ASTM D6402-99(2009)
(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:
The temperature conditions under which the solutions were prepared and stored and the temperature at which the current analysis is performed;
The uniformity and consistency of the Kaolin paste layer deposited onto the filter paper;
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 analysis 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 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.
General Information
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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: D6402 − 99 (Reapproved2009)
Standard Test Method for
Determining Soluble Solids and Insolubles in Extracts of
Vegetable Tanning Materials
This standard is issued under the fixed designation D6402; 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.
1. Scope 2.2 ALCA Methods:
A21 Soluble Solids and Insolubles
1.1 This test method is intended for use in determining the
quantity of soluble solids and insolubles in solutions of tannin
3. Terminology
extracts, water extracts of vegetable tanning materials, or
3.1 Definitions:
tanning liquors. This test method is applicable to the analysis
3.1.1 insolubles—non-volatile materials present in tannin
of liquid, solid, pasty, and powdered tannin extracts and to the
extracts and raw or spent materials that are dissolved or
water extracts of raw or spent materials.
suspended in water and do not pass through a filtering process
1.2 The values stated in SI units are to be regarded as
described in this method.
standard. No other units of measurement are included in this
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
tanninextracts(PracticesD4901orD4905)orthewaterextract
2. Referenced Documents
fromraworspentmaterials(PracticeD6405)isdriedovernight
2.1 ASTM Standards: in a forced-air oven (Test Method D4902) and the quantity of
D4901 Practice for Preparation of Solution of Liquid Veg-
solid residue remaining is determined and used to calculate the
etable Tannin Extracts total solids for that sample (Test Method D4903). Another
D4902 Test Method for Evaporation and Drying of Analyti-
aliquot of the same solution is passed through a specified
cal Solutions filtering procedure and the quantity of solid residue remaining
D4903 Test Method for Total Solids and Water in Vegetable
in the filtrate is determined and used to calculate the soluble
Tanning Material Extracts solids for that sample. The difference between the total solids
D4905 Practice for Preparation of Solution of Solid, Pasty
and the soluble solids is defined as the insolubles for that
and Powdered Vegetable Tannin Extracts sample.
D6403 Test Method for Determining Moisture in Raw and
5. Significance and Use
Spent Materials
D6405 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
which are insoluble solids in a solution of tannin extract or in
the water extract from raw or spent materials prepared for
tannin analysis.
This test method is under the jurisdiction ofASTM Committee D31 on Leather
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, 2009. Published July 2009. Originally
prepared from raw or spent materials.
approved in 1999. Last previous edition approved in 2004 as D6402 – 99 (2004).
DOI: 10.1520/D6402-99R09.
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 (2009)
5.3 The soluble solids are defined as the portion of the total standard filter paper. A 100 mL aliquot of the clear filtrate
solidswhicharedissolvedinthewaterandpassthroughafilter should have less than 0.001 g of residue after evaporation and
prepared by depositing a layer of Kaolin paste onto a standard oven-drying in a platinum dish.
filter paper.
6.9 Balance, analytical balance which will weigh up to 100
5.4 The insolubles are defined as the portion of the total g with an accuracy of 6 0.1 mg (6 0.0001 g).
solids which do not pass through the standard filter paper
6.10 Drying Oven, a forced-air convection oven (or
prepared with the layer of Kaolin paste.
mechanical-convection draft oven) capable of maintaining a
5.5 The results of this test method are dependent on a great temperature of 100 6 2.0°C.
many variables but particularly upon:
6.11 Thermometer, accurate to 6 0.2°C used to check and
5.5.1 The temperature conditions under which the solutions
monitor the oven set point.
were prepared and stored and the temperature at which the
6.12 Dessicator, any convenient form or size, using any
current analysis is performed;
normal dessicant.
5.5.2 The uniformity and consistency of the Kaolin paste
layer deposited onto the filter paper;
7. Test Specimen
5.5.3 The rate of solution run-out from the pipette; etc. It is,
7.1 The specimen shall consist of 100 mL of the solution
therefore, essential that the method be followed exactly in
prepared as described in Practices D4905, D4901,or D6405
order to obtain reproducible results both among specimens
and after passing through the filtering process described in this
within a laboratory and for analyses between laboratories.
test method.
6. Apparatus and Reagents
8. Procedure
6.1 Tannin Dish, crystallizing dish, borosilicate glass, 50
8.1 Place a pleated filter paper in a 100 to 125 mm funnel.
mm tall, 70 mm outside diameter. The bottom corner shall be
8.1.1 Fold the filter paper to contain 32 evenly divided
rounded to a radius of 6 mm, the bottom shall be flat and not
pleats.
cupped in the center, and the top edge shall be rounded and
8.2 Add to 2.0 g of kaolin in a clean glass container (a 250
polished.
mL beaker works well) 25 mL of the well-mixed analytical
6.2 Watch Glass, a suitable size (approximately 150 mm
solution (which has been prepared as described in Practices
diameter) to be used as a cover for the funnel and filter paper
D4901, D4905,or D6405) and stir the mixture with a glass
and a suitable size (75 mm) to be used as a cover for the tannin
stirring rod to form a smooth paste.Then add an additional 200
dishes.
mL of the well-mixed analytical solution (making 225 mL
6.3 Pipet, 100 mL capacity, preferably with a wide orifice total) and again stir the mixture to a uniform suspension.
approximately 2.4 mm ( ⁄32 in.) diameter and 15-25 sec
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