Standard Test Method for Determination of Beryllium in Copper-Beryllium Alloys by Phosphate Gravimetric Method

SIGNIFICANCE AND USE
This test method for the chemical analysis of metals and alloys is primarily intended to test such materials for compliance with compositional specifications. It is assumed that all who use these test methods will be trained analysts capable of performing common laboratory procedures skillfully and safely. It is expected that work will be performed in a properly equipped laboratory.
SCOPE
1.1 This test method describes the determination of beryllium in copper-beryllium alloys in percentages from 0.1 % to 3.0 % by the phosphate gravimetric method.
1.2 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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 hazard statements are given in Section 9.

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Status
Historical
Publication Date
30-Apr-2011
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ASTM E2824-11 - Standard Test Method for Determination of Beryllium in Copper-Beryllium Alloys by Phosphate Gravimetric Method
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: E2824 − 11
Standard Test Method for
Determination of Beryllium in Copper-Beryllium Alloys by
Phosphate Gravimetric Method
This standard is issued under the fixed designation E2824; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope 3. Terminology
1.1 This test method describes the determination of beryl- 3.1 For definitions of terms used in this method, refer to
lium in copper-beryllium alloys in percentages from 0.1 % to Terminology E135.
3.0 % by the phosphate gravimetric method.
4. Summary of Test Method
1.2 Units—The values stated in SI units are to be regarded
4.1 Beryllium is precipitated as the phosphate, which is
as standard. No other units of measurement are included in this
filtered, ignited, and weighed as beryllium pyrophosphate.
standard.
Interfering elements, if present, may be complexed with
1.3 This standard does not purport to address all of the
(ethylenedinitrilo) tetraacetate solution.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
5. Significance and Use
priate safety and health practices and determine the applica-
5.1 This test method for the chemical analysis of metals and
bility of regulatory limitations prior to use. Specific hazard
alloys is primarily intended to test such materials for compli-
statements are given in Section 9.
ance with compositional specifications. It is assumed that all
who use these test methods will be trained analysts capable of
2. Referenced Documents
performing common laboratory procedures skillfully and
2.1 ASTM Standards:
safely. It is expected that work will be performed in a properly
E29 Practice for Using Significant Digits in Test Data to
equipped laboratory.
Determine Conformance with Specifications
E50 Practices for Apparatus, Reagents, and Safety Consid-
6. Interferences
erations for Chemical Analysis of Metals, Ores, and
6.1 The elements ordinarily present in beryllium-copper
Related Materials
alloys do not interfere.
E135 Terminology Relating to Analytical Chemistry for
Metals, Ores, and Related Materials
7. Apparatus
E173 Practice for Conducting Interlaboratory Studies of
7.1 Electrodes for Electroanalysis—Recommended station-
Methods for Chemical Analysis of Metals (Withdrawn
ary type platinum electrodes are described in 7.1.1 and 7.1.2.
1998)
The surface of the platinum electrode should be smooth, clean,
E255 Practice for Sampling Copper and Copper Alloys for
and bright to promote uniform deposition and good adherence.
the Determination of Chemical Composition
Deviations from the exact size and shape are allowable. In
E1601 Practice for Conducting an Interlaboratory Study to
instances where it is desirable to decrease the time of deposi-
Evaluate the Performance of an Analytical Method
tion and agitation of the electrolyte is permissible, a generally
availablerotatingtypeofelectrodemaybeemployed.Cleaning
of the electrode by sandblasting is not recommended.
This test method is under the jurisdiction of ASTM Committee E01 on
7.1.1 Cathodes—Platinum cathodes may be either open or
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
responsibility of Subcommittee E01.05 on Cu, Pb, Zn, Cd, Sn, Be, theirAlloys, and
closed cylinders formed from sheets that are plain or
Related Metals.
perforated, or from gauze. Gauze cathodes are recommended;
Current edition approved May 1, 2011. Published July 2011. DOI: 10.1520/
preferably from 50-mesh gauze woven from approximately
E2824-11.
0.21 mm diameter wire. The top and bottom of gauze cathodes
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
should be reinforced by doubling the gauze about 3 mm onto
Standards volume information, refer to the standard’s Document Summary page on
itself, or by the use of platinum bands or rings. The cylinder
the ASTM website.
should be approximately 30 mm in diameter and 50 mm in
The last approved version of this historical standard is referenced on
www.astm.org. height. The stem should be made from a platinum alloy wire
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E2824 − 11
such as platinum-iridium, platinum-rhodium, or platinum- 11. Rounding Calculated Values
ruthenium, having a diameter of approximately 1.3 mm. It
11.1 Calculated values shall be rounded to the desired
should be flattened and welded the entire length of the gauze.
number of places as directed in Practice E29.
The overall height of the cathode should be approximately 130
mm.Acathode of these dimensions will have a surface area of
12. Preparation of Apparatus
135 cm exclusive of the stem.
12.1 Cathode—Clean the cathode in hot HNO , (1 + 1),
7.1.2 Anodes—Platinum anodes may be a spiral type when
rinse with distilled water, rinse in two separate baths of ethanol
anodic deposits are not being determined, or if the deposits are
or acetone. Dry at a low temperature, (110 °C for 3 to 5 min),
small (as in the electrolytic determination of lead when it is
and cool to room temperature in a desiccator.
present in concentrations below 0.2 %). Spiral anodes should
be made from 1.0 mm or larger platinum wire formed into a
12.2 Anode—Clean in HCl, (1 + 1), rinse with distilled
spiralofseventurnshavingaheightofapproximately130mm. water.
Aspiral anode of these dimensions will have a surface area of
12.3 Weigh the cathode to the nearest 0.1 mg and record the
9cm . When both cathode and anode plates are to be
weight. The anode does not have to be weighed.
determined,theanodeshouldbemadeofthesamematerialand
design as the electrode described in 7.1.1. The anode cylinder
13. Procedure
should be approximately 12 mm in diameter and 50 mm in
13.1 Transfer 5.00 g of sample to a 300-mL electrolysis
height and the overall height of the anode should be approxi-
beaker. Add 42 mL of the H SO -HNO mixture, cover, and
2 4 3
mately 130 mm. A gauze anode of these dimensions will have
allow to stand a few minutes until the reaction has nearly
a surface area of 54 cm exclusive of the stem.
ceased.Heatat80°Cto90°Cuntildissolutioniscompleteand
7.1.3 Gauze cathodes are recommended where rapid elec-
brown fumes have been expelled. Wash down the cover glass
trolysis is used.
and the sides of the beaker and dilute to about 175 mL(enough
8. Reagents
to submerge the cathode when it is inserted).
8.1 AmmoniumAcetate Solution (500 g/L)—Dissolve 500 g
...

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