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ASTM E378-97

(Test Method)

Standard Test Method for Spectrographic Analysis of Silver by the Powder Technique (Withdrawn 2004)

Standard Test Method for Spectrographic Analysis of Silver by the Powder Technique (Withdrawn 2004)

SCOPE
1.1 This test method covers the spectrographic analysis of silver for the following elements in the ranges indicated:  Element Concentration Range, % Copper 0.0001 to 0.1 Lead 0.0001 to 0.05 Zinc 0.001 to 0.01 Bismuth 0.0001 to 0.01 Palladium 0.001 to 0.005 Chromium 0.0001 to 0.005 Iron 0.0001 to 0.005 Nickel 0.0001 to 0.005 Manganese 0.0001 to 0.005 Tin 0.0001 to 0.005
1.2 This test method is designed for the analysis of commercial and high-purity silver samples in the form of needles, chips, cast bars, or sheet stock.  
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.

General Information

Status
Withdrawn
Publication Date
09-Apr-1997
Withdrawal Date
18-Jul-2004
ICS
77.120.99 - Other non-ferrous metals and their alloys
Technical Committee
E01 - Analytical Chemistry for Metals, Ores, and Related Materials
Current Stage
Ref Project

Relations

Referred By
ASTM B413-97a(2021) - Standard Specification for Refined Silver
Effective Date
10-Apr-1997

