DRC-2011-005650 - 0901a0688023082c

Page 1 of 1
Sonja Robinson - Part 1 White Mesa Mill Nitrate Investigation Work Plan Revision, Docket No,
UGW09-03
mmmMmmMmmmmM/mM^^ wmmmmmmsmmmMm.
From: Jo Ann Tischler <[e-mail]>
To: Rusty Lundberg <[e-mail]>
Date: 5/13/2011 7:48 PM
Subject: Part 1 White Mesa Mill Nitrate Investigation Work Plan Revision, Docket No.
UGW09-03
CC: Loren Morton <[e-mail]>, Thomas Rushing ii <[e-mail]>,
"[e-mail]" <Robert_D_Baird@URS
"[e-mail]" <[e-mail]>, David Frydenlund
<[e-mail]>, Kathy Weinel <[e-mail]>,
Harold Roberts <[e-mail]>, David Turk
<[e-mail]>, "'Dan Erskine'" <[e-mail]>, Rob
Sengebush <[e-mail]>, Angela Persico <[e-mail]>, Justin
Jayne <[e-mail]>
Attachments: Ltr to R Lundberg 05.13.1 INitrate work plan comment response and transmittal.pdf;
Nitrate WP Rev 5.13.11 per URS- text tables figs.pdf
Attached please find Denison Mines (USA) Corp.'s:
• response to Utah Division of Radiation Control's ("DRC's") comment letter of May 11, 2011 regarding
the Nitrate Investigation work Plan
• word searchable pdf digital blacklme and redline copies of the revised Work Plan dated May 13, 2011 -
text, tables, and figures.
A second email with the appendices will follow this transmittal. The full files were too large for one email.
Per email instructions from Tom Rushing on May 12, 2011, hard copies of this version were not required.
Please contact me if you have any questions on this transmittal.
Your truly,
Jo Ann Tischler ^
Jo Ann Tischler
Director, Compliance and Permitting
t: 303-389-4132 | f: 303-389-4125
1050 17th Street, Suite 950
Denver, GO, US, 80265
DENISON MINES (USA) CORP
\AA/vw.denisonmines.Gom
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file://C:\Documents and Settings\Sdrobinsoil\Local Settings\Temp\XPgrpwise\4DD0D62Eh. 5/16/2011
Figures
Tables
JfnT~l Designation: 02488 -Oga ~ INnRHAnONAL
Standard Practice for
Description and Identification of Soils (Visual-Manual
Procedure)1
This standard is issued under the fixed designation D2488; the numher immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope*
1.1 This practice covers procedures for the description of
soils for engineering purposes.
1.2 This practice also describes a procedure for identifying
soils, at the option of the user, based on the classification
system described in Test Method D2487. The identification is
based on visual examination and manual tests. It must be
clearly stated in reporting an identification that it is based on
visual-manual procedures.
1.2.1 When precise classification of soils for engineering
purposes is required, the procedures prescribed in Test Method
D2487 shall be used.
1.2.2 In this practice, the identification portion assigning a
group symbol and name is limited to soil particles smaller than
3 in. (75 mm).
1.2.3 The identification portion of this practice is limited to
naturally occurring soils (either intact or disturbed).
NOTE I-This practice may be used as a descriptive system applied to
such materials as shale, claystone, shells, crushed rock, etc. (see Appendix
X2).
1.3 The descriptive information in this practice may be used
with other soil classification systems or for materials other than
naturally occurring soils.
1.4 The values stated in inch-pound units are to be regarded
as standard. The values given in parentheses are mathematical
conversions to SI units that are provided for information only
and are not considered standard.
1.5 This standard does not purport to address all of the
safety problems, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. For specific
precautionary statements see Section 8.
1.6 This practice offers a set of instructions for performing
one or more specific operations. This document cannot replace
I This practice is under the jurisdiction of ASTM Committee Dl8 on Soil and
Rock and is the direct responsibility of Subcommittee D18.07 on Identification and
Classification of Soils.
Current edition approved June 15, 2009. Published July 2009. Originally
approved in 1966. Last previous edition approved in 2009 as 02488 -09. DOl:
10.1520ID2488·09A.
education or experience and should be used in conjunction
with professional judgment. Not all aspects of this practice may
be applicable in all circumstances. This ASTM standard is not
intended to represent or replace the standard of care by which
the adequacy of a given professional service must be judged,
nor should this document be applied without consideration of
a project's many unique aspects. The word "Standard" in the
title of this document means only that the document has been
approved through the ASTM consensus process.
2. Referenced Documents
2.1 ASTM Standards:2
D653 Terminology Relating to Soil, Rock, and Contained
Fluids
D 1452 Practice for Soil Exploration and Sampling by Auger
Borings
D1586 Test Method for Penetration Test (SPT) and Split-
Barrel Sampling of Soils
D1587 Practice for Thin-Walled Tube Sampling of Soils for
Geotechnical Purposes
D2113 Practice for Rock Core Drilling and Sampling of
Rock for Site Investigation
D2487 Practice for Classification of Soils for Engineering
Purposes (Unified Soil Classification System)
D3740 Practice for Minimum Requirements for Agencies
Engaged in Testing and/or Inspection of Soil and Rock as
U sed in Engineering Design and Construction
D4083 Practice for Description of Frozen Soils (Visual-
Manual Procedure)
3. Terminology
3.1 Definitions-Except as listed below, all definitions are
in accordance with Terminology D653.
NOTE 2-For particles retained on a 3-in. (75-mm) US standard sieve,
the following definitions are suggested:
Cobbles-particles of rock that will pass a 12-in. (300-mm) square
opening and be retained on a 3-in. (75-mm) sieve, and
2 For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard's Document Summary page on
the ASTM website.
* A Summary of Changes section appears at the end of this standard.
Copyright ©ASTM International. 100 Barr Harbour Dr .• P.O. Box C·700 West Conshohocken. Pennsylvania 19426·2959. United States
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<0 02488 -09a
Boulders-particles of rock that will not pass a 12-in. (300-mm) square
opening.
3.1.1 clay-soil passing a No. 200 (75-jlm) sieve that can be
made to exhibit plasticity (putty-like properties) within a range
of water contents, and that exhibits considerable strength when
air-dry. For classification, a clay is a fine-grained soil, or the
fine-grained portion of a soil, with a plasticity index equal to or
greater than 4, and the plot of plasticity index versus liquid
limit falls on or above the "A" line (see Fig. 3 of Test Method
D2487).
3.1.2 gravel-particles of rock that will pass a 3-in. (75-
mm) sieve and be retained on a No.4 (4.75-mm) sieve with the
following subdivisions:
coarse-passes a 3-in. (75-mm) sieve and is retained on a
3f4-in. (19-mm) sieve.
fine-passes a 3f4-in. (19-mm) sieve and is retained on a No.
4 (4.75-mm) sieve.
3.1.3 organic clay-a clay with sufficient organic content to
influence the soil properties. For classification, an organic clay
is a soil that would be classified as a clay, except that its liquid
limit value after oven drying is less than 75 % of its liquid limit
value before oven drying.
3.1.4 organic silt-a silt with sufficient organic content to
influence the soil properties. For classification, an organic silt
is a soil that would be classified as a silt except that its liquid
limit value after oven drying is less than 75 % of its liquid limit
value before oven drying.
3.1.5 peat-a soil composed primarily of vegetable tissue in
various stages of decomposition usually with an organic odor,
a dark brown to black color, a spongy consistency, and a
texture ranging from fibrous to amorphous.
3.1.6 sand-particles of rock that will pass a No.4 (4.75-
mm) sieve and be retained on a No. 200 (75-jlm) sieve with the
following subdivisions:
coarse-passes a No.4 (4.75-mm) sieve and is retained on
a No. 10 (2.00-mm) sieve.
medium-passes a No. 10 (2.00-mm) sieve and is retained
on a No. 40 (425-jlm) sieve.
fine-passes a No. 40 (425-jlm) sieve and is retained on a
No. 200 (75-jlffi) sieve.
3.1.7 silt-soil passing a No. 200 (75-jlffi) sieve that is
nonplastic or very slightly plastic and that exhibits little or no
strength when air dry. For classification, a silt is a fine-grained
soil, or the fine-grained portion of a soil, with a plasticity index
less than 4, or the plot of plasticity index versus liquid limit
falls below the "A" line (see Fig. 3 of Test Method D2487).
4. Summary of Practice
4.1 Using visual examination and simple manual tests, this
practice gives standardized criteria and procedures for describ-
ing and identifying soils.
4.2 The soil can be given an identification by assigning a
group symbol(s) and name. The flow charts, Fig. la and Fig. 1 b
for fine-grained soils, and Fig. 2, for coarse-grained soils, can
be used to assign the appropriate group symbol(s) and name. If
the soil has properties which do not distinctly place it into a
specific group, borderline symbols may be used, see Appendix
X3.
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NOTE 3-It is suggested that a distinction be made between dual
symbols and borderline symbols.
Dual Symbol-A dual symbol is two symbols separated by a hyphen,
for example, GP-GM, SW-SC, CL-ML used to indicate that the soil has
been identified as having the properties of a classification in accordance
with Test Method D2487 where two symbols are required. Two symbols
are required when the soil has between 5 and 12 % fines or when the liquid
limit and plasticity index values plot in the CL-ML area of the plasticity
chart.
Borderline Symbol-A borderline symbol is two symbols separated by a
slash, for example, CLlCH, GM/SM, CLIML. A borderline symbol should
be used to indicate that the soil has been identified as having properties
that do not distinctly place the soil into a specific group (see Appendix
X3).
5. Significance and Use
5.1 The descriptive information required in this practice can
be used to describe a soil to aid in the evaluation of its
significant properties for engineering use.
5.2 The descriptive information required in this practice
should be used to supplement the classification of a soil as
determined by Test Method D2487.
5.3 This practice may be used in identifying soils using the
classification group symbols and names as prescribed in Test
Method D2487. Since the names and symbols used in this
practice to identify the soils are the same as those used in Test
Method D2487, it shall be clearly stated in reports and all other
appropriate documents, that the classification symbol and name
are based on visual-manual procedures.
5.4 This practice is to be used not only for identification of
soils in the field, but also in the office, laboratory, or wherever
soil samples are inspected and described.
5.5 This practice has particular value in grouping similar
soil samples so that only a minimum number of laboratory tests
need be run for positive soil classification.
NOTE 4-The ability to describe and identify soils correctly is learned
more readily under the guidance of experienced personnel, but it may also
be acquired systematically by comparing numerical laboratory test results
for typical soils of each type with their visual and manual characteristics.
5.6 When describing and identifying soil samples from a
given boring, test pit, or group of borings or pits, it is not
necessary to follow all of the procedures in this practice for
every sample. Soils which appear to be similar can be grouped
together; one sample completely described and identified with
the others referred to as similar based on performing only a few
of the descriptive and identification procedures described in
this practice.
5.7 This practice may be used in combination with Practice
D4083 when working with frozen soils.
NOTE 5-Notwithstanding the statements on precision and bias con-
tained in this standard: The precision of this test method is dependent on
the competence of the personnel performing it and the suitability of the
equipment and facilities used. Agencies that meet the criteria of Practice
D3740 are generally considered capable of competent and objective
testing. Users of this test method are cautioned that compliance with
Practice D3740 does not in itself assure reliable testing. Reliable testing
depends on several factors; Practice D3740 provides a means for
evaluating some of those factors.
Joe Galemore (INTERA) pursuant to License Agreement. No further reproductions authorized.
<0 02488 -09a
GROUP SYMBOL GROUP NAME
< <30% plul No. 200 -=::::::::::::: <15'" plul No. 200 .. Lean clav
15·25'" plul No. 200 -===:::::::: ", .. nd ;::'" IIravel-Lellll clav wi1h .. nd CL ", .. nd <'" IIrev.l-L.an clay with IIra,,1
", .. nd ~'" of IIrawal <15'" IIravel .. Sendv lean clav ~3O'lIo plul No. 200-----=:::::::::::: ~15'" grawII .. Sendy INn clay with IIraw.1
--------", .. nd <'" graw.1 --=::::::::::: <15'" .. nd .. Grn.lIv 1.l1li cl.V
~16'" .. nd .. Grlvellv I .... clay with .. nd
<3O'lIo plus No. 200 ~ <15'" plus No. 200 .. Silt < 15·25'" plul No. 200 --=:::::::::::: ", .. nd ~'" IIrlw.l-Silt with .. nd ML '" .. nd <% IIrawal -Silt with gr.vel
~ ", .. nd ~'" of IIr.".1 -=::::::::::::: <15'" IIr.vel .. Sendy silt
~30'" plus No. 200 ~15'110 IIrlw.1 .. Sendy silt with grnel
'" lind <'" lI'evel --=::::::::::: <15'" lind .. Gr.veliv lilt
~15'11. send .. Grlvelly silt with lind
< <30'" plUI No. 200 oc::::::::::::: <15'" plul No. 200 .. Fit cliV
15.25% plul No. 200 -=::::::::::::: % .. nd;;::'" graw.1 -Fit claV with lind CH '" lind <'" gravel .. Fit cleV with llrewel
'" lind ~'" of g,avel ~ <15% grlvel .. $Indy fat clay ~3O'lIo plus No. 200-------;;::15% grnal .. SIIIIdy fit clay with grawel
-----.. '" lind <% gr.vel --=:::::::::::<15'" lind .. Grnallv fat cliV
~15'" lind .. Gravelly fit clay with lind
<3O'lIo plUI No. 200 ~ <15'" plul No. 200 .. Elastic lilt < ~ 15·25% plul No. 200 ~ % lind;::'" gra"l-Elastic 'lit with send MH '" lind <'II. IIra"l-Elastic silt with gravel
'" lind ;;::'11. of grlvel ~ <15'" gravel .. SIndv alastic silt ~3O'lIo plus No. 200 ---------~15% gr."el .. Sandy .Iastic ,ilt with gravel
-----'" lind <% gr."e' ~ <15% lind .. Gr.".11y .Ianic lilt ~ ~15'" lind .. Gravelly .Iastic silt with sand
NOTE l-Percentages are based on estimating amounts of fines. sand, and gravel to the nearest 5 %.
FIG. 1a Flow Chart for Identifying Inorganic Fine-Grained Soil (50 % or more tines)
GROUP SYMBOL GROUP NAME
< <30% plus No. 200 -=::::::::::::: <15% plus No. 200 • Organic soil
15·25% plul No. 200 ~" sand~" IIr.",1 • OrganIC sotl with .. nd OL /OH ----" .. nd <" .rnel _ Organic soil with gra,.1
______ " IInd~" .ravll ~ <15% .r .. 11 .. Sandy 0rtl.nic soil ~30% plus No. 200 ___ ---~15'" IIr .. 11 .. Sandy or,lnic soli with .r .....
" lind <" Ilrawl' ~ <15'110 lind .. Grawelly organic soil
---~15'11o lind .. Gr.".lIy organic soil with lind
NOTE l-Percentages are based on estimating amounts of fines, sand, and gravel to the nearest 5 %.
FIG. 1 b Flow Chart for Identifying Organic Fine-Grained Soil (50 % or more fines)
6. Apparatus
6.1 Required Apparatus:
6.1.1 Pocket Knife or Small Spatula.
6.2 Useful Auxiliary Apparatus:
6.2.1 Test Tube and Stopper (or jar with a lid).
6.2.2 Hand Lens.
7. Reagents
7.1 Purity of Water-Unless otherwise indicated, references
to water shall be understood to mean water from a city water
supply or natural source, including non-potable water.
7.2 Hydrochloric Acid-A small bottle of dilute hydrochlo-
ric acid, Hel, one part Hel (10 N) to three parts water (This
reagent is optional for use with this practice). See Section 8.
8. Safety Precautions
8.1 When preparing the dilute Hel solution of one part
concentrated hydrochloric acid (IO N) to three parts of distilled
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water, slowly add acid into water following necessary safety
precautions. Handle with caution and store safely. If solution
comes into contact with the skin, rinse thoroughly with water.
8.2 Caution-Do not add water to acid.
9. Sampling
9.1 The sample shall be considered to be representative of
the stratum from which it was obtained by an appropriate,
accepted, or standard procedure.
NOTE 6---Preferably, the sampling procedure should be identified as
having been conducted in accordance with Practices 01452, 01587, or
02113, or Test Method 01586.
9.2 The sample shall be carefully identified as to origin.
NOTE 7-Remarks as to the origin may take the form of a boring
number and sample number in conjunction with a job number, a geologic
stratum, a pedologic horizon or a location description with respect to a
permanent monument, a grid system or a station number and offset with
respect to a stated centerline and a depth or elevation.
Joe Galemore (INTERA) pursuant to License Agreement. No further reproductions authorized.
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TABLE 3 Criteria for Describing Moisture Condition
Description
Dry
Moist
Wet
Criteria
Absence of moisture, dusty, dry to the touch
Damp but no visible water
Visible free water, usually soil is below water table
TABLE 4 Criteria for Describing the Reaction With HCI
10.14 A local or commercial name or a geologic interpre-
tation of the soil, or both, may be added if identified as such.
10.15 A classification or identification of the soil in accor-
dance with other classification systems may be added if
identified as such.
11. Identification of Peat
11.1 A sample composed primarily of vegetable tissue in Description Criteria --:------------------------various stages of decomposition that has a fibrous to amor-
WNOenaek No visible reaction phous texture, usuaIly a dark brown to black color, and an Some reaction, with bubbles forming slowly
Strong Violent reaction, with bubbles forming immediately organic odor, shaIl be designated as a highly organic soil and ~.......::..-----~---...:.---.:..;....---:::--~~----shall be identified as peat, PT, and not subjected to the
identification procedures described hereafter.
