^ I : ' ft ¦ s
!i ¦. h - >
METHOD 13 12
SYNTHETIC PRECIPITATION LEACH TEST FOR SOILS
1.0 SCOPE AND APPLICATION
1-. 1 Method 13 12 is des iqned to determine the mobility of '
both orqanic arid inorganic contaminants present in soils.
1.2 If a total analysis of the soil demonstrates that in-
dividual contaminants are not present.in the-„soi„l, or that they
are present but at such low concentrations that the appropriate
regulatory thresholds could not possibly be exceeded, Method
13 12 need not be run.
i-'S rr-A RPGiOH i ur.f..r;v
2.0 SUMMARY OF METHOD	(SSL2n
2.1 The particle size of the soil is reduced (if necessary)
and is extracted with an amount of extraction fluid equal to 20
times the weight of the soil. The extraction fluid employed is
a function of the region of the country where the soil site is
located. A special extractor vessel is used when testing for
volatiles. Followinq extraction, the liquid extract is separated
from the soil by 0.6-0.8 um glass fiber filter.
3.0 INTERFERENCES
3.1 Potential interferences that may be encountered during
analys i s are discussed in the individual analytical methods.
4.0 APPARATUS AND MATERIALS	'
4.1	Agitation apparatus - an acceptable agitation apparatus
is one which is capable of rotating the extraction vessel in an
end-over-end fashion at 30 + 2 rpm (see Figure 1). Suitable
devices known to EPA are identified in Table 2.
4.2	Extraction vessel - acceptable extraction vessels are
those that are listed below:
4.2.1 Zero Headspace Extraction Vessel (ZHE) - This
device is for use only when the soil is being tested for the
mobility of volatile constituents (see Table 1). The ZHE is an
extraction vessel that allows for liquid/solid separation within
the device and which effectively precludes headspace (as depicted
in Figure 3). This type of vessel allows for initial liquid/solid
separation, extraction, and final extract filtration without
having to open the vessel (see Step 4.3.1). These vessels shall
have an internal volume of 500 to 600 mL and be equipped to
accommodate a 9 0-mm filter. Suitable ZHE devices known to EPA
are identified in Table 3. These devices contain viton O-rinqs
which should be replaced frequently. For the ZHE to be acceptable
for use, the piston within the ZHE should be able to be moved
1312-1
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with approximately 15 psi or less. If it takes more pressure
to move the piston, the O-rinqs in the device should be replaced.
F£ this does not solve the problem, the ZHE is unacceptable for
1312 analyses and the manufacturer should be contacted. The ZHE
should be checked after every extraction. If the device con-
tains a built-in pressure gauge, pressurize the device to
50 psi, allow it to stand unattended for 1 hour, and recheck
the pressure. If the device does not have a built-in pressure
gauge, pressurize the device to 50 psi, submerge it in water
and check for the presence of air bubbles escaping from any
of the fittings. If pressure is lost, check all fittinqs and
inspect and replace O-rings, if necessary. Retest the device.
If leakage problems cannot be solved, the manufacturer should
be contacted.
4.2.2	When the soil is being evaluated for other than
volatile contaminants, an extraction vessel that does not pre-
clude headspace (e.g. a 2-liter bottle) is used. Suitable
extraction vessels include bottles made from various materials,
depending on the contaminants to be analyzed and the nature of the
waste (see Step 4.3.3). It is recommended that borosilicate
glass bottles be used over other types of glass, especially
when inorganics are of concern. Plastic bottles may be used
only if inorganics are to be investigated. Bottles are available
from a number of laboratory suppliers. When this type of ex-
traction vessel is used, the filtration device discussed in
Step 4.3.2 is used for initial liquid/solid separation and final
extract filtration.
4.2.3	Some ZHEs use gas pressure to actuate the ZHE piston,
while others use mechanical pressure (see Table 3). Whereas
the volatiles procedure (see Step 7.4) refers to pounds-per-
square inch (psi), for the mechanically actuated piston, the
pressure applied is measured in torque-inch-pounds. Refer to
the manufacturer's instuctions as to the proper conversion.
4.3 Filtration devices - It is recommended that all filtrations
performed in a hood.
