ASTM D6406-99

Standard Test Method for Analysis of Sugar in Vegetable Tanning Materials

SCOPE
1.1 This test method covers determining the sugars present in vegetable tanning materials.
1.2 The values stated in SI units are to be regarded as the standard. The inch-pound units given in parentheses are for information only.
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: 09-May-1999
• ICS: 59.140.10 - Processes and auxiliary materials
• Technical Committee: D31 - Leather
• Drafting Committee: D31.01 - Vegetable Leather

Relations

• Replaced By: ASTM D6406-99(2004) - Standard Test Method for Analysis of Sugar in Vegetable Tanning Materials
• Effective Date: 01-Apr-2004
• Referred By: ASTM D4899-99(2020) - Standard Practice for Analysis of Vegetable Tanning Materials—General
• Effective Date: 10-May-1999

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D 6406 – 99
Standard Test Method for
Analysis of Sugar in Vegetable Tanning Materials
This standard is issued under the fixed designation D 6406; 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 3.1.2 glucose—a simple sugar with formula C H O , and
6 12 6
known to exist in d-, l-, and racemic forms. The term
1.1 This test method covers determining the sugars present
commonly refers to the sweet, colorless, water-soluble dex-
in vegetable tanning materials.
trorotatory form that occurs widely in nature and is the usual
1.2 The values stated in SI units are to be regarded as the
form in which carbohydrate is assimilated by animals. The
standard. The inch-pound units given in parentheses are for
term glucose can also refer to a light-colored syrup made from
information only.
corn starch.
1.3 This standard does not purport to address all of the
3.1.3 sugar—any of various water-soluble compounds that
safety concerns, if any, associated with its use. It is the
vary widely in sweetness and comprise the oligosaccharides
responsibility of the user of this standard to establish appro-
including sucrose.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
4. Summary of Test Method
2. Referenced Documents 4.1 An analytical strength solution (that is, 4.00 6 0.25 g
tannin per litre) of the tanning material is analyzed for reducing
2.1 ASTM Standards:
sugars and total sugars by the Munson and Walker procedure.
D 4901 Practice for Preparation of Solution of Liquid Veg-
etable Tannin Extracts
5. Significance and Use
D 4905 Practice for Preparation of Solution of Solid, Pasty,
2 5.1 This test method is used to determine the quantity of
and Powdered Vegetable Tannin Extracts
sugar present in vegetable tanning materials or vegetable
D 6401 Test Method for Determining Non-Tannins and
2 tannin extracts. The amount of the reducing sugars, total
Tannin in Extracts of Vegetable Tanning Materials
sugars, and non-reducing sugars in a sample of material or
D 6403 Test Method for Determining Moisture in Raw and
2 extract can be determined by this method.
Spent Materials
5.2 Because of the possibility of errors in this test method it
D 6404 Practice for Sampling Vegetable Materials Contain-
2 is essential that the method be followed exactly in order to
ing Tannin
obtain reproducible results both among specimens within a
D 6405 Practice for Extraction of Tannins from Raw and
2 laboratory and for analyses between laboratories.
Spent Materials
D 6408 Test Method for Analysis of Tannery Liquors
6. Apparatus and Reagents
2.2 ALCA Methods:
3 6.1 Saturated Solution of Normal Lead Acetate.
A30 Sugar in Tanning Materials
6.2 Dipotassium Hydrogen Phosphate, Anhydrous
3. Terminology (K HPO ), dried in an oven at 100°C for 16 h then stored in a
2 4
tightly stoppered bottle.
3.1 Definitions:
6.3 Toluene, assay $ 99.5 %.
3.1.1 dextrose—d-glucose.
6.4 Fehling’s Solutions, A and B.
6.5 Hydrochloric Acid, concentrated (sp.gr. 1.18).
This test method is under the jurisdiction of ASTM Committee D-31 on Leather
6.6 Kerosene, commercial grade.
and is the direct responsibility of Subcommittee D31.01 on Vegetable Leather. This
6.7 Saturated Solution of Sodium Hydroxide.
method has been adapted from and is a replacement for Method A30 of the Official