TABLE 5 Criteria for Describing Consistency
Description Criteria 12. Preparation for Identification
-ve-ry-s-Oft"";"'---T-h-um-b-w-ill-p-e-ne-tr-a-te-s-o-il-m-o-re-t-ha-n-1-in-. -(2-5-m-m-)-----12.1 The soil identification portion of this practice is based
Soft Thumb will penetrate soil about 1 in. (25 mm) on the portion of the soil sample that will pass a 3-in. (75-mm)
Firm Thumb will indent soil about '14 in. (6 mm) . Th I h 3' (75 ) . I b Hard Thumb will not indent soil but readily indented with thumbnail SIeve. e arger t an -Ill. -mm partiC es must e re-
Very hard Thumbnail will not indent soil moved, manuaIly, for a loose sample, or mentaIly, for an intact
-'-------------------------sample before classifying the soil.
Description
Weak
Moderate
Strong
TABLE 6 Criteria for Describing Cementation
Criteria
Crumbles or breaks with handling or linle finger pressure
Crumbles or breaks with considerable finger pressure
Will not crumble or break with finger pressure
TABLE 7 Criteria for Describing Structure
12.2 Estimate and note the percentage of cobbles and the
percentage of boulders. Performed visuaIly, these estimates
will be on the basis of volume percentage.
NOTE 9-Since the percentages of the particle-size distribution in Test
Method 02487 are by dry weight, and the estimates of percentages for
gravel, sand, and tines in this practice are by dry weight, it is recom-
mended that the report state that the percentages of cobbles and boulders
are by volume.
Description Criteria 12.3 Of the fraction of the soil smaIler than 3 in. (75 mm),
-------------------------estimate and note the percentage, by dry weight, of the gravel, Stratified Alternating layers of varying material or color with layers at
least 6 mm thick; note thickness sand, and fines (see Appendix X4 for suggested procedures).
Laminated Alternating layers of varying material or color with the
layers less than 6 mm thick; note thickness
Fissured Breaks along definite planes of fracture with linle
resistance to fracturing
Slickensided Fracture planes appear polished or glossy, sometimes
Blocky
Lensed
Homogeneous
striated
CoheSive soil that can be broken down into small angular
lumps which resist further breakdown
Inclusion of small pockets of different soils, such as small
lenses of sand scattered through a mass of clay; note
thickness
Same color and appearance throughout
mum particle size, 1112 in. (will pass a 1 Ih-in. square opening
but not a 3/4-in. square opening).
10.11.3 Cobble or Boulder Size-If the maximum particle
size is a cobble or boulder size, describe the maximum
dimension of the largest particle. For example: maximum
dimension, 18 in. (450 mm).
10.12 Hardness-Describe the hardness of coarse sand and
larger particles as hard, or state what happens when the
particles are hit by a hammer, for example, gravel-size particles
fracture with considerable hammer blow, some gravel-size
particles crumble with hammer blow. "Hard" means particles
do not crack, fracture, or crumble under a hammer blow.
10.13 Additional comments shaIl be noted, such as the
presence of roots or root holes, difficulty in drilling or augering
hole, caving of trench or hole, or the presence of mica.
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NOTE 10000Since the particle-size components appear visually on the
basis of volume, considerable experience is required to estimate the
percentages on the basis of dry weight. Frequent comparisons with
laboratory particle-size an alyses should be made.
12.3.1 The percentages shaIl be estimated to the closest 5 %.
The percentages of gravel, sand, and fines must add up to
100%.
12.3.2 If one of the components is present but not in
sufficient quantity to be considered 5 % of the smaller than
3-in. (75-mm) portion, indicate its presence by the term trace,
for example, trace of fines. A trace is not to be considered in the
total of 100 % for the components.
13. Preliminary Identification
13.1 The soil is fine grained if it contains 50 % or more
fines. FoIlow the procedures for identifying fine-grained soils
of Section 14.
13.2 The soil is coarse grained if it contains less than 50 %
fines. FoIlow the procedures for identifying coarse-grained
soils of Section 15.
14. Procedure for Identifying Fine-Grained Soils
14.1 Select a representative sample of the material for
examination. Remove particles larger than the No. 40 sieve
(medium sand and larger) until a specimen equivalent to about
a handful of material is available. Use this specimen for
performing the dry strength, dilatancy, and toughness tests.
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14.2 Dry Strength:
14.2.1 From the specimen, select enough material to mold
into a ball about I in. (25 mm) in diameter. Mold the material
until it has the consistency of putty, adding water if necessary.
14.2.2 From the molded material, make at least three test
specimens. A test specimen shall be a ball of material about 1/2
in. (12 mm) in diameter. Allow the test specimens to dry in air,
or sun, or by artificial means, as long as the temperature does
not exceed 60°C.
14.2.3 If the test specimen contains natural dry lumps, those
that are about 1/2 in. (12 mm) in diameter may be used in place
of the molded balls.
NOTE II-The process of molding and drying usually produces higher
strengths than are found in natural dry lumps of soil.
14.2.4 Test the strength of the dry balls or lumps by
crushing between the fingers. Note the strength as none, low,
medium, high, or very high in accorance with the criteria in
Table 8. If natural dry lumps are used, do not use the results of
any of the lumps that are found to contain particles of coarse
sand.
14.2.5 The presence of high-strength water-soluble cement-
ing materials, such as calcium carbonate, may cause excep-
tionally high dry strengths. The presence of calcium carbonate
can usually be detected from the intensity of the reaction with
dilute hydrochloric acid (see 10.6).
14.3 Dilatancy:
14.3.1 From the specimen, select enough material to mold
into a ball about V2 in. (12 mm) in diameter. Mold the material,
adding water if necessary, until it has a soft, but not sticky,
consistency.
14.3.2 Smooth the soil ball in the palm of one hand with the
blade of a knife or small spatula. Shake horizontally, striking
the side of the hand vigorously against the other hand several
times. Note the reaction of water appearing on the surface of
the soil. Squeeze the sample by closing the hand or pinching
the soil between the fingers, and note the reaction as none,
slow, or rapid in accordance with the criteria in Table 9. The
reaction is the speed with which water appears while shaking,
and disappears while squeezing.
14.4 Toughness:
14.4.1 Following the completion of the dilatancy test, the
test specimen is shaped into an elongated pat and rolled by
hand on a smooth surface or between the palms into a thread
about lis in. (3 mm) in diameter. (If the sample is too wet to roll
easily, it should be spread into a thin layer and allowed to lose
Description
None
Low
Medium
High
Very high
TABLE 8 Criteria for Describing Dry Strength
Criteria
The dry specimen crumbles into powder with mere pressure
of handling
The dry specimen crumbles into powder with some finger
pressure
The dry specimen breaks into pieces or crumbles with
considerable finger pressure
The dry specimen cannot be broken with finger pressure.
Specimen will break into pieces between thumb and a hard
surface
The dry specimen cannot be broken between the thumb and a
hard surface
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TABLE 9 Criteria for Describing Dilatancy
Description Criteria
None No Visible change in the specimen
Slow Water appears slowly on the surface of the specimen during
shaking and does not disappear or disappears slowly upon
squeezing
Rapid Water appears quickly on the surface of the specimen during
shaking and disappears quickly upon squeezing
some water by evaporation.) Fold the sample threads and reroll
repeatedly until the thread crumbles at a diameter of about lis
in. The thread will crumble at a diameter of lis in. when the soil
is near the plastic limit. Note the pressure required to roll the
thread near the plastic limit. Also, note the strength of the
thread. After the thread crumbles, the pieces should be lumped
together and kneaded until the lump crumbles. Note the
toughness of the material during kneading.
14.4.2 Describe the toughness of the thread and lump as
low, medium, or high in accordance with the criteria in Table
10.
14.5 Plasticity-On the basis of observations made during
the toughness test, describe the plasticity of the material in
accordance with the criteria given in Table 11.
14.6 Decide whether the soil is an inorganic or an organic
fine-grained soil (see 14.8). If inorganic, follow the steps given
in 14.7.
14.7 Identification of Inorganic Fine-Grained Soils:
14.7.1 Identify the soil as a lean clay, CL, if the soil has
medium to high dry strength, no or slow dilatancy, and medium
toughness and plasticity (see Table 12).
14.7.2 Identify the soil as a fat clay, CH, if the soil has high
to very high dry strength, no dilatancy, and high toughness and
plasticity (see Table 12).
14.7.3 Identify the soil as a silt, ML, if the soil has no to low
dry strength, slow to rapid dilatancy, and low toughness and
plasticity, or is nonplastic (see Table 12).
14.7.4 Identify the soil as an elastic silt, MH, if the soil has
low to medium dry strength, no to slow dilatancy, and low to
medium toughness and plasticity (see Table 12).
NOTE l2-These properties are similar to those for a lean clay.
However, the silt will dry quickly on the hand and have a smooth, silky
feel when dry. Some soils that would classify as MH in accordance with
the criteria in Test Method D2487 are visually difficult to distinguish from
lean clays, CL. It may be necessary to perform laboratory testing for
proper identification.
14.8 Identification of Organic Fine-Grained Soils:
14.8.1 Identify the soil as an organic soil, OLlOH, if the soil
contains enough organic particles to influence the soil proper-
ties. Organic soils usually have a dark brown to black color and
TABLE 10 Criteria for Describing Toughness
Description Criteria
Low Only slight pressure is required to roll the thread near the
plastic limit. The thread and the lump are weak and soft
Medium Medium pressure is required to roll the thread to near the
plastic limit. The thread and the lump have medium stiffness
High Considerable pressure is required to roll the thread to near the
plastic limit. The thread and the lump have very high
stiffness
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TABLE 11 Criteria for Describing Plasticity
Description Criteria
Nonplastic A 'la-in. (3-mm) thread cannot be rolled at any water content
low The thread can barely be rolled and the lump cannot be
formed when drier than the plastic limit
Medium The thread is easy to roll and not much time is required to
reach the plastic limit. The thread cannot be rerolled after
reaching the plastic limit. The lump crumbles when drier
than the plastic limit
High It takes considerable time rolling and kneading to reach the
TABLE 12
plastic limit. The thread can be rerolled several times after
reaching the plastic limit. The lump can be formed without
crumbling when drier than the plastic limit
15.3.2 Identify the soil as a poorly graded gravel, GP, or as
a poorly graded sand, SP, if it consists predominantly of one
size (uniformly graded), or it has a wide range of sizes with
some intermediate sizes obviously missing (gap or skip
graded).
15.4 The soil is either a gravel with fines or a sand with fines
if the percentage of fines is estimated to be 15 % or more.
15.4.1 Identify the soil as a clayey gravel, GC, or a clayey
sand, SC, if the fines are clayey as determined by the
procedures in Section 14.
15.4.2 Identify the soil as a silty gravel, GM, or a silty sand,
SM, if the fines are silty as determined by the procedures in
Section 14.
15.5 If the soil is estimated to contain 10 % fines, give the
-------------------------....,s""oil a dual identification using two group symbols.
Identification of Inorganic Fine-Grained Soils from
Manual Tests
Soil Dry Strength Dilatancy Toughness
15.5.1 The first group symbol shall correspond to a clean
------------------------gravel or sand (GW, GP, SW, SP) and the second symbol shall
Symbol and Plasticity
Ml None to low Slow to rapid low or thread cannot be
correspond to a gravel or sand with fines (GC, GM, SC, SM).
15.5.2 The group name shall correspond to the first group
symbol plus the words "with clay" or "with silt" to indicate the ------=--~---':....---------=:--------p..;.la li.city characteristics of the fines. For example: "weIl-
formed
Cl Medium to high None to slow Medium
MH low to medium None to slow low to medium
CH High to very high None High
may have an organic odor. Often, organic soils will change
color, for example, black to brown, when exposed to the air.
Some organic soils will lighten in color significantly when air
dried. Organic soils normally will not have a high toughness or
plasticity. The thread for the toughness test will be spongy.
NOTE 13-Jn some cases, through practice and experience, it may be
possible to further identify the organic soils as organic silts or organic
clays, OL or OH. Correlations between the dilatancy, dry strength,
toughness tests, and laboratory tests can be made to identify organic soils
in certain deposits of similar materials of known geologic origin.
14.9 If the soil is estimated to have 15 to 25 % sand or
gravel, or both, the words "with sand" or "with gravel"
(whichever is more predominant) shall be added to the group
name. For example: "lean clay with sand, CL" or "silt with
gravel, ML" (see Fig. l a and Fig. 1 b). If the percentage of sand
is equal to the percentage of gravel, use "with sand."
14.10 If the soil is estimated to have 30 % or more sand or
gravel, or both, the words "sandy" or "gravelly" shall be added
to the group name. Add the word "sandy" if there appears to be
more sand than gravel. Add the word "gravelly" if there
appears to be more gravel than sand. For example: "sandy lean
clay, CL", "gravelly fat clay, CR", or "sandy silt, ML" (see Fig.
l a and Fig. 1 b). If the percentage of sand is equal to the percent
of gravel, use "sandy."
15. Procedure for Identifying Coarse-Grained Soils
(Contains less than 50 % fines)
15.1 The soil is a gravel if the percentage of gravel is
estimated to be more than the percentage of sand.
15.2 The soil is a sand if the percentage of gravel is
estimated to be equal to or less than the percentage of sand.
15.3 The soil is a clean gravel or clean sand if the
percentage of fines is estimated to be 5 % or less.
15.3.1 Identify the soil as a well-graded gravel, GW, or as a
well-graded sand, SW, if it has a wide range of particle sizes
and substantial amounts of the intermediate particle sizes.
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graded gravel with clay, GW-GC" or "poorly graded sand with
silt, SP-SM" (see Fig. 2).
15.6 If the specimen is predominantly sand or gravel but
contains an estimated 15 % or more of the other coarse-grained
constituent, the words "with gravel" or "with sand" shall be
added to the group name. For example: "poorly graded gravel
with sand, GP" or "clayey sand with gravel, SC" (see Fig. 2).
15.7 If the field sample contains any cobbles or boulders, or
both, the words "with cobbles" or "with cobbles and boulders"
shall be added to the group name. For example: "silty gravel
with cobbles, GM."
16. Report
16.1 The report shall include the information as to origin,
and the items indicated in Table 13.
NOTE 14---Example: Clayey Gravel with Sand and Cobbles, GC-
About 50 % fine to coarse, subrounded to subangular gravel; about 30 %
fine to coarse, subrounded sand; about 20 % fines with medium plasticity,
high dry strength, no dilatancy, medium toughness; weak reaction with
HCl; original field sample had about 5 % (by volume) subrounded
cobbles, maximum dimension, 150 mm.
In-Place Conditions-Firm, homogeneous, dry, brown
Geologic Interpretation-Alluvial fan
NOTE IS-Other examples of soil descriptions and identification are
given in Appendix Xl and Appendix X2.
NOTE 16--If desired, the percentages of gravel, sand, and fines may be
stated in terms indicating a range of percentages, as follows:
Trace-Particles are present but estimated to be less than 5 %
Few-5 to 10 %
Little-IS to 25 %
Some-30 to 45 %
Mostly-50 to 100 %
16.2 If, in the soil description, the soil is identified using a
classification group symbol and name as described in Test
Method D2487, it must be distinctly and clearly stated in log
forms, summary tables, reports, and the like, that the symbol
and name are based on visual-manual procedures.
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TABLE 13 Checklist for Description of Soils
1. Group name
2. Group symbol
3. Percent of cobbles or boulders, or both (by volume)
4. Percent of gravel, sand, or fines, or ali three (by dry weight)
5. Particle-size range:
Gravel-fine, coarse
Sand-fine, medium, coarse
6. Particle angularity: angular, subangular, subrounded, rounded
7. Particle shape: (if appropriate) flat, elongated, flat and elongated
B. Maximum particle size or dimension
9. Hardness of coarse sand and larger particles
10. Plasticity of fines: nonplastic, low, medium, high
11. Dry strength: none, low, medium, high, very high
12. Dilatancy: none, slow, rapid
13. Toughness: low, medium, high
14. Color (in moist condition)
15. Odor (mention only if organic or unusual)
16. Moisture: dry, moist, wet
17. Reaction with HCI: none, weak, strong
For intact samples:
1 B. Consistency (fine-grained soils only): very soft, 50ft, firm, hard, very hard
19. Structure: stratified, laminated, fissured, slickensided, lensed, homo-
geneous
20. Cementation: weak, moderate, strong
21 . Local name
22. Geologic interpretation
23. Additional comments: presence of roots or root holes, presence of mica,
gypsum, etc., surface coatings on coarse-grained particles, caving or
sloughing of auger hole or trench sides, difficulty in augering or excavating,
etc.
17. Precision and Bias
17.1 This practice provides qualitative information only,
therefore, a precision and bias statement is not applicable.
18. Keywords
18.1 classification; clay; gravel; organic soils; sand; silt; soil
classification; soil description; visual classification
APPENDIXES
(Nonmandatory Information)
Xl. EXAMPLES OF VISUAL SOIL DESCRIPTIONS
Xl.l The following examples show how the information
required in 16.1 can be reported. The information that is
included in descriptions should be based on individual circum-
stances and need.
XU.l Well-Graded Gravel with Sand (GW)-About 75 %
fine to coarse, hard, subangular gravel; about 25 % fine to
coarse, hard, subangular sand; trace of fines; maximum size, 75
mm, brown, dry; no reaction with Hei.
Xl.1.2 Silty Sand with Gravel (SM)-About 60 % predomi-
nantly fine sand; about 25 % silty fines with low plasticity, low
dry strength, rapid dilatancy, and low toughness; about 15 %
fine, hard, subrounded gravel, a few gravel-size particles
fractured with hammer blow; maximum size, 25 mm; no
reaction with Hel (Note-Field sample size smaller than
recommended).
In-Place Conditions-Firm, stratified and contains lenses of
silt 1 to 2 in. (25 to 50 mm) thick, moist, brown to gray;
in-place density 106 Ib/ft3; in-place moisture 9 %.