4.3.1 Zero-Headspace Extractor Vessel (see Figure 3) -
When the waste is being evaluated for volatiles, the zero-
headspace extraction vessel is used for filtration. The device
shall be capable of supporting and keeping in place the fiber
filter, and be able to withstand the pressure needed to accomplish
separation (50 psi).
NOTE: When is it suspected that the glass fiber filter
has been ruptured, an in-line glass fiber filter may be
used to filter the material within the ZHE.
4.3.2 Filter holder - when the soil is being evaluated
for other than volatile compounds, a filter holder capable of
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supporting a glass fiber filter and able to withstand 50 psi
or more of pressure shall be used. These devices shall have a
minimum internal volume of 300 mL and be equipped to accomodate
a minimum filter size of 47 mm (filter holders having an
internal capacity of 1.5 liters or greater are recommended).
4.3.3 Materials of construction - filtration devices shall
be made of inert materials which will not leach or absorb soil
components. Glass, polytetraf luoroethylene (PTFE) or type 316
stainless steel equipment may be used when evaluating the mobility
of both organic and inorganic components. Devices made of high
density polyethylene (HDPE) , polypropylene, or polyvinyl chloride
may be used only when evaluating the mobility of metals. Boro-
silicate glass bottles are recommended for use over other types
of glass bottles, especially when inorganics are constituents
of concern.
4.4	Filters - filters shall be made of borosilicate glass
fiber, shall have an effective pore size of 0.6 - 0.8 um and
shall contain no binder materials. Filters known to EPA to meet
these requirements are identified in Table 5. When evaluating the
mobility of metals, filters should be acid-washed prior to use
by rinsing with 1.0N nitric acid followed by three consecutive rinses
with deionized distilied water (a minimum of 1-liter per rinse is
recommended). Glass fiber filters are fragile and should be handled
with care.
4.5	pH meters - any of the commmonly available pH meters are
acceptable.
4.6	ZHE extract collection devices - TEDLAR bags, glass, stain-
less steel or PTFE gas tight syringes are used to collect the volatile
extract.
4.7	Laboratory balance - any laboratory balance accurate to
within + 0.01 g may be used (all weight measurements are to be within
+ 0. 1 <3) •
4.8	ZHE extraction fluid transfer devices - any device capable
of transferring the extraction fluid into the ZHE without changing
the nature of the extraction fluid is recommended.
5.0 REAGENTS
5.1 Reagent water - reagent water is defined as water in
which 3° interferent is not observed at or above the method
detection limit of the analyte(s) of interest. For non-volatile
extractions, ASTM Type II water, or equivalent meets the definition
of reagent water. For volatile extractions, it is recommended
that reagent water be qenerated by any of the following methods.
Reagent water should be monitored periodically for impurities.
1312-3
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5.1.1	Reagent water for volatile extractions may be
generated by passing tap water through a carbon filter bed
containing about 500 g of activated carbon (Calgon Corp.,
Filtrasorb 300 or eguivalent).
5.1.2	A water purification system (Millipore Super-Q or
equivalent) may also be used to generate reagent water for
volatile extractions.
5.1.3	Reagent water for volatile extractions may also
be prepared by boiling water for 15 minutes. Subsequently,
while maintaining the water temperature at 90 + 5°C, bubble
a contaminant-free inert gas (e.g. nitrogen) through the
water for 1 hour. While still hot, transfer the water to a
narrow-mouth screw-cap bottle under zero headspace and seal
with a Teflon lined septum and cap.
5.2	Sulfuric acid/nitric acid (60/40 weight percent mixture)
H2SO4/HNO3. Cautiously mix 60 g of concentrated sulfuric acid with
40 g of concentrated nitric acid.
5.3	Extraction-fluids:
5.3.1	Extraction fluid #1 - this fluid is made by adding
the 60/40 weight percent mixture of sulfuric and nitric acids
to reagent water until the pH is 4.20 + 0.05.
5.3.2	Extraction fluid #2 - this fluid is made by adding
the 60/40 weight percent mixture of sulfuric and nitric acids
to reagent water until the pH is 5.00 + 0.05.
5.3.3	Extraction fluid	#3 - this fluid is reagent water
(ASTM Type II water, or equivalent) used to determine cyanide
leachabi1i ty.
Note; It is suggested that these extxraction fluids be moni-
tored frequently for impurities. The pH should be
checked prior to use	to ensure that these fluids are
made up accurately.
