ASTM D6402-99(2004)
(Test Method)Standard Test Method for Determing Soluble Solids and Insolubles in Extracts of Vegetable Tanning Materials
Standard Test Method for Determing Soluble Solids and Insolubles in Extracts of Vegetable Tanning Materials
SIGNIFICANCE AND USE
This test method is used to determine the proportion of the total solids which are soluble solids and that proportion which are insoluble solids in a solution of tannin extract or in the water extract from raw or spent materials prepared for tannin analysis.
The specimens are aliquots from the analytical solutions prepared from tannin extracts or the water extract solutions prepared from raw or spent materials.
The soluble solids are defined as the portion of the total solids which are dissolved in the water and pass through a filter prepared by depositing a layer of Kaolin paste onto a standard filter paper.
The insolubles are defined as the portion of the total solids which do not pass through the standard filter paper prepared with the layer of Kaolin paste.
The results of this test method are dependent on a great many variables but particularly upon:
5.5.1 The temperature conditions under which the solutions were prepared and stored and the temperature at which the current analysis is performed;
5.5.2 The uniformity and consistency of the Kaolin paste layer deposited onto the filter paper;
5.5.3 The rate of solution run-out from the pipette; etc. It is, therefore, essential that the method be followed exactly in order to obtain reproducible results both among specimens within a laboratory and for analyses between laboratories.
SCOPE
1.1 This test method is intended for use in determining the quantity of soluble solids and insolubles in solutions of tannin extracts, water extracts of vegetable tanning materials, or tanning liquors. This test method is applicable to the anlysis of liquid, solid, pasty, and powdered tannin extracts and to the water extracts of raw or spent materials.
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.
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Standards Content (Sample)
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Designation:D6402–99(Reapproved2004)
Standard Test Method for
Determining Soluble Solids and Insolubles in Extracts of
Vegetable Tanning Materials
This standard is issued under the fixed designation D 6402; 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 A21 Soluble Solids and Insolubles
1.1 This test method is intended for use in determining the
3. Terminology
quantity of soluble solids and insolubles in solutions of tannin
3.1 Definitions:
extracts, water extracts of vegetable tanning materials, or
3.1.1 insolubles—non-volatile materials present in tannin
tanning liquors. This test method is applicable to the analysis
extracts and raw or spent materials that are dissolved or
of liquid, solid, pasty, and powdered tannin extracts and to the
suspended in water and do not pass through a filtering process
water extracts of raw or spent materials.
described in this method.
1.2 The values stated in SI units are to be regarded as the
3.1.2 soluble solids—non-volatile materials present in tan-
standard.
nin extracts and raw or spent materials that are dissolved or
1.3 This standard does not purport to address all of the
suspended in water and pass through a filtering process
safety concerns, if any, associated with its use. It is the
described in this method.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
4. Summary of Test Method
bility of regulatory limitations prior to use.
4.1 An aliquot of the analytical solution prepared from
tannin extracts (Practices D 4901 or D 4905) or the water
2. Referenced Documents
extract from raw or spent materials (Practice D 6405) is dried
2.1 ASTM Standards:
overnight in a forced-air oven (Test Method D 4902) and the
D 4901 Practice for Preparation of Solution of Liquid Veg-
quantity of solid residue remaining is determined and used to
etable Tannin Extracts
calculate the total solids for that sample (Test Method D 4903).
D 4902 Test Method for Evaporation and Drying of Ana-
Another aliquot of the same solution is passed through a
lytical Solutions
specified filtering procedure and the quantity of solid residue
D 4903 TestMethodforTotalSolidsandWaterinVegetable
remaining in the filtrate is determined and used to calculate the
Tanning Material Extracts
soluble solids for that sample. The difference between the total
D 4905 Practice for Preparation of Solution of Solid, Pasty,
solidsandthesolublesolidsisdefinedastheinsolublesforthat
and Powdered Vegetable Tannin Extracts
sample.