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Xl.l.3 Organic Soil (OUOH)-About 100 % fines with
low plasticity, slow dilatancy, low dry strength, and low
toughness; wet, dark brown, organic odor; weak reaction with
Hei.
Xl.1.4 Silty Sand with Organic Fines (SM)-About 75 %
fine to coarse, hard, sub angular reddish sand; about 25 %
organic and silty dark brown nonplastic fines with no dry
strength and slow dilatancy; wet; maximum size, coarse sand;
weak reaction with Hei.
Xl.1.5 Poorly Graded Gravel with Silt, Sand, Cobbles and
Boulders (GP-GM)-About 75 % fine to coarse, hard, sub-
rounded to subangular gravel; about 15 % fine, hard, sub-
rounded to subangular sand; about 10 % silty nonplastic fines;
moist, brown; no reaction with Hel; original field sample had
about 5 % (by volume) hard, subrounded cobbles and a trace of
hard, subrounded boulders, with a maximum dimension of 18
in. (450 mm).
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X2. USING THE IDENTIFICATION PROCEDURE AS A DESCRIPTIVE SYSTEM FOR SHALE, CLAYSTONE,
SHELLS, SLAG, CRUSHED ROCK, AND THE LIKE
X2.1 The identification procedure may be used as a
descriptive system applied to materials that exist in-situ as
shale, claystone, sandstone, siltstone, mudstone, etc., but con-
vert to soils after field or laboratory processing (crushing,
slaking, and the like).
X2.2 Materials such as shells, crushed rock, slag, and the
like, should be identified as such. However, the procedures
used in this practice for describing the particle size and
plasticity characteristics may be used in the description of the
material. If desired, an identification using a group name and
symbol according to this practice may be assigned to aid in
describing the material.
X2.3 The group symbol(s) and group names should be
placed in quotation marks or noted with some type of distin-
guishing symbol. See examples.
X2.4 Examples of how group names and symbols can be
incororated into a descriptive system for materials that are not
naturally occurring soils are as follows:
X2.4.1 Shale Chunks-Retrieved as 2 to 4-in. (50 to 100-
mm) pieces of shale from power auger hole, dry, brown, no
reaction with HCI. After slaking in water for 24 h, material
identified as "Sandy Lean Clay (CL)"; about 60 % fines with
medium plasticity, high dry strength, no dilatancy, and medium
toughness; about 35 % fine to medium, hard sand; about 5 %
gravel-size pieces of shale.
X2.4.2 Crushed Sandstone-Product of commercial crush-
ing operation; "Poorly Graded Sand with Silt (SP-SM)"; about
90 % fine to medium sand; about 10 % nonplastic fines; dry,
reddish-brown.
X2.4.3 Broken Shells-About 60 % uniformly graded
gravel-size broken shells; about 30 % sand and sand-size shell
pieces; about 10 % nonplastic fines; "Poorly Graded Gravel
with Silt and Sand (GP-GM)."
X2.4.4 Crushed Rock-Processed from gravel and cobbles
in Pit No.7; "Poorly Graded Gravel (GP)"; about 90 % fine,
hard, angular gravel-size particles; about 10 % coarse, hard,
angular sand-size particles; dry, tan; no reaction with HCI.
X3. SUGGESTED PROCEDURE FOR USING A BORDERLINE SYMBOL FOR SOILS WITH TWO POSSIBLE
IDENTIFICATIONS.
X3.1 Since this practice is based on estimates of particle
size distribution and plasticity characteristics, it may be diffi-
cult to clearly identify the soil as belonging to one category. To
indicate that the soil may fall into one of two possible basic
groups, a borderline symbol may be used with the two symbols
separated by a slash. For example: SC/CL or CLiCH.
X3.1.1 A borderline symbol may be used when the percent-
age of fines is estimated to be between 45 and 55 %. One
symbol should be for a coarse-grained soil with fines and the
other for a fine-grained soil. For example: GMlML or CLiSC.
X3.1.2 A borderline symbol may be used when the percent-
age of sand and the percentage of gravel are estimated to be
about the same. For example: GP/SP, SC/GC, GMiSM. It is
practically impossible to have a soil that would have a
borderline symbol of GW/SW.
X3.1.3 A borderline symbol may be used when the soil
could be either well graded or poorly graded. For example:
GW IGP, SW ISP.
X3.1.4 A borderline symbol may be used when the soil
could either be a silt or a clay. For example: CLIML, CHIMH,
SCISM.
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X3.1.5 A borderline symbol may be used when a fine-
grained soil has properties that indicate that it is at the
boundary between a soil of low compressibility and a soil of
high compressibility. For example: CLlCH, MHIML.
X3.2 The order of the borderline symbols should reflect
similarity to surrounding or adjacent soils. For example: soils
in a borrow area have been identified as CH. One sample is
considered to have a borderline symbol of CL and CH. To
show similarity, the borderline symbol should be CH/CL.
X3.3 The group name for a soil with a borderline symbol
should be the group name for the first symbol, except for:
CLiCH lean to fat clay
MLlCL clayey silt
CLIML silty clay
X3.4 The use of a borderline symbol should not be used
indiscriminately. Every effort shall be made to first place the
soil into a single group.
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X4. SUGGESTED PROCEDURES FOR ESTIMATING THE PERCENTAGES OF GRAVEL, SAND,
AND FINES IN A SOIL SAMPLE
X4.1 Jar Method-The relative percentage of coarse-and
fine-grained material may be estimated by thoroughly shaking
a mixture of soil and water in a test tube or jar, and then
allowing the mixture to settle. The coarse particles will fall to
the bottom and successively finer particles will be deposited
with increasing time; the sand sizes will fall out of suspension
in 20 to 30 s. The relative proportions can be estimated from
the relative volume of each size separate. This method should
be correlated to particle-size laboratory determinations.
The percentages of sand and fines in the minus sieve size No.
4 material can then be estimated from the wash test (X4.3).
X4.2 Visual Method-Mentally visualize the gravel size
particles placed in a sack (or other container) or sacks. Then,
do the same with the sand size particles and the fines. Then,
mentally compare the number of sacks to estimate the percent-
age of plus No.4 sieve size and minus No.4 sieve size present.
X4.3 Wash Test (for relative percentages of sand and
fines)-Select and moisten enough minus No.4 sieve size
material to form a I-in (2S-mm) cube of soil. Cut the cube in
half, set one-half to the side, and place the other half in a small
dish. Wash and decant the fines out of the material in the dish
until the wash water is clear and then compare the two samples
and estimate the percentage of sand and fines. Remember that
the percentage is based on weight, not volume. However, the
volume comparison will provide a reasonable indication of
grain size percentages.
X4.3.1 While washing, it may be necessary to break down
lumps of fines with the finger to get the correct percentages.
XS. ABBREVIATED SOIL CLASSIFICATION SYMBOLS
XS.l In some cases, because of lack of space, an abbrevi-
ated system may be useful to indicate the soil classification
symbol and name. Examples of such cases would be graphical
logs, databases, tables, etc.
Prefix:
s = sandy
g = gravelly
Suffix:
s = with sand
g = with gravel
c = with cobbles
b = with boulders
XS.2 This abbreviated system is not a substitute for the full
name and descriptive information but can be used in supple-
mentary presentations when the complete description is refer-
enced.
XS.4 The soil classification symbol is to be enclosed in
parenthesis. Some examples would be:
XS.3 The abbreviated system should consist of the soil
classification symbol based on this standard with appropriate
lower case letter prefixes and suffixes as:
Group Symbol and Full Name
Cl, Sandy lean clay
SP-SM, Poorly graded sand with slit and gravel
GP, poorly graded gravel with sand, cobbles, and
boulders
Ml, gravelly silt with sand and cobbles
SUMMARY OF CHANGES
Abbreviated
s(Cl)
(SP-SM)g
(GP)scb
g(Ml)sc
Committee D 18 has identified the location of selected changes to this standard since the last issue
(D2488 -09) that may impact the use of this standard, (Approved June IS, 2009.)
(1) Revised Section 1.2.3.
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Appendix B
EPA Method 1312
METHOD 1312
SYNTHETIC PRECIP ITATION LE ACHING PRO CEDURE
1.0 SCOPE AND APPLICATION
1.1 Method 1312 is designed to determine the mobility of both organic
and inorganic analytes present in liquids. soils. and wastes.
2.0 SUMMARY OF METHOD
2.1 For liquid samples (~. those containing less than 0.5 % dry
solid material). the sample. after filtration through a 0.6 to 0.8 pm glass fiber
filter. is defined as the 1312 extract.
2.2 For samples containing greater than 0.5 % solids. the liquid phase.
if any. is separated from the solid phase and stored for later analysis; the
particle size of the solid phase is reduced. if necessary. The solid phase is
extracted with an amount of extraction fluid equal to 20 times the weight of the
solid phase. The extraction fluid employed is a function of the region of the
country where the sample site is located if the sample is a soil. If the sample
is a waste or wastewater. the extraction fluid employed is a pH 4.2 solution.
A special extractor vessel is used when testing for volatile analytes (see Table
1 for a list of volatile compounds). Following extraction. the liquid extract
i s separated from the so l id phase by filtration through a 0.6 to 0.8 pm glass
fiber filter.
2.3 If compatible (~. multiple phases will not form on combination).
the initial liquid phase of the waste is added to the liquid extract. and these
are analyzed together. If incompatible. the liquids are analyzed separately and
the results are mathematically combined to yield a volume-weighted average
concentration.
3.0 INTERFERENCES
3.1 Potential interferences that may be encountered during analysis are
discussed in the individual analytical methods.
4.0 APPARATUS AND MATERIALS
4.1 Agitation apparatus: The agitation apparatus must be capable of
rotating the extraction vessel in an end-over-end fashion (s ee Figure 1) at 30
± 2 rpm. Suitable devices known to EPA are identified in Table 2.
CD-ROM
4.2 Extraction Vessels
4.2.1 Zero Headspace Extraction Vessel (ZHE). This device is for
use only when the sample is being tested for the mobility of volatile
analytes (~. those listed in Table 1). The ZHE (depicted in Figure 2)
allows for liquid/solid separation within the dev i ce and effectively
precludes headspace. This type of vessel allows for initial liquid/solid
1312 - 1 Revision 0
September 1994
in Step 4.2.1 is used for filtration. The device shall be capable of
supporting and keeping in place the glass fiber filter and be able to
withstand the pressure needed to accomplish separation (50 psig).
NOTE: When it is 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 sample is evaluated for other than
volatile analytes, a filter holder capable of supporting a glass fiber
filter and able to withstand the pressure needed to accomplish separation
may be used. Suitable filter holders range from simple vacuum units to
relatively complex systems capable of exerting pressures of up to 50 psig
or more. The type of filter holder used depends on the properties of the
material to be filtered (see Step 4.3.3). These devices shall have a
minimum internal volume of 300 mL and be equipped to accommodate a minimum
filter size of 47 mm (filter holders having an internal capacity of 1.5 L
or greater, and equipped to accommodate a 142 mm diameter filter, are
recommended). Vacuum filtration can only be used for wastes with low
solids content «10 %) and for highly granular, liquid-containing wastes.
All other types of wastes should be filtered using positive pressure
filtration. Suitable filter holders known to EPA are listed in Table 4.
4.3.3 Materials of Construction: Extraction vessels and
filtration devices shall be made of inert materials which will not leach
or absorb sample components of interest. Glass, polytetrafluoroethylene
(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 (HOPE), polypropylene (PP), or polyvinyl
chloride (PVC) may be used only when evaluating the mobility of me t als.
Borosilicate glass bottles are recommended for use over other types of
glass bottles, especially when inorganics are analytes of concern.
4.4 Filters: Filters shall be made of borosilicate glass fiber, shall
contain no binder materials, and shall have an effective pore size of 0.6 to
0.8 -~m. Filters known to EPA which meet these specifications are identified in
Table 5. Pre-filters must not be used. When evaluating the mobility of metals,
filters shall be acid-washed prior to use by rinsing with 1N nitric acid followed
by three consecutive rinses with reagent water (a minimum of 1-L per rinse is
recommended). Glass fiber filters are fragile and should be handled with care.
4.5 pH Meters: The meter should be accurate to ± 0.05 units at 25°C.
4.6 ZHE Extract Collection Devices: TEDLAR®2 bags or glass, stainless
steel or PTFE gas-tight syringes are used to collect the initial liquid phase and
the final extract when using the ZHE device. These devices listed are
recommended for use under the following conditions:
2TEDLAR® is a registered trademark of Du Pont.
CD-ROM 1312 - 3 Revision 0
September 1994
4.6.1 If a waste contains an aqueous liquid phase or if a waste
does not contain a significant amount of nonaqueous liquid (~, <1 % of
total waste), the TEDLAR® bag or a 600 mL syringe should be used to collect
and combine the initial liquid and solid extract.
4.6.2 If a waste contains a significant amount of nonaqueous
liquid in the initial liquid phase (~, >1 % of total waste), the
syringe or the TEDLAR® bag may be used for both the initial solid/liquid
separation and the final extract filtration. However, analysts should use
one or the other, not both.
4.6.3 If the waste contains no initial liquid phase (is 100 %
solid) or has no significant solid phase (is <0.5% solid) , either the
TEDLAR® bag or the syringe may be used. If the syringe is used. discard
the first 5 mL of liquid expressed from the device. The remaining
aliquots are used for analysis.
4.7 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 acceptable (~, a positive displacement or peristaltic
pump, a gas-tight syringe. pressure filtration unit (see Step 4.3.2), or other
ZHE device).
4.8 Laboratory Balance: Any laboratory balance accurate to within ±
0.01 grams may be used (all weight measurements are to be within ± 0.1 grams).
4.9 Beaker or Erlenmeyer flask, glass, 500 mL.
4.10 Watchglass, appropriate diameter to cover beaker or Erlenmeyer
flask .
4.11 Magnetic stirrer.
5.0 REAGENTS
5.1 Reagent grade chemicals shall be used in all tests. Unless
otherwise indicated. it is intended that all reagents shall conform to the
specifications of the Committee on Analytical Reagents of the American Chemical
Society, where such specifications are available. Other grades may be used,
provided it is first ascertained that the reagent is of sufficiently high purity
to permit its use without lessening the accuracy of the determination.
5.2 Reagent Water. Reagent water is defined as water in which an
interferant is not observed at or above the method's detection limit of the
analyte(s) of interest. For nonvolatile extractions, ASTM Type II water or
equivalent meets the definition of reagent water. For volatile extractions, it
is recommended that reagent water be generated by any of the following methods.
Reagent water should be monitored periodically for impurities.
CD -ROM
5.2.1 Reagent water for volatile extractions may be generated
by passing tap water through a carbon filter bed containing about 500
grams of activated carbon (Calgon Corp., Filtrasorb-300 or equivalent).
1312 - 4 Revision 0
September 1994
5.2.2 A water purification system (Millipore Super-Q or
equivalent) may also be used to generate reagent water for volatile
extractions.
5.2.3 Reagent water for volatile extractions may also be prepared
by boiling water for 15 minutes. Subsequently, while maintaining the
water temperature at 90 ± 5 degrees C, bubble a contaminant-free inert gas
(~. 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.
5.3 Sulfuric acid/nitric acid (60/40 weight percent mixture) H2S04/HN03 •
Cautiously mix 60 g of concentrated sulfuric acid with 40 g of concentrated
nitric acid. If preferred, a more dilute H2S04/HN~ acid mixture may be prepared
and used in steps 5.4.1 and 5.4.2 making it easier to adjust the pH of the
extraction fluids.
5.4 Extraction fluids.
5.4.1 Extraction fluid #1: This fluid is made by adding the
60/40 weight percent mixture of sulfuric and nitric acids (or a suitable
dilution) to reagent water (Step 5.2) until the pH is 4.20 ± 0.05. The
fluid is used to determine the leachability of soil from a site that is
east of the Mississippi River, and the leachability of wastes and
wastewaters.
NOTE : Solutions are unbuffered and exact pH may not be attained .
5.4.2 Extraction fluid #2: This fluid is made by adding the
60/40 weight percent mixture of sulfuric and nitric acids (or a suitable
dilution) to reagent water (Step 5.2) until the pH is 5.00 ± 0.05. The
fluid is used to determine the leachability of soil from a site that is
west of the Mississippi River.
5.4.3 Extraction fluid #3: This fluid is reagent water (Step
5.2) and is used to determine cyanide and volatiles leachability.
NOTE: These extraction fluids should be monitored frequently for
impurities. The pH should be checked prior to use to ensure that
these fluids are made up accurately. If impurities are found or
the pH is not within the above specifications, the fluid shall be
discarded and fresh extraction fluid prepared.
5.5 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 There may be requirements on the minimal size of the field sample
depending upon the physical state or states of the waste and the analytes of
concern. An aliquot is needed for the preliminary evaluations of the percent
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solids and the particle size. An aliquot may be needed to conduct the
nonvolatile analyte extraction procedure. If volatile organics are of concern.
another aliquot may be needed. Quality control measures may require additional
aliquots. Further. it is always wise to collect more sample just in case
something goes wrong with the initial attempt to conduct the test.
6.3 Preservatives shall not be added to samples before extraction.
6.4 Samples may be refrigerated unless refrigeration results in
irreversible physical change to the waste. If precipitation occurs. the entire
sample (including precipitate) should be extracted.
6.5 When the sample is to be evaluated for volatile analytes. care
shall be taken to minimize the loss of volatiles. Samples shall be collected and
stored in a manner intended to prevent the loss of volatile analytes (~.
samples should be collected in Teflon-lined septum capped vials and stored at
4°C. Samples should be opened only immediately prior to extraction).
6.6 1312 extracts should be prepared for analysis and analyzed as soon
as possible following extraction. Extracts or portions of extracts for metallic
analyte determinations must be acidified with nitric acid to a pH < 2. unless
precipitation occurs (see Step 7.2.14 if precipitation occurs). Extracts should
be preserved for other analytes according to the guidance given in the individual
analysis methods. Extracts or portions of extracts for organic analyte
determinations shall not be allowed to come into contact with the atmosphere
(.L..h. no headspace) to prevent losses. See Step 8.0 (Quality Control) for
acceptable sample and extract holding times.
