ASTM C1220-98(2004)
(Test Method)Standard Test Method for Static Leaching of Monolithic Waste Forms for Disposal of Radioactive Waste
Standard Test Method for Static Leaching of Monolithic Waste Forms for Disposal of Radioactive Waste
SCOPE
1.1 This test method covers the relative chemical durability of simulated and radioactive monolithic waste forms, such as glasses, ceramics, or cermets, in various test solutions at temperatures
1.2 This test method can be used to distinguish differences in the leaching behavior of various simulated or radioactive waste forms under the specific conditions of the test based on analysis of the test solution. Data from this test are used to calculate the normalized elemental mass loss from specimens exposed to aqueous solutions at temperatures
1.3 Specimen surfaces may be altered during this test. These altered surfaces may be used to study the reaction of monolithic waste forms during static exposure to solutions.
1.4 This test method must be performed in accordance with all applicable quality assurance requirements for acceptance of the data.
1.5 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 appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For a specific hazard statement, see 7.3.2.
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Designation:C1220–98(Reapproved2004)
Standard Test Method for
Static Leaching of Monolithic Waste Forms for Disposal of
Radioactive Waste
This standard is issued under the fixed designation C1220; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope C1174 Practice for Prediction of the Long-Term Behavior
of Materials, Including Waste Forms, Used in Engineered
1.1 This test method covers the relative chemical durability
Barrier Systems (EBS) for Geological Disposal of High-
of simulated and radioactive monolithic waste forms, such as
Level Radioactive Waste
glasses, ceramics, or cermets, in various test solutions at
D1125 Test Methods for Electrical Conductivity and Resis-
temperatures <100°C under low surface-area-to-volume (S/V)
tivity of Water
ratio conditions.
D1129 Terminology Relating to Water
1.2 This test method can be used to distinguish differences
D1193 Specification for Reagent Water
in the leaching behavior of various simulated or radioactive
D1293 Test Methods for pH of Water
waste forms under the specific conditions of the test based on
E177 Practice for Use of the Terms Precision and Bias in
analysis of the test solution. Data from this test are used to
ASTM Test Methods
calculate the normalized elemental mass loss from specimens
2.2 EPA Document:
exposed to aqueous solutions at temperatures <100°C.
TestMethodsforEvaluatingSolidWaste,Physical/Chemical
1.3 Specimensurfacesmaybealteredduringthistest.These
Methods
altered surfaces may be used to study the reaction of mono-
lithic waste forms during static exposure to solutions.
3. Terminology
1.4 This test method must be performed in accordance with
3.1 Definitions:
all applicable quality assurance requirements for acceptance of
3.1.1 accumulated dose—the sum of the absorbed doses
the data.
received by the system considered regardless of whether it is
1.5 This standard does not purport to address all of the
exposed to radiation in a continuous or discontinuous fashion.
safety concerns, if any, associated with its use. It is the
3.1.2 accuracy—the closeness of agreement between the
responsibility of the user of this standard to establish appro-
accepted reference value and individual results (Practice
priate safety and health practices and determine the applica-
E177).
bility of regulatory limitations prior to use. For a specific
3.1.2.1 Discussion—In its usage in this test method, accu-
hazard statement, see 7.3.2.
racy includes the effects of precision and bias. The term is
2. Referenced Documents applied to measurements wherein a specific standard reference
is available such as NIST standard mass and reference solu-
2.1 ASTM Standards:
tions traceable to a standards organization. The term “accurate
C1109 Practice for Analysis of Aqueous Leachates from
to within” a specified range means that individual measure-
Nuclear Waste Materials Using Inductively Coupled
ments on a reference standard are always within the specified
Plasma-Atomic Emission Spectroscopy
range, for example, within 2°C of a certified NIST thermo-
couple, within 0.5 mg of a NISTstandard mass or within 10%
ThistestmethodisunderthejurisdictionofASTMCommitteeC26onNuclear of the value for a reference solution.
Fuel Cycle and is the direct responsibility of Subcommittee C26.07 on Waste
3.1.3 actinide—any element with atomic number of 89 to
Materials.
103.
CurrenteditionapprovedJune1,2004.PublishedJuly2004.Originallyapproved
3.1.4 bias of a measurement process—a generic concept
in 1992. Last previous edition approved in 1998 as C1220–98. DOI: 10.1520/
C1220-98R04.
relatedtoaconsistentorsystematicdifferencebetweenasetof
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on SW846A, 3rd Ed., Revision 1, U.S. Environmental Protection Agency, Wash-
the ASTM website. ington, DC, December 1987.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
C1220–98 (2004)
testresultsfromtheprocessandanacceptedreferencevalueof meet objectives that include evaluation of waste forms for
the property being measured (Practice E177). comparative purposes. In the test method, three reference
3.1.5 chemical durability—the resistance of a glass, ce- leachants are used: high-purity water and two solutions
ramic, or cermet test specimen to the release of its constituents (silicate/bicarbonate and brine) that approximate fluids that the
toanaqueoussolutionunderthespecificconditionsofthistest. wasteformmayencounterinageologicrepository.Inaddition
3.1.5.1 Discussion—The response of glass, ceramics, or to the reference leachants, others may be used. The test is for
cermets under other conditions is outside the scope of this test application to simulated waste forms and to radioactive speci-
method. mens.
