HR)
S. OTHER VOCs (ppi/vol)
(I/HR)
6. TOTAL VOCs (ppi/vol)
(I/HR)
0.60
2.000E-04
0.30
2.000E-04
BDL
BDL
I.W
9.000E-04
0.80
3.000E-04
3.60
1.600E-03
0.50
2.000E-04
0.30
2.000E-04
BDL
BDL
2.20
l.OOOE-03
2.20
9.000E-04
S.20
2.300E-03
0.53
6.000E-04
0.20
4.000E-04
BDL
BDL
1.80
2.500E-03
1.20
1.400E-03
3.73
4.900E-03
-
-
-
-
-
-
-
-
-
-
-
-
0.50
2.000E-04
0.30
2.000E-04
BM.
BDL
1.80
9.000E-04
1.60
7.000E-04
4.20
2.000E-03
BDL
BOL
BDL
BDL
BDL
BDL
1.30
6.000E-04
4.00
1.800E-03
5.30
2.400E-03
0.30
4.000E-04
0.10
2.000E-04
BDL
BDL
1.40
2.000E-03
2.03
2.700E-03
3.B3
5.300E-03
-
-
-
-
-
-
-
-
-
-
-
-
BDL
BDL
BDL
BDL
BDL
BDL
1.50
8.000E-04
2.00
7.000E-04
3.50
1.500E-03
BDL
BDL
BDL
BDL
BDL
BDL
2.10
1.100E-03
5.50
-LJOOE-03
7.60
3.800E-03
BDL
BDL
BDL
BDL
BDL
BOL
1.47
2.300E-03
2.77
3.800E-03
4.23
6.100E-03
-
-
-
-
-
.
-
.
.
.
.
»
BDL
BDL
BDL
BDL
BDL
BDL
8.10
4.200E-03
5.30
2.500E-03
13.40
4.700E-03
BDL
BDL
BDL
BDL
BDL
BDL
2.40
1.200E-03
1.20
5.000E-04
3.60
1.700E-03
BDL
BDL
BDL
BDL
BDL
BDL
4.33
6.700E-03
2.53
3.500E-03
6.87
1.020E-02
-
.
-
-
-
.
-
.
.
.
.
.
BDL
BDL
BDL
BDL
BDL
BDL
6.00
2.600E-03
3.60
1.400E-03
9.60
4.000E-03
BDL
BDL
BDL
BDL
BDL
BDL
2.60
1.100E-03
1.20
5.000E-04
3.80
1.600E-03
BDL
BDL
BDL
BDL
BDL
BDL
5.03
6.500E-03
3.03
3.600E-03
8.07
1.010E-02
-
-
-
-
-
.
.
.
.
.
.
„
358105.00
5.193E-02
F-18
-------
PARAMETER
RUN 19
RUN 20
RUN 21
RUN 22
RUN 23
RUN 24
3. NOI5TURE
t. PROCESS AIR (Z/vol)
(t/HR)
1. ENTHALPY (BTU/f)
b. INFILTRATION AIR U/vol!
(t/HR)
1. ENTHALPY (BTU/t)
c. KANIFOLO II (I/voI)
(t/HR)
d. flANIFOLD 12 (Z/vol)
(I/HRI
e. MANIFOLD 13 (I/voI)
(t/HR)
f. AFTERBURNER INLET (I/voli
(t/HR)
1. ENTHALPY (BTU/t)
q. STACK (l/vol)
(t/HR)
4. FLOHRATE
i. PROCESSOR INLET (HACFH)
(OSCFN)
(t/HR)
b. INFILTRATION AIR (DSCFH)
(t/HR)
c. MANIFOLD tl (HACFH)
(DSCFH)
It/HR)
d. MANIFOLD 12 (NACFH)
(DSCFH)
(t/HR)
e. MANIFOLD 13 (HACFH)
(DSCFH)
(t/HR)
{. AFTERBURNER INLET (HACFH)
(DSCFH)
(t/HR)
g. STACK (HACFH)
(OSCFH)
(t/HR)
5. PARTICULATE EfllSS-ABI/STACK (6R/HACFR)
(6R/DSCFR)
(t/HR)
6. HYDROSEN CHLORIDE EMISSIONS (t/DSCFH)
(t/HR)
7. CARBON DIOIIDE EMISSIONS (2/val)
(t/HR)
8. OIY6EN EMISSIONS C/vol)
(t/HR)
9. CARBON MONOIIDE EMISSIONS (I/vol I
(I/HR)
1.90
2.00
1147.40
1.90
2. 48
1097.10
1.70
1.90
1147.60
1.70
2.33
1097.50
2.20
2.10
1149.30
2.20
4.00
1098.40
2.40
2.50
1147.80
2.40
4.10
1100.90
2.30
2.30
1149.30
2.30
2.87
1101.40
0.80
0.94
1091.00
0.80
1.23
1091.00
14.40
39.30
1158.05
10.00
27.00
1156.30
14.80
47.20
1161.55
10.40
31.10
1133.80
8.44
20.40
1135.00
6.90
20.00
1110.30
48.90
37.60
170.00
45.60
206.00
49.80
38.40
173.00
48.10
217.00
44.00
33.40
151.00
63.40
286.00
47.50
36.00
163.00
59.40
268.00
47.00
35.40
160.00
43.40
196.00
42.60
41.70
186.00
54.40
246.00
135.00
83.20
376.00
593.00
113.00
522.00
132.00
86.50
390.00
480.00
98.00
451.00
160.00
96.80
437.00
517.00
98.80
454.00
136.00
95.40
431.00
640.00
127.00
586.00
111.00
78.80
356.00
624.00
12B.OO
see. oo
120.00
96.10
434.00
681.00
142.00
649.00
F-19
-------
PARAMETER
RUN 19
RUN 20
RUN 21
RUN 22
RUN 23
RUN 24
10. ENERGY - AIR/ROISTURE
a. PROCESS AIR INLET (BTU/HR)
1. SPECIFIC HEAT (BTU/*f)
2. flOISTURE (BTU/HR)
t>. INFILTRATION AIR INLET (BTU/HR)
1. SPECIFIC HEAT (BTU/IF)
2. NOI5TURE (BTU/HR)
c. AFTERBURNER INLET (BTU/HR)
1. SPECIFIC HEAT (BTU/IF)
2. KGISTURE (BTU/HR)
OIL SVSTEfl PARAHETERS
1. TEMPERATURE
*. SCREH INLET 1C)
b. StREM OUTLET/TROUGH INLET (C)
c. TROUGH OUTLET (C)
2. PRESSURE
i. SCREH INLET (PSI6)
b. SCREN OUTLET/TROUGH INLET (PSI6)
3. FLOHRATE (6PH)
(i/HR)
4. HEAT RELEASED
a. INLET (BTU/HR)
1. SPECIFIC HEAT-INLET (BTU/IF)
b. OUTLET (BTU/HR)
1. SPECIFIC HEAT-OUTLET (BTU/IF)
5ROPANE SYSTEM PARAHETERS
1. PROPANE CONSUMPTION (SCFR)
(I/HR)
PROCESSOR PARAMETERS
1. SCREW SPEED (SEC/REV)
HEAT LOSS (BTU/HR)
1. PERCENT TOTAL HEAT (BTU/HR)
.
8394.14
2.411E-01
2294. BO
3983.20
2.399E-01
2718.06
21211. 81
2.41SE-01
45511.37
292.51
283.33
282.22
33.52
9.92
12.50
6293. 36
2144122.45
6.100E-01
2039033.54
6.000E-01
2.30
0.26
129.00
42860.14
40.78
.
8542.27
2.411E-01
2180.82
4289.60
2.399E-01
2560.99
21493.02
2.415E-01
31220.10
298.89
290.10
290.56
37.00
11.99
13.00
6545.10
2294392.86
6.150E-01
2197712.63
6.050E-01
1.93
0.22
189.63
53470.83
55.31
.
7587.03
2.4I1E-01
2413.53
5777.08
2.399E-01
4394.37
25613.51
2.416E-01
54825.16
299.36
293.79
295.17
36.83
12.00
12.80
6444.40
2262445.30
6.1SOE-01
2214403.20
6.100E-01
2.01
0.23
162.10
-22319.54
-46.46
*
8048.50
2.411E-01
2869.50
5760.67
2.399E-01
4510.85
17511.60
2.407E-01
35261.18
221.13
211.37
207.91
23.05
7.72
9.70
4883.65
1148774.14
5.470E-01
1061399.45
5.350E-01
2.57
0.29
127.00
51546.51
58.99
.
8039.24
2.411E-01
2643.39
4297.66
2.399E-01
3156.68
14772.82
2.407E-01
23154.00
221.72
213.39
210.25
23.00
10.00
8.80
4430.53
1044761.12
5.470E-OI
981995.96
5.400E-01
2.64
0.30
184.23
39392.26
62.76
•••••» • • •! • n • i
2984.45
2.398E-01
1025.54
3905.19
2.39BE-01
1342.66
11587.42
2.401E-01
22206.00
144.71
138.88
138.88
28.00
8.15
11.40
5739.55
809129.59
4.820E-01
773624.49
4.780E-01
2.64
0.30
124.79
9513.94
26.80
F-20
-------
i:
PARAMETER
V CONTROL PARAMETERS
1. TARGET SOIL RESIDENCE TIHE (HIM
». TARGET SCREM SPEED (SEC/REV)
2. TARGET SOIL DISCHARGE TEMP (0
3. TARGET AIR IKLET TEHP (C)
4. TARGET AIR FLDK RATE (DSCFH)
3. SOIL SYSTEM PARAMETERS
1. TEMPERATURE
t. FEED SOIL
b. PROCESSED SOIL (C)
2. VOCs
a. PIED SOIL
i. DICHLOROETHrLENE-LAB lug/kg)
CORRESP lug/kg)
(t/HR)
2. TRICHLORQETHYLENE-LAJ (ug/kg)
CORRESP (ug/kg)
(I/HR)
3. TETRACHLOROETHYLENE-LAB (ug/kg)
CDRRESP (ug/kg)
(f/HR)
4. ZYLEHE-LAB (ug/kg)
CORRESP (ug/kg)
(t/HR)
5. OTHER VOCs-LAB (ug/kg)
1 CORRESP (ug/kg)
(t/HR)
6. TOTAL VOCs-LAB (ug/kg)
CORRESP (ug/kg)
(t/HR)
b. PROCESSED SOIL
1. DICHLOROETHYLENE (ug/kg)
(t/HR)
2. TRICHLOROETHYLEME (ug/kg)
(t/HR)
3. TETRACHLOROETHYLENE (ug/kg)
(t/HR)
4. IYLENE (ug/kg)
(t/HR)
5. OTHER VOCs (ug/kg)
(t/HR)
6. TOTAL VOCs (ug/kg)
(t/HR)
