ASTM D4655-95(2017)

Standard Test Methods for Sulfates in Leather (Total, Neutral, and Combined Acid)

SIGNIFICANCE AND USE
3.1 These test methods are used to determine the basicity of leather when used in accordance with Test Method D4654.
SCOPE
1.1 These test methods are intended for use in determining the total, neutral, and combined acid sulfate in mineral-tanned leather.  
1.2 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.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Historical
• Publication Date: 31-Mar-2017
• ICS: 59.140.30 - Leather and furs
• Technical Committee: D31 - Leather
• Drafting Committee: D31.06 - Chemical Analysis

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D4655 − 95 (Reapproved 2017)
Standard Test Methods for
1
Sulfates in Leather (Total, Neutral, and Combined Acid)
This standard is issued under the fixed designation D4655; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope 4.3 Crucible, Gooch, with porous porcelain filter (optional).
1.1 These test methods are intended for use in determining
5. Reagents
the total, neutral, and combined acid sulfate in mineral-tanned
5.1 Ammonium Hydroxide Solution, (0.1 N)—7 mL/L re-
leather.
agent grade concentrate NH OH. Optional: Potassium dihydro-
4
1.2 The values stated in SI units are to be regarded as
gen phosphate, 0.1 molar solution (13.6 g/L KH PO ) or
2 4
standard. No other units of measurement are included in this
sodium dihydrogen phosphate, 0.1 molar solution (13.8 g/ L
standard.
NaH PO -H O).
2 4 2
1.3 This standard does not purport to address all of the
5.2 Hydrochloric Acid Solution, (1.5 N)—125 mL/L reagent
safety concerns, if any, associated with its use. It is the
grade concentrate hydrochloric acid.
responsibility of the user of this standard to establish appro-
5.3 Barium Chloride Solution—(BaCl ·2H O), 1 %.
priate safety and health practices and determine the applica- 2 2
bility of regulatory limitations prior to use.
5.4 Sodium Hydroxide Solution, 0.01 N, 0.4 g/L.
1.4 This international standard was developed in accor-
5.5 Mixed Indicator, consisting of 60 mL of a 0.1 % solution
dance with internationally recognized principles on standard-
of methyl red and 40 mL of a 0.1 % solution of methylene blue,
ization established in the Decision on Principles for the
both in 95 % alcohol.
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
6. Sampling, Test Specimens, and Test Units
Barriers to Trade (TBT) Committee.
6.1 The specimen for each determination shall consist of 1
2. Referenced Documents g leather from the composite sample (See Practice D2813).
2
2.1 ASTM Standards:
6.2 Two specimens from the composite sample shall be
D2813 Practice for Sampling Leather for Physical and tested for each determination.
Chemical Tests
7. Procedure
D4654 Test Method for Sulfate Basicity in Leather
7.1 Total Sulfates—Weigh the specimen to the nearest mil-
3. Significance and Use
ligram and record the value as W . Transfer the specimen to a
1
3.1 These test methods are used to determine the basicity of
250-mL volumetric flask and add 200 mL of 0.1 N ammonium
leather when used in accordance with Test Method D4654.
hydroxide or 0.1 molar potassium or sodium dihydrogen
phosphate solution. Immerse the flask up to the neck in a bath
4. Apparatus
of boiling water. Thoroughly wet all products by swirling
4.1 Volumetric Flask, 250 mL.
occasionally. After 2 h cool the flask to room temperature, and
make up to volume with distilled water, shake, and without
4.2 Filter paper, ashless, fine grained and porcelain crucible.
delay filter through a folded filter paper. Discard the first 20 to
1
25 mL of the filtrate. Pipette 200 mL of the filtrate into a 600
These test methods are under the jurisdiction of ASTM Committee D31 on
Leather and are the direct responsibility of Subcommittee D31.06 on Chemical mL beaker and add about 20 mL of 1.5 N hydrochloric acid.
Analysis. This test method was developed in cooperation with the American Leather
Heat the solution to boiling and while boiling and stirring the
Chemists Assn. (Method D20–1956).