D 6403 Test Method for Determining Moisture in Raw and
Spent Materials
5. Significance and Use
D 6405 Practice for Extraction of Tannins from Raw and
5.1 This test method is used to determine the proportion of
Spent Materials
the total solids which are soluble solids and that proportion
2.2 ALCA Methods:
which are insoluble solids in a solution of tannin extract or in
the water extract from raw or spent materials prepared for
This test method is under the jurisdiction ofASTM Committee D31 on Leather
tannin analysis.
and is the direct responsibility of Subcommittee D31.01 on Vegetable Leather. This
5.2 The specimens are aliquots from the analytical solutions
test method has been adapted from and is a replacement for Method A21 of the
prepared from tannin extracts or the water extract solutions
Official Methods of the American Leather Chemists Association.
Current edition approved April 1, 2004. Published May 2004. Originally prepared from raw or spent materials.
approved in 1999. Last previous edition approved in 1999 as D 6402 – 99.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Official Methods of the American Leather Chemists Association. Available
Standards volume information, refer to the standard’s Document Summary page on from the American Leather Chemists Association, University of Cincinnati, P.O.
the ASTM website. Box 210014, Cincinnati, OH 45221-0014.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D6402–99 (2004)
5.3 The soluble solids are defined as the portion of the total 6.9 Balance, analytical balance which will weigh up to 100
solidswhicharedissolvedinthewaterandpassthroughafilter g with an accuracy of 6 0.1 mg (6 0.0001 g).
prepared by depositing a layer of Kaolin paste onto a standard 6.10 Drying Oven, a forced-air convection oven (or
filter paper. mechanical-convection draft oven) capable of maintaining a
5.4 The insolubles are defined as the portion of the total temperature of 100 6 2.0°C.
solids which do not pass through the standard filter paper 6.11 Thermometer, accurate to 6 0.2°C used to check and
prepared with the layer of Kaolin paste.
monitor the oven set point.
5.5 The results of this test method are dependent on a great 6.12 Dessicator, any convenient form or size, using any
many variables but particularly upon:
normal dessicant.
5.5.1 The temperature conditions under which the solutions
were prepared and stored and the temperature at which the
7. Test Specimen
current analysis is performed;
7.1 The specimen shall consist of 100 mL of the solution
5.5.2 The uniformity and consistency of the Kaolin paste
prepared as described in Practices D 4905, D 4901, or D 6405
layer deposited onto the filter paper;
and after passing through the filtering process described in this
5.5.3 The rate of solution run-out from the pipette; etc. It is,
test method.
therefore, essential that the method be followed exactly in
order to obtain reproducible results both among specimens
8. Procedure
within a laboratory and for analyses between laboratories.
8.1 Place a pleated filter paper in a 100 to 125 mm funnel.
6. Apparatus and Reagents 8.1.1 Fold the filter paper to contain 32 evenly divided
pleats.
6.1 Tannin Dish, crystallizing dish, borosilicate glass, 50
8.2 Add to 2.0 g of kaolin in a clean glass container (a 250
mm tall, 70 mm outside diameter. The bottom corner shall be
mL beaker works well) 25 mL of the well-mixed analytical
rounded to a radius of 6 mm, the bottom shall be flat and not
solution (which has been prepared as described in Practices
cupped in the center, and the top edge shall be rounded and
D 4901, D 4905, or D 6405) and stir the mixture with a glass
polished.
stirring rod to form a smooth paste.Then add an additional 200
6.2 Watch Glass, a suitable size (approximately 150 mm
mL of the well-mixed analytical solution (making 225 mL
diameter) to be used as a cover for the funnel and filter paper
total) and again stir the mixture to a uniform suspension.
and a suitable size (75 mm) to be used as a cover for the tannin
Immediately pour the suspension onto the pleated filter paper
dishes.
in the funnel and collect the filtrate in the container in which
6.3 Pipet, 100 mL capacity, preferably with a wide orifice
3 the solution and kaolin were mixed. After approximately 40
ap
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