c. REMOVAL EFFICIENCY
1. DICHLOROETHYLENE (I)
2. TRICHLOROETHYLENE (I)
3. TETRACHLOROETHYLENE (1)
4. ZYLENE 12)
5. OTHER VOCs (!)
6. MAJOR 4 CONTAMINANTS ID
7. TOTAL VOCs (I)
RUN 25
60.00
128.57
50.00
25.00
100.00
14.16
59.84
35000.00
35000.00
6.106E-03
1100000.00
1100000.00
1.919E-01
470000.00
470000.00
8.200E-02
37000.00
37000.00
6.455E-03
•8600.00
•8600.00
1.500E-03
1650600.00
1650600.00
2.BBOE-01
13000.00
2.0B9E-03
21000.00
3.374E-03
8600.00
1.3B2E-03
890.00
1.430E-04
451.00
7.246E-05
43941.00
7.060E-03
65.79
9B.24
98.31
97.78
95.17
97.56
97.55
RUN 26
60.00
128.57
30.00
25.00
100.00
17.67
62.84
«30000.00
•30000.00
4.653E-03
2300000.00
2300000.00
3.567E-01
890000.00
890000.00
1.380E-01
87000.00
87000.00
1.349E-02
•17000.00
•17000.00
2.637E-03
3324000.00
3324000.00
5.155E-01
3300.00
4.533E-04
52000.00
7.143E-03
48000.00
6.593E-03
5800.00
7.967E-04
2890.00
3.970E-04
111990.00
1.538E-02
90.26
98.00
95.22
94.10
84.94
97.08
97.02
RUN 27
60.00
128.57
HAZ
25.00
75.00
18.75
174.58
BDL
BDL
BDL
83000.00
83000.00
1.697E-02
120000.00
120000.00
2.454E-02
«23000.00
•23000.00
4.704E-03
BDL
BDL
BDL
226000.00
226000.00
4.622E-02
•390.00
7.079E-05
1900.00
3.449E-04
•270.00
4.901E-05
#27.00
4.901E-06
•172.00
3.122E-05
2759.00
' 5.008E-04
-
97.97
99.80
99.90
-
98. 98
98.92
RUN '28
90.00
192.86
flAZ
25.00
75.00
19.16
185.00
•6700.00
•6700.00
7.319E-04
430000.00
430000.00
4.697E-02
340000.00
340000.00
3.714E-02
49000.00
49000.00
5.353E-03
6200.00
6200.00
6.773E-04
831900.00
831900.00
9.0B8E-02
•90.00
8.257E-06
•130.00
1.193E-05
BDL
BDL
BDL
BDL
•700.00
6.42E-05
920.00
8.440E-05
98.87
99.97
100.00
100.00
90.5:
99.98
99.91
F-21
-------
PARAMETER
RUM 25
RUN 26
RUN 27
RUN 28
3. HOISTURE
a. EXCAVATED SOIL (Z)
b. FEED SOIL C)
(t/HR)
1. ENTHALPY (STU/t)
c. PROCESSED SOIL (I)
(I/HR)
1. ENTHALPY (BTU/«)
4. MASS FLONRATE
a. FEED SOIL
1. NET BASIS (I/HR)
2. DRY BASIS (I/HR)
fa. PROCESSED SOIL
1. NET BASIS (I/HR)
2. DRY BASIS (I/HR)
5. DENSITY
a. FEED SOIL (t/CU FT)
b. PROCESSED SOIL (I/OJ FT)
6. ENERGY - SOIL/MOISTURE
a. SOIL IN
1. INERT SOIL (BTU/HR)
2. NOISTURE (BTU/HR)
b. SOIL OUT
1. INERT SOIL (BTU/HR)
2. HOISTURE (BTU/HR)
AIR SYSTEM PARAKETERS
1. TEMPERATURE
a. AMBIENT AIR (C)
b. HEATER EFFLUENT/PROC INLET
c.
(C)
INFILTRATION AIR (C)
d. MANIFOLD II (C)
e. MANIFOLD 12 (C)
i. MANIFOLD 13 (C)
g. AFTERBURNER INLET (C)
h. STACK
2. VOCs
a. AMBIENT AIR
1. TOTAL VOCs (ppi/vol)
(I/HR)
b. MANIFOLD II
1. OICHLOROETHYLENE (ppi/vol)
(I/HR)
2. TRICHLOROETHYLENE (ppi/vol)
(I/HR)
3. TETRACHLOROETHYLENE (ppi/vol)
(I/HR)
4. IYLENE (ppi/vol)
(I/HR)
5. OTHER VOCs (ppi/vol)
(I/HR)
6. TOTAL VOCs (ppi/vol)
(I/HR)
174.46
153.43
160.66
153.43
86. 92
76.11
1764.08
519.73
4287.21
779.25
17.00
17.00
17.00
43.00
51.00
67.00
44.00
890.00
BOL
BDL
21.00
18.20
21.34
32.05
3.00
4.11
112.89
155.10
133.24
137.36
133.24
98.51
72.96
1700.29
684.08
3866.92
463.46
20.00
20.00
20.00
50.00
63.00
75.00
52.00
896.00
BDL
BDL
10.60
10.70
24.78
34.05
1.00
1.81
317.43
204.51
179.69
161.50
179.69
.
80.90
2362.86
843.64
12442.97
575.98
21.00
21.00
21.00
91.00
118.00
145.00
91.00
901.00
BDL
BDL
109.24
91.65
91.74
91.65
84.63
1218.70
613.48
6690.32
30.93
21.00
21.00
21.00
71.00
103.00
146.00
88.00
903.00
BDL
BDL
F-22
-------
PARAMETER RUN 25 RUN 26 RUN 27 RUN 28
c. MANIFOLD 12
1. 0ICHIOROETHYLEKE (ppi/vol) ....
(I/HR) ....
2. TRICHLOROETHYLENE (ppi/vol) ....
(l/Hfi) ....
3. TETRACHLQRQETHYLENE (ppi/vol) ....
(I/HR) ....
4. IYLENE (ppi/vol) ....
(I/HR) ....
5. OTHER VOCs (ppi/vol) ....
(I/HR) ....
6. TOTAL VOCs Ippi/vol) ....
(I/HR) ....
d. MANIFOLD 13
1. B1CHLOROETHYLEME (ppi/vol) ....
(I/HR) ....
2. TRICHLOROETHYLENE (ppi/volI ....
(I/HR) ....
3. TETRACHLOROETHYLENE (ppi/vol) ....
(l/Hfi) ....
4. XYLWE (ppi/vol) ....
(I/HR) ....
5. OTHER VOCs (ppi/vol) ....
(I/HR) - - -
t>. TOTAL VOCs (ppi/vol) ....
(I/HR) ....
t. AFTERBURNER INLET
1. B1CHLOROETHYLENE lpp»/vo]) ....
(I/HR) ....
2. TRICHLOROETHYLENE (ppi/vol) ....
(I/HR) ....
3. TETRACHLOROETHYLENE (ppi/vol) ....
(I/HR) ....
4. IYLENE
-------
PARAMETER
RUN 23
RUN 26
RUN 27
RUN 28
HOISTURf
t.
b.
PROCESS AIR (I/vol)
(I/HR)
1. ENTHALPY (BTU/t)
INFILTRATION AIR (I/vol)
(I/HR)
1. ENTHALPY (BTU/t)
1.00
1.20
1088.90
1.00
1.68
1088.90
1.00
1.20
1091.50
1.00
1.56
1091.50
1.00
0.93
1092.30
1.00
1.11
1092.30
1.20
1.00
1092.30
1.00
1.79
1092.30
c. HANIFOLO tl (l/vol)
(f/HR)
d. HANIFOLD 12 (I/vol)
(I/HR)
t. MANIFOLD 13 (I/vol)
(I/HR)
f. AFTERBURNER INLET (I/vol)
(t/HR)
1. ENTHALPY (BTU/i)
9. STACK (I/vol)
(I/HR)
4. FLOURATE
a. PROCESSOR INLET (UACFH)
(DSCFH)
(I/HR)
b. INFILTRATION AIR (DSCFN)
(I/HR)
c. flANIFOLO II (MACFH)
(DSCFH)
(I/HR)
d. HANIFOLO 12 (HACFK)
(DSCFN)
(I/HR)
e. MANIFOLD 13 INACFH)
(DSCFH)
(I/HR)
4. AFTERBURNER INLET (MACFH)
(DSCFH)
(t/HR)
q. STACK UACFH)
(OSCFH)
(t/HR)
5. PARTICULAR EHISS-ABI/STACK (6R/HACFH)
(SR/DSCFH)
(t/HR)
6. HYDROGEN CHLORIDE EHISSIONS (l/DSCFfll
(t/HR)
7. CARBON DIDIIDE EfllSSIONS (I/vol)
(I/HR)
8. OXY6EN EHISSIQNS (I/vol)
(I/HRI
9. CARBON nONOXIDE EHISSIONS (I/vol)
(t/HR)
5.40
16.40
1109.90
6.90
20.00
1116.20
11.00
25.00
1144.40
8.00
20.20
1142.40
43.90
43.60
197.00
59.40
267.00
43.00
42.30
191.00
55.10
249.00
33.70
33.00
149.00
39.10
176.00
31.50
30.50
138.00
52.50
237.00
125.00
103.00
464.00
621.00
118.00
540.00
124.00
97.40
440.00
720.00
158.00
723.00
107.00
72.10
325.00
494.00
111.00
511.00
119.00
83.00
375.00
559.00
121.00
555.00
F-24
-------
PARAMETER
RUN 25
RUN 26
RUN 27
RUN 28
§
'[I
10. ENERGY - AIR/MOISTURE
». PROCESS AIR INLET (BTU/HR)
1. SPECIFIC HEAT (BTU/tf)
2. MOISTURE (BTU/HR)
b. INFILTRATION AIR INLET (BTU/HR)
1. SPECIFIC HEAT (BTU/IF)
2. MOISTURE (BTU/HR)
c. AFTERBURNER INLET (BTU/HR)
1. SPECIFIC HEAT (BTU/IFI
2. MOISTURE (BTU/HR)
\ OIL SYSTEM PARAMETERS
1. TEMPERATURE
i. SCREH INLET (C)
b. SCREN OUTLET/TROUGH INLET (C)
c. TROU6H OUTLET (C)
2. PRESSURE
j. SCREH INLET (PSIB)
b. SCREH OUTLET/TROUGH INLET (PSIE)
3. aONRATE (6PM)
(I/HR)
4. HEAT RELEASED
i. INLET (BTU/HR)
1. SPECIFIC HEAT-INLET (BTU/IF)
b. OUTLET (BTU/HR)
1. SPECIFIC HEAT-OUTLET 1BTU/IF)
PROPANE SYSTEM PARAMETERS
1. PROPANE CONSUMPTION (SCFM)
(I/HR)
PROCESSOR PARAMETERS
1. SCREH SPEED (SEC/REV)
HEAT LOSS (BTU/HR)
1. PERCENT TOTAL HEftT (BTU/HR)
2957.26
2.398E-01
1306.68
4008.07
2.39BE-01
1832.75
12386.39
2.401E-01
18202.36
144.71
139.18
137.78
30.00
B.50
11.90
5991.28
844617.08
4.820E-01
796851.62
4.750E-01
2.78
0.32
124.23
24496.81
51.29
3114.52
2.398E-01
1309.80
4060.29
2.39BE-01
1704.13
13274.41
2.402E-01
22324.00
148.20
144.02
140.56
30.00
9.50
11.60
5840.24
846242.60
4.B50E-01
798967.26
4.800E-01
2.73
0.31
125.50
19919.67
42.14
2493.97
2.398E-01
1015.84
2945.90
2.39BE-01
1210.17
15336.04
2.410E-01
28610.00
294.03
277.36
260.69
20. B8
10.38
7.60
3826.36
1310011.51
6.100E-01
1112400.76
5.800E-01
2.13
0.24
125.65
151518.15
76.68
2309.85
2.398E-01
1092.30
3966.92
2.398E-01
1953.84
17207.40
2.410E-01
23076.48
289.13
275.24
264.41
18.22
10.33
6.20
3121.51
1043279.09
4.050E-01
927537.12
5.850E-01
2.51
0.29
183.43
79891.92
69.03
F-25
-------
APPENDIX G
MASS/ENERGY BALANCES
6060A
-------
o
I
Stream Number 12345C78*
Description
Inerts (Ib/hr)
VOC's - Oichloroelhylene (Ib/hr)
Trjchloroethylene (Ib/hr]
Tetrachloroethylene (Ib/hr]
Xylene (Ib/hr)
Olher VOC's (Ib/hr)
Moisture (Ib/hr)
Oil (Ib/hr)
Air (Ib/hr)
Water Vapor (Ib/hr)
F'.,.ticulate (Ib/hr)
Hydrochloric Acid (Ib/hr)
Carbon Dioxide (Ib/hr)
Oxygen (Ib/hr)
Carbon Monoxide (Ib/hr)
Propane (Ib/hr)
Total Mass (Ib/hr)
Average Temp ("F)
Specific Heat/HeaWng Value (Btu/lb)
Heat Rate (Btu/hr)
Soil
Feed
IM '%
HIM
PW
AIM,
HDL
*m.
J« *•
Itl l«
J*
19 VI
Ott
Inlet
«n it
/•«
itt jj
Process
Air
Inlet
]M ••
1 M
• 1
II <>
Infil-
tration
Air
11* «0
> 14
• I
M II
Oil
Outlet
«»• It
210
i M. n
Soil
Dis-
charge
in t)
•M.
•M.
•M.
HOC
•IX,
1) 1 1
II)
I* 0«
• 971,41
Off-
Gas
Dis-
charge
•M.
MM.
urn.