5.4	Analytical standards shall be prepared according to the
appropriate analytical method.
6.0 SAMPLE COLLECTION, PRESERVATION, AND HANDLING
6.1	All samples shall be collected using	an appropriate
sampling plan.
6.2	At least two separate representative	samples of a soil
should be collected. The first sample is used	to determine if the
soil requires particle-size reduction and, if desired, the percent
solids of the soil. The second sample is used	for extraction
of volatiles and non-volatiles.
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6.3	Preservatives shall not be added to samples.
6.4	Samples shall be refrigerated to minimize loss of volatile
organics and to retard biological activity.
6.5	When the soil is to be evaluated for volatile contaminants,
care should be taken to minimize the loss of volatiles. Samples
shall be taken and stored in a manner to prevent the loss of
volatile contaminants. If possible, it is recommended that any
necessary particle-size reduction be conducted as the sample is
being taken.
6.6. 1312 extracts should be prepared for analysis and
analyzed as soon as possible following extraction. If they need
to be stored, even for a short period of time, storage shall be at
4°C, and samples for volatiles analysis shall not be allowed to
come into contact with the atmosphere (i.e. no headspace). See
Section 8.0 (Quality Control) for acceptable sample and extract
holding times.
7.0 PROCEDURE
7.1	The preliminary 1312 evaluations are performed on a mini-
mum 100 g representative sample of soil that will not actually under-
go 1312 extraction (designated as the first sample in Step 6.2).
7.1.1	Determine whether the soil requires particle-size
reduction. If the soil passes through a 9.5 nun (0. 375-inch)
standard sieve, particle-size reduction is not required
(proceed to Step 7.2). If portions of the sample do not
pass through the sieve, then the oversize portion of the
soil will have to be prepared for extraction by crushing
the soil to pass the 9.5 mm sieve.
7.1.2	Determine the percent solids if desired.
7.2	Procedure when volatiles are not involved - Enough
solids should be generated for extraction such that the volume
of 1312 extract will be sufficient to support all of the analyses
required. However, a minimum sample size of 100 grams shall
be used. If the amount of extract generated by a single 1312
extract will not be sufficient to perform all of the analyses,
it is recommended that more than one extraction be performed and
the extracts be combined and then aliquoted for analysis.
7.2.1	Weigh out a representative subsample of the soil and
transfer to the filter holder extractor vessel.
7.2.2	Determine the appropriate extraction fluid to use.
If the soil is from a site that is east of the Mississippi
River, extraction fluid #1 should be used. If the soil is
from a site that is west of the Mississippi River, extraction
fluid #2 should be used. If the soil is to be tested for
cyanide leachabi1ity, extraction fluid #3 should be used.
1312-5
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Note: Extraction fluid 13 {reagent water) must be used
when evaluating cyanide-containing soils because leaching
of cyanide-containing soils under acidic conditions may
result in the formation of hydrogen cyanide gas.
7.2.3	Determine the amount of extraction fluid to add
based on the following formula:
amount of extraction fluid (mL) = 20 x weight of soil (g)
Slowly add the amount of appropriate extraction fluid to the
extractor vessel. Close the extractor bottle tightly (it
is recommended that Teflon tape be used to ensure a tight
seal), secure in rotary extractor device, and rotate at 30
+ 2 rpra for 18+2 hours. Ambient temperature (i.e. temper-
ature of room in which extraction is to take place) shall
be maintained at 22 + 3°C during the extraction period.
Note: As agitation continues, pressure may build up within the
extractor bottle for some types of soil (e.g. limed or
calcium carbonate containing soil may evolve gases such as
carbon dioxide). To relieve excess pressure, the extractor
bottle may be periodically opened (e.g. after 15 minutes,
30 minutes, and 1 hour) and vented into a hood.
7.2.4	Following the 18 + 2 hour extraction, the material in
the extractor vessel is separated into its component liquid and
solid phases by filtering through a glass fiber filter.
7.2.5	Following collection of the 1312 extract it is re-
commended	that the pH of the extract be recorded. The extract ¦'
should be	immediately aliquoted for analysis and properly
preserved	(metals aliquots must be acidified with nitric
acid to pH < 2; all other aliquots must be stored under
refrigeration (4°C) until analyzed). The 1312 extract
shall be prepared and analyzed according to appropriate
analytical methods. 1312 extracts to be analyzed for metals,
other than mercury, shall be acid digested.