solution, add 20 mL of a 1 % solution of barium chloride
Current edition approved April 1, 2017. Published April 2017. Originally
dropwise. Keep the covered beaker in a warm place at least for
approved in 1987. Last previous edition approved in 2012 as D4655–95 (2012).
DOI: 10.1520/D4655-95R17.
2 h and preferably overnight.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
7.1.1 Filter the precipitate through a fine grained ashless
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
filter paper and wash with hot water until free from chloride. A
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. weighed Gooch crucible or a weighed porous crucible may be
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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D4655 − 95 (2017)
used as an alternative for the filtration. Transfer the paper with % neutral sulfate ~SO !
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D4655 − 95 (Reapproved 2012) D4655 − 95 (Reapproved 2017)
Standard Test Methods for
1
Sulfates in Leather (Total, Neutral, and Combined Acid)
This standard is issued under the fixed designation D4655; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope
1.1 These test methods are intended for use in determining the total, neutral, and combined acid sulfate in mineral-tanned
leather.
1.2 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.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2
2.1 ASTM Standards:
D2813 Practice for Sampling Leather for Physical and Chemical Tests
D4654 Test Method for Sulfate Basicity in Leather
3. Significance and Use
3.1 These test methods are used to determine the basicity of leather when used in accordance with Test Method D4654.
4. Apparatus
4.1 Volumetric Flask, 250 mL.
4.2 Filter paper, ashless, fine grained and porcelain crucible.
4.3 Crucible, Gooch, with porous porcelain filter (optional).
5. Reagents
5.1 Ammonium Hydroxide Solution, (0.1N)—7 mL/L reagent grade concentrate NH OH. Optional: Potassium dihydrogen
4
phosphate, 0.1 molar solution (13.6 g/L KH PO ) or sodium dihydrogen phosphate, 0.1 molar solution (13.8 g/ L NaH PO -H O).
2 4 2 4 2
5.2 Hydrochloric Acid Solution, (1.5 N)—125 mL/L reagent grade concentrate hydrochloric acid.
5.3 Barium Chloride Solution—(BaCl ·2H O), 1 %.
2 2
5.4 Sodium Hydroxide Solution, 0.01 N, 0.4 g/L.
5.5 Mixed Indicator, consisting of 60 mL of a 0.1 % solution of methyl red and 40 mL of a 0.1 % solution of methylene blue,
both in 95 % alcohol.
1
These test methods are under the jurisdiction of ASTM Committee D31 on Leather and are the direct responsibility of Subcommittee D31.06 on Chemical Analysis. This
test method was developed in cooperation with the American Leather Chemists Assn. (Method D20–1956).
Current edition approved April 1, 2012April 1, 2017. Published April 2012 April 2017. Originally approved in 1987. Last previous edition approved in 20062012 as
D4655–95 (2006).(2012). DOI: 10.1520/D4655-95R12.10.1520/D4655-95R17.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D4655 − 95 (2017)
6. Sampling, Test Specimens, and Test Units
6.1 The specimen for each determination shall consist of 1 g leather from the composite sample (See Practice D2813).
6.2 Two specimens from the composite sample shall be tested for each determination.
7. Procedure
7.1 Total Sulfates—Weigh the specimen to the nearest milligram and record the value as W . Transfer the specimen to a 250-mL
1
volumetric flask and add 200 mL of 0.1 N ammonium hydroxide or 0.1 molar potassium or sodium dihydrogen phosphate solution.
Immerse the flask up to the neck in a bath of boiling water. Thoroughly wet all products by swirling occasionally. After 2 h cool
the flask to room temperature, and make up to volume with distilled water, shake, and without delay filter through a folded filter
paper. Discard the first 20 to 25 mL of the filtrate. Pipette 200 mL of the filtrate into a 600 mL beaker and add about 20 mL of
1.5 N hydrochloric acid. Heat the solution to boiling and while boiling and stirring the solution, add 20 mL of a 1 % solution of
barium chloride dropwise. Keep the covered beaker
...