M»t
*f>L
• 10 «•
11. It
no
•* tl
!•*•! 4t
Stack
Exhaust
Heat
Loss
!••'• t)
For Thermal Stripping (X VOC't »om Soil Wot SHidf
Al iMWrkcnny Army Depot (LEAD) OwmlWf tbufg PA
IWtlTONHM
lots' cx jti« r
Jn«M utm Jojo
Till I BU
E&IIQF G-1 MATEWAL/EMERQY BALANCE
HGUBt« FOR TEST RUN 1
»"• None
11/as
??«! 01 tl
Notes BDL - Below Detection Level
-------
Stream Number
Description
Inerts (Ib/hr)
VOC'a - Dichloroettiylene flb/hr)
Trichloroetiylene (t>/hr)
TefracnloroelnyMne (Ib/hr)
Xylene (to/hr)
Olher VOC's (Ib/hr)
Moisture (Ib/hr)
Oil (Ib/hr)
Air (Ib/hr)
Water Vapor (Ib/hr)
Paniculate (Ib/hr)
Hydrochloric Acid (Ib/hr)
Carbon Dioxide (Ib/hr)
Oxygen (Ib/hr)
Carbon Monoxide (Ib/hr)
Propane (Ib/hr)
Tnlal Uau flh/hfl
Average Temp (°F)
Specific Heat/Heating Value (Blu/lb)
HAal Ral* fftht/hrt
1
Soil
Feed
!*• M
1 II • !•"'
*.«> • It*1
_l
1 •• • l« '
21 •»
It
1* 1*
2
Oil
Inlet
%•*• S*
111
»• •!
3
Process
Air
Inlet
m M
t i*
>•>
«• »*
4 "
Infil-
tration
Air
1)1 M
>-%«
• 1
tt 4»
s
Oil
Outlet
MM. It
JM
M M
«
Soil
Dis-
charge
itt t«
i.ii • i«'4
T ir • i«~'
~
t).i\
Ml
II It
7
Oil-
Gas
Dis-
charge
i. ->
« 41 • It*1
1 «••!•'
Ill M
II It
tl
~l tt
•
Slack
Exhaust
•
Heal
Loss
For Thermal Skipping ol VOC't from Sort PrtcM Study
Al Lcn.wh.wwiy Aimy O*K* (LEAD) Chwi*».ttur0. PA
FK2UREQ-2 MATERIAL/ENERGY BAUNCE
FOR TEST RUN 2
11/15
nsi-01-u
Notes DDL - Below Detection Level
-------
Stream Number
Description
Inerts (Ib/hr
VOC's - Dichloro«lhylen0 (Ib/hr)
Trlchlofoettiytene (Ib/hr;
Tetrachloroelhylene (Ib/hr;
Xylene (Ib/hr;
Other VOC's (Ib/hr)
Moisture (Ib/hr)
Oil (Ib/hr)
Air (Ib/hr)
Water Vapor (Ib/hr)
Participate (Ib/hr)
Hydrochloric Acid (Ib/hr)
Carbon Dioxide (Ib/hr)
Oxygen (Ib/hr)
Carbon Monoxide (Ib/hr)
Propane (Ib/hr)
Total Mass (Ib/hr)
Average Temp (°F)
Specific Heal/Heating Value (Btu/lb)
Heat Rate (Btu/hr)
1
Soil
Feed
ttt 99
m.
4 t* • in"
* tl • It"1
• M * It'1
MM.
4t IT
it* •<
u
ii «4
2
OH
Inlet
«n K
1*9
M It
3
Process
Air
Intel
11* ••
1 4t
t«
It If
4
Infil-
tration
Air
!•>.•>•
>.**
•4
It 11
s
CXI
Outlet
M« U
1*0
tt •«
6
Soil
Dis-
charge
114 *•
MM.
1 U • It*'
»OL
•DL
If .ft
111
11.1*
7
Off-
Gas
Dis-
Charge
•«,
4 *• • It*1
» M • |»'*
MM,
»• M
1* M
Itl
111 t»
•
Stack
Exhaust
•
tj^^a
neai
Loss
For T>Mrm« Stripping otVOClkom Sol PM Study
At itttii^iiin Army DWMM HEAD) Owi*«*urg. PA
FIGURE G-3 MATERIAL/ENERGY BALANCE
FOR TEST RUN 3
II/K
2W1 01
Notes BOL - Below Detection Level
IOTM-*
_
-------
O
I
Stream Number
Description
Inert* (to/hf)
VOC's • OicMoroethylene (Ib/hr)
TricMofoethylene (Ib/hr)
Tetrachloroethylene (Ib/hr)
Xylene (Ib/hr)
Otter VOC's (Ib/hr)
Moisture (Ib/hr)
Oil (Ib/hr)
Air (Ib/hr)
Water Vapor (Ib/hr)
Paniculate (Ib/hr)
Hydrochloric Acid (Ib/hr)
Carbon Dioxide (Ib/hr)
Oxygen (Ib/hr)
Carbon Monoxide (Ib/hr)
Propane (Ib/hr)
TViflal iJa«« fltl/hrl
Average Temp (°F)
specific Heai/neaong value (WU/IDJ
1
Soil
Feed
114 11
Mt
I.I* • I*"1
J.tl • !•"*
».«T • 1« *
1.?? • !•'*
M.I*
?«
2
Oil
Inlet
II*
3
Process
Air
Inlet
I 4»
in
4
Inlil-
tralion
Air
1 M
•4
s
Oil
Outlet
Itt
•
Soil
Dis-
charge
I»4 4J
ML
l.tt • It*1
l.»I • !«"*
I.»F > !«''
l.)l
?l>
7
OM-
Gas
Dis-
Charge
«•
ML
Mt,
twt.
U.M
14*
•
Stack
Exhaust
•
Heal
Loss
MO1OK
mtUHO»
fa ThwnHl SkipiMng ol VOC'i horn Sod (Mot Study
Al l4MWrli«nnr Army Ot^KM (LCAOI Cruunb4wK>u>«. PA
IMtlOMIUI
f CMHtf* FtM4Inv
-------
o
I
tn
Stream Number
Description
Inerts (Ib/hr)
VOC's - Dlchloroethylene (Ib/hr)
Trlchloroethylene (Ib/hr)
TetracMoroethylene (Ib/hr)
Xylene (Ib/hr)
Other VOC's (Ib/hr)
Moisture (Ib/hr)
Oil (Ib/hr)
Air (Ib/hr)
Water Vapor (Ib/hr)
Participate (Ib/hr)
Hydrochloric Acid (Ib/hr)
Carbon Dioxide (Ib/hr)
Oxygen (Ib/hr)
Carbon Monoxide (Ib/hr)
Propane (Ib/hr)
Total Mass (Ib/hr)
Average Terhp (°F)
Specific Heat/Heating Value (*u/B>)
Heal naw (Biu/nrj
1
Soil
Feed
141. ••
1 M • It'1
» «f • H"1
1 11 • !•*'
i M . 1. '
1 >• * !•"'
ft 11
III 11
r*
11 ••
2
Oil
Inlet
Mil M
MIt.M
HI
IT4.4I
3
Process
Air
Intel
1*1 M
».»»
Itl.M
l«f
41 1*
4
Infil-
tration
Air
in ••
l M
IM.M
r»
>• l)
5
Oil
Outlet
Mil. tS
Mil M
' Itl
l«l t4
«
Soil
Dis-
charge
!«• tt
«.
1 1* • I4*1
MN.
•m.
Ml
i •'
Ml t>
IM
«1 tl
7
O«-
Gas
Dis-
Cnarge
1 M • !•"'
1 •• • 1C'1
t 11 • ll'1
» «• • !•"'
1 11 . !•"'
It* ••
4«.lt
«l. 91
IM
IM.M
•
Stack
Exhaust
9
Heat
Loss
ItlMIt •!
For Th«rm«l Suppin
Al t^nxlunny A/my OwxHdEAO) Chwxtwlbufg PA
FIGURE G-5 MATERIAL/ENERGY BALANCE
FOR TEST RUN S
<•» Non« !'••"'
t/»5
1 01 II
Notes. BDL - Below Detection Level
-------
o
I
Stream Number
Description
Inert* (Ib/hr)
VOC't - DteMoroettytone (fc/hr)
TricMoroetiytone (fc/hr)
TetracMoroettiytone (fc/hr)
Xytene (fc/hr)
Ofier VOCs (fc/hr)
Moisture (Jb/hr)
Oil (fc/hr)
Ak (fc/hr)
Water Vapor (fc/hr)
Parkculate (fc/hr)
Hydrochloric Acid (fc/hr)
Carbon Dioxide (fc/hr)
Oxygen (fc/hr)
Carbon Monoxide (fc/hr)
Propane (fc/hr)
Total Mass (fc/hr)
Average Temp (°F)
Specific Heat/Heating Value (Btu/fc)
Heat Rate (Btu/hr)
1
Soil
Feed
M4 tl
1 II . It"'
I.It
1 *l • It''
1.11 . It '
1 41 • It'1
1i. l»
Itl M
It
» II
Hit 11
2
Oil
Inlet
«tM ••
4*14. M
»)•
»vt<
m*4» IS
a
Process
Air
Intel
III M
I.M
lll.tt
tl
4Mt.t1
4
Infil-
tration
Air
111 M
l.st
Itl.SS
tl
Hl« It
s
Oil
Outlet
4tM.M
4tl4.M
>tt
itum. it
6
Soil
Dis-
charge
W4.ll
I.M m It '
l.lt • lt~'
>.t« • It"1
14. It
lit. 14
Itl
IMtl.tl
7
Oil-
Gas
Dis-
charge
i tt
I.M • It"'
l.tt • It"1
Itt tt
U It
Itt. It
III
mtt.ii
•
Slack
Exhaust
i>»
•
Heat
Loss
Ulitt II
Fw TlwnMlSk*
1M»ONM»
|«fSt CHfltf M n
Mt >IS tl< MM
"IIIIIUU4I
FIGURE O-« MATERIAL/ENENGV BALANCE
FOR TEST RUN*
n/ss
I2SI-OI -II
Notes. BDL - Below Detection Level
-------
o
I
Stream Number
Description
Inerts (Ib/hr)
VOC's - Dlchloroelhylene (Ib/hr)
Trichtoroelhytene (Ib/hr]
Tetrachloroelhylene (Ib/hr]
Xylene (Ib/hr)
Other VOC's (Ib/hr)
Moisture (Ib/hr)
Oil (Ib/hr)
Air (Ib/hr)
Water Vapor (Ib/hr)
Particulate flb/hr)
Hydrochloric Acid (Ib/hr)
Carbon Dioxide (Ib/hr)
Oxygen (Ib/hr)
Carbon Monoxide (Ib/hr)
Propane (Ib/hr)
Total Mass (Ib/hr)
Average Temp (°F)
Specific Heal/Healing Value (Btu/lb)
Heat Rale (Btu/hr)
1
SON
Feed
m »i
« t» • t«~*
• •* • it* *
) It • It"*
J tt » !•' *
•M.
11 M
i*
i* *t
2
OM
Inlet
It 14 11
lit
T* •»
3
Process
Air
Inlet
IM M
I >•
1*T
tl.tl
4
Infil-
tration
Air
Ili.W
> '<
•1
11 II
5
Oil
Outlet
)t!4 M
IM
It *»
<
Soil
Dis-
charge
ii* *»
4 l» • It"'
1 It • lt'^
-
•OL
>t «•
114
M 4«
7
on-
Gas
Dis-
charge
•et
•M.
1MB !•' '
•M.
• 14 ••
11 4t
IM
It 14
•
Slack
Exhaust
IT '4
9
• J_-.a
rWal
Loss
For Th*n»ISMpp*ogolVOC«lromSoi(Pl»0(S»iio>
Al L«tt«r1i«nnv Army Depot HEAD) Chambefaburg PA
FIGURE 07 MATERIAL/ENERGY BALANCE
FOR TEST RUN 7
11/85
Notes BDL - Below Detection Level
tWMM. 16
??«l 01 M I
-------
/hr)
Moisture (t>/hr)
Oil (Ib/hr)
Air (Ib/hr)
Water Vapor (fc/hr)
Partin ilnlA flH /Hrl
Hydrochloric Acid (to/hr)
Carbon Dioxide (Ib/hr)
Oxygen (Ib/hr)
Carbon Monoxide (Ib/hr)
Propane (Ib/hr)
T/ital iJae* fMi/hrt
Average Temp (°F)
Specific Heat/Healing Value (Blu/lb)
MAJI| RalA JRtn/hrl
1
Soil
Feed
>•• t*
> a« • n"1
• •* * it'1
1 TS . ,.->
J It • Iff*
1. 1 1 • I0"'
«• *•
• 1
JJ 1'
2
Oil
Inlet
4tl« »*
!*•
«1 *i
3
Process
Air
Intel
Iffi.M
2 ft*
•«
IS •*
4
Infil-
tration
Air
>H M
1 Jt
M
11 II
5
Oil
Outlet
OM M
III
M 't
6
Soil
Dis-
charge
10. M
> •• > !• '
».!> • It*1
t !• • !•*'
1 II m !•'*
1) M
111
It It
1
Oil-
Gas
Dis-
charge
i •• • i*"1
1 » • !•"'
!.»• • It'1
•M.