7.2.6	The contaminant concentrations in the 1312 extract are
compared to thresholds in the clean closure guidance manual.
Refer to Section 8.0 for Quality Control requirements.
7.3 Procedure when volatiles are involved:
7.3.1 The ZHE device is used to obtain 1312 extracts for
volatile analysis only. Extract resulting from the use of the
ZHE shall not be used to evaluate the mobility of non-volatile
analytes (e.q. metals, pesticides, etc.). The ZHE device
has approximately a 500 mL internal capacity. Although a minimum
sample size of 100 g was required in the Step 7.2 procedure, the
ZHE can only accommodate a maximum of 25 g of solid , due to the
need to add an amount of extraction fluid equal to 20 times the
1312-6
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weight of the soil. The ZHE is charged with sample only once and
the device is not opened until the final extract has been col-
lected. Although the following procedure allows for particle-
size reduction during the conduct of the procedure, this could
result in the loss of volatile compounds. If possible particle-
size reduction (see Step 7.1.1) should be conducted on the
sample as it is being taken (e.g., particle-size may be reduced
by crumbling). If necessary particle-size reduction may be
conducted during the procedure. In carrying out the following
steps, do not allow the soil to be exposed to the atmosphere for
any more time than is absolutely necessary. Any manipulation of
these materials should be done when cold (4°C) to minimize the
loss of volatiles. Pre-weigh the evaculated container which
will receive the filtrate (see Step 4.6), and set aside. If
using a TEDLAR® bag, all air must be expressed from the device.
7.3.2	Place the ZHE piston within the body of the ZHE (it
may be helpful first to moisten the piston O-rings slightly with
extraction fluid). Adjust the piston within the ZHE body to a
height that will minimize the distance the piston will have to
move once it is charged with sample. Secure the gas inlet/outlet
flange (bottom flange) onto the ZHE body in accordance with the
manufacturer's instructions. Secure the glass fiber filter
between the support screens and set aside. Set liquid inlet/out-
let flange (top flange) aside.
7.3.3	Quantitatively transfer 25 g of soil to the ZHE.
Secure the filter and support screens into the top flange of the
device and secure the top flange to the ZHE body in accordance
with the manufacturer's instructions. Tighten all ZHE fittings
and place the device in the vertical position (gas inlet/outlet
flange on the bottom). Do not attach the extraction collection
device to the top plate. Attach a gas line to the gas inlet/out-
let valve (bottom flange) and, with the liquid inlet/outlet
valve (top flange) open, begin applying gentle pressure of 1-10
psi to a maximum of 50 psi to force most of the headspace out of
the device.
7.3.4	With the ZHE in the vertical position, attach a
line from the extraction fluid reservoir to the liquid inlet/
outlet valve. The line used shall contain fresh extraction
fluid and should be preflushed with fluid to eliminate any air
pockets in the line. Release gas pressure on the ZHE piston
(from the gas inlet/outlet valve), open the liquid inlet/
outlet valve, and begin transferring extraction fluid (by
pumping or similar means) into the ZHE. Continue pumping
extraction fluid into the ZHE until the appropriate amount of
fluid has been introduced into the device.
7.3.5	After the extraction fluid has been added, immediately
close the inlet/outlet valve and disconnect the extraction fluid
line. Check the ZHE to ensure that all valves are in their closed
positions. Physically rotate the device in an end-over-end fashion
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2 or 3 times. Reposition the ZHE in the vertical position with,
the liquid inlet/outlet valve on top. Put 5-10 psi behind the
piston (if nesessary) and slowly open the liquid inlet/outlet
valve to bleed out any headspace (into a hood) that may have
been introduced due to the addition of extraction fluid.
This bleedinq shall be done quickly and shall be stopped at th^
first appearance of liquid from the valve. Re-pressurize the
ZHE with 5-10 psi and check all ZHE fittings to ensure that
they are closed.
7.3.6	Place the ZHE in the rotary extractor apparatus (if
it is not already there) and rotate the ZHE at 30+2 rpm for
18+2 hours. Ambient temperature (i.e. temperature of the room
in which extraction is to occur) shall be maintained at 22 + 3°c
during agitation.