7.0 PROCEDURE
7.1 Preliminary Evaluations
Perform preliminary 1312 evaluations on a minimum 100 gram aliquot of
sample. This aliquot may not actually undergo 1312 extraction. These
preliminary evaluations include: (1) determination of the percent solids (Step
7.1.1); (2) determination of whether the waste contains insignificant solids and
is. therefore. its own extract after filtration (Step 7.1.2); and (3)
determination of whether the solid portion of the waste requires particle size
reduction (Step 7.1.3).
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7.1.1 Preliminary determination of percent solids: Percent
solids is defined as that fraction of a waste sample (as a percentage of
the total sample) from which no liquid may be forced out by an applied
pressure. as described below.
7.1.1.1 If the sample will obviously yield no free
liquid when subjected to pressure filtration (~, is 100% solid),
weigh out a representative subsample (100 g minimum) and proceed
to Step 7.1.3.
7.1.1.2 If the sample is liquid or multiphasic.
liquid/solid separation to make a preliminary determination of
percent solids is required. This involves the filtration device
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discussed in Step 4.3.2, and is outlined in Steps 7.1.1.3 through
7.1.1.9.
7.1.1.3 Pre-weigh the filter and the container that will
receive the filtrate.
7.1.1.4 Assemble filter holder and filter following the
manufacturer's instructions. Place the filter on the support
screen and secure.
7.1.1.5 Weigh out a subsample of the waste (100 gram
minimum) and record the weight.
7.1.1.6 Allow slurries to stand to permit the solid phase
to settle. Samples that settle slowly may be centrifuged prior to
filtration. Centrifugation is to be used only as an aid to
filtration. If used, the liquid should be decanted and filtered
followed by filtration of the solid portion of the waste through
the same filtration system.
7.1.1.7 Quantitatively transfer the sample to the filter
holder (liquid and solid phases). Spread the sample evenly over
the surface of the filter. If filtration of the waste at 4QC
reduces the amount of expressed liquid over what would be expressed
at room temperature, then allow the sample to warm up to room
temperature in the device before filtering.
Gradually apply vacuum or gentle pressure of 1-10 psig,
until air or pressurizing gas moves through the filter. If this
point is not reached under 10 psig, and if no additional liquid has
passed through the filter in any 2-minute interval, slowly increase
the pressure in 10 psig increments to a maximum of 50 psig. After
each incremental increase of 10 psig, if the pressuri zing gas has
not moved through the filter, and if no additional liquid has
passed through the filter in any 2-minute interval, proceed to the
next 10-psig increment. When the pressurizing gas begins to move
through the filter, or when liquid flow has ceased at 50 psig
(~, filtration does not result in any additional filtrate within
any 2-minute period), stop the filtration .
.tillI.E.: If sample material (>1 % of original sample weight) has
obviously adhered to the container used to transfer the sample to
the filtration apparatus, determine the weight of this residue and
subtract it from the sample weight determined in Step 7.1.1.5 to
determine the weight of the sample that will be filtered.
NOTE: Instantaneous application of high pressure can degrade the
glass fiber filter and may cause premature plugging.
7.1.1.8 The material in the filter holder is defined as
the solid phase of the sample, and the filtrate is defined as the
liquid phase.
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NOTE: Some samples, such as oily wastes and some paint wastes,
will obviously contain some material that appears to be a liquid,
but even after applying vacuum or pressure filtration, as outlined
in Step 7.1.1.7, this material may not filter. If this is the
case, the material within the filtration device is defined as a
solid. Do not replace the original filter with a fresh filter
under any circumstances. Use only one filter.
7.1.1.9 Determi ne the wei ght of the 1 i qui d phase by
subtracting the weight of the filtrate container (see Step 7.1.1.3)
from the total weight of the filtrate-filled container. Determine
the weight of the solid phase of the sample by subtracting the
weight of the liquid phase from the weight of the total sample, as
determined in Step 7.1.1.5 or 7.1.1.7.
Record the weight of the liquid and solid phases.
Calculate the percent solids as follows:
Weight of solid (Step 7.1.1.9)
Percent solids x 100
Total weight of waste (Step 7.1.1.5 or 7.1.1.7)
7.1.2 If the percent solids determined in Step 7.1.1.9 is equal
to or greater than 0.5%, then proceed either to Step 7.1.3 to determine
whether the solid material requires particle size reduction or to Step
7.1.2.1 if it is noticed that a small amount of the filtrate is entrained
in wetting of the fi lter. If the percent sol ids determi ned inStep
7.1.1.9 is less than 0.5%, then proceed to Step 7.2.9 if the nonvolatile
1312 analysis is to be performed, and to Step 7.3 with a fresh portion of
the waste if the volatile 1312 analysis is to be performed.
7.1.2.1 Remove the sol i d phase and fi 1 ter from the
filtration apparatus.
7.1.2.2 Dry the filter and solid phase at 100 ± 20°C
until two successive weighings yield the same value within ± 1 %.
Record the final weight.
Caution: The drying oven should be vented to a hood or other
appropriate device to eliminate the possibility of fumes from the
sample escaping into the laboratory. Care should be taken to
ensure that the sample will not flash or violently react upon
heating.
7.1.2.3 Calculate the percent dry solids as follows:
Percent
dry solids
(Weight of dry sample + filter) -tared weight of filter
x 100
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Initial weight of sample (Step 7.1.1.5 or 7.1.1.7)
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7.1.2.4 If the percent dry solids is less than 0.5%.
then proceed to Step 7.2.9 if the nonvolatile 1312 analysis is to
be performed. and to Step 7.3 if the volatile 1312 analysis is to
be performed. If the percent dry solids is greater than or equal
to 0.5%. and if the nonvolatile 1312 analysis is to be performed.
return to the begi nni ng of thi s Step (7.1) and. wi th a fresh
portion of sample. determine whether particle size reduction is
necessary (Step 7.1.3).
7.1.3 Determination of whether the sample requires particle-size
reduction (particle-size is reduced during this step): Using the solid
portion of the sample. evaluate the solid for particle size. Particle-
size reduction is required. unless the solid has a surface area per gram
of material equal to or greater than 3.1 cmz• or is smaller than 1 cm in
its narrowest dimension (hL. is capable of passing through a 9.5 mm
(0.375 inch) standard sieve). If the surface area is smaller or the
particle size larger than described above. prepare the solid portion of
the sample for extraction by crushing. cutting. or grinding the waste to
a surface area or particle size as described above. If the solids are
prepared for organic volatiles extraction. special precautions must be
taken (see Step 7.3.6).
NOTE: Surface area criteria are meant for filamentous (~.
paper. cloth. and similar) waste materials. Actual measurement of
surface area is not required. nor is it recommended. For materials
that do not obviously meet the criteria. sample-specific methods
woul d need to be developed and employed to measure the surface
area. Such methodology is currently not available.
7.1.4 Determination of appropriate extraction fluid:
7.1.4.1 For soils. if the sample is from a site that is
east of the Mississippi River. extraction fluid #1 should be used.
If the sample is from a site that is west of the Mississippi River.
extraction fluid #2 should be used.
7.1.4.2
should be used.
For wastes and wastewater. extraction fluid #1
7.1.4.3 For cyanide-containing wastes and/or soils.
extraction fluid #3 (reagent water) must be used because leaching
of cyanide-containing samples under acidic conditions may result
in the formation of hydrogen cyanide gas.
7.1.5 If the aliquot of the sample used for the preliminary
evaluation (Steps 7.1.1 -7.1.4) was determined to be 100% solid at Step
7.1.1.1. then it can be used for the Step 7.2 extraction (assuming at
least 100 grams remain). and the Step 7.3 extraction (assuming at least 25
grams remain). If the aliquot was subjected to the procedure in Step
7.1.1.7. then another aliquot shall be used for the volatile extraction
procedure in Step 7.3. The aliquot of the waste subjected to the
procedure in Step 7.1.1.7 might be appropriate for use for the Step 7.2
extraction if an adequate amount of solid (as determined by Step 7.1.1.9)
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was obtained. The amount of solid necessary is dependent upon whether a
sufficient amount of extract will be produced to support the analyses. If
an adequate amount of solid remains, proceed to Step 7.2.10 of the
nonvolatile 1312 extraction.
7.2 Procedure When Volatiles Are Not Involved
A minimum sample size of 100 grams (solid and liquid phases) is
recommended. In some cases, a larger sample size may be appropriate, depending
on the solids content of the waste sample (percent solids, See Step 7.l.1),
whether the initial liquid phase of the waste will be miscible with the aqueous
extract of the solid, and whether inorganics, semivolatile organics, pesticides.
and herbicides are all analytes of concern. Enough solids should be generated
for extraction such that the volume of 1312 extract will be sufficient to support
all of the analyses required. If the amount of extract generated by a single
1312 extraction will not be sufficient to perform all of the analyses. more than
one extraction may be performed and the extracts from each combined and aliquoted
for analysis.
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7.2.1 If the sample will obviously yield no liquid when subjected
to pressure filtration (~, is 100 % solid. see Step 7.1.1), weigh out
a subsample of the sample (100 gram minimum) and proceed to Step 7.2.9.
7.2.2 If the sample is liquid or multiphasic. liquid/solid
separation is required. This involves the filtration device described in
Step 4.3.2 and is outlined in Steps 7.2.3 to 7.2.8.
7.2.3 Pre-weigh the container that will receive the filtrate.
7.2.4 Assemble the filter holder and filter following the
manufacturer's instructions. Place the filter on the support screen and
secure. Acid wash the filter if evaluating the mobility of metals (see
Step 4.4).
NOTE: Acid washed filters may be used for all nonvolatile
extractions even when metals are not of concern.
7.2.5 Weigh out a subsample of the sample (100 gram minimum) and
record the weight. If the waste contains <0.5 % dry solids (Step 7.1.2),
the liquid portion of the waste. after filtration. is defined as the 1312
extract. Therefore. enough of the sample should be filtered so that the
amount of filtered liquid will support all of the analyses required of the
1312 extract. For wastes containing >0.5 % dry solids (Steps 7.1.1 or
7.1.2), use the percent solids information obtained in Step 7.1.1 to
determine the optimum sample size (100 gram minimum) for filtration.
Enough solids should be generated by filtration to support the analyses to
be performed on the 1312 extract.
7.2.6 Allow slurries to stand to permit the solid phase to settle.
Samples that settle slowly may be centrifuged prior to filtration. Use
centrifugation only as an aid to filtration. If the sample is
centrifuged. the liquid should be decanted and filtered followed by
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filtration of the solid portion of the waste through the same filtration
system.
7.2.7 Quantitatively transfer the sample (liquid and solid phases)
to the filter holder (see Step 4.3.2). Spread the waste sample evenly
over the surface of the filter. If filtration of the waste at 4°C reduces
the amount of expressed 1 i qui d over what woul d be expressed at room
temperature, then allow the sample to warm up to room temperature in the
device before filtering.
Gradually apply vacuum or gentle pressure of 1-10 psig, until air
or pressurizing gas moves through the filter. If this point if not
reached under 10 psig, and if no additional liquid has passed through the
filter in any 2-minute interval, slowly increase the pressure in 10-psig
increments to maximum of 50 psig. After each incremental increase of 10
psig, if the pressurizing gas has not moved through the filter, and if no
additional liquid has passed through the filter in any 2-minute interval,
proceed to the next 10-psig increment. When the pressurizing gas begins
to move through the filter, or when the liquid flow has ceased at 50 psig
(~, filtration does not result in any additional filtrate within a
2-minute period), stop the filtration.
NOTE: If waste material (>1 % of the original sample weight) has
obviously adhered to the container used to transfer the sample to
the filtration apparatus, determine the weight of this residue and
subtract it from the sample weight determined in Step 7.2.5, to
determine the weight of the waste sample that will be filtered.
NOTE:Instantaneous application of high pressure can degrade the
glass fiber filter and may cause premature plugging.
7.2.8 The material in the filter holder is defined as the solid
phase of the sampl e, and the fi 1 trate is defi ned as the 1 i qui d phase.
Weigh the filtrate. The liquid phase may now be either analyzed (see Step
7.2.12) or stored at 4°C until time of analysis.
NOTE: Some wastes, such as oily wastes and some paint wastes, will
obviously contain some material which appears to be a liquid. Even
after applying vacuum or pressure filtration, as outlined in Step
7.2.7, this material may not filter. If this is the case, the
material within the filtration device is defined as a solid, and
is carried through the extraction as a solid. Do not replace the
original filter with a fresh filter under any circumstances. Use
only one filter.
7.2.9 If the sample contains <0.5% dry solids (see Step 7.1.2),
proceed to Step 7.2.13. If the sample contains >0.5 % dry solids (see
Step 7.1.1 or 7.1.2), and if particle-size reduction of the solid was
needed in Step 7.1.3, proceed to Step 7.2.10. If the sample as received
passes a 9.5 mm sieve, quantitatively transfer the solid material into the
extractor bottle along with the filter used to separate the initial liquid
from the solid phase, and proceed to Step 7.2.11.
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7.2.10 Prepare the solid portion of the sample for extraction by
crushing, cutting, or grinding the waste to a surface area or particle-
size as described in Step 7.1.3. When the surface area or particle-size
has been appropriately altered, quantitatively transfer the solid material
into an extractor bottle. Include the filter used to separate the initial
liquid from the solid phase.
NOTE: Sieving of the waste is not normally required. Surface area
requirements are meant for filamentous (~. paper, cloth) and
similar waste materials. Actual measurement of surface area is not
recommended. If sieving is necessary, a Teflon-coated sieve should
be used to avoid contamination of the sample.
7.2.11 Determi ne the amount of extraction fl ui d to add to the
extractor vessel as follows:
20 x % solids (Step 7.1.1) x weight of waste
filtered (Step 7.2.5 or 7.2.7)
Weight of
extraction fluid
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Slowly add this amount of appropriate extraction fluid (see Step
7.1.4) to the extractor vessel. Close the extractor bottle tightly (it is
recommended that Teflon tape be used to ensure a tight seal), secure in
rota ry extractor devi ce, and rotate at 30 ± 2 rpm for 18 ± 2 hours.
Ambient temperature (~, temperature of room in which extraction takes
place) shall be maintained at 23 ± 2°C during the extraction period.
NOTE: As agitation continues, pressure may build up within the
extractor bottle for some types of sample (~, limed or calcium
carbonate-containing sample may evolve gases such as carbon
dioxide). To relieve excess pressure, the extractor bottle may be
periodically opened (~, after 15 minutes, 30 minutes, and 1
hour) and vented into a hood.
7.2.12 Following the 18 ± 2 hour extraction, separate the material
in the extractor vessel into its component 1 i qui d and sol i d phases by
filtering through a new glass fiber filter, as outlined in Step 7.2.7.
For final filtration of the 1312 extract, the glass fiber filter may be
changed, if necessary, to facilitate filtration. Filter(s) shall be
acid-washed (see Step 4.4) if evaluating the mobility of metals.
7.2.13 Prepare the 1312 extract as follows:
7.2.13.1 If the sample contained no initial liquid phase,
the filtered liquid material obtained from Step 7.2.12 is defined
as the 1312 extract. Proceed to Step 7.2.14.
7.2.13.2 If compatible (~, multiple phases will not
result on combination), combine the filtered liquid resulting from
Step 7.2.12 with the initial liquid phase of the sample obtained
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The ZHE device has approximately a 500 mL internal capacity. The ZHE can
thus accommodate a maximum of 25 grams of solid (defined as that fraction of a
sample from which no additional liquid may be forced out by an applied pressure
of 50 psig), due to the need to add an amount of extraction fluid equal to 20
times the weight of the solid phase.
Charge the ZHE with sample only once and do not open the device until the
final extract (of the solid) has been collected. Repeated filling of the ZHE to
obtain 25 grams of solid is not permitted.
Do not allow the sample, the initial liquid phase, or the extract 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 loss
of volatiles.
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7.3.1 Pre-weigh the (evacuated) filtrate collection container
(see Step 4.6) and set aside. If using a TEOLAR® bag, express all l i quid
from the ZHE device into the bag, whether for the initial or final
liquid/solid separation, and take an aliquot from the liquid in the bag
for analysis. The containers listed in Step 4.6 are recommended for use
under the conditions stated in Steps 4.6.1-4.6.3.
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
fl ui d). Adjust the pi ston withi n the ZHE body to a hei ght that wi 11
minimize the distance the piston will have to move once the ZHE is charged
with sample (based upon sample size requirements determined from Step 7.3,
Step 7.1.1 and/or 7.l.2). 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/outlet flange (top flange) aside.
7.3.3 If the sample is 100% solid (see Step 7.1.1), weigh out
a subsample (25 gram maximum) of the waste, record weight, and proceed to
Step 7.3.5.
7.3.4 If the sample contains <0.5% dry solids (Step 7.1.2), the
liquid portion of waste, after filtration, is defined as the 1312 extract.
Filter enough of the sample so that the amount of filtered liquid will
support all of the volatile analyses required. For samples containing
2.0.5% dry solids (Steps 7.l.1 and/or 7.l.2), use the percent solids
information obtained in Step 7.1.1 to determine the optimum sample size to
charge into the ZHE. The recommended sample size is as follows:
7.3.4.1 For samples containing <5% solids (see Step
7.1.1), weigh out a 500 gram subsample of waste and record the
weight.
7.3.4.2 For wastes containing >5% solids (see Step
7.1.1), determine the amount of waste to charge into the ZHE as
follows:
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25
Weight of waste to charge ZHE x 100
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percent solids (Step 7.1.1)
Weigh out a subsample of the waste of the appropriate size and
record the weight.