4lt ••
II. M
IM
M t«
•
Slack
Exhaust
)14 ••
M.«i
1 « • !•"'
«t ••
• 1 SI
»UL
1141
•
Heat
Loss
Fo< Th«fmal Stripping ol VOC t fcom Sol PikM Study
Al Ltftwhwrny Aimy D*pcrt (LEAD) CrwitiMrsburg PA
• •MSI CHtSHH Pf*MSvtvAMA i
JPMONI lit **7 HMO
till* •> »••
FIGURE Q-t MATERIAL/ENERGY BALANCE
FOR TEST RUN I
It'SS
7?*l 01 II
Notes. BDL - Below Detection Level
-------
O
I
Stream Number 1234S67B9
Description
Inerts (Ib/hr)
VOC's - Dichtoroethytene (Ib/hr)
Trichloroelhylene (Ib/hr)
Tetrachloroethylene (Ib/hr)
Xylene (Ib/hr]
Other VOC s (Ib/hr)
Moisture (Ib/hr)
Oil (Ib/hr)
Air (Ib/hr)
Water Vapor (Ib/hr)
Paniculate (Ib/hr)
Hydrochloric Acid (Ib/hr)
Carbon Dioxide (Ib/hr)
Oxygen (Ib/hr)
Carbon Monoxide (Ib/hr)
Propane (Ib/hr)
Total Mass (Ib/hr)
Average Temp (T)
Specific Heal/Healing Value (Btu/fc)
Heal Rate (Btu/hr)
Soil
Feed
!•« »4
1 M • IB"1
1 O * It*'
. >» . 1. '
I »» • It'1
1 II * I**1
II J»
• •
)4 •>
Oil
Intel
»m •>
4«
»*. !•
Process
Air
Inlet
141 0*
J.tt
1M
Infil-
tration
Air
tt« M
I. tr
*l
Oil
Outlet
«•».«*
• •4
Soil
Dis-
charge
Ill.T)
1 t« • !•"'
1 t> • I*"1
ii n
n«
0«-
Gas
Dis-
Charge
i t« . i. '
i «• . i» '
M* •*
II M
lit
*
Stack
Exhaust
««• M
tl *•
!.••
11. »•
41. H
•M.
I«*I
Keai
Loss
4»^4» *«
Fat r>wrn«l Stripping alVOC'i»o
-------
o
I
Stream Number
Description
Inerts (Ib/hr)
.
VOC's - DichkxoettiylerM (Ib/hr)
TrichkMroelhylene (Ib/hr)
Telrachloroelhylene (Ib/hr)
Xylene (Ib/hr)
Other VOC's (Ib/hr)
Moisture (Ib/hr)
Oil (Ib/hr)
Air (Ib/hr)
Water Vapor (Ib/hr)
Paniculate (to/hr)
Hydrochloric Acid (Ib/hr)
Carbon Dioxide (to/hr)
Oxygen (Ib/hr)
Carbon Monoxide (Ib/hr)
Propane (Ib/hr)
loiai Mass (iD/nr)
Average Temp (°F)
« u_
Specific Heat / Heating Value (Btu / ID)
.
Heat Rale (Blu/hr)
1
Soil
Feed
III 4«
.a
. M . i.-'
, .. . ,. '
1 f*
, .. . i. '
1» 41
•4
2
Oil
Inlet
Ult »
• If
3
Process
Air
Inlet
Ul.M
J M
111
4
Inlil-
tration
Air
ID ••
i it
*i
5
Oil
Outlet
MVO.Sf
Mi
6
Soil
Dis-
charge
ni.i>
1 11 !•"*
I.M • !•*'
».J« • It"1
MM.
• .II
>!•
7
ON-
Gas
Dis-
charge
I.M . !•"'
I.M1
».>t . !•"'
M*.M
II «•
l«4
•
Slack
Exhaust
••• M
M >»
1 »
\t fl*
4k )•
.^
II»4
t
Heal
Loss
fa TlWfin*! Stripping olVOCikoM Sod PikM Study
Al LMMrkwwy Afmy O^xX (LEAD) CtumlMirtMiB. PA
|M»•» mo
FIGURE G-10 MATERIAL/ENERGY BALANCE
FOR TEST RUN 10
II/U
tttl-OMI
Notes BDL - Below Detection Level
-------
o
I
Stream Number 1234SI7lt
Description
Inerls (Ib/hr)
VOC's - Dichloroetiytone (Ib/hr)
Trichloroethylene (Ib/hr]
Tetrachloroelhylene (Ib/hr)
Xylene (Ib/hr)
CHher VOC's (Ib/hr)
Moisture (Ib/hr)
Oil (Ib/hr)
Air (Ib/hr)
Water Vapor (Ib/hr)
Participate flb/hr)
Hydrochloric Acid (Ib/hr)
Carbon Dioxide (Ib/hr)
Oxygen (Ib/hr)
Carbon Monoxide (Ib/hr)
Propane (Ib/hr)
Total Mas* (Ib/hr)
Average Temp (0F)
Specific Heat/Heating Value (Bhi/lb)
Heal Rate (Btu/hr)
Soil
Feed
141 )1
• •» m It"'
tun It'1
1 •• • !•''
1 M • It*'
* 1*. I.''
IVit
••
Oil
Inlet
• 111 M
»M
Process
Air
Inlet
14* ••
1 1*
M*
Infil-
tration
Air
1IT.M
> ?•
It
Oil
Outlet
*•»! M
<«•
Soil
Dis-
charge
in 11
4.11 « !•**
1 •• H !• *
> 71
Ml. ft
m
)• «3
Off-
Gas
Dis-
Charge
I.Tt m It*'
1 •• • It"1
ITT •«
It ••
l«t t*
114
IM.t«
Stack
Exhaust
M<>
Heat
Loss
IMItl «1
For n«rn«ISMp|i4ngolVOC'»lraiNS<)«PMSlupal (LEAD) CtwrtMrfeurg. PA
I of si ovum n w«n»«M« inn
FIGURE G-t 1 MATERIAL/ENERGY BALANCE
FOR TEST RUN 11
M««-OMI
Notes BOL - Below Detection Level
-------
Stream Number
Description
Inert* (Ib/hr)
VOC's - Dichioroethytone (to/hr)
Trichloroettiylene (Ib/hr)
TetracMoroetiylene (tt>/hr|
Xytene (to/hr)
Otter VOC's (Ib/hr)
Moisture (Ib/hr)
Oil (Ib/hr)
Air (Ib/hr)
Water Vapor (Ib/hr)
Paniculate (to/hr)
Hydrochloric Acid (Ib/hr)
Carbon Dioxide (Ib/hr)
Oxygen (Ib/hr)
Carbon Monoxide (Ib/hr)
Propane (Ib/hr)
Average Temp (°F)
Specific Heal/Heating Value (Btu/lb)
i
Soil
Feed
lit *4
ft. IJ • It"1
1 •• • It"*
i rt * i*'1
J. 1> • !•''
t l» • !•"'
11.11
• 1
21 n
2
Oil
Intel
in* ••
t%v
MB )l
3
Process
Air
Inlet
III M
1 M
!•!
41 44
4
Infil-
tration
Air
i«* ••
i M
•i
» 14
s
Oil
OuUel
Ml« M
111
Itt 11
•
Soil
Dis-
charge
III.94
1 >« • !•*'
4 J»
1M
«l f*
7
Off-
Gas
Dis-
charge
i.n » w"1
114 «t
11 '•
41.
144
Itl.ll
•
Stack
Exhaust
u»
1
Heat
Loss
Fo* That mri Slftp9*naolVOC'i Irom SoriPikM Study
PA
FIGURE Q-1J MATERIAL/ENERGY BALANCE
FOR TEST RUN 12
Non*
11 /IS
2711 01-11
Notes. BDL - Below Detection Level
-------
o
I
Stream Number
Description
Inerts (Ib/hr)
VOC'S - Dichloroelhylene (Ib/hr)
Trlchloroethylene (Ib/hr)
Tetrachloroelhylene (Ib/hr)
Xylenc (Ib/hr)
Other VOC's (Ib/hr)
Moisture (Ib/hr)
OH (Ib/hr)
Air (Ib/hr)
Water Vapor (Ib/hr)
Paniculate flb/hr)
Hydrochloric Acid (Ib/hr)
Carbon Dioxide (Ib/hr)
Oxygen (Ib/hr)
Carbon Monoxide (Ib/hr)
Propane (Ib/hr)
Tntal &£«•• flh/Krl
Average Temp (°F)
Heat Rale (Biu/nr)
1
Soil
Feed
!»• It
4 41 » It"7
1 11 « IB '
> I* • 1t"J
» tl « It" '
) If • It"'
tt. 17
U
2
Oil
Inlet
411*. 14
4W
3
Process
Air
Inlet
Itl. M
1 tt
It
4
InDI-
tration
Air
lit M
1.4*
»t
5
Oil
Outlet
4JJ» 14
I4f
J«> 1
6
Soil
Dis-
charge
itt.it
* II » !•"'
• a] « !•"'
I *
• l«
14T
'
7
Ofl-
Gas
Dis-
charge
• !• • 1»~'
4 •• • I**1
1 M • !•" '
IT! M
It »•
llf
•
Stack
Exhaust
it)*
•
Heat
Loss
For Tb«rm.«l SMppIng ol VOC't from SoH PMM SdMty
Al LM«rli«nny Army D«pOl (LEAD) Chambwsburg PA
FIGURE Q-13 MATEIMAL/ENEROV BALANCE
FOR TEST RUN 13
2?tl 01 II
Notes BDL - Below Detection Level
-------
Stream Number
Description
towns (Ib/hr)
VOC's - Dichkxoetiylene (to/hr)
Trichkxoetiylene (to/hr)
Tetrachtoroetiylene (Ib/hr)
Xytene (Ib/hr)
Ot>er VOC's (Ib/hr)
Moisture (Ib/br)
Oil (Ib/hr)
Air (Ib/hr)
Water Vapor (Ib/hr)
Paniculate (Ib/hr)
Hydrochloric Acid (Ib/hr)
Carbon Dioxide (Ib/hr)
Oxygen (Ib/hr)
Carbon Monoxide (Ib/hr)
Propane (Ib/hr)
TVifal A4tt«« /Ih/hrk
Average Temp (°F)
Specific Heal/Heating Value (Btu/lb)
Heat Rale (Blu/hr)
1
Soil
Feed
111 »»
T *l » I*''
1 1* • I**1
J.It • It"1
I.M a !•'*
• l» • J0'1
1* •)
)t
If »0
UM kO
2
Oil
Inlet
•111 JJ
4*»
III •*
1 )0«TI 1 M
3
Process
Air
Inlet
2M.M
J %•
ir
II tl
«• 12 t»
4
mill-
(ration
Air
no «•
a *;
IT
II II
ft 4* •*
S
Oil
Outlet
41I» »
441
Ml »*
IIITMt 54
6
Soil
Dis-
charge
Hi ii
1 II m !•'*
MM.
1 M m U"*
• IS
141
t».7>
l*»*l *T
7
OK
Gas
Dis-
charge
> M • !•"'
>. »• • !•'*
4.M • I**1
41* ••
IS.lt
Itl
12* «•
SttM 41
•
Slack
Exhaust
I«2T
9
Heal
Loss
llt>»* •!