7.3.7	Following the 18+2 hour agitation period, check
the pressure behind the ZHE piston by quickly opening and closing
the gas inlet/outlet valve and noting the escape of gas. If the
pressure has not been maintained (i.e. no gas release observed),
the device is leaking. Check the ZHE for leaking and redo the
extraction with a new sample of soil. If the pressure within
the device has been maintained, the material in the extractor
vessel is separated into its component liquid and solid phases.
7.3.8	Attach the evacuated pre-weighed filtrate collection
container to the liquid inlet/outlet valve and open the valve.
Begin applying gentle pressure of 1-10 psi to force the liquid
phase into the filtrate collection container. If no additional
liquid has passed through the filter in any 2 minute interval,
slowly increase the pressure in 10-psi increments to a maximum of
50 psi. After each incremental increase of 10 psi/ if no addition|
liquid has passed through the filter in any 2 minute interval,
proceed to the next 10 psi increment. When liquid flow has
ceased such that continued pressure filtration at 50 psi does
not result in any additional filtrate within any 2 minute period,
filtration is stopped. Close the inlet/outlet valve, discontinue
pressure to the piston, and disconnect the filtration collection
contai ner.
NOTE: Instantaneous application of high pressure can
degrade the glass fiber filter and may cause
premature plugging.
7.3.9	Following collection of the 1312 extract, the extract
should be immediately aliquoted for analysis and stored with
minimal headspace at 4°C until analyzed. The 1312 extract will be
prepared and analyzed according to the appropriate analytical
methods.
8.0 QUALITY CONTROL
8.1 All data, including quality assurance data, should be
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maintained and available for reference or inspection.
8.2	A minimum of one blank (extraction fluid # 1) for every
10 extractions that have been conducted in an extraction vessel
shall be employed as a check to determine if any memory effects
from the extraction equipment are occurring.
8.3	For each analytical batch (up to twenty samples), it is
recommended that a matrix spike be performed. Addition of matrix
spikes should occur once the 1312 extract has been generated
(i.e. should not occur prior to performance of the 1312 procedure).
The purpose of the matrix spike is to monitor the adequacy of the
analytical methods used on the 1312 extract and for determining
if matrix interferences exist in analyte detection.
8.4	All quality control measures described in the appropriate
analytical methods shall be followed.
8.5	The method of standard addition shall be employed for
each analyte if: 1) recovery of the compound from the 1312
extract is not between 50 and 150%, or 2) if the concentration of
the constituent measured in the extract is within 20% of the
appropriate regulatory threshold. If more than one extraction is
being run on samples of the same waste (up to twenty samples),
the method of standard addition need be applied only once and the
percent recoveries applied on the remainder of the extractions.
8.6	Samples must undergo 1312 extraction within the following
time period after sample receipt: Volatiles, 14 days; Semi-
Volatiles, 40 days; Mercury, 28 days; and other Metals, 180 days.
1312 extracts shall be analyzed after generation and preservation
within the following periods: Volatiles, 14 days; Semi-Volatiles,
40 days; Mercury, 28 days; and other Metals, 180 days.
9.0 METHOD PERFORMANCE
9.1 None available.
10.0 REFERENCES
10. 1 None available.
1312-9
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TABLE 1. -- VOLATILE CONTAMINANTS
Compounds
CAS No.
Acetone	
Acrylonitrile	
Benzene	
n-Butyl alcohol	
Carbon disulfide	
Carbon tetrachloride	
Chlorobenzene	
Chloroform	
1,2-Dichloroe thane	
1,1-Di chloroethylene	
Ethyl acetate	
Ethyl benzene			
Ethyl ether	
Isobu tanol	
Methanol	
Methylene chloride 	
Methyl ethyl ketone 	
Methyl isobutyl ketone 	
1,1,1,2-Tetrachloroethane	
1,1,2,2-Tetrachloroethane	
Tetrachloroethylene 	
Tolulene 	
1.1.1-Trichloroethane		
1.1.2-Trichloroethan	e	
Trichloroethylene 	
Trichlorofluoromethane	
1,1,2-Trichloro-l,2,2-trifluoroethane
Vinyl chloride	
Xylene 	
67-
107-
71-
71-
75-
56-
108-
67-
107-
75-
141-
100-
60-
78-
67-
75-
78-
108-
630-
79-
127-
108-
71-
79-
79-
75-
76-
75-
1330-
¦64-1
¦13-1
•43-2
36-6
15-0
¦23-5
90-7
66-3
06-2
•35-4
78-6
•41-4
29-7
83-1
56-1
09-2
93-3
10-1
20-6
34-5
18-4
88-3
55-6
00-5
01-6
69-4
13-1
01-7
20-7
1312-10
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TABLE 2. — SUITABLE ROTARY AGITATION APPARATUS1
Company
Location
Model
Analytical Testing and
Consulting Services, Inc.
