ASTM D6402-99
(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
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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Designation: D 6402 – 99
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 3. Terminology
1.1 This test method is intended for use in determining the 3.1 Definitions:
quantity of soluble solids and insolubles in solutions of tannin 3.1.1 insolubles—non-volatile materials present in tannin
extracts, water extracts of vegetable tanning materials, or extracts and raw or spent materials that are dissolved or
tanning liquors. This test method is applicable to the analysis suspended in water and do not pass through a filtering process
of liquid, solid, pasty, and powdered tannin extracts and to the described in this method.
water extracts of raw or spent materials. 3.1.2 soluble solids—non-volatile materials present in tan-
1.2 The values stated in SI units are to be regarded as the nin extracts and raw or spent materials that are dissolved or
standard. suspended in water and pass through a filtering process
1.3 This standard does not purport to address all of the described in this method.
safety concerns, if any, associated with its use. It is the
4. Summary of Test Method
responsibility of the user of this standard to establish appro-
4.1 An aliquot of the analytical solution prepared from
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. tannin extracts (Practices D 4901 or D 4905) or the water
extract from raw or spent materials (Practice D 6405) is dried
2. Referenced Documents
overnight in a forced-air oven (Test Method D 4902) and the
2.1 ASTM Standards: quantity of solid residue remaining is determined and used to
D 4901 Practice for Preparation of Solution of Liquid Veg- calculate the total solids for that sample (Test Method D 4903).
etable Tannin Extracts Another aliquot of the same solution is passed through a
D 4902 Test Method for Evaporation and Drying of Ana- specified filtering procedure and the quantity of solid residue
lytical Solutions remaining in the filtrate is determined and used to calculate the
D 4903 Test Method for Total Solids and Water in Vegetable soluble solids for that sample. The difference between the total
Tanning Material Extracts solids and the soluble solids is defined as the insolubles for that
D 4905 Practice for Preparation of Solution of Solid, Pasty, sample.
and Powdered Vegetable Tannin Extracts
5. Significance and Use
D 6403 Test Method for Determining Moisture in Raw and
5.1 This test method is used to determine the proportion of
Spent Materials
D 6405 Practice for Extraction of Tannins from Raw and the total solids which are soluble solids and that proportion
which are insoluble solids in a solution of tannin extract or in
Spent Materials
2.2 ALCA Methods: the water extract from raw or spent materials prepared for
tannin analysis.
A21 Soluble Solids and Insolubles
5.2 The specimens are aliquots from the analytical solutions
prepared from tannin extracts or the water extract solutions
prepared from raw or spent materials.
This test method is under the jurisdiction of ASTM Committee D-31 on Leather
5.3 The soluble solids are defined as the portion of the total
and is the direct responsibility of Subcommittee D31.01 on Vegetable Leather. This
solids which are dissolved in the water and pass through a filter
test method has been adapted from and is a replacement for Method A21 of the
prepared by depositing a layer of Kaolin paste onto a standard
Official Methods of the American Leather Chemists Association.
Current edition approved May 10, 1999. Published August 1999.
filter paper.
Annual Book of ASTM Standards, Vol 15.04.
5.4 The insolubles are defined as the portion of the total
Official Methods of the American Leather Chemists Association. Available
solids which do not pass through the standard filter paper
from the American Leather Chemists Association, University of Cincinnati, P.O.
Box 210014, Cincinnati, OH 45221-0014. prepared with the layer of Kaolin paste.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 6402
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.
8.1.1 Fold the filter paper to contain 32 evenly divided
6. Apparatus and Reagents
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
approximately 2.4 mm ( ⁄32 in.) diameter and 15-25 second
mL of the filtrate has been collected, swirl it, to pick up kaolin
delivery time.
remaining on the sides and bottom of the container, and return
6.4 Graduated Cylinder, standard laboratory grade with at
to the funnel. During this and subsequent operations, keep
least 225 mL capacity.
funnels and containers covered with watch glasses to avoid
6.5 Glass Rods, soft glass stirring rods with rounded,
changes due to evaporation, and maintain the te
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