For TlwiMl Skipping ol VOC't fcom Soil Prfol Smtfr
At L««trh«nnyArmyO«pot
-------
O
Stream Number
Description
Inerts (Ib/hr)
VOC's - Dlchloroetiylene (Ib/hr)
Trichlofoethyteoe (Ib/hr)
Tetrachtoroelhylene (Ib/hr)
Xytene (Ib/hr)
Other VOC's (Ib/hr)
Moisture (Ib/hr)
Oil (Ib/hr)
Air (Ib/hr)
Water Vapor (Ib/hr)
Paniculate flb/hr)
Hydrochloric Acid (Ib/hr)
Carbon Dioxide (Ib/hr)
Oxygen (Ib/hr)
Carbon Monoxide (Ib/hr)
Propane (Ib/hr)
loiai Mass (ro/nr)
Average Temp (°F)
SpecHIc Heat/Healing Value (Btu/fo)
Heat Rate (Btu/hr)
1
Sod
Feed
lit II
1 51 • I*"1
1 tl • I*"1
1 II • It'1
1 It • It"1
t If • It'1
II. tt
« tl
It It
lt*t IT
2
OH
Intel
ITU •!
ui
HI II
i mf?t M
3
Process
Air
Inlet
Itl.M
I.«
11
II 1)
tttt tt
4
Infil-
tration
Air
Itt.M
I 11
T»
II »•
Mlt It
5
OH
Outlet
DM t]
IK
l«. M
ii>7i«t t)
6
Sotl
Dis-
charge
11* «i
1 t« H It'*
• >* • It" '
f «T • It*4
1 *1 • It'4
1.4t
lt»
M.lf
tTt« It
7
Off-
Gas
Dis-
charge
4 tt • It'1
J.«4 • It"'
I It • It'1
t tt • It'1
ITt tt
11 It
ItT
HI. 11
•!•*«. 11
•
Stack
Exhaust
tttt
9
Heat
Loss
Hint 51
For TtMrrMlStrippingolVOCtlromSodWkHShirty
At t»««ek«ooy Army O^xM (LEAD) ClwnlwrAufg PA
FIGURE Q-15 MATERIAL/ENERGY BALANCE
FOR TEST RUN IS
11 IK
1 01 II
Notes BOL • Below Detection Level
-------
o
I
Stream Number
Description
Inert* . (K>/hr)
VOC't - Dichloroelhylene (Ib/hr)
TricMoroelhytene (Ib/hr)
TetoacMoroetiylene (Ib/hr)
Xytene (Ib/hr)
Other VOC's (Ib/hr)
Moisture (to/hr)
Oil (Ib/hr)
Air (Ib/hr)
Water Vapor (Ib/hr)
Paniculate (Ib/hr)
Hydrochloric Acid (Ib/hr)
Carbon Dioxide (Ib/hr)
Oxygen (Ib/hr)
Carbon Monoxide (Ib/hr)
Propane (Ib/hr)
Total MUM llh/hrt
Average Temp (°F)
Specific Heal/Heating Value (Btu/lb)
Heat Rate (Blu/hr)
1
Soil
Feed
l« M
1 1* • It"'
4 1* a !•*'
I It • It'1
1 •« • It*1
1 M • It'1
•i at
*»
If II
2
Oil
Inlet
**»«. *»
«U
J U M
3
Process
Air
Inlet
!•> •*
I.It
II
«.«!
4
Intil-
lra(ion
Air
115 ••
1,1V
Tl
J» »*
S
Oil
Outlet
1M4.IS
>>l
lit •)
6
Soil
Dis-
charge
Hi »«
m.
•w.
ML
I » > !•"'
ML
» !•
1*4
» II
7
0«-
Gas
Dis-
charge
I.U • It'1
f.lS • It'1
l.»t • It'1
l.tt • It*'
t.M • lt~*
• 21 M
lf.lt
lit
III. t«
••At* IT
•
Slack
Exhaust
UJI
•
Heat
Loss
S4«l) «l
for Thermal Stripping of VOCt Worn Sorf Pihx Sludv
Al L«tl«fk«nny Army 0«pol (IE*D» Ch»mb4Hi*>otg. PA
|
-------
o
I
Stream Number
Description
Inerts (Ib/hr)
vuo s - uicnioroemyiene (io/nr)
TrichkHoelhytene (Ib/hr)
Tetrachloroethytene (Ib/hr)
Xylene (Ib/hr)
Other VOC's (Ib/hr)
Moisture (Ib/hr)
Oil (Ib/hr)
Air (Ib/hr)
Water Vapor (Ib/hr)
Paniculate (Ib/hr)
Hydrochloric Acid (Ib/hr)
Carbon Dioxide (Ib/hr)
Oxygen (Ib/hr)
Carbon Monoxide (Ib/hr)
Propane (Ib/hr)
Tnlttl &£••• fttl/hrl
Average Temp (T)
Specific Heal/Healing Value (Btu/lb)
Heat Raw (wu/nr)
1
Soil
Feed
It* *l
-1
1 T» • It"'
i '
l.M » It"1
-
M. IT
«•
l» T»
2
Oil
Inlet
44lt • »
4«t
ll» «•
3
Process
Air
Inlet
l<> M
l.lt
I)
»l •*
4
Infil-
tration
Air
XI M
1 M
Tl
II •*
5
O»
Outlet
44lfl) IT
1T«
It5 14
«
Soil
Dis-
charge
114 *l
•n.
moL
I.I) • !«"*
•OL
• . n
15*
M 41
7
Ofl-
Gas
Dis-
charge
,j
1 T» • It/1
a 14 * !•*'
1 M » I*"1
•DR.
• 4*.tf>
11. 4t
!*•
111. II
•
Stack
Exhaust
!(••
9
Heat
Loss
For TtwnMl Shipping olVOCifcom So* foot 9iu*i
Al l«fl»rti»n-i» Amy DxxMflEADt »«n*wjbu
-------
I
-4
X)
Stream Number
Description
Inerts . (Ib/hr
VOC's - Dichkxoetiylene (Ib/hr
Trichloroetiytene (Ib/hr
Tetrachloroetiytene (Ib/hr)
Xylene (Ib/hr)
Of»er VOC's (Ib/hr)
Moisture (Ib/hr)
Oil (Ib/hr)
Air (Ib/hr)
Water Vapor (Ib/hr)
Paniculate (Ib/hr)
Hydrochloric Acid (Ib/hr)
Carbon Dioxide (Ib/hr)
Oxygen (Ib/hr)
Carbon Monoxide (Ib/hr)
Propane (Ib/hr)
Total Mass (Ib/hr)
Average Temp (°F|
Specific Heat/Healing Value (Blu/lb)
Hnal RA!A /Rtn/hrl
1
Soil
Feed
1*1. M
1 M • II"
1 14 • l« '
J •> « II"
I.M • II*'
J II • !•"
11.41
414 tl
14
II 14
2
Oil
Inlet
4IIJ 41
41 It 41
11)
III 04
3
Process
Air
Inlet
1IJ M
)-!•
m ii
in
11.14
4
Infil-
tration
Air
111 M
1 M
j«.n
il
14.41
s
Oil
Outlet
4'lJ.tl
«1I> tl
]•!
Ill *1
•
Soil
Dis-
charge
!•!.!%
T.tl * !•"
1 «t • I*"1
*.M • I*"1
9.M m lit'1
» %»
)•• 14
111
11 I*
7
Off-
Gas
Dis-
charge
1 M • I**1
a t» » i**1
I.M • I**1
1 M « !»"'
41) ••
11 *•
444 »l
144
lll.l«
•
Stack
Exhaust
14*4
t
Heat
Loss
Fot rowm* Sttippmg ol VOC'« fcom Sod PikK Skudy
At t«N*rlt«mnyArmyO«po<(L£AO| OwmbttstNUg PA
f SI CHtSUn PtMMSViVAMA )«1M
.1 >t)«U
M tl »*»
riGURE O-14 MATERIAL/ENERGY BALANCE
FOR TEST RUN II
2MI-OI-1I
Notes: BOL - Below Detection Level
-------
o
I
Stream Number
Description
Inerts (Ib/hr)
VOC's - Dichloroethytene (Ib/hr)
Trichloroettiylene (Ib/hr)
Telrachloroelhylene (Ib/hr)
Xylene (Ib/hr)
Other VOC's (Ib/hr)
Moisture (Ib/hr)
Oil (Ib/hr)
Air (Ib/hr)
Water Vapor (Ib/hr)
Particulate (Ib/hr)
Hydrochloric Acid (Ib/hr)
Carbon Dioxide (Ib/hr)
Oxygen (Ib/hr]
Carbon Monoxide (Ib/hr]
Propane (Ib/hr]
Total Mass (Ib/hr)
Average Temp (°F]
Specific Heat/Heating Value (Btu/lb)
Heal P>8te (Btu/hr)
1
Soil
Feed
ItS 1*
4-«t • It'*
t t» • It"*
1 « • It'^
1MB It' '
1 «r P It'1
14 4t
] 1! 41
It
It 41
2
Oil
Inlet
•ni »
•Itt U
»«
M» »•
3
Process
Air
Inlet
17* M
I M
m M
i»
•> 11
4
Infil-
tration
Air
It* ••
1.4t
Itt.4t
tl
11.14
s
OH
Outlet
»j»i it
•1*1. it
»4t
I*< tt
6
Soil
Dis-
charge
IM U
1.*) • It-'
I 9* m It"1
l.»5 « It "*
1 ^»
l««.*t
41%
It.tt
7
on-
Gas
Dis-
charge
4 tt • It**
•«,
1 \» m It'1
IT* *•
I* It
4M It
114
1*0 tt
*t>M It
1
Stack
Exhaust
itti
9
Heat
Loss
For Tlwrm*ISMp|»*n»olVOC'tfromSoNWWShidy
At l«n«cfc»ooy ArmyO»pOt|UAD) Chambvrsburg PA
I wisi CMtsitft *t wenvMtw i
FIGURE G-1« MATERIAL/ENERGY BALANCE
FOR TEST RUN 1*
Noftt
11/85
2781-01 II
Notes BDL - Below Detection Level
-------
i
KJ
O
Stream Number 123454711
Description
Inerts . (Ib/hr)
VOC's - Dichloroethylene (Ib/hr)
Trichloroelhylene (Ib/hr)
Telrachloroelhylene (Ib/hr)
Xylene (Ib/hr)
Ottier VOC's (Ib/hr)
Moisture (Ib/hr)
Oil 1 M
1 tt
|l«.*t
*«
kl.ll
10 111 0*
Infil-
tration
Air
a i i . ot
1. 11
no 11
•j
II 21
40*0 M
Oil
Outlet
«>«> Je
4MV I*
5)1
m.'«
mmi tl
Soil
Os
charge
111 41
ML
fr.21 « It*1
ML
1 It H It*'
4 *4 m It*5
• .II
111 4«
• IS
• 5 21
imi j*
OH-
Gas
Dis-
charge
4 M . 1. *
2.W « I*"*
•Ot
1 •• l It* '
I.JO • It**
1*4) 00
J» 00
411 41
lit
124 41
12M1 11
Slack
Exhaust
)«»•
Heat
Loss
tMIO II
For Tlwmd Stripping ol VOC'i hom Soil PikX Study
Al LMMrkcnny Army Depot (LEAD) Crtwnbwibura PA
• •MSIONiMr
|««$1 CHtSlIM rflMSVtVAM* ItMO
FIGURE G-20 MATERIAL/ENERGY BALANCE
FOR TEST RUN 20
*•» Non« \r*vu
2MI-OI II
Notes: BDL - Below Detection Level
-------
o
I
K)
Stream Number
Description
Inerts (Ib/hr)
VOC's - Dichloroethylene (Ib/hr)
Trichloroethylene (Ib/hr)
Tetrachloroethylene (tt>/hr)
Xytene (Ib/hr)
Other VOC's (Ib/hr)
Moisture (Ib/hr)
Oil (Ib/hr)
Air (Ib/hr)
Water Vapor (Ib/hr)
Participate (tb/hr)
Hydrochloric Acid (Ib/hr)
Carbon Dioxide (Ib/hr)
Oxygen (Ib/hr)
Carbon Monoxide (Ib/hr)
Propane (Ib/hr)
Average Temp (°F)
1
Soli
Feed
112 M
MIL
I 1. . ..-*
•W.
* H • It'*
i •! • IB" '
41 «*
Tf
2
Oil
Inlet
•444 «0
411
3
Process
Air
Inlet
Iff M
I. It
]••
4
Inlil-
Iration
Air
«4 M
« M
14
5
Oil
Outlet
««44 ««
S«l
6
Soil
Dis-
charge
in i»
MM,
I.I) « !•"*
KM.
1 It
4)1
7
OH-
Gas
Dis-
charge
•OL
•M.