7.3.5 If particle-size reduction of the solid portion of the
sample was required in Step 7.1.3, proceed to Step 7.3.6. If particle-
size reduction was not required in Step 7.1.3, proceed to Step 7.3.7.
7.3.6 Prepare the sample for extraction by crushing, cutting, or
grinding the solid portion of the waste to a surface area or particle size
as described in Step 7.1.3.1. Wastes and appropriate reduction equipment
should be refrigerated. if possible. to 4°C prior to particle-size
reduction. The means used to effect particle-size reduction must not
generate heat in and of itself. If reduction of the solid phase of the
waste is necessary, exposure of the waste to the atmosphere should be
avoided to the extent possible.
NOTE: Si evi ng of the waste is not recommended due to the
possibility that volatiles may be lost. The use of an
appropriately graduated ruler is recommended as an acceptable
alternative. Surface area requirements are meant for filamentous
(~, paper, cloth) and similar waste materials. Actual
measurement of surface area is not recommended .
When the surface area or part icle-size has been appropriately
altered, proceed to Step 7.3.7.
7.3.7 Waste slurries need not be allowed to stand to permit the
solid phase to settle. Do not centrifuge samples prior to filtration.
7.3.8 Quantitatively transfer the entire sample (liquid and solid
phases) quickly 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.
Note: If sample material (>1% of original sample weight) has
obviously adhered to the container used to transfer the sample to
the ZHE, determine the weight of this residue and subtract it from
the sample weight determined in Step 7.3.4 to determine the weight
of the waste sample that will be filtered.
Attach a gas line to the gas inlet/outlet valve (bottom flange)
and. with the liquid inlet/outlet valve (top flange) open. begin applying
gentle pressure of 1-10 psig (or more if necessary) to force al l headspace
slowly out of the ZHE device into a hood. At the f i rst appearance of
liquid from the liquid inlet/outlet valve, quickly close the valve and
discontinue pressure. If filtration of the waste at 4°C reduces the
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amount of expressed liquid over what would be expressed at room
temperature, then allow the sample to warm up to room temperature in the
device before filtering. If the waste is 100 % solid (see Step 7.1.1),
slowly increase the pressure to a maximum of 50 psig to force most of the
headspace out of the device and proceed to Step 7.3.12.
7.3.9 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 psig to force the liquid phase of the
sample 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-psig increments to a maximum of 50 psig. After each
incremental increase of 10 psig, if no additional liquid has passed
through the filter in any 2-minute interval, proceed to the next 10-psig
increment. When liquid flow has ceased such that continued pressure
filtration at 50 psig does not result in any additional filtrate within a
2-minute period, stop the filtration. Close the liquid inlet/outlet
valve, discontinue pressure to the piston, and disconnect and weigh the
filtrate collection container.
NOTE: Instantaneous application of high pressure can degrade the
glass fiber filter and may cause premature plugging.
7.3.10 The material in the ZHE is defined as the solid phase of
the sample and the filtrate is defined as the liquid phase.
NOTE: Some samples, such as oily wastes and some paint wastes,
will obviously contain some material which appears to be a liquid.
Even after applying pressure filtration, this material will not
filter. If this is the case, the material within the filtration
device is defined as a solid, and is carried through the 1312
extraction as a solid.
If the original waste contained <0.5 % dry solids (see Step 7.1.2),
this filtrate is defined as the 1312 extract and is analyzed directly.
Proceed to Step 7.3.15.
7.3.11 The liquid phase may now be either analyzed immediately
(see Steps 7.3.13 through 7.3.15) or stored at 4°C under minimal headspace
conditions until time of analysis. Determine the weight of extraction
fluid #3 to add to the ZHE as follows:
20 x % solids (Step 7.1.1) x weight
of waste filtered (Step 7.3.4 or 7.3.8)
Weight of extraction fluid
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7.3.12 The foll owi ng steps detai 1 how to add the appropri ate
amount of extraction fluid to the solid material within the ZHE and
agitation of the ZHE vessel. Extraction fluid #3 is used in all cases
(see Step 5.4.3).
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7.3.12.1 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
1 i ne. Rel ease gas pressure on the ZHE pi ston (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.
7.3.12.2 After the extraction fluid has been added.
immediately close the liquid inlet/outlet valve and disconnect the
extraction fluid line. Check the ZHE to ensure that all valves are
in their closed positions. Manually rotate the device in an
end-over-end fashion 2 or 3 times. Reposition the ZHE in the
vertical position with the liquid inlet/outlet valve on top.
Pressurize the ZHE to 5-10 psig (if necessary) and slowly open the
liquid inlet/outlet valve to bleed out any heads pace (into a hood)
that may have been introduced due to the addition of extraction
fluid. This bleeding shall be done quickly and shall be stopped
at the first appearance of liquid from the valve. Re-pressurize
the ZHE with 5-10 psig and check all ZHE fittings to ensure that
they are closed.
7.3.12.3 Place the ZHE in the rotary extractor apparatus
(if it is not already there) and rotate at 30 ± 2 rpm for 18 ± 2
hours. Ambi ent temperature (~, temperature of room in whi ch
extraction occurs) shall be maintained at 23 ± 2°C during
agitation.
7.3.13 Fo 11 owi ng the 18 ± 2 hour agi tat i on peri od. 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 (~. no gas release observed). the ZHE is leaking.
Check the ZHE for leaking as specified in Step 4.2.1. and perform the
extraction again with a new sample of waste. If the pressure within the
device has been maintained. the material in the extractor vessel is once
again separated into its component liquid and solid phases. If the waste
contained an initial liquid phase, the liquid may be filtered directly
into the same filtrate collection container (~. TEDLAR® bag) holding the
initial liquid phase of the waste. A separate filtrate collection
container must be used if combining would create multiple phases. or there
is not enough volume left within the filtrate collection container.
Filter through the glass fiber filter. using the ZHE device as discussed
in Step 7.3.9. All extracts shall be filtered and collected if the TEDLAR®
bag is used. if the extract is multiphasic. or if the waste contained an
initial liquid phase (see Steps 4.6 and 7.3.1).
1ill.I.E: An in-line glass fiber filter may be used to filter the
material within the ZHE if it is suspected that the glass fiber
filter has been ruptured
1312 -17 Revision 0
September 1994
spike concentration may be as low as one half of the analyte
concentration. but may not be less than five times the method detection
limit. In order to avoid differences in matrix effects. the matrix spikes
must be added to the same nominal volume of 1312 extract as that which was
analyzed for the unspiked sample.
8.2.3 The purpose of the matrix spike is to monitor the
performance of the analytical methods used. and to determine whether
matrix interferences exist. Use of other internal calibration methods.
modification of the analytical methods. or use of alternate analytical
methods may be needed to accurately measure the analyte concentration in
the 1312 extract when the recovery of the matri x spi ke is below the
expected analytical method performance.
8.2.4
formula:
Matrix spike recoveries are calculated by the following
%R (% Recovery) = 100 ( X, -Xu) / K
where:
X, = measured value for the spiked sample
Xu measured value for the unspiked sample. and
K known value of the spike in the sample.
8.3 All quality control measures described in the appropriate analytical
methods shall be followed.
8.4 The use of internal calibration quantitation methods shall be
employed for a metallic contaminant if: (1) Recovery of the contaminant from the
1312 extract is not at least 50% and the concentration does not exceed the
appropriate regulatory level. and (2) The concentration of the contaminant
measured in the extract is within 20% of the appropriate regulatory level.
CD-ROM
8.4.1. The method of standard additions shall be employed as the
internal calibration quantitation method for each metallic contaminant.
8.4.2 The method of standard additions requires preparing
calibration standards in the sample matrix rather than reagent water or
blank solution. It requires taking four identical aliquots of the
solution and adding known amounts of standard to three of these aliquots.
The forth aliquot is the unknown. Preferably. the first addition should
be prepared so that the resulting concentration is approximately 50% of
the expected concentration of the sample. The second and third additions
should be prepared so that the concentrations are approximately 100% and
150% of the expected concentration of the sample. All four aliquots are
maintained at the same final volume by adding reagent water or a blank
solution. and may need dilution adjustment to maintain the signals in the
linear range of the instrument technique. All four aliquots are analyzed.
8.4.3 Prepare a plot. or subject data to linear regression. of
instrument signals or external-calibration-derived concentrations as the
dependant variable (y-axis) versus concentrations of the additions of
standards as the independent variable (x-axis). Solve for the intercept
1312 -19 Revision 0
September 1994
of the abscissa (the independent variable, x-axis) which is the concentra -
tion in the unknown.
8.4.4 Alternately, subtract the instrumental signal or external-
calibration-derived concentration of the unknown (unspiked) sample from
the instrumental signals or external-calibration-derived concentrations of
the standard additions. Plot or subject to linear regression of the
corrected instrument signals or external-calibration-derived concentra-
tions as the dependant variable versus the independent variable. Derive
concentrations for the unknowns using the internal calibration curve as if
it were an external calibration curve.
8.5 Samples must undergo 1312 extraction within the following time
periods:
SAMPLE MAXIMUM HOLDING TIMES (days)
From: Fi e 1 d From: 1312 From: Prepara-Total
Collec-extrac-tive Elapsed
tion tion extrac-Time
tion
To: 1312 To: Prepara-
extrac-tive To: Determi -
tion extrac-native
tion analysis
Volatiles 14 NA 14 28
Semi-
volatiles 14 7 40 61
Mercury 28 NA 28 56
Metals,
except 180 NA 180 360
mercury
NA = Not Applicable
If sample holding times are exceeded, the values obtained will be considered
minimal concentrations. Exceeding the holding time is not acceptable in
establishing that a waste does not exceed the regulatory level. Exceeding the
holding time will not invalidate characterization if the waste exceeds the
regul atory 1 evel .
9.0 METHOD PERFORMANCE
9.1 Precision results for semi-volatiles and metals: An eastern soil
with high organic content and a western soil with low organic content were used
for the semi-volatile and metal leaching experiments. Both types of soil were
analyzed prior to contaminant spiking. The results are shown in Table 6. The
concentration of contaminants leached from the soils were reproducible, as shown
CD-ROM 1312 -20 Revision 0
September 1994
by the moderate relative standard deviations (RSDs) of t he recoveries (averaging
29% for t he compounds and elements ana lyzed).
9.2 Precision results for volatiles: Four different soils were spiked
and tested for the extraction of volatiles. Soils One and Two were from western
and eastern Superfund sites. SOlls Th r ee and Four were mixtures of a western
soil with low organic content and two different municipal sludges. The results
are shOwn in Table 7. Extract conce ntrations of volatile organics from the
eastern soil were lower th an from the wester n soil . Repl icate leachl ngs of Soils
Three and Four showed lower precision than the leachates from the Superfund
soil s.
10.0 REFERENCES
1. Environmental Monitoring Systems labor atory. RPe rformance Testing of
Method 1312 : OA Suppo rt for RCRA Testing : Project Report". EPA/600/4-
89/022 . EPA Contract 68-03-3249 to Lockheed Engineering and Sciences
Company . June 1989 .
2. Research Triangle Institute . Rlnterlaboratory Comparison of Methods 1310.
1311. and 1312 for lead in Soil-. U.S. EPA Cont r act 68-01-7075. November
1988 .
CO'ROM 1312 . 21 Revision 0
Septembe r 1994
Table 1. Volatile Analytes l
Compound CAS No.
Acetone
Benzene
n-Butyl alcohol
Carbon disulfide
Carbon tetrachloride
Chlorobenzene
Chloroform
1.2-Dichloroethane
1.1-D1chloroethylene
Ethyl acetate
Ethyl benzene
Ethyl ether
Isobutanol
Methanol
Methylene chloride
Methyl ethyl ketone
Methyl fsobutyl ketone
Tetrachloroethylene
Toluene
1.1.1 . -Tri chI oroethane
Trichloroethylene
Trich l orofluoromethane
1.1.2-Trichloro-l .2.2-trifluoroethane
Vinyl chloride
Xylene
67 -64-1
71-43-2
71-36-3
75-15-0
56-23-5
108-90-7
67-66-3
107-06-2
75-35-4
141-78-6
100-41-4
60-29-7
78-83-1
67-56-1
75-09-2
78-93-3
108-10-1
127-18-4
108 -88-3
71-55-6
79-01-6
75-69-4
76-13-1
75-01-4
1330-20-7
I When testing for any or all of these analytes. the zero-headspace extractor
vessel shall be used instead of the bottle extractor .
CO-ROM J312 -22 Revision 0
September 1994
Table l . Suitable Rotary Agitation Apparatus'
Company location Model No.
Analytical Testing and Warrington . PA 4~vessel extractor (DC2DS):
Consulting Services. [phone] a-vessel extractor (DC201 :
Inc. ll-vessel extractor (DC20B)
Associated Design and Alexandria , VA 2·vessel (3740-2) :
Manufacturing Company [phone] 4-vessel (3740-4);
6-vessel (3740-61 :
8-vessel (3740-81 :
12-vessel (3740-12) :
24 -vessel (3740-24)
Envi ronmental Machine and Lynchbu rg . VA 8-vessel (08-00-001
Design . Inc. [phone] 4-vessel (04-00-001
IRA Machine Shop and Santurce. PR 8~vessel (011001)
Laboratory (8091 752-4004
Lars Lande Manufacturing Wh itmore La ke. MI lO-vessel (lOVREl
[phone] 5-vessel ( 5VREl
Mil 1 i pore Corp. 8edford . MA 4-ZH E or
[phone] 4 I-liter
bottle extractor
(YT300RAHW)
, Any device that rotates the extraction vessel in an end~over-end fashion at 30
±2 rpm is acceptable.
CO-ROM 1312 -23 Revision 0
September 1994
Table 3. Suitable Zero-Headspace Extractor Vessels '
Company
Analytical Testing &
Consulting Services , Inc .
Associated Design and
Manufacturing Company
Lars Lande Manufacturing1
Millipore Corporation
Envi ronme ntal Machine
and Desig n, Inc .
Location
Warrington, PA
[phone]
Alexandria , VA
[phone]
Whitmore Lake , MI
(313) 44 9-4116
Bedford, MA
[phone]
Lynchburg , VA
(804 ) 845-6424
Model No .
CI02 , Mechanical
Pressure Device
3745-ZHE . Gas
Pressure Device
ZHE-ll , Gas
Pressure Device
YT30090HW, Gas
Pressure Device
VOLA-TOXi. Gas
Pressure Devi ce
1 Any device that meets the specifications listed in Step 4.2.1 of the method is
suitabl e.
2 This device uses a 110 mm filter .
CD-ROM 1312 -24 Revision 0
September 1994
Table 4. Suitable Filter Holdersl
Modell
Company Location Catalogue 1t Size
Nucleopore Corporation Pleasanton , CA 425910 142 mm
[phone] 410400 47 mm
Micro Filtration Dublin . CA 302400 142 mm
Systems [phone] 311400 47 mm
[phone]
Mi11ipore Corporation Bedford . MA YT30142HW 142 mm
(800) 225 -3384 XXlO04700 47 mm
1 Any device capable of separating the liquid from the solid phase of the waste
is suitable, providing that i t i s chemically compatible with the waste and the
constituents to be analyzed. Plastic devices (not listed above) may be used when
only inorganic analytes are of concern. The 142 mm size filter holder is
recommended.
COmpany
Mil1ipore Corporation
Nuc1eopore Corporation
Whatman Laboratory
Products, Inc.
Micro Filtration
Systems
Table 5. Suitable Filter Media l
Location
Bedford . MA
[phone]
Pleasa nton . CA
[phone]
Clifton, NJ
[phone]
Dublin . CA
[phone]
(415) 828 -6010
Model
AP40
211625
GFF
GF75
Pore
Size
(llm)
0.7
0.7
0.7
0.7
1 Any f i lter that meets the specifications in Step 4.4 of the Method is suitable .
CD-ROM 1312 -25 Re vision 0
September 1994
TABLE 6 . METHOO 1312 PRECISION RESULTS FOR SEMI·VOLATILES ANO METALS
Eastern Soil (pH (\ .2) Western Soil (pH 5 .0)
Amount Amount Amount
SE:iked Recovered' % RSD Recovered~ \; RSD
(1l9) (j.1g) (lJg )
FORTIFIED ANALYTES
bis(2-chloroethyl)-
ether 1040 834 12 .5 616 14 .2
2-Chlorophenol 1620 1010 6 .8 525 54 .9
1,4-DichloLobenzene 2000 3<4 12.3 272 34 .6
l ,Z-Dichlorobenzene 8920 1010 8 .0 1520 28 .4
2-Methylphenol 3940 1860 ,., 1130 32 .6
Nitrobenzene 1010 812 10 .0 457 21.3
2,(\-Dimethylphenol 1460 200 18 .4 18 87 .6
Hexachlorobutadiene 6300 95 12.9 280 22 .8
AcenaphLbene 3640 210 8.1 310·" 7 .7
2 ,4-Dinitrophenol 1300 896 ...... 6.1 23'· 15 .7
2,4-Dinitrotoluene 1900 1150 5 .4 585 54.4
Hexachlorobenzene 1840 3 .7 12 .0 10 173 .2
gamma BHe (Lindane) 7440 230 16.3 1240 55 .2
beta BHe 6'0 35 13.3 65.3 51. 1
METALS
Lead 5000 70 '.3 10 51.1
Cadmium 1000 387 2.3 91 71.3
• -Triplicate analyses.
"* -Duplicate analyses; one value was rejected as an outlier at the 90%
confidence level using the Dixon Q test.
