ASTM E1371-90(1999)

Standard Test Method for Gravimetric Determination of Phosphorus in Phosphorus-Copper Alloys or Phosphorus-Copper-Silver Alloys

SCOPE
1.1 This test method covers the gravimetric determination of phosphorus in phosphorus-copper or phosphorus-copper-silver alloys containing 1 to 15% phosphorus.
1.2 This standard does not purport to address 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: Historical
• Publication Date: 09-Feb-1999
• ICS: 77.040.30 - Chemical analysis of metals
• ICS: 77.120.30 - Copper and copper alloys
• Technical Committee: E01 - Analytical Chemistry for Metals, Ores, and Related Materials

Relations

• Replaced By: ASTM E1371-05 - Standard Test Method for Gravimetric Determination of Phosphorus in Phosphorus-Copper Alloys or Phosphorus-Copper-Silver Alloys (Withdrawn 2006)
• Effective Date: 25-Jul-2005
• Referred By: ASTM B950-22 - Standard Guide for Editorial Procedures and Form of Product Specifications for Copper and Copper Alloys
• Effective Date: 10-Feb-1999
• Referred By: ASTM B644-11(2017) - Standard Specification for Copper Alloy Addition Agents
• Effective Date: 10-Feb-1999

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: E 1371 – 90 (Reapproved 1999)
Standard Test Method for
Gravimetric Determination of Phosphorus in Phosphorus-
Copper Alloys or Phosphorus-Copper-Silver Alloys
This standard is issued under the fixed designation E 1371; 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 safely. It is expected that the work will be performed in a
properly equipped laboratory.
1.1 This test method covers the gravimetric determination
of phosphorus in phosphorus-copper or phosphorus-copper-
5. Interferences
silver alloys containing 1 to 15 % phosphorus.
5.1 Silver is complexed as diamminesilver (I). Copper is
1.2 This standard does not purport to address the safety
complexed as tetraminecopper (II).
concerns, if any, associated with its use. It is the responsibility
5.2 When present, tin interferes by forming insoluble stan-
of the user of this standard to establish appropriate safety and
nic phosphate. Other elements which form insoluble phos-
health practices and determine the applicability of regulatory
phates or hydroxides in ammoniacal solution also interfere.
limitations prior to use.
6. Apparatus and Reagents
2. Referenced Documents
6.1 Magnesium Chloride Precipitant—Dissolve 65 g of
2.1 ASTM Standards:
magnesium chloride (MgCl ) and 140 g of ammonium chloride
E 29 Practice for Using Significant Digits in Test Data to
2 (NH Cl) in 500 mL water, add 375 mL of NH OH, dilute to 1
4 4
Determine Conformance with Specifications
L with water, and mix.
E 173 Practice for Conducting Interlaboratory Studies of
3 6.2 Potassium Chlorate Solution—Dissolve 10 g of potas-
Methods for Chemical Analysis of Metals
sium chlorate (KClO ) in 200 mL water.
E 255 Practice for Sampling Copper and Copper Alloys for
Determination of Chemical Composition
7. Sampling
3. Summary of Test Method 7.1 Select the sample so as to be representative of the
material to be analyzed.
3.1 After dissolution of the sample in nitric acid, phospho-
7.2 For procedures for sampling the material, refer to
rus is precipitated with ammoniacal magnesium chloride.
Practice E 255.
Magnesium ammonium phosphate is separated by filtration and
redissolved with dilute hydrochloric acid. Phosphorus is repre-
8. Procedure
cipitated with ammoniacal magnesium chloride, then filtered,
8.1 Select and weigh a sample in accordance with the
ignited, and weighed as magnesium pyrophosphate.
following:
4. Significance and Use
Tolerance in Sample
Phosphorus, % Sample Weight, g
Weight, mg
4.1 This test method for the chemical analysis of metals and
alloys is primarily intended to test such materials for compli- 0.25 to 2.0 2.0 0.4
2.0 to 10.0 1.0 0.3
ance with compositional specifications. It is assumed that all
10.0 to 15.0 0.5 0.2
who use this method will be trained analysts capable of
8.2 Place the weighed sample in a 400-mL beaker. Add 20
performing common laboratory procedures skillfully and
mL of HNO (1 + 1). Heat to dissolve the sample and boil to
expel the oxides of nitrogen. Add 10 mL of potassium chlorate
solution to complete the oxidation of the phosphorus to
This test method is under the jurisdiction of ASTM Committee E-1 on
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
phosphate. Continue boiling and evaporate to between 5 and 10
responsibility of Subcommittee E01.03 on Precious Metals.
mL then cool. If crystals appear, add a few millilitres of water
Current edition approved July 27, 1990. Published September 1990.
2 to dissolve them. A faint cloudiness in the solution may
Annual Book of ASTM Standards, Vol 14.02.
Annual Book of ASTM Standards, Vol 03.05. indicate the presence of silver chloride.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E 1371
TABLE 1 Statistical Information—Phosphorus
8.3 Dilute to 125 mL and heat to boiling. Remove from heat
and carefully add 25 mL of magnesium chloride precipitant Phosphorus
Test Material R1, E173 R2, E173
Found, %
followed by 50 mL of NH OH. Stir with a glass rod, leaving
Copper Phosphorus Powder 2.37 .021 .039
the rod in the beaker. Cool overnight to allow for complete
2.50 % Phosphorus
precipitation.
Copper Phosphorus Powder 7.11 .075 .107
8.4 Set up a vacuum filter using a glass funnel and 12.5-cm
7.00 % Phosphorus
Copper Phosphorus Powder 14.19 .175 .273
low porosity, ashless filter paper with a 9-cm hardened ashless
15.0 % Phosphorus
filter paper as a support. Moisten these with water and pack
with enough filter pulp to fill the funnel about ⁄4 in. from the
bottom. Transfer the solution and precipitate to the funnel and
muffle furnace at 1700°F (927°C) and ignite for 1 h, or until the
rinse the beaker three times with NH OH (1 + 19). Some of the
4 precipitate is pure white. Cool in a desiccator and weigh.
precipitate may sti
...