•«.
<>'.»
«> 1*
4I4.II
I«l
8
Stack
Exhaust
i«t*
•
» i *
• rOtil
Loss
For nxxm
Al t«t»*ti«in» AtmyO«poiaEAO) Ch»n*enbuig PA
r>» nit« a u«
FIGURE G-21 MATf RIAL/ENERGY BALANCE
FOR TEST RUN 21
««• Non« *"»•<
1-01-
Notes SOL - Below Detection Level
-------
O
KJ
K)
Stream Number
Description
Inerts (Ib/hr)
VOC's - Dichloroettiylene (Ib/hr)
Trichloroelhylene (Ib/hr)
Tetrachloroethylene (Ib/hr)
Xylene (Ib/hr)
Other VOC's (Ib/hr)
Moisture (Ib/hr)
Oil (Ib/hr)
Air (Ib/hr)
Water Vapor (Ib/hr)
Paniculate (Ib/hr)
Hydrochloric Acid (Ib/hr)
Carbon Dioxide (Ib/hr)
Oxygen (Ib/hr)
Carbon Monoxide (Ib/hr)
Propane (Ib/hr)
Tnlal Ma«« flh/hrt
Average Temp (°F)
Specific Heal/Heating Value (Btu/lb)
Heat Rate (Blu/hr)
1
Soil
Feed
1*1 J*
•OL
1 It * !•'*
1 »• H It"*
t II . 1*'
1 »• • 1»"
14 »«
II
ai a*
<*** u
2
Oil
Inlet
4*11 tt
419
I1V 21
II4|1'4 14
3
Process
Air
Inlet
Ul M
J.»t
lit
t* tl
10*11 Ol
4
Infil-
tration
Air
1*1 M
4. 14}
ft
»» M
102 '1 \l
S
Oil
Outlet
4111. »4
«•«
111. 14
10*1 l*» 4)
. •
Soil
Dis-
charge
141. Jt
ML
J II • l« '
!.»• • !•"*
l.JI M !•"*
!.•< • !•'*
• I*
lift
11.14
• lit M
7
O«-
Gas
Dis-
charge
•M.
•M.
•M.
t. M • !•"'
I.M . ..-'
411. ••
ll.lt
lit
Il4.il
42 m ft
I
Slack
Exhaust
ii»
I
Heat
Loss
51)44 51
For Thwmai Skipping ol VOC't fcom Soil PikM Study
Al LMMrh«nny Army D4>pol (IEAO) Ch«m6«fibo.g PA
FIGURE Q-22 MATERIAL/ENERGY BALANCE
FOR TEST RUN 22
None
11/IS
am 01-11
10.*—4JN
Notes. BOL - Below Detection Level
-------
o
I
K)
Stream Number
Description
Inerts (Ib/hr)
VOC's - Dtchloroethylene (Ib/hr)
Trichloroethylene (Ib/hr)
Tetrachloroelhytone (Ib/hr)
Xylene (Ib/hr)
Other VOC's (Ib/hr)
Moisture (Ib/hr)
Oil (Ib/hr)
Air (Ib/hr)
Water Vapor (Ib/hr)
Particulate (Ib/hr)
Hydrochloric Acid (Ib/hr)
Carbon Dioxide (Ib/hr)
Oxygen (Ib/hr)
Carbon Monoxide (Ib/hr)
Propane (Ib/hr)
i otai Ma 99 fio/nr)
Average Temp ("F)
Specific Heat/Heating Value (Btu/lb)
Heat Rate (Btu/hr)
1
Soil
Feed
»4 II
» Tl • It"'
1 « • lt"%
1, « • It'4
• 31 V It"1
1 »« • It"'
It.tl
•«
11 7*
2
Oil
Inlet
44 It »»
411
m.ti
3
Process
Air
Inlet
IM.M
1 It
IN
tvti
4
Infil-
tration
Air
iti •*
> •»
• I
IT «•
S
Oil
Outlet
4IM.1I
«!•
191 *4
6
Soil
Dis-
charge
t4.lt
* Tl • It"1
1 M » It"'
1 « * It"*
1. It • It"'
t. Tt
HI
41 01
r
Off-
Gas
Dis-
charge
tot.
•04.
tOL
« M • It"1
nt.tt
11.41
I'l
Itt Tt
•
Stack
Exhaust
Kll
t
Heat
Loss
191*1 11
Foi TbtxiMl Stripping o!VOC'llromSa«Pllal Study
At Itmocktmo, Afmy O*>pol aCAO) Ch»n*.>.*>o.9 PA
FIGURE G 23 MATEIWAL/CNEIIQY BALANCE
FOR TEST RUN 23
°~ I1/8S
2MI-01-11
Notes BDL - Below Detection Level
-------
Stream Number
Description
Inerts (Ib/hr)
VOC's - Dichloroethylene (Ib/hr)
Trichloroelhylene (Ib/hr)
Telrachloroethylene (Ib/hr)
Xylene (Ib/hr)
Other VOC's (Ib/hr)
Moisture (Ib/hr)
Oil (Ib/hr)
Air (Ib/hr)
Water Vapor (Ib/hr)
Paniculate (Ib/hr)
Hydrochloric Acid (Ib/hr)
Carbon Dioxide (Ib/hr)
Oxygen (Ib/hr)
Carbon Monoxide (Ib/hr)
Propane (Ib/hr)
Tnlal Mace (IK/hrk
Average Temp (°F(
Specific Heat / Healing Value (Btu / Ib)
1
Soil
Feed
m •)
1 It • !•'*
J tt » It'2
».•> • li J
1 *• « !•* '
' *l > It'1
J* »1
hi
IT |*
2
Oil
Inlet
»M» Si
1V1
140 «f
3
Process
Air
Inlet
!•••••
• 14
«»
Jl 11
4
Infil-
tration
Air
)«4 M
l.ll
4ft
II 11
s
Oil
Outlet
till It
1»)
114 II
•
Soil
Dis-
charge
iii.ii
ft. 14 • !•'*
1 41 . II"*
4.14
141
II 14
7
OH
Gas
Dis-
charge
1.14 . II" '
J 11 k ll"1
414 II
1» 41
III
II 41
•
Slack
Exhaust
III!
•
Heal
Loss
Foi Thermal Stripping ol VOC'ft fcom Soil Pttol Study
At L«IMrli«nny Army O^KM (LCAO» Chamb«r9tHjfg PA
I CMf SUM l**#«$nvM*A 19WO
Jit *M MX
FIGURE O-24 MATERIAL/ENERGY BALANCE
FOR TEST RUN 24
Nona
II/S5
22*1-01-11
Notes BDL - Below Detection Level
-------
1
O
I
ro
Ln
Stream Number
Description
Inert s (Ib/hr)
VOC's - Dtchloroelhylene (Ib/hr)
Trichloroethylene (Ib/hr)
Tetrachloroelhylene (Ib/hr)
Xylene (Ib/hr)
Other VOC's (Ib/hr)
Moisture (Ib/hr)
Oil (Ib/hr)
Air (Ib/hr)
Water Vapor (Ib/hr)
Paniculate (Ib/hr)
Hydrochloric Acid (Ib/hr)
Carbon Dioxide (Ib/hr)
Oxygen (Ib/hr)
Carbon Monoxide (Ib/hr)
Propane (Ib/hr)
Total Mass (Ib/hr)
Average Temp (°F)
Specific Heat/Heating Value (Btu/lb)
Heal Rate (Btu/hr)
1
Soil
Feed
1)1 4 1
t.ll • It
1 «1 • It*'
• /• • It'1
• 4» . !•"
1 tt • It"
ltj.»4
IT4 *t
It
1 1 a*
2
Oil
Inlet
1MI 10
1*01 It
1*1
MO »>
3
Process
Air
Inlet
m.oo
!.]•
1*0.10
<)
II tl
4
Infil-
tration
Air
2*1 ft
1 «•
tit tl
• 1
11. 14
5
Oil
Outlet
«»i 10
1MI 11
!••
1 M.M
•
Soil
Dis-
charge
i«i «>
1 Of • 10* '
1 17 • 10* *
in . 10"'
1 «1 • 10"*
1 It • I0~*
1.11
100 00
MO
tl.SI
7
ow-
Gas
Dis-
charge
4 10 . 10 '
1 00 • 10"'
0 04 • 10"'
i.ll • 10*'
1 41 • IO'1
401.00
10.40
400.0*
III
01 04
•
Stack
Exhaust
1014
»
Heat
Loss
For Thojrrml Stripping ol VOC'i tram Son PiMSIuoV
At l«n*rli*nny Army Depot (LEAD) CrwmbOfjDurg PA
IWVSTONWAV
fi! .71 MII CMUIW «n«nv«x« I
l»oo>'m
nu>nuo>
FIGURE 0-25 MATERIAL/ENERGY BALANCE
FOR TEST RUN 25
N00«
Notes BDL - Below Detection Level
-------
Stream Number 1234567*9
Description
Inerls . (Ib/hr)
VOC's - Dtchloroelhyfene (Ib/hr)
Trichloroethylene (Ib/hr)
Telrachloroetiylene (Ib/hr)
Xylene (Ib/hr)
Other VOC's (Ib/hr)
Moisture (Ib/hr)
Oil (Ib/hr)
Air (Ib/hr)
Water Vapor (Ib/hr)
Paniculate (Ib/hr)
Hydrochloric Acid (Ib/hr)
Carbon Dioxide (Ib/hr)
Oxygen (Ib/hr)
Carbon Monoxide (Ib/hr)
Propane (Ib/hr)
Total Mass (Ib/hr)
Average Temp (°F)
Specific Heat / Heating Value (Bin / Ib)
Heal Rate (Btu/hr)
Soil
Feed
UI.14
4.»1 * I0~
1 11 Ji !•'
1 H • !•*
l.ll • !•"'
l.»4 • !•*
11.14
h4
1% II
Oil
Inlet
«4» J«
Jtt
144 10
Process
Air
Intel
1*1 M
1.2*
»•
JI 02
Infil-
tration
Air
>4» ••
1 »»
»•
) 1 4)1
Oil
Outlet
*I4*.J4
III
1 It ••
Soil
Dis-
charge
111.14
1.14 • It'1
4.11
11) It
141 II
ll.il
Off-
Gas
Dis-
charge
).» • !•"'
1 14 . ,.->
44*. e«
/« ••
4tfi W
11*
)I l«
Slack
Exhaust
U4*
Heat
Loss
l»*t* «4
fo> Thwmal Sbtpfxng ol VOC't fcom Soil PiKM Study
Al l«fl4Hk«ony Aimy Depot (LEAD) ClUMntwobutg. PA
|MSt CMfSltM Pt*wfi
E lit Ml MM
"HIM HUM
FIGURE O-tt MATERIAL/ENERGY BALANCE
FOR TEST RUN M
vx» Non* |>iMiO»«iia»
2211 01 II
II/U
Notes BDL - Below Detection Level
-------
J —1
O
I
to
Stream Number
Description
Inerts (Ib/hr
VOC's - Dichloroethylene (Ib/hr)
Trichloroethytene (Ib/hr;
Tetrachloroettiylene (Ib/hr]
Xylene (lb/hr|
Olher VOC's (Ib/hr)
Moisture (Ib/hrj
Oil (Ib/hr)
Air (Ib/hr)
Water Vapor (Ib/hr)
Paniculate (Ib/hr)
Hydrochloric Acid (Ib/hr)
Carbon Dioxide (fc/hr)
Oxygen (Ib/hr)
Carbon Monoxide (Ib/hr)
Propane (Ib/hr)
Tntnl Ma«« tlh/hrl
Average Temp (°F)
Specific Heat/Heating Value (Blu/fb)
HM| Ruin IRtn/hrl
1
Soil
Feed
u» ••*
MM.
1 »• • !•''
i 41 * l«~*
4 It « It"1
tfX.
I*. >*
it
1* ••
2
OH
Inlet
!•)• U
""
«l
141.14
3
Process
Air
Inlet
14* ••
• «l
»•
Jl 41
4
Infil-
tration
Air
l>« M
1 II
>•
>1 41
s
Oil
Outlet
It?* U
!•>
>»• 7]
6
Soil
Dis-
charge
i>« if
•n.
4 ft • It'^
km.
t *i
14i
11 11
7
Off-
Gas
Ois-
Charge
MK.
t 45 • I**1
•04.