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ASTM E378-97 - Standard Test Method for Spectrographic Analysis of Silver by the Powder Technique (Withdrawn 2004)ASTM E378-97 - Standard Test Method for Spectrographic Analysis of Silver by the Powder Technique (Withdrawn 2004)
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ASTM E378-97 - Standard Test Method for Spectrographic Analysis of Silver by the Powder Technique (Withdrawn 2004)
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Please contact ASTM International (www.astm.org) for the latest information.
Designation:E378–97
Standard Test Method for
Spectrographic Analysis of Silver by the Powder Technique
This standard is issued under the fixed designation E 378; 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 covers the spectrographic analysis of 3.1 For definitions of terms used in this test method, refer to
silver for the following elements in the ranges indicated: Terminology E 135E 135.
Element Concentration Range, %
4. Summary of Test Method
Copper 0.0001 to 0.1
Lead 0.0001 to 0.05
4.1 Samples and standards are prepared in the form of dry
Zinc 0.001 to 0.01
silver nitrate powder and packed into the craters of specially
Bismuth 0.0001 to 0.01
Palladium 0.001 to 0.005
shaped graphite cup electrodes.The spectra are produced using
Chromium 0.0001 to 0.005
dc arc excitation and recorded photographically. Intensity
Iron 0.0001 to 0.005
ratios of selected pairs of analytical lines and internal standard
Nickel 0.0001 to 0.005
Manganese 0.0001 to 0.005
lines are determined photometrically. Concentrations are read
Tin 0.0001 to 0.005
from an analytical curve relating log intensity ratio to log
1.2 This test method is designed for the analysis of com- concentration.
mercial and high-purity silver samples in the form of needles,
5. Significance and Use
chips, cast bars, or sheet stock.
1.3 This standard does not purport to address all of the 5.1 Refined silver is marketed on purity. This test method is
safety concerns, if any, associated with its use. It is the suitable for analysis of refined silver for compliance with
responsibility of the user of this standard to establish appro- Specification B 413B 413.
priate safety and health practices and determine the applica-
6. Apparatus
bility of regulatory limitations prior to use.
6.1 Excitation Source providing a 12-A dc arc.
2. Referenced Documents
6.2 Spectrograph having sufficient resolving power and
2.1 ASTM Standards: linear dispersion to separate the analytical lines from other
B 413 Specification for Refined Silver lines in the spectrum of the sample in the spectral region from
E50 Practices for Apparatus, Reagents and Safety Precau- 2500 to 3500 Å. An instrument having a reciprocal linear
tions for Chemical Analysis of Metals dispersion of 5 to 10 Å/mm in the first order satisfies these
E115 Practice for Photographic Processing in Optical conditions.
Emission Spectrographic Analysis 6.3 Photographic Processing Equipment providing devel-
E116 Practice for Photographic Photometry in Spectro- opment, fixing, washing, and drying operations and conform-
chemical Analysis ing to the requirements of Practice E 115E115.
E 130 Practice for Designation of Shapes and Sizes of 6.4 Microphotometer conforming to criteria of Practice
Graphite Electrodes E 409E 409.
E 135 Terminology Relating to Analytical Chemistry for 6.5 Calculating Board to convert microphotometer read-
Metals, Ores, and Related Materials ings to log intensity ratios and concentrations.
E 409 Practice For Description and Performance of the
7. Reagents and Materials
Microphotometer
7.1 Purity and Concentration of Reagents—The purity and
concentration of the chemical reagents used in preparing the
This test method is under the jurisdiction of ASTM Committee E-1 on
standards and samples shall conform to the requirements
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
prescribed in Practices E 50E50.
responsibility of Subcommittee E01.03 on Precious Metals.
Current edition approved April 10, 1997. Published June 1997. Originally
7.2 Electrodes—The sample electrode shall be high-purity
´1
published as E 378 – 68. Last previous edition E 378 – 83 (1992) .
Type S-4 and the counter electrode high-purity Type C-1 as
Annual Book of ASTM Standards, Vol 02.04.
3 described in Practice E 130E 130.
Annual Book of ASTM Standards, Vol 03.05.
Annual Book of ASTM Standards, Vol 03.06.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Please contact ASTM International (www.astm.org) for the latest information.
E378–97
TABLE 1 Analytical and Internal Standard Lines
7.3 Silver Nitrate, High-Purity.
˚
Element Analytical Line, A Concentration Range,
NOTE 1—Detection limits will be affected by the amount of impurity
Copper 3247.54 0.0001 to 0.005
elements contained in the silver nitrate.
2961.16 0.005 to 0.1
7.4 Metals and Metal Salts —Bismuth, copper, iron, lead,
Lead 2833.06 0.0001 to 0.005
nickel, palladium, and zinc as metals; chromium as chromium
2873.32 0.001 to 0.05
nitrate; manganese as manganese sulfate monohydrate; and tin
Zinc 3345.02 0.001 to 0.01
as sodium stannate.
7.5 Photographic Emulsion.
Bismuth 3067.72 0.0001 to 0.005
7.6 Photographic Processing Solutions— The formulas for
2897.98 0.001 to 0.01
photographic processing solutions are given in Practice
Palladium 3242.70 0.001 to 0.005
E115E115.
Chromium 3021.56 0.0001 to 0.005
2835.63
8. Preparation of Standards
8.1 SilverNitrateStockSolution(1mL = 1gAg)—Dissolve Iron 3021.07 0.0001 to 0.005
2999.51 0.001 to 0.005
315.0 g of high-purity silver nitrate (AgNO ) in 150 mL of
water in a 200-mL volumetric flask and dilute to volume.
Nickel 3002.49 0.0001 to 0.005
8.2 Element Stock Solutions (1 mL = 0.5 mg of each 3050.82
element)—Dissolve 100 mg of each metal in 10 mL of nitric
Manganese 2801.06 0.0001 to 0.005
acid (HNO , 1 + 1); dissolve 770 mg of chromium nitrate
2798.27
[Cr(NO ) ·9 H O] and 308 mg of manganese sulfate monohy-
3 2 2
Tin 2839.99 0.0001 to 0.005
drate (MnSO ·H O) in 10 mL of water; combine element
4 2
2863.33
solutions in a 200-mLvolumetric flask and dilute with water to
Silver 3099.12 internal standard
volume.
8.2.1 Diluted Stock Solution—Make dilutions of the ele-
ment stock solutions with water to contain 0.05 mg and 0.005
10. Preparation of Apparatus
mg of each element.
8.2.2 Tin Stock Solution (1 mL = 0.5 mg Sn)—Dissolve 225
10.1 Electrode System—Firmly pack the dried silver nitrate
mg of sodium stannate (NaSnO ·3H O) in water in a 200-mL
powder level full into the crater of a preformed graphite
3 2
volumetric flask and dilute to volume.
electrode Type S-4 and insert in the lower electrode holder as
the anode. Insert a Type C-1 counter electrode in the upper
NO
...

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