Standard Practice for Flux Fusion Sample Distribution (Withdrawn 2001)

SCOPE
1.1 This practice covers flux fusion sample decomposition and dissolution for the determination of SiO2 as well as many other oxides in glasses, ceramics, and raw materials. The solutions are analyzed by atomic spectroscopy methods. Analyte concentrations ranging from trace to major levels can be measured in these solutions, depending on the sample weights and dilution volumes used during preparation.
1.2 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. Specific precautionary statements are given in Section 8.

General Information

Status
Withdrawn
Publication Date
09-Jul-1996
Withdrawal Date
09-Jun-2001
Technical Committee
Drafting Committee
Current Stage
Ref Project

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ASTM C1342-96 - Standard Practice for Flux Fusion Sample Distribution (Withdrawn 2001)
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NOTICE: This standard has either been superseded and replaced by a new version or
withdrawn. Contact ASTM International (www.astm.org) for the latest information.
Designation: C 1342 – 96
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Practice for
1
Flux Fusion Sample Dissolution
This standard is issued under the fixed designation C 1342; the number 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.
1. Scope 3.2 With appropriate sample preparation, the solution result-
ing from this procedure can be analyzed for trace metals by
1.1 This practice covers flux fusion sample decomposition
inductively coupled plasma-atomic emission spectroscopy
and dissolution for the determination of SiO as well as many
2
(ICP-AES), inductively coupled plasma-mass spectrometry
other oxides in glasses, ceramics, and raw materials. The
(ICP-MS), and flame atomic absorption spectroscopy.
solutions are analyzed by atomic spectroscopy methods. Ana-
lyte concentrations ranging from trace to major levels can be
4. Significance and Use
measured in these solutions, depending on the sample weights
4.1 This practice describes a method for fusing and dissolv-
and dilution volumes used during preparation.
ing silicate and refractory matrix samples for subsequent
1.2 This standard does not purport to address all the safety
analysis for trace metals and radionuclides. Glass vitrification
concerns, if any, associated with its use. It is the responsibility
plant feeds and product can be characterized using this
of the user of this standard to establish appropriate safety and
dissolution method, followed by the appropriate analysis of the
health practices and determine the applicability of regulatory
resulting solutions as described in Test Methods C 1109 and
limitations prior to use. Specific precautionary statements are
C 1111.
given in Section 8.
4.2 This practice has been used to analyze round robin
2. Referenced Documents simulated nuclear waste glass samples.
4.3 This practice can be used for bulk analysis of glass
2.1 ASTM Standards:
samples as described in Test Methods C 1220 and C 1285.
C 1109 Test Method for Analysis of Aqueous Leachates
4.4 This practice is a companion to Practice C 1317. These
from Nuclear Waste Materials Using Inductively Coupled
2
procedures can be used to dissolve borosilicate glasses con-
Plasma-Atomic Emission Spectrometry
taining nuclear wastes for subsequent analysis.
C 1111 Test Method for Determining Elements in Waste
Streams by Inductively Coupled Plasma-Atomic Emission
5. Technical Precautions
2
Spectroscopy
5.1 This procedure is not useful for the determination of
C 1220 Test Method for Static Leaching of Monolithic
2 boron or sodium since these elements are contained in the flux
Waste Forms for Disposal of Radioactive Waste
material.
C 1285 Test Methods for Determining Chemical Durability
5.2 The user is cautioned that with analysis by ICP emis-
of Nuclear Waste Glasses: The Product Consistency Test
2 sion, flame atomic absorption, and ICP-MS, the high sodium
(PCT)
concentrations from the flux may cause interferences.
C 1317 Practice for Dissolution of Silicate or Acid Resistant
2 5.3 Elements that form volatile species under these alkaline
Matrix Samples
3
fusion conditions may be lost during the fusion process (that is,
D 1193 Specifications for Reagent Water
As and Sb).
3. Summary of Practice
6. Apparatus
3.1 A ground sample is weighed into a platinum crucible,
6.1 Platinum Crucibles,30mL.
and an appropriate amount of alkaline flux (Na CO and
2 3
6.2 Balance, analytical type, precision to 0.1 mg.
Na B O ) is added. The mixture is fused in a muffle furnace
2 4 7
6.3 Furnace, with heating capacity to 1000°C.
(950°C for 25 min), cooled to room temperature, dissolved
6.4 Crucible Tongs (cannot be made of iron, unless using
with hydrochloric acid, and diluted to an appropriate volume
platinum-clad tips).
for subsequent analysis.
6.5 Polytetrafluoroethylene (PTFE) Beaker, 125-mL capac-
ity.
1
6.6 Magnetic Stir Bar, PTFE-coated (0.32 to 0.64 cm).
This practice is under the jurisdiction of ASTM Committee C-26 on Nuclear
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
6.7 Magnetic Stirrer.
Test.
6.8 Mortar and Pestle, agate or alumina (or equivalent
Current edition approved July 10, 1996. Published September 1996.
2
grinding apparatus).
Annual Book of ASTM Standards, Vol 12.01.
3
Annual Book of ASTM Standards, Vol 11.01. 6.9 Sieves, 100 mesh.
1

---------------------- Page: 1 ----------------------
C 1342
7. Reagents and Materials platinum crucible on an analytical balance to 60.1 mg. The
sample size is dependent on the analyte con
...

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