115. ••
1^ M
m.«
!*•
FIGURE G-27 MATERIAL/ENEMY BALANCE
FOR TEST RUN 27
1I/8S
2?8I 01
Notes BDL - Below Detection Level
-------
i
NJ
00
Stream Number
Description
Inerts (Ib/hr)
VOC's - Dichlofoethyiene (Ib/hr)
Trichloroeftylene (Ib/hr)
Tetrachloroethylene (Ib/hr)
Xylene (Ib/hr)
Other VOC's (Ib/hr)
Moisture (Ib/hr)
Oil (Ib/hr)
Air (Ib/hr)
Water Vapor (Ib/hr)
Participate (Ib/hr)
Hydrochloric Acid (Ib/hr)
Carbon Dioxide (Ib/hr)
Oxygen (Ib/hr)
Carbon Monoxide (Ib/hr)
Propane (Ib/hr)
Total Mass (Ib/hr)
Average Temp (°F|
Specific Heat/Healing Value (Btu/lb)
t
Soil
Feed
ti »*
I. 11 • 14"*
«. 14 • !•*'
>.»! • !•"'
t.n • 14" '
4.M • !•'*
IT »t
l«t 1«
tr
It »
2
Oil
Inlet
1111 41
till 41
5)1
114 It
3
Process
Air
Inlet
111 ••
1 M
1 1* 04
It
It II
4
Infil-
tration
Air
jn t«
i it
ii« if
i«
?«.>*
S
Oil
Outlet
mi.ti
im.ti
»M
1»7 14
6
Soil
Dis-
charge
II 4S
I.It > li"*
m
•a.
• .Of
tl '4
lit
fl »*
7
Off-
Gas
Dis-
Oharge
4 It . !«"'
I.JI • 1C"1
V It • I*"1
l>> »
34.10
l»).lff
1*4
141.41
I
Slack
Exhaust
I4»l
•
Heat
Loss
fw Th»m»ISliippMiflo( VCX; tfcomSwl Pool Study
Al UnwfcMwy A>my Otpol (LEAD) ClumlM»bu
-------
APPENDIX H
SUPPLEMENTAL DATA
Table H-l Moisture content in the processed soil.
Table H-2 Mass flow rate of feed soil and processed soil.
Table H-3 Comparison of total VOC's as measured by the CEM
system and GC/MS analysis.
Table H-4 Summary of MM1 data from Test Run 2
(6 August 1985)
Table H-5 Summary of MM1 data from Test Run 4
6 August 1985) .
Table H-6 Summary of MM1 data from Test Run 5
9 August 1985) .
Table H-7 Moisture content in the air discharge stream.
Table H-8 Temperature of the air discharge stream.
6060A
-------
H. SUPPLEMENTAL DATA
H.I Moisture content of processed soils. The moisture
content in the processed soil varied with changes in the
operating conditions. The moisture content of the processed
soils is shown, in matrix format, for all operating conditions
in Table H-l.
H.2 Mass flow rate of soils. The mass flow rate of the
feed and processed soils were monitored regularly during the
,— pilot study. As expected, the mass flow rate of the processed
1 soils varied with changes in the operating conditions and
moisture content in the soil. The mass flow rates of the feed
and processed soil streams are summarized in Table H-2.
H.3 VOC concentrations in off-gas manifold as determined
by continuous emission monitoring (GEM) system and mobile mass
spectrometer. In addition to the laboratory GC/MS analyses,
( . two other modes of analysis were used to analyze the discharge
gas in the three legs of the manifold system: 1) a CEM system,
and 2} a mobile mass spectrometer. The CEM system utilized
( portable field instruments to measure the gross VOC
concentrations in the linear range from 1 to 600 ppm relative
to the calibration gas (benzene). An AID photoionization
detector was used during Test Runs 1 through 11. An OVA was
', used during Test Runs 12 through 23, and test runs 25 through
28. A summary of the gross VOC concentrations as measured by
the CEM system is shown for each manifold leg in Table H-3. For
r- comparison, the total VOC concentrations as detected by GC/MS
techniques are also given. As shown, the average deviation
(i.e., 100% x [1 - (GC/MS)/CEM]) corresponding to the AID
detector was SB.93 percent. The average deviation corresponding
f to the OVA was 54.00 percent. The large variance between the
..; VOC's measured by the CEM system and GC/MS analyses indicates
that the portable monitors are not adequate to accurately
f - quantify VOC's in the air stream. The portable instruments are
' far less sophisticated analytically and extreme precision is
not expected. However, analysis of Table H-3 indicates that the
instrument readings are generally in the same order of
i magnitude as the GC/MS results. The portable monitors,
therefore, can be used to obtain real-time estimates of VOC
emissions in the air discharging the thermal processor.
' A Bruker MM1 mobile mass spectrometer was also utilized
during Test Runs 2, 4, and 5 conducted on 6 August 1985, 8
August 1985, and 9 August 1985, respectively. The MM1 was used
to qualitatively identify VOC's in the discharge air stream.
The data generated by the MM1 during Test Runs 2, 4, and 5 are
shown in Tables H-4 through H-6. The MM1 identified only those
H-l
6060A
-------
I. AMMwrt Air Mri T
i
K>
60
90
390
450
300
100
OtO
TABLE H-1 MOISTURE CONTENT IN THE PROCESSED SOIL
(PERCENT BY WEIGHT)
-------
I. Ambtonl Air InM T*mpt»*tur*
75
90
Fwd
PtOCMMd
ProcnMd
ProcmMd
ProcctMd
PlOCMMd
FMd
PfOCMMd
14463
1M7S
1744*
16086
15510
13736
?04St
taiso
10924
91 74
Not •vlluilsd
TABLE H-2 MASS FLOW RATE OF FEED SOIL AND PROCESSED SOIL
(WET BASIS - LB/HR)
-------
TABLE H-3.
COMPARISON OF TOTAL VOC' S AS MEASURED BY THE CEM
SYSTEM AND GC/MS ANALYSES (PPM BY VOLUME)
CEM system
Test
run
Mani-
fold
1
Mani-
fold
2
Mani-
fold
3
GC/MS
Analyses
Afterburner
inlet
Deviation
Between CEM
System and
GC/MS Analyses
(percent)
I. Phase I Test Runs
AID
1
2
3
4
5
6
7
8
9
10
11 '
5
768
6
3
831
768
3
368
365
1,240
437
5
812
8
3
809
695
2
484
390
1,320
426
5
778
24
3
800
592
2
707
325
1,200
381
<1
704
7.7
1.1
936
1,122
519 (7,
206
515
3,620
519
Average
80.00
10.43
39.21
63.33
15.08
63.80
314.29)*
60.36
43.06
188.83
25.16
58.93
'B. OVA
12
13
14
15
16
17
IS
(Average
331
117
167
550
399
142
17
OVA Devi
494
133
202
607
537
157
17
ation -
477
122
130
533
576
115
17
Phase
426
88
258
544
503
196
5.3
I Test Runs:
1.84
29.03
55. 11
3.43
0.20
42 .03
68.82
28.64)
•Excluded as outlier
H-4
6060A
-------
TABLE H-3. (Continued)
GC/MS
Analyses
Test
run
Mani-
fold
1
Mani-
fold
2
Mani-
fold
3
CEM system
Afterburner
inlet
Deviation
Between CEM
System and
GC/MS Analyses
(percent)
I. Phase II Test Runs
A. OVA
19
20
21
22
23
2.4
2.0
1.6
3.6
10.8
3.6
4.2
3.5
3.4
9.6
5.2
5.3
7.6
3.6
3.8
70
54
100
44
39
94.67
92.90
96.77
84.39
79.32
(Average OVA Deviation -
Phase II Test Runs: 89.41)
Average 54.00 percent
r
H-5
6060A
-------
TABLE H-4. SUMMARY OF MM1 DATA FROM TEST RUN 2 (6 AUGUST 1985)
Tarqet Compounds
Number 1,2-Di- 1,1,1-
of deter- chloro- Trichloro-
Manifold minations ethene ethane
Baseline1
1
2
3
1
2
3
1
2
3
Baseline1
1
3
1
2
3
1
2
3
1
2
3
Baseline1
6
3
5
4
6
3
3
2
4
3
3
2
6
2
3
3
4
5
3
3
2
3
4
4
4
4
4
4
4
5
4
3
4
5
4
4
4
5
4
4
4
4
4
3
.0-3
.3-5
.7-5
.3-4
.6-4
.1-4
.3-4
.3-4
.1
.8-4
.3-4
.5-4
.1
.4-5
.7-5
.9-5
.0-5
.7-4
.7-4
.6-4
.9
.5-4
.9-4
.9
.0
.0
.9
.8
.9
.5
.7
.9
.0
.8
.4
.0
.3
.2
.9
.9
.9
.8
.8
2.9-3.7
4.1-5.0
4.8-5.0
4.8-5.0
4.4-4.9
4.1-4.8
4.2-4.4
4.3-4.9
4.9
4.7-4.8
2.5-3.9
4.5-4.8
4.9-5.0
4.4-5.0
4.5-4.8
4.9-5.3
5.1
5.0-5.1
4.8-4.9
4.4-4.9
4.9-5.0
4.8-4.9
3.9-4.0
(arbitary log units)
Aliphatic
hydro-
carbons
3
4
4
5
4
4
4
5
4
4
5
4
4
4
4
5
4
4
.6-4.5
.4-5.2
.9-5.3
.9-5.3
.8-5.1
.4-5.0
.7-4.8
.4-5.0
.0-5.1
.8-5.1
.7-4.8
.0-4.8
.2-5.3
.6-5.1
.2-4.4
.0-5.1
.9-5.0
.8-5.1
.9
.7-5.0
.0
.6-5.0
.8
Chloro-
form
3.9-4.9
4.5-4.9
4.0-4.9
3.7-4.6
3.8-4.6
4.1-4.4
4.0-4.6
4.7
4.3-4.7
3.9-4.4
4.8-4.9
3.7-4.5
4.2-4.4
4.7-4.8
4.6-4.8
4.7-4.8
4.5-4.6
4.3-4.6
4.6-4.7
4.4-4.6
3.9
Oichloro-
me thane
2
3
3
3
3
3
3
3
3
3
2
4
3
3
3
4
4
4
.6-3.
.6-4.
.9-4.
.8-4.
.2-4.
.0-4.
.8-4.
.3-3.
.9-4.
.3-3.
.9-3..
.5
.5
.2-3.
— — —
.9
.0
.0
.4
2
5
6
7
0
0
0
9
0
5
9
3
'Reading taken in area where process was operating - represents
background in that area.
6060A
H-6
-------
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vv v — ^ to^co co f*»r*tO mvto v^to cr ^CMin ^cntn mcoso CMO%O
CM CM CMPOPO pococo CM po m PO po co m po m po CM mmm m m PO rococo m m PO
C9 tfi ^t rfi v ^r ^3 CM ^9 co ^r f*o in v ^r co j"i ^ CM ^r co ^o m ^c* uo en m co ^^ ^o po
0* «l
c c
CM CO ^"CMPO ^CMCO VI *• CM PO ^ CM CO — CMCO VI ^CMP". ^ CM CO ^ CM CO ^~ CM PO
ie
-------
TABLE H-6. SUMMARY OF MM1 DATA FROM TEST RUN 5 (9 AUGUST 1985)
Number Tetra-
Mani- of deter- chloro-
fold minations ethene
3
1
2
3
1
2
3
1
2
3
Baseline1
6
7
5
3
4
2
3
4
5
3
1
3.
4.
4.
4.
4.
4.
4.
4.
4.
4.
2.
7-4.5
2-4.6
1-4.5
3-4.4
1-4.5
5-4.8
5-4.9
6-4.8
7-5.1
9-5.1
9
1,1,1-
Trichloro-
ethene
5.
5.
5.
5.
5.
6.
5.
6.
6.
6.
4.
3-6.0
8-5.9
9-6.2
9
9-6.3
1-6.4
8-6.2
0-6.2
0-6.4
5-6.8
1
Target
Chloro-
form
4.
»•
4.
4.
4.
4.
4.
4.
4.
4.
3.
