ASTM E129-74(1993)E01

Test Method for Spectrographic Analysis of Thermionic Nickel Alloys by the Powder Techniques (Withdrawn 1999)

SCOPE
1.1 This test method covers the determination of the following elements in thermionic nickel alloys in the concentration ranges shown:  
1.2 The test method has been designed for inspection testing of nickel alloy thermionic cathodes. It is equally applicable to the determination of the elements listed in 1.1 in any nickel alloy where the nickel content is greater than 98.0%, provided the total sample available exceeds 50 mg.  Note 1-The concentration ranges of the elements listed in 1.1 have been established through cooperative testing of secondary standards and by preparation of synthetic standards provided in the method. The scope is underwritten by three primary spectrochemical standards.  Cooperative testing of the first two of these standards has provided supporting data for this method.  
1.3 The values stated in inch-pound units are to be regarded as the standard.  
1.4 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 appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Withdrawn
• Publication Date: 31-Dec-1992
• Withdrawal Date: 09-May-1999
• Technical Committee: E01 - Analytical Chemistry for Metals, Ores, and Related Materials
• Drafting Committee: E01.08 - Ni and Co and High Temperature Alloys

Standards Content (Sample)

ASTM EL29 74 - 0759510 0533956 8Lb m
AMERICAN SOCIETY FOR TESTING AND MATERIALS
Designation: E 129 - 74 (Reapproved 1993)”
1916 Race St. Philadelohia. Pa 19103
Reprinted from the Annual Book of AS&4 &andards. Copyright ASTM
If not listed in the current combined index, will appear in the next edition.
Standard Test Method for
Spectrographic Analysis of Thermionic Nickel Alloys by the
Powder Technique’
This standard is issued under the fixed designation E 129; 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 reapprowL
‘I NOTE-Section 17 was added editorially in December 1993.
E 115 Practice for Photographic Processing in Optical
1. Scope
Emission Spectrographic Analysis4
1.1 This test method covers the determination of the fol-
E 116 Practice for Photographic Photometry in Spectro-
lowing elements in thermionic nickel alloys in the concentra-
chemical Analysis4
tion ranges shown:
E 130 Practice for Designation of Shapes and Sixes of
Concentration Range, %
Element
Graphite Electrodes4
0.01 to 1.0
Cobalt
E 135 Terminology Relating to Analytical Chemistry for
0.001 to 0.50
Copper
Metals, Ores, and Related Materials4
Iron 0.005 to 0.30
Magnesium 0.005 to 0.30
3. Terminology
0.005 to 0.30
Manganese
Aluminum 0.003 to 0.30
3.1 Definitions-For definitions of terms used in this test
0.003 to 0.10
Chromium
method, refer to Terminology E 135.
0.003 to 0. IO
Silicon
Titanium 0.003 to 0. IO
4. Summary of Test Method
1.2 The test method has been designed for inspection
4.1 The sample is dissolved in dilute nitric acid and
testing of nickel alloy thermionic cathodes. It is equally
evaporated to dryness and baked. The oxide powder is then
applicable to the determination of the elements listed in 1.1
in any nickel alloy where the nickel content is greater than mixed with graphite powder which acts as a buffer and
98.0 %, provided the total sample available exceeds 50 mg. diluent. This mixture is packed into the crater of a graphite
cup. Direct-current arc excitation is employed. The spectra
NOTE l-The concentration ranges of the elements listed in 1.1 have
are recorded photographically. Intensity ratios of selected
been established through cooperative testing of secondary standards and
pairs of analytical lines and internal standard nickel lines are
by preparation of synthetic standards provided in the method. The scope
is underwritten by three primary spectrochemical standank Coopera- determined photometrically. The concentration of each
tive testing of the first two of these standards has provided supporting
element is read from an analytical curve relating the log
data for this method.’
intensity ratio to log concentration.
1.3 The values stated in inch-pound units are to be
5. Apparatus
regarded as the standard.
5.1 Sample Preparation Equipment-A mortar and pestle
