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

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 the 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.

General Information

Status
Historical
Publication Date
14-May-1995
Technical Committee
Drafting Committee
Current Stage
Ref Project

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ASTM D4655-95(2001) - Standard Test Methods for Sulfates in Leather (Total, Neutral, and Combined Acid)
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D 4655 – 95 (Reapproved 2001)
Standard Test Methods for
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Sulfates in Leather (Total, Neutral, and Combined Acid)
This standard is issued under the fixed designation D 4655; 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 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
1.1 These test methods are intended for use in determining
methylene blue, both in 95 % alcohol.
the total, neutral, and combined acid sulfate in mineral-tanned
leather.
6. Sampling, Test Specimens, and Test Units
1.2 The values stated in SI units are to be regarded as the
6.1 The specimen for each determination shall consist of 1
standard.
g leather from the composite sample (See Practice D 2813).
1.3 This standard does not purport to address all of the
6.2 Two specimens from the composite sample shall be
safety concerns, if any, associated with its use. It is the
tested for each determination.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
7. Procedure
bility of regulatory limitations prior to use.
7.1 Total Sulfates—Weigh the specimen to the nearest
2. Referenced Documents milligram and record the value asW .Transfer the specimen to
1
a 250-mL volumetric flask and add 200 mL of 0.1 N ammo-
2.1 ASTM Standards:
nium hydroxide or 0.1 molar potassium or sodium dihydrogen
D 2813 Practice for Sampling Leather for Physical and
2 phosphate solution. Immerse the flask up to the neck in a bath
Chemical Tests
2 of boiling water. Thoroughly wet all products by swirling
D 4654 Test Method for Sulfate Basicity in Leather
occasionally.After 2 h cool the flask to room temperature, and
3. Significance and Use make up to volume with distilled water, shake, and without
delay filter through a folded filter paper. Discard the first 20 to
3.1 These test methods are used to determine the basicity of
25 mL of the filtrate. Pipette 200 mL of the filtrate into a 600
leather when used in accordance with Test Method D 4654.
mL beaker and add about 20 mL of 1.5 N hydrochloric acid.
4. Apparatus
Heat the solution to boiling and while boiling and stirring the
solution, add 20 mL of a 1 % solution of barium chloride
4.1 Volumetric Flask, 250 mL.
dropwise. Keep the covered beaker in a warm place at least for
4.2 Filter paper, ashless, fine grained and porcelain crucible.
2 h and preferably overnight.
4.3 Crucible, Gooch, with porous porcelain filter (optional).
7.1.1 Filter the precipitate through a fine grained ashless
5. Reagents
filter paper and wash with hot water until free from chloride.A
weighed Gooch crucible or a weighed porous crucible may be
5.1 Ammonium Hydroxide Solution, (0.1 N)—7 mL/L re-
used as an alternative for the filtration. Transfer the paper with
agentgradeconcentrateNH OH.Optional:Potassiumdihydro-
4
the precipitate to a weighed crucible and ignite gently, either
gen phosphate, 0.1 molar solution (13.6 g/L KH PO)or
2 4
over a gas burner or in a muffle oven at 900°C for 1 h. Cool the
sodium dihydrogen phosphate, 0.1 molar solution (13.8 g/ L
crucible in a desiccator, weigh, and record the value of the
NaH PO -H O).
2 4 2
BaSO as W .
5.2 HydrochloricAcid Solution, (1.5 N)—125 mL/Lreagent 4 2
7.2 Neutral Sulfates—Weigh the specimen to the nearest
grade concentrate hydrochloric acid.
milligram and record the value asW .Transfer the specimen to
5.3 Barium Chloride Solution—(BaCl ·2H O), 1 %. 3
2 2
a 250-mL volumetric flask and add 200 mL of distilled water.
5.4 Sodium Hydroxide Solution, 0.01 N, 0.4 g/L.
Immerse the flask up to the neck in boiling water. Thoroughly
wet all particles by swirling occasionally. After 2 h cool flask
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These test methods are under the jurisdiction of ASTM Committee D31 on
to room temperature, make up to volume with distilled water,
Leather and are the direct responsibility of Subcommittee D31.06 on Chemical
shake and without delay filter through a folded filter. Discard
Analysis—General. This test method was developed in cooperation with the
thefirst20to25mLofthefiltrate.Pipette200mLofthefiltrate
American Leather Chemists Assn. (Method D 20–1956).
Current edition approved May 15, 1995. Published July 1995. Originally into a 600-mL beaker and titrate with 0.01 N sodium hydrox-
e1
published as D 4655 – 87. Last previous edition D 4655 – 87 (1993) .
ide, using a few drops of the methyl red/methylene blue
2
Annual Book of ASTM Standards, Vol 15.04.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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