Warrington, PA
(215) 343-4490
4-vessel
devi ce
Associated Design and
Manufacturing Company
Alexandria, VA
(703) 549-5999
4-vessel
6-vessel
devi ce,
device
Environmental Machine
and Design, Inc.
Lynchburg, VA
(804) 845-6424
4-vessel
6-vessel
devi ce,
devi ce
IRA Machine Shop and
Laboratory
Santurce, PR
(809) 752-4004
16-vessel
device
Lars Lande Manufacturing
Whitmore Lake, MI
(313) 449-4116
10-vessel
5-vessel
devi ce
device
Millipore Corp.
Bedford, MA
(800) 225-3384
4-vessel ZHE device
or 4-one litter
bottle extractor
device
REXNORD
Milwaukee, WI
(414) 643-2850
6-vessel
devi ce
lAny device that rotates the extraction vessel in an end-over-enct
fashion at 30 + 2 rpm is acceptable.
TABLE 3. — SUITABLE ZERO-HEADSPACE EXTRACTOR VESSELS
Company
Location
Model No.
Analytical Testing
suiting Services,
& Con-
ine.
Warrington, PA,
(215)'343-4490
C102, Mechanical
Pressure Device
Associated Design
facturing Co.
& Manu-
Alexandria, VA
(703) 549-5999
3740-ZHB, Gas
Pressure Device
Lars Lande Mfg.

Whitmore Lake, MI
(313) 449-4116
Gas Pressure
Device
Millipore Corp.

Bedford, MA,
(800) 225-3384
SD1 P581 C5, Gas
Pressure Device
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TABLE 4. — SUITABLE ZHE FILTER HOLDERS1
Company
Location
Model
Size
Micro Filtration Systems
Dublin, CA
(415) 828-6010
302400
14 2 mm
Millipore Corp.
Bedford, MA
(800) 225-3384
YT30142HW
XX1004700
14 2 mm
4 7 mm
Nucleopore Corp.
Pleasanton, CA
(800) 882-7711
425910
410400
14 2 mm
4 7 mm
^Any device capable of separating the liquid from the solid phase of
the soil is suitable, providing that it is chemically compatible with
the soil and the constitutents to be analyzed. Plastic devices (not
listed above) may be used when only inorganic contaminants are of con
cern. The 142 mm size filter holder is recommended.
TABLE 5. — SUITABLE FILTER MEDIA
Company
Location
Model
Si ze^
Millipore Corp.
Bedford, MA
(800) 225-3384
AP 40
r-
•
o
Nucleopore Corp.
Pleasanton, CA
(415) 463-2530
211625
0.7
Whatman Laboratory
Products, Inc.
Clifton, NJ
(201) 773-5800
GFF
0.7
^Nominal pore size
1312-12
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December
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Figure 1. Rotary Agitation
1312- \1
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gure 2. Zero-Headspace Extraction Vessel
liquid inlet/outlet valve
i t i
-f i 1 ter	
•waste and
extraction
fluid
piston
->¦ top flange
-V body
VITON O-rings

bottom flange
I
pressurizing gas inlet/outlet valve
1312-14
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METHOD 1312
SYNTHETIC ACID PRECIPITATION LEACH TEST FOR SOILS
c
lUtt
J
7 • i Soil atapl*
7.3 !•
MMicl* dn
r«4ietl«i
MClMiqr?
IU
7.a l«4ui
•U«
by
crushing
M-T.l r«i«n
ntiwtln >t nil
t*r If k««r«; m
1*1 f»r nluUt
•r(iilci
T.«
¦•Hnliti I) ti
X»I (far nlitllta)
•»; 3) llltntlai
f»r
ucnlttUii
'Aialyla fey
•PFr«»rUta
HtWtl
1312-iS
Revi si on
December
0
1988

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