CO'ROM 1312 . 26 Revision 0
September 1994
TABLE 7 -METHOD 1312 PRECISION RESULTS FOR VOLATILES
Compound Name
Acetone
Acrylonitrile
Benzene
n-Butyl Alcohol
(l-Butanol)
Carbon disulfide
Carbon tetrachloride
Chlorobenzene
Chloroform
1,2-Dichloroethane
1,1-0ichloroethane
Ethyl acetate
Ethylbenzene
Ethyl ether
Isobutanol (4-Methyl
-l-propanol)
Methylene chloride
Methyl ethyl ketone
(2-Butanone)
Methyl isobutyl
ketone
1, 1, 1,2-Tetrachloro-
ethane
1, 1,2, 2-Tetrachloro-
ethane
Tetrachloroethene
Toluene
1,1,1-Trichloro-
ethane
1, 1, 2-Trichloro-
ethane
Trichloroethene
Trichloro-
f1uoromethane
1,1,2-Trichloro-
trif1uoroethane
Vinyl chloride
* Triplicate analyses
Soil No.1
(Western)
Avg.
%Rec.* %RSO
44.0
52.5
47.8
55.5
21.4
40.6
64.4
61. 3
73.4
31. 4
76 .4
56.2
48.0
0.0
47.5
56.7
81.1
69.0
85.3
45.1
59.2
47.2
76.2
54.5
20.7
18.1
10.2
12.4
68.4
8.29
2.91
16.4
18.6
6.76
8.04
4.59
14.5
9.65
9.22
16.4
NO
30.3
5.94
10.3
6.73
7.04
12.7
8.06
16.0
5.72
11.1
24.5
26.7
20.3
** Six replicate analyses
*** Five replicate analyses
CD-ROM
Soil No.2
(Eastern)
Avg.
%Rec.* %RSO
43.8
50.5
34.8
49.2
12.9
22.3
41. 5
54.8
68.7
22.9
75.4
23.2
55.1
0.0
42 .2
61. 9
88.9
41.1
58.9
15.2
49.3
33.8
67.3
39.4
12.6
6.95
7.17
1312 -27
2.25
70.0
16.3
14.6
49.5
29.1
13.1
16.4
11 .3
39.3
4 .02
11. 5
9.72
NO
42.9
3.94
2.99
11. 3
4.15
17.4
10.5
22 .8
8.43
19.5
60.1
58.0
72.8
Soil No.3
(Western and
Sludge)
Avg.
%Rec.** %RSO
116.0
49.3
49.8
65.5
36.5
36.2
44.2
61. 8
58.3
32.0
23.0
37.5
37.3
61. 8
52.0
73.7
58.3
50.8
64.0
26.2
45.7
40.7
61. 7
38.8
28.5
21.5
25.0
11.5
44.9
36.7
37.2
51. 5
41.4
32.0
29 .1
33.3
54.4
119.8
36.1
31. 2
37.7
37.4
31. 3
32.6
31. 5
25.7
44.0
35.2
40.6
28.0
40 .9
34.0
67.8
61. 0
Soil No.4
(Western and
Sludge)
Avg.
%Rec.*** %RSO
21. 3
51.8
33.4
73.0
21.3
24.0
33.0
45.8
41.2
16.8
71.4
4.6
41.1
l3.9
31. 5
34.0
24.9
38.6
37.8
26.4
11.0 115.5
27.2 28.6
42.0 17.6
76.0 12.2
37.3 16.6
40.6 39.0
39.8 40.3
36.8 23.8
53.6 15.8
18 .6 24.2
31.4 37.2
26.2 38.8
46.4 25.4
25.6 34.1
19.8 33.9
15.3 24.8
11.8 25.4
Revision a
September 1994
Appendix C
Soil Boring Log Form
~,.", ~~~
InLiE=lA LOG OF BORING
= ~ MEZ (Page of )
Project Name: Date Started ; Driller ;
Date Completed : Depth to Water :
Drilling Method : Logged By :
Sampling Method ; Northing ;
Project#: Drilling Company : Easting :
ro E E ~ ~ 0. 0.
d & &
Depth Q) Q) c Q)
~ Q) "0 In a. Ol ·8 DESCRIPTION en
E C g ()
Feet C\l Q) ::c en en a.. Z () :>
0 r--
5-
10-
15-
20-
25-
30-
35-
40 -
Notes:
Coordinate System -
Site Location: Drilling Co: Soil Boring Log Depth to Water (ft): Boring No.:
(Field)
Drilling Method: Driller: Total Depth (ft): Date: Drilling Start:
Drilling Equipment: Northing: Easting: Borehole Diameter: Date: Drilling Finish:
"','_ "'-0' • ___ -_ .. ,.. .... ,..-_ .. -....-' ..... ___ • _. -___ 0 ',
Depth In uses Descriptor Soli Type Color PartiCal Grading Angularltyl Density Plasticity Moisture Odor PIDr % Sample Comments ~eetlB.L.SI SIze shaoe FID Rae. N.oJlnt.
Sandy SAND very fine poor angular (sand or gravel) non-plastic dry none
very loose
Clayey CLAY fine well subangular loose slightly plastic moist organic
dense
Silty SILT medium subrounded very dense plastic wet hydrocarbon
Gravelly GRAVEL coarse rounded (silt or clay) very plasitc
very soft
soft
hard
very hard
Depth in uses Descriptor Soil Type Color Part/cal Grading Angularltyl Density Plasticity Moisture Odor % Sample Comments Feet IBLSI Size shaoe Rac. No/lnt.
Sandy SAND very fine poor angular (sand or gravel) non-plastic dry none
very loose
Clayey CLAY fine well subangular loose slightly plastic moist organic
dense
Silty SILT medium subrounded very dense plastic wet hydrocarbon
Gravelly GRAVEL coarse rounded (silt or clay) very plasitc
very soft
soft
hard
very hard
Depth In uses DescrIptor Soli Type Color Partlcal Grading Angularityl Density Plasticity Moisture Odor % Sample Comments -
F_IBlSI Silo .. "h, ..... R ..... lfo.llnt.
Sandy SAND very fine poor angular (sand or gravel) non-plastic dry none
very loose
Clayey CLAY fine well subangular loose slightly plastic moist organic
dense
Silty SILT medium subrounded very dense plastic wet hydrocarbon
Gravelly GRAVEL coarse rounded (silt or clay) very plasitc
very soft
soft
hard
very hard
Depth In uses Descriptor Soli Type Color Partlcar Grading Angularityl Density Plasticity Moisture Odor % Sample Comments Feet (BLS) Size shape Rae. No.nnt.
Sandy SAND very fine poor angular (sand or gravel) non-plastic dry none
very loose
Clayey CLAY fine well subangular loose slightly plastic moist organic
dense
Silty SILT medium subrounded very dense plastic wet hydrocarbon
Gravelly GRAVEL coarse rounded (silt or clay) very plasitc
very soft
soft
hard
-_. ---------very hard --'-------_.
o .0 ..., o
to ~ ::l ~I
~ I
~ '" 0
~
~ u '" e-!!-
'" o ;; N g
'" a
-~=; ~
InLC::rJl LOG OF SOIL BORING: SB-03
!:== ... ~~ (Page 1 of 1)
Project Name: Date Star1ed : 10/23109 Driller ! J. Aguire
Date Completed : 10123109 Depth to Water :NA
Santa Fe River Assessment Drilling Method : HSA (7-314 00) Logged By : E. Romesser
Sampling Method : continuous (5' intelVat) X Coordinate : 1731486.02990
Project #: NME-VR2-SR Drilling Company ; Rodgers & Co" Inc, Y Coordtnate ; 1705469,01180
'iij
2: QJ
C u E Depth QJ QJ c..
in 0.. a: .e, DESCRIPTION (fJ -.., u E c 0 Feet <IS QJ (fJ
(fJ CL a:: :::J
0 SILTY SAND trace Cobbles, brown (5YR 4/6)
NA NA
SM
I--Fill: SILTY SAND little Gravel (up to 2"), dark brown (7.5YR 3/2). fine to medium gravel, coal & brick
5-pieces
60124 <1 SAND some Gravel & Cobbles, reddish (2.5YR 7/6), fine-to medium-grained sand, fine to coarse
gravel & cobbles SW
'--
10-Not Sampled: boulder, augered down to 11.5' bgs
.--Tesuque formation contact
30130 <1 SAND, reddish (2.5YR 7/6), line-grained sand (little medium grained), subangular, moist
SAND, reddish (2.5YR 5/8), fine-grained sand, 5ubangular, dry SP
I--
15-SAND trace Gravel, reddish (2,5YR 4/8), fine-to coarse-grained sand, subangular, fine gravel,
60143 <1 subangular
I\..SAND little Gravel, reddish (2.5YR 4/8), fine-to coarse-grained sand, fine gravel, strongly cemented,
laminar layers at -12" from bottom
I--
20-
IX
SAND, reddish (2.5YR 4/8). fine-to coarse-grained sand, subangular to subrounded, 2' cobble, dry
60/48 <1
SAND little Gravel, reddish (2.5YR 4/8), fine-to coarse-grained sand, subanglar to subrounded, fine to
<-coarse gravel, subangular to subrounded, strongly cemented, dry SW
25-SAND little Gravel, reddish (2.5YR 4/8), fine-to coarse-grained sand, subanglar to subrounded, fine to
60/44 <1
coarse gravel, subangular to subrounded, strongly cemented, 2' cobbles, dry
I--
30-
IX
SAND little Gravel, reddish (2.5YR 4/8), fine-to coarse-grained sand, subanglar to subrounded, fine to
coarse gravel, subangular to subrounded, strongly cemented, 2' cobbles, dry
60/29 <1
SAND, reddish (2.SYR 4/8), fine-grained sand, very thin laminar SP f--
35-18124 <1 SAND, reddish (2 5YR 4/8), fine-to coarse-grained sand, subangular, strongly cemented (sample SW
taken 1'1/2' spill spoon)
Bottom of Boring at 35.5' bgs
40-
Notes: 5. Groundwater nol encountered -monitoring well not installed. Soil boring
1. Post hole 0-4' bgs abandoned with bentonite/cement slurry on 10123109
2. NA; Not Applicable.
3. Refusat at 35.5' bgs, Split Spoon: blow counts IS,GD 175.
4. X; Sampte inteNal sent lor laboratory analysis.
~ I CL « a: C!l
'.-
*:: .
.l~
' ,
-" , ..
-, ':'.
"
,
'.
: .
Appendix D
Standard Guide for Direct Push Soil Sampling for Environmental Site
Characterizations
a Designation: D 6282 -98 (Reapproved 2005)
. ~U I' INTfiRNAnONAL
Standard Guide for
Direct Push Soil Sampling for Environmental Site
Characterizations 1
T~~ standard is issued under the fixed designation D 6282; the number immediately following the designation indicates the year of
ongInal .adopMn or, In . the case of rev.lsl~n, the year of last revision. A number in parentheses indicates the year of last reapprova!. A
superscnpt epsIlon (El indIcates an edltonal change since the last revision or reapprova\.
1. Scope
1.1 This guide addresses direct push soil samplers, which
also may be driven into the ground from the surface or through
prebored holes. The samplers can be continuous or discrete
interval units. Samplers are advanced by a combination of
static push, or impacts from hammers, or vibratory methods, or
a combination thereof, to the depth of interest. The guide does
not cover open chambered samplers operated by hand such as
augers, agricultural samplers operated at shallow depths, or
side wall samplers. This guide does not address single sam-
pling events in the immediate base of the drill hole using rotary
drilling equipment with incremental drill hole excavation.
Other sampling standards, such as Test Methods D 1586 and
D 1587 and Practice D 3550 apply to rotary drilling activities.
This guide does not address advancement of sampler barrel
systems with methods that employ cuttings removal as the
sampler is advanced. Other drilling and sampling methods may
apply for samples needed for engineering and construction
applications.
1.2 Guidance on preservation and transport of samples, as
given in Guide D 4220, mayor may not apply. Samples for
chemical analysis often must be subsampled and preserved for
chemical analysis using special techniques. Practice D 3694
provides information on some of the special techniques re-
quired. Additional information on environmental sample pres-
ervation and transportation is available in other references (1,
2).2 Samples for classification may be preserved using proce-
dures similar to Class A. In most cases, a direct push sample is
considered as Class B in Practice D 4220 but is protected,
representative, and suitable for chemical analysis. The samples
taken with this practice do not usually produce Class C and D
(with exception of thin wall samples of standard size) samples
for testing for engineering properties, such as shear strength
and compressibility. Guide D 4700 has some information on
mechanical soil sampling devices similar to direct push tech-
1 This guide is under the jurisdiction of ASTM Cornmillee D18 on Soil and Rock
and is the direct responsibility of Subcommittee D18.21 on Ground Water and
Vadose Zone Investigation.
Current edition approved Jan. I, 2005. Published February 2005. Originally
approved in 1998. Last previous edition approved in 1998 as D 6282-98.
2 The boldface numbers in parentheses refer to the list of references at the end of
this standard.
niques, however, it does not address most direct push sampling
methods. If sampling is for chemical evaluation in the Vadose
Zone, consult Guide D 4700 for any special considerations.
1.3 Field methods described in this guide, include the use of
discreet and continuous sampling tools, split and solid barrel
samplers and thin walled tubes with or without fixed piston
style apparatus.
1.4 Insertion methods described include static push, impact,
percussion, other vibratory/sonic driving, and combinations of
these methods using direct push equipment adapted to drilling
rigs, cone penetrometer units, and specially designed
percussion/direct push combination machines. Hammers pro-
viding the force for insertion include drop style, hydraulically
activated, air activated and mechanical lift devices.
1.5 Direct push soil sampling is limited to soils and uncon-
solidated materials that can be penetrated with the available
equipment. The ability to penetrate strata is based on hammer
energy, carrying vehicle weight, compactness of soil, and
consistency of soil. Penetration may be limited or damage to
samplers and conveying devices can occur in certain subsur-
face conditions, some of which are discussed in 5.5. Successful
sample recovery also may be limited by the ability to retrieve
tools from the borehole. Sufficient retract force must be
available when attempting difficult or deep investigations.
1.6 This guide does not address the installation of any
temporary or permanent soil, ground water, vapor monitoring,
or remediation devices.
1.7 The practicing of direct push techniques may be con-
trolled by local regulations governing subsurface penetration.
Certification, or licensing requirements, or both, may need to
be considered in establishing criteria for field activities.
1.8 The values stated in SI units are to be regarded as
standard: however, dimensions used in the drilling industry are
given in inch-pound units by convention. Inch-pound units are
used where necessary in this guide.
1.9 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
Copyright ©ASTM Intemalional.100BarrHarborDrive.POBoxC700.WestConshohocken.PA19426-2959. United States.
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1.10 This guide offers an organized collection of informa-
tion or a series of options and does not recommend a specific
course of action. This document cannot replace education or
experience and should be used in conjunction with professional
judgment. Not all aspects of this guide may be applicable in all
circumstances. This ASTM standard is not intended to repre-
sent or replace the standard of care by which the adequacy of
a given professional service must be judged, nor should this
document be applied without consideration of a projects's
many unique aspects. The word "Standard" in the title of this
document means only that the document has been approved
through the ASTM consensus process.
2. Referenced Documents
2.l ASTM Standards: 3
D 653 Terminology Relating to Soil, Rock and Contained
Fluids
D 1586 Test Method for Penetration Test and Split-Barrel
Sampling of Soils
D 1587 Practice for Thin-Wall Tube Sampling of Soils
D 2488 Practice for Description and Identification of Soils
(Visual-Manual Method)
D 3550 Practice for Ring-Lined Barrel Sampling of Soils
D 3694 Practices for Preparation of Sample Containers and
for Preservation of Organic Constituents
D 4220 Practices for Preserving and Transporting Soil
Samples
D 4700 Guide for Soil Sampling from the Vadose Zone
D 5088 Practice for Decontamination of Field Equipment
Used at Nonradioactive Waste Sites
D 5092 Practice for Design and Installation of Ground
Water Monitoring Wells in Acquifers
D 5299 Guide for Decommisioning of Ground Water Wells,
Vadose Zone Monitoring Devices, Boreholes, and Other
Devices for Environmental Activities
D 5434 Guide for Field Logging of Subsurface Explora-
tions of Soil and Rock
D 6001 Guide for Direct-Push Water Sampling for Geoen-
vironmental Investigations
3. Terminology
3.1 Definitions-General definitions for terminology used
in this guide are in accordance with Terminology D 653.
Definitions for terms related to direct push water sampling for
geoenvironmental investigations are in accordance with Guide
D 6001.
3.1.1 assembly length, n-Iength of sampler body and riser
pipes.
3.1.2 borehole, n-a hole of circular cross-section made in
soil or rock.
3.1.3 casing, n-pipe furnished in sections with either
threaded connections or bevelled edges to be field-welded,
which is installed temporarily or permanently to counteract
3 For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard's Document Summary page on
the ASTM website.
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caving, to advance the borehole, or to isolate the interval being
monitored, or combination thereof.
3.1.4 caving/sloughing, n-the inflow of unconsolidated
material into an unsupported borehole that occurs when the
borehole walls lose their cohesive strength.
3.1.5 decontamination, n-the process of removing unde-
sirable physical or chemical constituents, or both, from equip-
ment to reduce the potential for cross-contamination.
3.1.6 direct push sampling, n-sampling devices that are
advanced into the soil to be sampled without drilling or
borehole excavation.
3.1.7 extension rod, n-hollow steel rod, threaded, in vari-
ous lengths, used to advance and remove samplers and other
devices during direct pushing boring. Also known as drive rod.
In some applications, small diameter solid extension rods are
used through hollow drive rods to activate closed samples at
depth.
3.1.8 incremental drilling and sampling, n-insertion
method where rotary drilling and sampling events are alter-
nated for incremental sampling. Incremental drilling often is
needed to penetrate harder or deeper formations.
3.1.9 percussion driving, n-insertion method where rapid
hammer impacts are performed to advance the sampling
device. The percussion normally is accompanied with the
application of a static down-force.
3.1.10 push depth, n-the depth below a ground surface
datum to which the lower end, or tip, of the direct-push
sampling device is inserted.
3.1.11 sample interval, n-defined zone within a subsurface
strata from which a sample is gathered.