1.4 This standard does not purport to address all of the
made of material that will not contaminate the sample with
safety problems, if any, associated with its use. It is the
any of the elements to be determined, or a dental
responsibility of the user of this standard to establish appro-
amalgamatofl utilizing a plastic vial and a plastic ball. If a
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. mortar and pestle are used, highly polished agate may be
employed for alI determinations except silicon, highly pol-
ished sapphire for all determinations except aluminum, or
2. Referenced Documents
high polished tool steel for all determinations except iron.
2.1 ASTM Standards: 5.2 Excitation Source-A d-c arc source capable of pro-
E 50 Practices for Apparatus, Reagents, and Safety Pre- viding a current of 8.0 to 12.0 A.
cautions for Chemical Analysis of Metals4
5.3 Spectrograph, having sufficient resolving power and
linear dispersion to separate clearly the analytical lines from
other lines in the spectrum of the sample in the spectral
* This test method is under the jurisdiction of ASTM Committee E-l on
region 2400 to 4500 A. These conditions are satisfied by
Analytical Chemistry of Metals, Ores and Related Materials and is the direct
instruments having a reciprocal linear dispersion of 5 to 7
responsibility of Subcommittee E01.08 on Ni and Co and High Temperature
A/mm at 2800 A,
Alloys.
Current edition approved April 29, 1974. Published June 1974. Originally
5.4 Photographic Processing Equipment, providing devel-
published as E 129 - 57 T. Last previous edition E 129 - 61 (1972).
oping, fixing, washing, and drying operations and con-
2 National Institute of Standards and Technology nickel oxide standards Nos.
67 I, 672, and 673.
3 Appendix I to 1957 Report of Committee E-2, Proceedings, ASTEA, Am. Sot.
Testing Mats., Vol 57, 1957.
’ A dental amalgamator suitable for this purpose is sold under the trade name
l Annual Book of ASTM Slandards, Vol 03.05.
“Wig&Bug.”
ASTM EL29 74 - 0759530 0533957 752 -
(16 E 129
9. Preparations of Samples
forming to the requirements of Practice E 115.
5.5 Microphotometer, having a precision of f 1.0 % for
9.1 Dissolve samples in HNOs( 1+ 1). Approximately 0.5 g
transmittances between 5 and 90 %.
of representative sample shall be used if available, but a
5.6 Calculating Equipment-The use of a calculating
complete analysis can be made on 50 mg if the sample is
board shall be optional.
limited. Evaporate the solution to dryness in a platinum
evaporating dish and bake at WC for 20 min. Grind and
6. Reagents and Materials
mix thoroughly with a suitable mortar and pestle. Mix a
6.1 Purity and Concentration of Reagents-The purity portion of this powder with three parts by weight of graphite
and concentration of chemical reagents shall conform to the
powder.
requirements prescribed in Practices E 50.
10. Electrode System
6.2 Graphite Powder, highest purity obtainable, passing a
No. 100 (15~urn) sieve. 10.1 Place the sample electrode, filed level-full with stand-
6.3 Electrodes, high-putity graphite. The sample electrode ard or sample, in the lower electrode holder (anode). If the S-
shall be high-purity Type S-4 or S- 15 and the counter elec- 4 electrode is used, hold it in a water-cooled clamp, ifpossible,
trode high-purity Type C-6 or C-9 as described in Practice
for best resuhs. Position the external optics, including the
E 130. The electrode pair shah be standardized within the
gap, in such a manner that the resulting spectral lines
laboratory. represent radiant energy from the entire arc column, except
6.4 Metals or Metal Salts-Nickel, cobalt, copper, iron,
that both electrode tips shall be screened out. These condi-
magnesium, manganese, aluminum, chromium, and tita-
tions should be satisfied with an analytical gap of 3.0 mm.
nium as pure metals or as pure metal salts soluble in HNOs
11. Excitation and Exposure
(1+1).
6.5 Photographic Emulsions-Eastman Process, SA No, 1,
11.1 Produce and record the spectrum in accordance with
SA No. 2, or equivalent. Either films or plates may be used.
the following conditions:
6.6 Photographic Processing Solutions-The formulas for
Il. I. 1 Electrical Parameters:
proce
...