3.1.6 closed system—a system that precludes the transport 4.1.1 PTFE test vessels and PTFE specimen supports are
of matter into or out of the system. used, provided the integrated dose to a PTFE component from
3.1.7 high-purity water—ASTM Type I or Type II water all radiation (alpha, beta, or gamma) does not exceed 10 rad
with a maximum total matter content of 0.1 g/m , a minimum (100 Gy), which has been shown to not damage PTFE. If the
electrical resistivity of 16.67 MV·cm at 25°C, and no detect- integrateddosetothetestvesselandspecimensupportexceeds
able soluble silica (see Specification D1193 and Terminology 10 rad, 304L stainless steel or fused silica vessels and
D1129). specimen supports are to be used (in such tests involving brine
3.1.8 ion selective electrode (ISE)—a device for measuring leachants, fused silica vessels and components must be used
F-. because of the corrosion of stainless steel by the brine) (see
3.1.9 leachant—a solution used, or intended for use, in Note 1).
leaching.
NOTE 1—These modifications to the test method are required when
3.1.10 leachate—the solution resulting from a leach test.
using highly radioactive waste forms.
3.1.11 leaching—the action of removing soluble constitu-
4.2 Separate specimen and leachant volumes are required
ents from a solid into a solution.
for each data point. The test results are based on leachate
3.1.12 monolithic specimens—specimens that are physi-
analyses in all cases and include examination of the leached
cally one coherent piece, as opposed to powdered specimens
specimen surface after long-duration tests.
that consist of many small pieces of irregular configuration.
Monolithic specimens may consist of several individual
5. Significance and Use
phases, but they must be bound in a stable coherent configu-
5.1 This test method is intended principally to distinguish
ration.
differences in the leaching behavior of candidate monolithic,
3.1.13 nuclear waste forms—solidmaterialsinwhichradio-
inorganic, radioactive waste forms under low S/V ratio condi-
active wastes have been immobilized.
tions. The test method can be used to produce altered solid
3.1.14 open system—a system that permits the transport of
specimens to study the reaction of monolithic waste forms
matter into or out of the system, e.g., O and/or CO diffusion
2 2
during static exposure to solutions. Data from this test may
into or out of the system.
form part of the larger body of data that is necessary in the
3.1.15 polytetrafluoroethylene (PTFE)—a material pro-
logical approach to long-term prediction of waste form behav-
duced from various monomers that are polymerized into the
ior, as described in Practice C1174. In particular, solution
plastic.
concentrations and characterization and altered surfaces may
3.1.16 precision of a measurement process—a generic con-
be used in the testing of geochemical modelling codes. This
cept related to the closeness of agreement between test results
test method excludes study of powdered or organic materials.
obtained under prescribed like conditions from the measure-
This test method can be used as either a “characterization” or
ment process being evaluated (Practice E177). In this test
“accelerated” test under the protocol of Practice C1174, men-
method, precision will be measured by either standard devia-
tioned above.
tion or relative standard deviation.
5.2 The total absorbed dose for each PTFE test vessel may
3.2 Abbreviations:
not exceed 10 rad (100 Gy) during the lifetime of the vessel.
3.2.1 EDX—energy-dispersive x-ray fluorescence instru-
Hence,arecordoftheabsorbeddoseeachvesselreceivesmust
ment (or analysis).
be maintained.
3.2.2 ICP—inductively coupled plasma.
5.2.1 More radiation-resistant materials are used when test-
3.2.3 PFA—perfluoroalkoxy.
ing in radiation fields where the accumulated absorbed dose
3.2.4 SEM—scanningelectronmicroscope(ormicroscopy).
exceeds 10 rad (see Note 1).
3.2.5 TEM—transmission electron microscope (or micros-
5.3 Bothaeratedanddeaeratedsolutionsmaybeusedinthis
copy).
test method. However, when testing highly radioactive speci-
3.2.6 XRD—x-ray diffractometer (or diffraction).
mens,testswithdeaeratedsolutionsaremandatorytominimize
4. Summary of Test Method
radiolysis effects of nitrogen (see Note 1). Control of the
oxygen fugacity is not part of this test method. Such control
4.1 Specimensofknownvolumeandgeometricsurfacearea
andmeasurementmayberequiredforspecificusesofleaching
are immersed in the reference leachants without agitation for
defined time periods at defined temperatures. The S/V ratio is
−1
held constant within 0.5 of 10.0 m .Three reference tempera-
Strachan, D. M., “Effect of Gamma Irradiation on Simulated Waste Glass
tures, 40°, 70°, and 90°C, and a number of specific time
Leaching and on the Leach Vessel,” Journal of the American Ceramic Society,
periods are identified in a series of test matrices established to 66[9], C-158 -C-160, 1983.