5-4.9
5-4.9
6-4.9
6-4.7
6-4.8
1-4.9
6-5.0
7-4.9
9
1
compounds (arbitrary log units)
1,2-Di-
chloro-
ethene
4.9-5.4
5.2-5.4
4.8-5.0
4.5-5.3
5.1-5.5
4.9-5.1
5.0-5.4
5.0-5.3
5.4-5.9
ND
Xylenes
4.7-5.0
4.8-5.0
4.9-5.1
4.7-4.9
4.8-5.1
4.9-5.1
4.7-5.2
4.7-5.1
5.0-5.2
3.6
Tetra-
chloro-
e thane
4.4-4.9
4.6-4.9
4.6-4.8
4.2-4.7
4.7-4.9
4.6-4.9
4.5-4.9
4.7-5.0
5.0-5.3
3.5
Tri-
chloro-
ethane
4.5-4.9
4.6-5.0
4.4-4.7
4.7-5^0
4.3-5.0
4.6-4.8
4.8-5.1
4.5-5.1
4.7-4.9
4.6-5.0
ND
'Readings taken in area where process was operating - represents backgound in that
area.
ND = Not Detected
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I. Affiowfit JMf inwi TofnpofMuw
ac
i
VO
ThM
30
W
«0
•to
430
S40
•to
1M
Not *rtlu*Md >X:¥'1 • PIMM I T«*l Hunt
1100
H. Etovatod Air toM TwnpOTfcm
to
•rc»
'", I 4»4 * '.
•' *> ,
«M
144
1440
14(0
1000
TABLE H-7 MOISTURE CONTENT IN THE AIR DISCHARGE STREAM
(PERCENT BY WEIGHT)
-------
I. Ambtont a* Wei temperature
N. Elevated Air Mel Temperature
X
I
legend
Man Manifold
ABI Afterburner inlet
— No) elevated
Phaie I Teel Run*
TABLE H-8 TEMPERATURE OF T^E AIR DISCHARGE STREAM (°C)
-------
compounds for which it was mass calibrated with standards;
other compounds may have been present. Units on the summary
tables represent the logarithmic intensities of ions
characteristic to the target compounds (e.g., alphatic
hydrocarbons were semiquantified with ions at 57, 71, and 85
atomic mass units (AMU)). It is emphasized that since the MM1
was not calibrated for quantification, and the sampling method
(simply placing the probe 2 inches from the sampling port) was
not quantitative, the data can be used only in a relative
sense. The data cannot be converted to concentrations in air.
Further work is required to standardize instrument response and
establish sampling techniques before the logarithmic
intensities can be converted to a relative concentrations.
H.4 Moisture content in the air discharge stream. The
moisture content of the air discharge stream was monitored at
the afterburner inlet. The moisture content of the combined air
stream is shown for all operating conditions in Table H-7.
H.5 Temperature of the discharge air stream. The
temperature of the gases discharging the thermal processor were
monitored during each test run. Temperatures were monitored in
each leg of the manifold system as well as at the afterburner
inlet. Air discharge temperatures are summarized in Table H-8.
H-ll
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APPENDIX I
STATISTICAL ANALYTICAL APPROACH
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APPENDIX I
STATISTICAL ANALYTICAL APPROACH
Analysis Techniques. The multiple regression analysis
reduces the data to a linear equation, as discussed in Section
9, which can be used to predict important response variables.
The use of stepwise analysis allows the determination of
regression coefficients, while interactively specifying the
system equations via addition or deletion of singular variables.
As with any statistical tool, there are limitations in the
multiple regression technique; however, these limitations can be
overcome as discussed in the following subsections.
In the case of a nonlinear relationship between the input
variables and the response variable, the alternative procedures
include:
(a) Reduce the span of the analysis of the response
variable until an acceptable correlation is found.
(b) Transform the response variable, e.g.,
LN(Y) -a * bnXn
(c) Weigh each of the input variables, e.g.,
Y - a + b,w»xt + bjWzXit + ... + bnwnxn
(d) Use multiple regression as the initial iterative step
followed by analysis by a different technique to
finalize the correlation.
(e) Utilize the linear relationship in an estimation
capacity recognizing there may be variance from the
true relationship.
In order to determine the exact relationship between the
variables over a useful span, the third and fourth procedures
would have to be employed following each of a series of trial
operations similar to the test recently completed. This would
be very costly and time consuming and is impractical for this
analysis.
A correlation which minimizes the variance from the true
relationship could be developed using the third and fourth
procedures to analyze the data recorded from the completed
test. Although this procedure could extract some otherwise
indistinguishable relationships from the data, it would be very
time consuming and is also not within the scope of this project.
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The method generally accepted as the initial iterative step
is a combination of the first, second, and fifth procedures,
whereby a basic correlation would be developed followed by the
determination of its useful span. This data analysis is based
on this method.
One advantage of multiple regression is the ability to
simultaneously analyze unlimited numbers of input variables.
When computers are used to perform the analysis the number of
input variables may be limited by the software or hardware of
the computer. WESTON has utilized software and hardware which
can analyze all of the test variables simultaneously. A
Tektronix 4054 microcomputer and its associated plot-50
statistics: Multiple Linear Regression software package* was
utilized to perform the computations necessary for the iterative
steps.
It should be noted, however, that the number of calculations
required to solve the equations used in the analysis increases
factorially as each additional variable is included in the
analysis. Computer time should be a consideration when deciding
the number of input variables to be analyzed.
As the number of input variables increases, so does the
probability of coincidence (i.e., an input variable may not
actually be correlated to the response variable other than by
coincidence). While only additional testing can prove
correlation by coincidence, this factor can be discounted based
on scientific judgment and adjustment to the response
parameters.
Final solution. Application of the multiple regression
packages yielded ANOVA tables, regression tables, and summary
of successive significance of input variables.
The ANOVA table includes the following information*:
(a) SS - The sum of squares of the deviations.
(b) MS - The mean square, which is SS/df.
(c) df - Degress of freedom.
(d) F - The value of the F statistic, such that
.F - (Regression SS/df)/(Residual SS/df).
*Users Manual, Statistics; Multiple Linear Regression, Plot
50-4050D04, Tektronix, Inc., Beaverton, Oregon, July 1982.
*A glossary of statistical terms is provided in Table 1-1 at the
end of this appendix.
1-2
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(e) Pr >F - The probability that a value of a random
variable having the F-distribution takes on a value
greater than the value of F. A value less than 0.1
indicates significance of the F statistic and, conse-
quently, the overall system equations. Statisticians
normally associate a Pr >F value of less than 0.05
with a very significant hypothesis.
(f) R-square - The coefficient of determination, which
gives a measure of the linear association between the
dependent variable and the set of independent
variables. The R-square value indicates the
significance of the model (or variable) where 1.0
equals 100 percent.
(g) Rbar-square - An adjustment to R-square for its
tendency to increase as the number of independent
variables increases. The adjustment is
1 - ((I res*/(n-p))/< l(Yj-Y)l/(n-l))
(h) Root of Residual MS - The square root of the residual
mean square.
The regression table includes the following information for
•each variable coefficient in the regression equation:
(a) Estimate - The estimated value of -the coefficient.
(b) Standard Error - The standard error of the regression
coefficient estimates.
•(c) t - The value of the t-statistic, which is, for each
estimate:
Estimate/Standard Error.
(d) Pr >ABS(t) - The probability that the absolute value
of a random variable having the t-distribution takes
on a value greater than the absolute value of t. A
value of Pr >ABS(t) of less than O.I indicates
significance of the t-static and, consequently, the
estimated value of the coefficient. Statisticians
normally associate a Pr >ABS(t) value of less than
0.05 with a very significant hypothesis.
The value of the Durbin-Watson statistic can be used to test
whether the residuals are uncorrelated.
For each iterative step, both the forward and backward
stepping techniques are applied. The forward stepping analysis
allows the statistician to select a variable to be added to the
model, or the Tektronix 4054 will automatically select the
variable which is most significant of those remaining, and add
it to the model. The forward stepping technique determines the
marginal contribution of each variable added. The backward
stepping technique includes all of the selected variables to
determine interrelationships between the input variables and to
calculate an overall system equation.
1-3
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The iteration process was continued until significant and
practical system equations were developed. System equations
were rejected if:
(a) The probability that the hypothesized equation was not
correct exceeded 10 percent (Pr >F was not less than
0.1) .
(b) The significance of the equation did not approach 90
percent (R-square did not approach 0.9) or too many
variables were required to reach this level.
(c) The range of response variables for which a correlation
could be developed was too small.
Input variables were eliminated from the system equations
based on:
(a) Insignificant marginal contribution to the model
determined by the R-squared value computed during the
forward stepping process.
(b) A high probability that the hypothesized variable
coefficient was not correct as determined by the
analysis of the t statistic of the regression table
(Pr >ABS(t)).
(c) Scientific and intuitive reasoning suggesting
alternative correlations between the input variable in
question and the response variable.
(d) The coefficient of the input variable was corrective.
The system model is a set of simple linear equations which
describe certain system parameters and enable the projection of
responses to be calculated based on measureable input data. The
use of the system model can vary from a basis for an environ-
mental permit application to becoming an aid for system design
or ultimately a dynamic model. The intended use of the system
equations for the purposes of this report is the projection of
system requirements to aid in future technical and economic
feasibility analyses of thermal stripping as a decontamination
method for soils contaminated with VOC's as well as system
design.
1-4
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U
r:
TABLE 1-1. GLOSSARY OF STATISTICAL TERMINOLOGY
ANOVA table - Analysis of Variance table. The ANOVA table pro-
vides a useful summary of calculations about variability. It
contains sums of squares and mean square estimates of the two
sources of variability (regression and residuals) and their re-
spective degrees of freedom, the value of the F-statistic, R-
square, Rbar-square, and Pr >F.
Dependent variable - The variable to be described in terms of
others in the regression model.
Fitted values - Values of the dependent variable calculated from
the regression equation and existing values of the independent
variables in the model.
Independent variable - A variable used, possibly in conjunction
with other variables, to describe a given dependent variable.
Least squares - The least-squares method is a method of line-
fitting that determines parameter values to minimize the sum of
squares of the deviations (lengths of the vertical line seg-
ments) from the observed data points to the line.
Mean - The arithmetic average of a column of data.
Median - The middle value in an ordered column of data; that is,
the data value half way between the top and bottom.
Missing-data value - A numeric constant used as a place holder
for data missing from the data set.
Mode - The value that occurs most often in a data set.
Model - A statistical equation that expresses the supposed
(often only approximate) functional relation between variables.
Observation - A row of data in a data file.
Outliers - A pair of values being plotted is an outlier if the
value for one of the variables falls outside a specified number
of standard deviations from its mean. (Outliers for an index
plot are defined only on the variable for the y axis.) More gen-
erally, any discrepant value.
Pr >ABS(t) - The probability that the absolute value of a random
variable having the the t distribution takes on a value greater
than the value of the t statistic calculated as part of the re-
gression table.
1-5
6060A
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TABLE l-l. (Continued)
Pr >F - The probability that a random variable having the F dis-
tribution takes on a value greater than the value of the F sta-
tistic calculated as part of the ANOVA table.
Predicted value - The value of the dependent variable calculated
from the regression equation and new values of the independent
variables in the model.
Probability plot - Values of a variable plotted on a probability
scale. The horizontal scale refers to percentages of the proba-
bility distribution. The vertical scale, an ordinary arithmetic
scale, is for the variable. The degree to which the data lies on
a straight line indicates the closeness of fit of the sample
distribution to the theoretical distribution.
Raw data - The set of data values read from a data file and used
directly by an algorithm, as opposed to a set of data read from
a data file and manipulated by transformations before being
used.
Regression coefficient - The coefficients of the equation used
in a regression model.
Regression table - A table that provides a summary of regression
calculations. It contains parameter estimates, the standard er-
ror of the estimates, the value of the t statistic, the t proba-
bility, and the mean and standard deviation of the dependent
variable.
Residuals - The difference between the actual values and the
fitted values of the dependent variable (see definition for e) .
Response variable - Another name for a dependent variable.
Scatter plot - A scatter plot is a graphical display showing how
two variables are related to each other.
Standard deviation - The square root of the variance.
Standard error of the mean - The standard deviation of a set of
sample means.
Variance - The average of the sum of the squares of the devia-
tion of each observation from the mean of the variable.
1-6
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Distribution List
Copies
Defense Technical Information Center " 14
Cameron Station
Alexandria, Virginia 22314
Defense logistics Studies Information Exchange
US Army Logistics Management Center
Fort Lee, Virginia 23801
Conrander 32
US Anry Toxic and Hazardous Materials Agency
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Letterkenny Amy Depot
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-------