3.1.12 sample recovery, n-tbe length of material recovered
divided by the length of sampler advancement and stated as a
percentage.
3.1.13 soil core, n-cylindrical shaped specimen of sedi-
ments or other unconsolidated accumulations of solid particles
produced by the physical and chemical disintegration of rocks
and which mayor may not contain organic matter recovered
from a soil sampler.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 closed barrel sampler, n-a sampling device with a
piston or other secured device that is held to block the
movement of material into the barrel until the blocking device
is removed or released. Liners are required in closed barrel
samplers. Also may be referred to as a protected type sampler.
3.2.2 impact heads/drive heads, n-pieces or assemblies
that fit to top of the above ground portion of the direct push tool
assembly to receive the impact of the hammering device and
transfer the impact energy to sampler extensions.
3.2.3 open barrel sampler, n-sampling barrel with open
end allowing material to enter at any time or depth. Also may
be referred to as an unprotected type sampler.
3.2.4 piston lock, n-device to lock the sampler piston in
place to prevent any entry of a foreign substance into the
sampler chamber prior to sampling.
3.2.5 single tube system, n-a system whereby single
extension/drive rods with samplers attached are advanced into
the subsurface strata to collect a soil sample.
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3.2.6 solid barrel sampler, n-a soil sampling device con-
sisting of a continuous or segmented tube with a wall thickness
sufficient to withstand the forces necessary to penetrate the
strata desired and gather a sample. A cutting shoe and a
connecting head are attached to the barrel.
3.2.7 split barrel sampler, n-a soil sampling device con-
sisting of the two half circle tubes manufactured to matching
alignment, held together on one end by a shoe and on the other
by a connecting head.
3.2.8 two tube systems, n-a system whereby inner and
outer tubes are advanced simultaneously into the subsurface
strata to collect a soil sample. The outer tube is used for
borehole stabilization. The inner tube for sampler recovery and
insertion.
4. Summary of Guide
4.1 Direct push soil sampling consists of advancing a
sampling device into subsurface soils by applying static
pressure, by applying impacts, or by applying vibration, or any
combination thereof, to the above ground portion of the
sampler extensions until the sampler has been advanced to the
desired sampling depth. The sampler is recovered from the
borehole and the sample removed from the sampler. The
sampler is cleaned and the procedure repeated for the next
desired sampling interval. Sampling can be continuous for full
depth borehole logging or incremental for specific interval
sampling. Samplers used can be protected type for controlled
specimen gathering or unprotected for general soil specimen
collection.
5. Significance and Use
5.1 Direct push methods of soil sampling are used for
geologic investigations, soil chemical composition studies, and
water quality investigations. Examples of a few types of
investigations in which direct push sampling may be used
include site assessments, underground storage tank investiga-
tions, and hazardous waste site investigations. Continuous
sampling is used to provide a lithological detail of the
subsurface strata and to gather samples for classification and
index or for chemical testing. These investigations frequently
are required in the characterization of hazardous waste sites.
Samples, gathered by direct push methods, provide specimens
necessary to determine the chemical composition of soils, and
in most circumstances, contained pore fluids (3).
5.2 Direct push methods can provide accurate information
on the characteristics of the soils encountered and of the
chemical composition if provisions are made to ensure that
discrete samples are collected, that sample recovery is maxi-
mized, and that clean decontaminated tools are used in the
sample gathering procedure. For purposes of this guide, "soil"
shall be defined in accordance with Terminology D 653. Using
sealed or protected sampling tools, cased boreholes, and proper
advancement techniques can assure good representative
samples. Direct push boreholes may be considered as a
supplementary part of the overall site investigation or may be
used for the full site investigation if site conditions permit. As
such, they should be directed by the same procedural review
and quality assurance standards that apply to other types of
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subsurface borings. A general knowledge of subsurface condi-
tions at the site is beneficial.
5.3 Soil strata profiling to shallow depths may be accom-
plished over large areas in less time than with conventional
drilling methods because of the rapid sample gathering poten-
tial of the direct push method. More site time is available for
actual productive investigation as the time required for ancil-
lary activities, such as decontamination, rig setup, tool han-
dling, borehole backfill, and site clean-up is reduced over
conventional drilling techniques. Direct push soil sampling has
benefits of smaller size tooling, smaller diameter boreholes,
and minimal investigative derived waste.
5.4 The direct push soil sampling method may be used as a
site characterization tool for subsurface investigation and for
remedial investigation and corrective action. The initial direct
push investigation program can provide good soil stratigraphic
information depending on the soil density and particle size,
determine ground water depth, and provide samples for field
screening and for formal laboratory analysis to determine the
chemical composition of soil and contained pore fluids. Use of
this method, results in minimum site disturbance and no
cuttings are generated.
5.5 This guide may not be the correct method for investi-
gations in all cases. As with all drilling methods, subsurface
conditions affect the performance of the sample gathering
equipment and methods used. Direct push methods are not
effective for solid rock and are marginally effective in partially
weathered rock or very dense soils. These methods can be
utilized to determine the rock surface depth. The presence or
absence of ground water can affect the performance of the
sampling tools. Compact gravelly tills containing boulders and
cobbles, stiff clay, compacted gravel, and cemented soil may
cause refusal to penetration. Certain cohesive soils, depending
on their water content, can create friction on the sampling tools
which can exceed the static delivery force, or the impact energy
applied, or both, resulting in penetration refusal. Some or all of
these conditions may complicate removal of the sampling tools
from the borehole as well. Sufficient retract force should be
available to ensure tool recovery. As with all borehole advance-
ment methods, precautions must be taken to prevent cross
contamination of aquifers through migration of contaminants
up or down the borehole. Regardless of the tool size, the
moving of drilling and sampling tools through contaminated
strata carries risks. Minimization of this risk should be a
controlling factor in selecting sampling methods and drilling
procedures. The user should take into account the possible
chemical reaction between the sample and the sampling tool
itself, sample liners, or other items that may come into contact
with the sample (3, 4).
5.6 In some cases this guide may combine water sampling,
or vapor sampling, or both, with soil sampling in the same
investigation. Guides D 6001 and D 4700 can provide addi-
tional information on procedures to be used in such combined
efforts.
6. Criteria for Selection
6.1 Important criteria to consider when selecting sampling
tools include the following:
6.1.1 Size of sample.
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6.1.2 Sample quality (Class A,B,C,D) for physical testing.
Refer to Practice D 4220.
6.1.3 Sample handling requirements, such as containers,
preservation requirements.
6.1.4 Soil conditions anticipated.
6.1.5 Ground water depth anticipated.
6.1.6 Boring depth required.
6.1.7 Chemical composition of soil and contained pore
fluids.
6.1.8 Probability of cross contamination.
6.1.9 Available funds.
6.1.1 0 Estimated cost.
6.1 .11 Time constraints.
6.1.12 History of tool performance under anticipated con-
ditions (consult experienced users and manufacturers).
6.2 Important criteria to consider when selecting direct push
equipment include the following:
6.2.1 Site accessibility.
6.2.2 Site visibility.
6.2.3 Soil conditions anticipated.
6.2.4 Boring depth required.
6.2.5 Borehole sealing requirements.
6.2.6 Equipment performance history.
6.2.7 Personnel requirements.
6.2.8 Decontamination requirements.
6.2.9 Equipment grouting capability.
6.2.10 Local regulatory requirements.
7. Apparatus
7.1 General-A direct push soil sampling system consists
of a sample collection tool, hollow extension rods for advance-
ment, retrieval, and transmission of energy to the sampler, and
an energy source to force sampler penetration. Auxiliary tools
are required to handle, assemble and disassemble, clean, and
repair the sample collection tools and impact surfaces. Neces-
sary expendable supplies are sample containers, sample con-
tainer caps, sample liners, sample retainers, appropriate lubri-
cants, and personal safety gear.
7.2 Direct Push Tool Systems:
7.2.1 Two Tube System-An outer casing and an inner
extension rod with a sampler attached (see Fig. 1) are advanced
simultaneously into the soil for the length capacity of the
sampler. The sampler is removed from the borehole and a new
sampler barrel or plug bit is inserted for each increment of
depth. Two-tube sampling systems also may incorporate
sample gathering chambers that are fitted into the outer casing
shoe. These sample barrels are designed to create a minimum
of sample disturbance while gathering high quality specimens
(see Fig. 2). Samplers are held in the proper position by
different methods, such as extension rods, pneumatic or me-
chanical packers, spring activated latches, or other devices (see
Figs. 1 and 2). Locking devices must be strong enough to hold
the sampler while penetrating the sample strata. The outer
casing supports the borehole wall. Sample retrieval is expe-
dited by the cased hole and continuous sampling is simplified.
Continuous sampling may be a benefit to lithological logging.
A cased borehole can be sealed from the bottom up as the
casing is extracted (see Section 10). A cased hole may reduce
the risk of contamination migration down the borehole and
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sample cross contamination. The two-tube system is more
susceptible to soil friction because of its larger diameter and
may require larger direct push energy than single-tube systems.
An oversized drive shoe is sometimes used to reduce friction
and buckling but may increase the risk of contamination
migration down the borehole.
7.2.2 Single Tube System-The single tube system (see Fig.
3), uses a hollow extension/drive rod to advance and retrieve
the sampler. The sampler is attached to the bottom of the
extension/drive rod. A drive cap is added to the top of the
extension/drive rod and the sampler is pushed into the soil.
Extension/drive rods generally are smaller in diameter than the
sampler. The single tube system minimizes effort for discrete
interval sampling under many subsurface conditions. Tool
connection time per interval is reduced. Time of removal and
reinsertion of samplers into the borehole is affected by soil
conditions. Repeated movement of the sampler through con-
taminated subsurface strata may increase the risk of contami-
nation migration down the borehole. Bottom up borehole
sealing may require re-entry in soil formations that collapse
(see Section 10).
7.3 Samplers:
7.3.1 Split Barrel Samplers-Split barrel samplers (see Fig.
4) are available for use with direct push drilling methods and
are available in various sizes up to 3.0 in. (76.2-mm) inside
diameter. The inside tolerance should allow for use of liners.
Split barrel sampler shoes used in two tube systems must be of
sufficient diameter to prevent the intrusion of soil between the
outer diameter of the shoe and the inside wall of the outer tube.
Split barrel shoes should be replaced when the leading edge is
damaged. Damaged shoes can negatively affect sample recov-
ery. Samplers can be used with or without ball check value
fitted split barrel heads. The ball check prevents up hole fluids
from flowing down through the sample. Where soil sampling
will be performed below the water table, the split barrel head,
equipped with a ball check, should be used. The open split
barrel is best used with the two tube system because the outer
casing protects the borehole against cave-in or sloughing, or in
soils in which the borehole wall will not collapse. Split barrel
sealing systems are available. Split barrel sections can be
joined to create a sampler with a nominal sample length
capacity of 48 in. (1.22 m). It is understood that samplers with
usable lengths beyond 24 in. (0.61 m) are used to advantage in
certain soil types; however, the added weight of the soil sample
in the chamber and the added friction within the sampler may
prevent loose soils from entering the sampler, affecting sample
recovery and representativeness. Split barrel samplers can be
fitted with a basket to improve recovery in cohesionless soils.
Retainers are available in many styles and materials. Retainers
should allow the passage of softer soils. Stiff retainers can
reduce specimen recovery in soft soils.
7.3.2 Solid Barrel Samplers:
7.3.2.1 Open Solid Barrel Samplers-Open solid barrel (see
Fig. 5) samplers are used with all types of direct push sampling
systems. Solid barrels can have inside diameters ranging up to
3 in. (76.2 mm). Barrel lengths range from 6 in. (152.4 mm) to
5 ft (1.53 m). Solid barrel samplers may be one piece or
segmented. Sample liners should be used to facilitate removal
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~ D 6282 -98 (2005)
Can 8e Pushed With
AW or CPT Rods
All Stainless Construc'jon
Completely Sealed Untll
Opened For Sample RetrievaJ
/
Eas'J To Usa Ball Lock
Action -Push To Depth.
Retract 260mm To Open Sampler,
Push 240mm To Capture Sam pie
316 SS Sample Tubes
With Caps
25'mmx200mm
Sampler
FIG. 2 Sealed Sample Barrel, Single Tube System
cross contamination or in circumstances where borehole wall
stability cannot be assured. The shoe sealing device generally
is a point designed to allow the continuous flow of soil around
and past the sampler until such time as it is removed or
released. The piston point can be fitted with seals, such as "0"
rings at top and bottom to hold fluid out until sampling the
desired interval. The piston rod extends through the sample
retaining liner and must be released or removed for the soil to
enter (see Fig. 3, Fig. 5, Fig. 7). The piston can be removed
manually before sampling or be displaced by the soil entering
the sampler chamber. Using the displacement method can
result in reduced recovery if sampled soils do not have
sufficient strength to displace the piston. Pistons are locked in
place by several methods, such as a spring loaded latch. The
latch holds several balls (see Fig. 2, Fig. 7, Fig. 8) into a groove
in the latch coupling. When the latch is released by lifting up
on the latch stem, the balls slip back into the latch chamber
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allowing the piston to be removed. Another method uses a
locking screw. A reverse thread pin (Fig. 3, Fig. 6) is positioned
in the sampler head to prevent the piston from being displaced
by the soil when advancing the sampler. At the sampling
interval, small diameter extension rods are inserted through the
sampler extension/drive rods and rotated clockwise to unscrew
the locking pin. A third method uses an inflated packer. An
inflated packer (see Fig. 9) is attached to the top of the sampler
barrel. The sample barrel is lowered into position in the drive
casing and the packer inflated. The packer is deflated to release
and the sample barrel is recovered after being advanced the
sampling interval.
7.3.4 Thin Wall Tube-A 1.0-in. (25.4-mm) diameter thin
wall tube (see Fig. 10) is available for use with direct push
equipment and is manufactured according to Practice D 1587.
Thin wall tubes can be effective when used with dual tube
direct push systems as the borehole must be kept clear of
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completed so other functions can be performed while samples
are being processed. A backup tool system adaptable to and
within the capabilities of the power source should be available
should the original planned method prove unworkable. Mate-
rials for proper sealing of boreholes should always be available
at the site (5-7).
9. Procedure
9.1 While procedures for direct push soil sampling with two
common direct push methods are outlined here, other systems
may be available. As long as the basic principles of practice
relating to sampler construction and use are followed, other
systems may be acceptable.
9.2 General Set-Up-Select the boring location and check
for underground and overhead utilities and other site obstruc-
tions. Establish a reference point on the site for datum
measurements, and set the direct push unit over the boring
location. Stabilize and level the unit, raise the drill mast or
frame into the drilling position, and attach the hammer assem-
bly to the drill head if not permanently attached. Attach the
anvil assembly in the prescribed manner, slide the direct push
unit into position over the borehole, save a portion of the
sliding distance for alignment during tool advancement, and
ready the tools for insertion.
9.2.1 Tool Preparation-Inspect the direct push tools before
using, and clean and decontaminate as necessary. Inspect drive
shoes for damaged cutting edges, dents, or thread failures as
these conditions can cause loss of sample recovery and slow
the advancement rate. Where permissible, lubricate rod joints
with appropriate safe products, and check impact surfaces for
cracks or other damage that could result in failure during
operations. Assemble samples and install where required,
install sample retainers where needed, and install and secure
sampler pistons to ensure proper operation where needed.
9.2.2 Sample Processing-Sample processing should fol-
Iowa standard procedure to ensure quality control procedures
are completed. View sample in the original sampling device, if
possible. Open the sampling device with care to keep distur-
bance to a minimum. When using liners or thin wall tubes,
protect ends to prevent samples from falling out or being
disturbed by movement within the liner. Measure recovery
accurately, containerize as specified in the work plan or
applicable ASTM procedures, and label recovered samples
with sufficient information for proper identification. When
collecting samples for volatile chemical analysis, sample
specimens must be contained and preserved as soon as possible
to prevent loss of these components. Follow work plan
instructions or other appropriate documents (see Practice
D 3694) when processing samples collected for chemical
analysis.
9.3 Two Tube System:
9.3.1 Split Barrel Sampling (see Fig. I)-Assemble the
outer casing with the drive shoe on the bottom, attach the drive
head to the top of the outer casing, and attach the sampler to the
extension rods. Connect the drive head to the top of the
sampler extension rods, and insert the sampler assembly into
the outer casing. The sampler cutting shoe should contact the
soil ahead of the outer casing to prevent unnecessary sample
disturbance. The split spoon cutting shoe should extend a
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minimum of 0.25 in. (6.25 mm) ahead of the outer casing.
Greater extensions may improve recovery in soft formations.
Mark the outer casing to designate the required drive length,
position the outer casing and sampler assembly under the drill
head, and move the drill head downward to bring pressure on
the tool string. If soil conditions allow, advance the sampler/
casing assembly into the soil at a steady rate slow enough to
allow the soil to be cut by the shoe and move up inside the
sample barrel. If advancement is too rapid, it can result in loss
of recovery because of soil friction in the shoe. Occasional
hammer action during the push may help recovery by agitating
the sample surface. If soil conditions prevent smooth static
push advancement, activate the hammer to advance the sam-
pler. Apply a continuous pressure while hammering to expedite
soil penetration. The pressure required is controlled by subsur-
face conditions. Applications of excessive down pressure may
result in the direct push unit being shifted off the borehole
causing misalignment with possible tool damage. Stop the
hammer at completion of advancement of the measured sam-
pling barrel length. Release the pressure and move the drill
head off the drive head. Attach a pulling device to the extension
rods or position the hammer bail and retrieve the sampler from
the borehole. At the surface remove the sampler from the
extension rods and process. Soil classification is accomplished
easily using split barrel samplers as the specimen is available
readily for viewing, physical inspection and subsampling when
the barrel is opened. Clean, decontaminate, and reassemble the
sampler. Reattach the sampler to the extension rod, add the
necessary extension rod and outer casing to reach the next
sampling interval, and sound the borehole for free water before
each sample interval. If water is present, it may be necessary to
change sampling tools. Unequal pressure inside the casing may
result in blow-in of material disturbing the soil immediately
below the casing. Lower the sampler to its proper position, add
the drive heads, and repeat the procedure. If it is desired that
the pass through certain strata without sampling, install an
extension rod point in lieu of the sampler. When the sampling
interval is reached, remove the point and install the sampler.