C1220–98 (2004)
data but are beyond the scope of this test method. Preparation 6.2.2 Teflon vessels are considered to provide open systems
of deaerated leachants is covered in 7.2.2. because they are pervious to carbon dioxide and some water
5.4 The use of PTFE test vessels may result in some F− loss.
release from the vessel to the solution. For PTFE vessels that
6.2.3 Stainless steel and fused silica vessels are considered
meet the qualification requirements of this test method (see
to provide closed systems because they are impervious to
6.4), the amount of release at low radiation levels, <10 rad, is
carbon dioxide, and water loss is usually negligible.
not significant. Fluoride, at the concentrations encountered in
6.3 Test Vessel Size—The vessels shall have a diameter-to-
testswheretheradiationdoseislimitedtolessthan10 radand
height ratio between 0.5 and 2.0. Leach vessel volumes will
qualified PTFE is used, has not been demonstrated to have an
generally be between 20 mL and 1 L. The vessels shall be
effect on leaching behavior. The primary reason for limiting
sufficiently impervious and have a tight-fitting lid to limit
the integrated dose to PTFE vessels and specimen supports to
leachant loss during the test to less than 10% of the original
10 rad and requiring that the PTFE vessels be qualified is to
volume.Thespecimensupportshallbeconstructedofthesame
ensure that excessive fluoride releases do not occur (see Note
material as the vessel or of equally inert material and designed
1). In order to monitor fluoride releases, which could have an
tomaintainthespecimennearthecentroidoftheleachvolume,
influence on test results, analysis for F− concentration is a test
but must not contact more than 5% of the specimen surface
requirement.
area.
6.4 Identification of Vessels and Cleaning History—Vessel
6. Apparatus and Analytical Requirements
identification and the cleaning history of each vessel must be
6.1 Fig.1illustratesthebasicfeaturesofthetestequipment.
maintained during testing.
Thespecimenisheldnearthecentroidoftheleachvolume,for
6.4.1 Identification Marking—Aunique identifying number
example with a monofilament or by use of a coarsely woven
should be permanently marked on each leach vessel.The same
support screen.The specimen surface-area-to-leachant-volume
number should be permanently marked on the companion lid.
−1
(S/V) ratio must be within 0.5 of 10.0 m .
6.4.2 Record of Vessel Cleaning History—Each batch of
6.2 Test Vessel Material—The choice of material for con-
cleanedvesselsshallbelabeledwithauniquebatchnumber.A
struction of the test vessels will depend on the radiation field.
log book of the leach vessel number and date of cleaning shall
Whentestingisperformedinfieldsthatyieldanabsorbeddose
be kept. The date can be used as the batch number identifier if
of less than 10 rad, use PTFE PFA vessels that have been
only one batch has been cleaned on that date. Alternatively, a
qualified (see 6.4).
separate batch number can be assigned and recorded. In this
6.2.1 For fields where the absorbed dose exceeds 10 rad,
manner, any inconsistent test responses might be traced to
use fused silica or 304L stainless steel. If the vessel dose
improper cleaning of a batch of vessels or to a problem vessel.
exceeds 10 rad and the brine leachant is employed, fused
6.5 Qualification of PTFE Lot for Use as Test Vessels—
silica vessels are to be used (because of the corrosion of
Variations in manufacturing practice may cause particular lots
stainless steel by the brine). Use of the same vessel material
ofPTFEtohaveunacceptableamountsoffluoridereleasefrom
throughout the test matrix will allow an evaluation of the
PTFE vessels during leach tests. Therefore, the vessels from a
contribution to the leachate by the vessel, for example, silicon
particular lot must be qualified for use by performing a blank
from fused silica. (See Note 1.)
test for 28 days to ascertain and document that the fluoride
release is acceptably low for 28-day tests. The suitability of a
particular lot of PTFE for longer-term tests is dependent on
similar checks of fluoride release in blank tests conducted for
the longer test durations, which is a test requirement. That is,
the fluoride level must always be checked on the blanks and
leachates used during testing. It is imperative that the vessels
fortheblanksbefromthesamelotastheothervesselsusedfor
testing. Measurement of pH shall also be determined in these
qualification tests, as well as in the analyses of test leachates.
The test matrices in 9.5 require the use of blanks, which will
further document that excessive
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