Advance the sampler as described. Upon completion of the
borehole, remove the outer casing after instrumentation has
been set or as the borehole is sealed as described in Section 10
(6).
9.3.2 Two Tube System-Other Samplers:
9.3.2.1 Thin Wall Tubes-Thin wall tubes (see Fig. 10) can
be used with the dual tube system. Attach the tube to the tube
head using removable screws. Attach the tube assembly to the
extension rods and position at the base of the outer casing shoe
protruding a minimum of 0.25 in. (6.25 mm) to contact the soil
ahead of the outer casing. Advance the tube, with or without
the outer casing, at a steady rate similar to the requirements of
Practice D 1587. At completion of the advancement interval,
let the tube remain stationary for 1 min. Rotate the tube slowly
two revolutions to shear off the sample. Remove the tube from
the borehole, measure recovery, and classify soil. The thin wall
tube can be field extruded for on-site analysis or sealed in
accordance with Practice D 4220 and sent to the laboratory for
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soil for the sample increment. Rest sampler 1 min to allow
sample to conform to tube. Rotate tube one revolution to shear
off sample. Remove sampler assembly from borehole and
process sample (6).
9.3.2.3 Open Solid Barrel Samplers-Use solid barrel sam-
plers in advance of the outer casing where the soil conditions
could cause swelling of split barrel samplers, or where friction
against the outer casing precludes its advancement and sam-
pling must still be accomplished. The solid, single, or seg-
mented barrel sampler requires the use of liners for removal of
the sample. The sampler must be cleaned and decontaminated
before use. Use of the sampler follows the procedure described
in 9.3.1.
9.4 Single Tube System:
9.4.1 Open Solid Barrel Sampler (see Figs. 5 and 6)-
Attached the required liner to the cutting shoe by insertion into
the machined receptacle area or by sliding over the machined
tube. Insert the liner and shoe into the solid barrel, and attach
the shoe (6, 8-11). Attach the sampler head to the sampler
barrel providing a backing plate for the liner. Attach the
sampler assembly to the drive rod and the drive head to the
drive rod. Position the assembly under the hammer anvil and
advanced as described in 9.3.1. At completion of the sampling
increment, remove the sampler from the borehole. Remove the
filled sample liner from the barrel by unscrewing the shoe, cap
the liner for laboratory testing or spit open for field processing,
and advance the borehole by repeating the procedure. Because
the solid barrel cannot be opened for cleaning, it may require
more effort for cleaning and decontamination. The open solid
barrel sampler is used in soil formations that have sufficient
wall strength to maintain a borehole wall without sloughing or
cave-in. In soil formations not affording such structure, other
sampling methods may be required or the opening sealed. To
enhance recovery in some soil strata, it may be necessary to
vary the length of the sampling increment. Shorter increments
generally improve recovery because of lower sample friction
and compression inside the sampler chamber. Sample recovery
can be enhanced in some formations by intermittent use of the
percussion hammer (6, 8, 10, 11).
9.4.2 Closed Solid Barrel Sampler (see Figs. 5-7, Fig.
11 )-Insert or attach the sample liner to the shoe, and insert the
assembly into the solid barrel sampler. Install sample retaining
basket if desired. Attach the latch coupling or sampler head to
the sampler barrel, and attach the piston assembly with point
and" 0" rings if free water is present, to the latching mecha-
nism or holder. Insert the piston or packer into the liner to its
proper position so the point leads the sampler shoe. Set latch,
charge packer, or install locking pin, and attach assembled
sampler to drive rod. Add drive head and position under the
hammer anvil. Apply down pressure, hammer if needed, to
penetrate soil strata above the sampling zone. When the
sampling zone is reached, insert the piston latch release and
recovery tool, removing the piston, or insert the locking pin
removal/extension rods through the drive rods, tum counter-
clockwise, and remove the piston locking pin so the piston can
float on top of the sample, or release any other piston holding
device. Direct push or activate the hammer to advance the
sampler the desired increment. Retrieve the sampler from the
Copyright by ASTM Int'l (all rights reserved); Mon May 2 11 :39:30 EDT 201117
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borehole by withdrawing the extension/drive rods. Remove the
shoe, and withdraw the sample liner with sample for process-
ing. Clean and decontaminate the sampler, reload as described,
and repeat the procedure. Extreme stress is applied to the
piston when driving through dense soils. If the piston releases
prematurely, the sample will not be recovered from the correct
interval, and a resample attempt must be made. The piston
sampler can be used as a re-entry grouting tool for sealing
boreholes on completion if it is equipped with a removable
piston (5, 6, 7, 10, 11).
9.4.3 Standard Split Barrel Sampler-Attach the split spoon
to an extension rod or drill rod. Using a mechanical or
hydraulic hammer drive the sampler into the soil the desired
increment, as long as that increment does not exceed the
sampler chamber length. Remove the sampler from the bore-
hole, disassemble, and process sample. Standard split barrel
samplers can be used, as long as borehole wall integrity can be
maintained and the additional friction can be overcome. If
caving or sloughing occurs, the sampler tip should be sealed or
other sampling tools used (9).
9.5 Quality Control:
9.5.1 Quality Control-Quality control measures are neces-
sary to ensure that sample integrity is maintained and that
project data quality objectives are accomplished. By following
good engineering principles and applying common sense,
reliable site characterizations can be accomplished.
9.5.2 Water Checks-Water seeping into the direct push
casing or connecting rods from contaminated zones may
influence testing results. Periodically check for ground water
before inserting samplers into borehole or into outer casings in
the two tube system. If water is encountered, it may be
necessary to switch to the sealed piston type samplers to
protect sample integrity. Sealed piston type samples may not
always be water tight. Sealing of rod or casing joints can
prevent ground water from entering through the joints.
9.5.3 Datum Points-Establishment of a good datum refer-
ence is essential to providing reliable sample interval depths
and elevators. Select datum reference points that are suffi-
ciently protected from the work effort, and that can be located
for future reference. Field measurements should be to 0.1 ft
(3.05 mm). Measure extension rods as the bore advances to
locate sample depth. Mark rods before driving each sample
interval to determine accurate measurement of sample recovery
and to accurately log borehole depth.
9.5.4 Sample Recovery-Sample recovery should be moni-
tored closely and results documented. Poor recovery could
indicate a change in sampling method is needed, that improper
sampling practices are being conducted, or that sampling tools
are incorrect. Sample recovery involves both volume and
condition. Poor sample recovery should cause an immediate
review of the sampling program.
9.5.5 Decontamination-Follow established decontamina-
tion procedures. Taking shortcuts may result in erroneous or
suspect data.
10. Completion and Sealing
10.1 Completion-For boreholes recelvmg permanent
monitoring devices, completion should be in accordance with
Practice D 5092, site work plan, or regulatory requirements.
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o D 6282 -98 (2005)
10.2 Borehole Sealing-Seal direct push boreholes to mini-
mize preferential pathways for containment migration. Addi-
tional information and guidance on borehole sealing can be
found in Guide D 6001 and in Guide D 5299. State or local
regulations may control both the method and the materials for
borehole sealing. Regulations generally direct bottom up bore-
hole sealing as it is the surest and most permanent method for
complete sealing. High pressure grouting is available for use
with direct push technology for bottom up borehole sealing.
10.2.1 Sealing by Slurry, Two Tube System-Sound the
borehole for free water. If water exists in the casing, place the
extension rods, open-ended, to the bottom of the outer casing,
as a tremie. Mix the slurry to standard specifications prescribed
by regulation or work plan. Pump slurry through the extension!
drive rod until it appears at the surface of the outer casing.
Remove the extension rods. If no free water exists in the
borehole, the slurry can be placed by gravity. Top off the outer
casing as it is removed from the borehole.
10.2.1.1 Slurry Mixes-Slurry mixes used for slurry grout-
ing of direct push boreholes generally are of lower viscosity
because of the small diameter tremie pipes required. Usable
mixes are 6 to 8 gal (22.7 to 30.28 L) ofwater!94-lb (42.64-kg)
bag of cement with 5 Ib (2.27 kg) of bentonite or 24 to 36 gal
(90.84 to 136.28 L) of water to 50 lb (22.68 kg) of bentonite.
10.2.2 Sealing by Gravity-Two Tube System-Measure the
cased hole to ensure it is open to depth. Slowly add bentonite
chips or granular bentonite to fill the casing approximately 2 ft.
Withdraw the casing 2 ft and recheck depth. Hydrate the
bentonite by adding water. Repeat this procedure as the outer
casing is withdrawn. The bentonite must be below the bottom
of the casing during hydration. Wetness inside the rods may
affect the flow of granular bentonite to the bottom of the
casing. Fill the top foot of the borehole with material that is the
same as exists in that zone.
10.2.3 Borehole Sealing Single Tube System:
10.2.3.1 Gravity Sealing from Surface-If the soil strata
penetrated has sufficient wall strength to maintain an open
hole, then it may be possible to add sealing materials from the
surface. Dry bentonite chips or granular bentonite can be
placed by gravity. The borehole volume should be determined
and the borehole sounded every 10 ft (3 m) to ensure bridging
has not occurred. The bentonite should be hydrated by adding
approximately 1 pt (0.57 L) of water for each 5 ft of filled
borehole. Seal the surface with native material.
Copyright by ASTM Int'l (all rights reserved); Mon May 2 11 :39:30 EDT 2011 18
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10.2.3.2 Wet Grout Mix Tremie Sealing-Tremie sealing
methods can be used with single tube systems when borehole
wall strength is sufficient to maintain an open hole or when
extension rods with an expendable point are used to reenter the
borehole. The grout pipe should be inserted immediately after
the direct push tools are withdrawn or through the annulus of
the extension rods that have been reinserted down the borehole
for grouting. Care must be taken to not plug the end of the
grout pipe. Side discharge grout pipes also can be used to
prevent plugging.
10.2.4 Re-Entry Grouting-If the borehole walls are not
stable, the borehole can be re-entered by static pushing
grouting tools, such as an expendable point attached to the
extension/drive rods to the bottom of the original borehole.
Pump a slurry through the rods as they are withdrawn. High
pressure grouting equipment may be beneficial in pumping
standard slurry mixes through small diameter gravity pipes.
Care must be taken to ensure the original borehole is being
sealed.
11. Record Keeping
11.1 Field Report-The field report may consist of boring
log or a report of the sampling event and a description of the
sample. Soil samples can be classified in accordance with
Practice D 2488 or other methods as required for the investi-
gation (12). Prepare the log in accordance with standards set in
Guide D 5434 listing the parameters required for the field
investigation program. List all contaminants identified, instru-
ment readings taken, and comments on sampler advancement.
Record any special field tests performed and sample processing
procedures beyond those normally used in the defined inves-
tigation. Record borehole sealing procedures, materials used,
and mix formulas on the boring log. Surveyor otherwise locate
the boring site to provide a permanent record of its replace-
ment.
11 .2 Backfilling Record-Record the method of sealing,
materials used, and volume of materials placed in each
borehole. This information can be added to the field boring log
or recorded on a separate abandonment form.
12. Keywords
12.1 decontamination; direct push; ground water; sealing;
soil sampling
Justin Jayne (INTERA+Inc.) pursuant to License Agreement. No further reproductions authorized.
o D 6282 -98 (2005)
REFERENCES
(1) Ford, Patrick J., and Turine, Paul J., "Characterization of Hazardous
Waste Sites-A Methods Manual" Vol II, Available Sampling Methods,
Second Edition, (Appendix A: Sample Containerization and Preserva-
tion), December 1984, EPA-600/4-84-076.
(2) Mayfield, D., Waugh, J., and Green, R., "Environmental Sampling
Guide in Environmental Testing and Analysis Product News, Vol I, No.
I, April 1993.
(3) McLoy and Associates, Inc. "Soil Sampling and Analysis-Practice
and Pitfalls," The Hazardous Waste Consultant, Vol 10, Issue 6, 1992.
(4) Kay, 1. N., "Technical Note," "Symposium on Small Diameter Piston
Sampling with Cone Penetrometer Equipment," ASTM, 1991.
(5) Einearson, M.D., "Wire Line Sample Recovery System," Precision
Sampling Incorporated, San Fafae!, CA, 1995.
(6) Ruda, T.e., "Operating the Diedrich Drill ESP System Tools,"
LaPorte, IN, 1995.
(7) Sales Division, "GS-lOOO Series Grout System," Geoprobe System,
1996.
(8) Sales Division, "Catalogue of Products," Geoprobe, Inc., Standard
Operating Procedures, Technical Bulletin No. 93-660, 1993.
(9) Sales Division, "Catalogue of Products," Diedrich Drill, Inc., LaPorte,
IN, 1995.
(10) Sales Division, "Geoprobe Macro-Core Soil Sampler, Standard
Operating Procedure," Technical Bulletin No. 95-8500, November
1995.
(11) Sales Division, "Geoprobe AT-660 Series Large Bore Soil Sampler,
Standard Operating Procedures," Technical Bulletin No. 93-{i60,
Revised: June 1995.
(12) Boulding, 1.R., "Description and Sampling of Contaminated Soils: A
Field Pocket Guide," EPA-625/12-911002; 1991 (second edition
published in 1994 by Lewis Publishers).
ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
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(www.Bstm.org).
Copyright by ASTM Int'l (aU rights reserved); Mon May 2 11 :39:30 EDT 2011 19
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Appendix E
Nitrate Extraction and Field Test Procedure
Redlines
Table 2: Laboratory Analytical Parameters by Task and Media
Analyte Analytical Repe"l,. Holding Preservation Temperature
Method Practical rime Requirement
gU!!ntitation
Umll(POU
UR*
SPLP Leachate EPA NA 28 days None~ Cool to S6"C
1312*~ &--------------------------------------------________________ --{ Formatted: Superscript ]
Nitrate+Nitrite EPA353.~ __ O':<~~ ~l~ _ _ }~_c!.ay~ __ HzS04tO apH Cool to S6"C** ----<F..r-----------_._--
.... --------------...
-J Formatted: Superscript
-Formatted: Superscript
I
Chloride and EPA 300.0: Chloride-__ 2~ _d_ay~ __ None**~ Cool to S6"C** ----------________ A. __ -----------... Sulfate 0.1 mg/L -------------<: = 1 .... :_:_:: __ ;_:_~:....::_:_.:..::_:_--______ ____'
Sulfate -
0.75 mg/L
Ammonia as N EPA350.~_ __ O.:q~~L~_ _}~_d_ay~ __ HZS04tO apH Cool to S6"C** ----------_ ...
--, Formatted: Superscript -- --<?"-U ----""----------------_______________ --1 Formatted: Superscript
'-----
* Extraction Fluid 3 will be used. Standard extraction requires the addition of nit ric acid and sulfuric aCid during the leaching process. Since the
leachates will be analyzed for nitrate+nitrite as nitrogen and sulfate, the DI leaching process contemplated by the method (for cyanide
containing samples}will be used in lieu ofthe standard leaching procedure.
**Preservation and temperature requirements listed are for the leachates generated from the SPLP leaching procedure 1312 and for water
samples generated during QC activities such as DI Blanks and equipment blanks.
*** Sample containers will be 4 oz. glass or plastic laboratory supplied jars.
~ miu ~iM;I;iii~
Nitrate Investigation Revised Phase 1 Work Plan
White Mesa Mill Site
May 6,2011
Page 1 of2
~~lig~p!.S J~r;.an}lv~js of nitrate as njtrop;~n ~~'! a_n:!,!,9,!i~ ~~ ,!I!rpg~n_ ~i!1 b~ t~ken frp~ (H ~s..O _ml_po!ve~hJ~e!,~ !a_bp~~~ry-s~pplied sample
container preserved with H2S04 to a pH <2 and cooled to <6"C.
__ -1 Formatted: Superscript
2 Aliguots for analysis of sulfate and chloride will be taken from (1) 250 ml polyethylene laboratory-supplied sample container with no chemical
preservation but cooled to <6"C.
: M_e!'!.od }}1~ is !~o_"! ~~A_ "I.e~~ ~~~9~ fo! Evaluating 5~lid_ '{:J~~~'!'.!ly~<:.aY.s:~emica I Methods. Me.!h~d ~31? is_ d~!~d_ ~e.P1e_"!be.: 1~9~ ______ -{Formatted: Superscript
Revision 0,
~~!ho~~ for Chemical Analysis <;:If ~~ter and_ ~2~~hl[lvi[.on£l1e!ltal Pr.9tectio'! ~g~nS¥._E!,~i~~n_l"!~n!aJ ~o_n!toring Systems Labq,rat,9IY_-= ___ ..... _'~
Cincinnati (EMSL-Cn, EPA-600/4-7~20 •• R..evi?ec!.. M~rch 1~8~ an_d_ ~9.?~ ~_h~~e_app~c_ap~e:.. ___________________________________ ,\
", ",
5 Methods for the Determination of Inorganic Substances In Environmental Samples (EPA/60Q/R-93/10Q) "\ ~--------------------~ ------------------------------------------------,'
~ IntiC=lJi ~~~
Nitrate Investigation Revised Phase 1 Work Plan
White Mesa Mill Site
May 6,2011
Page 2 of2
\ \\'
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Formatted: Superscript
Formatted: Space After: 0 pt, Line spacing:
single, Don't adjust space between Latin and
Asian text, Don't adjust space between Asian
text and numbers
Formatted: Font: (Default) +Body, 11 pt
Formatted: Font: (Default) +Body, 11 pt
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Formatted: Superscript ----