6.8 Phenolphthalein Solution, 0.5 g dissolved in 100 mL of
Methods of the American Leather Chemists Association.
Current edition approved May 10, 1999. Published August 1999. 95 % ethanol.
Annual Book of ASTM Standards, Vol 15.04.
6.9 Tartaric Acid, powdered.
Official Methods of the American Leather Chemists Association. Available
from the American Leather Chemists Association, University of Cincinnati, P.O.
Box 210014, Cincinnati, OH 45221-0014.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 6406
6.10 Copper Sulfate Solution, prepared by dissolving 7. Test Specimen
69.278 g of CuSO •5H O in 1 L of distilled water and filtering
4 2
7.1 The specimen for the sugar analysis shall consist of 400
through asbestos.
mL of a solution of the tanning material of analytical strength
6.11 Alkaline Tartrate Solution, prepared by dissolving 346
(4.006 0.25 g tannin per L).
g of Rochelle salt (sodium potassium tartrate tetrahydrate) and
8. Procedure
100 g of sodium hydroxide in 1 L of distilled water. After
standing for two days the solution shall be filtered through
8.1 Sample the tanning material using Practice D 6404, and
asbestos.
prepare the analytical solution as described in Practices
6.12 Alcohol, 95 % ethyl alcohol.
D 4901, D 4905, D 6405, or D 6408.
6.13 Ether, diethyl ether.
8.2 Detannization of Analytical Solution:
6.14 Filter Paper , 21.5 cm diameter, pleated to contain 32
8.2.1 Add to 400 mL of the analytical solution 50 mL of a
evenly divided creases.
saturated lead acetate solution. Shake the mixture well and
6.15 Funnel, 100-125 mm top diameter, 60° angle bowl, and
allow to stand for 5 to 10 min.
150 mm stem length.
NOTE 1—It is important that the mixture of liquor and lead acetate
6.16 Watch Glasses, a suitable size (approximately 150 mm
solution be very well shaken. Good results are obtained by placing the
diameter) to be used as a cover for the funnel and filter paper.
solution mixture in shake bottles and running in the shake machine for 10
6.17 Graduated Cylinder, standard laboratory grade with
min (as described in Test Method D 6401) to ensure complete detanniza-
500 mL capacity.
tion of the liquor. The mixture filters better after complete detannization.
Complete detannization also results in less danger of residual quantities of
6.18 Pipets, capable of measuring and transferring 100 mL,
unreacted lead which may exceed the capacity of the potassium phosphate
50 mL, and 7.5 mL.
to remove and which could then interfere in the final copper precipitation
6.19 Beakers, 400 mL, low form.
step.
6.20 Erlenmeyer Flasks, 500 mL capacity.
8.2.2 Then filter the mixture through a folded filter paper
6.21 Reflux Condensers, to connect to the top of the
and return the filtrate to the filter until it is clear. Continue
Erlenmeyer flasks.
filtration until 360 to 380 mL of the clear filtrate has been
6.22 Heat Source, either a Bunsen burner or a hotplate.
collected; this may take an hour or more to accomplish. Cover
6.23 Volumetric Flasks, 200 mL capacity.
the funnel during the filtration.
6.24 Filtering Crucibles, either porcelain crucibles of Fine
8.2.3 Measure the volume of the collected filtrate in a
porosity or Gooch-asbestos crucibles prepared as follows:
graduated cylinder. Remove the excess lead from this filtrate
6.24.1 Digest finely divided long fibered asbestos with nitric
by adding dried dipotassium hydrogen phosphate (K HPO )at
acid (diluted 1 to 3) for 2 to 3 days.
2 4
the rate of 2.5 g (6 0.1 g) phosphate per 100 mL of the filtrate.
6.24.2 Wash the asbestos free from acid.
After addition of the phosphate shake the mixture well for 4 to
6.24.3 Digest the asbestos with 10 % sodium hydroxide
5 min and then filter through a folded filter paper. Allow time
solution for two to three days.
for the solution to drain completely from the lead phosphate.
6.24.4 Wash the asbestos free from alkali.
Cover the funnel during the filtration.
6.24.5 Prepare the Gooch crucible by making a bottom layer
8.3 Determination of Reducing Sugars:
of 6.4 mm ( ⁄4 in.) thickness using the coarser particles of
8.3.1 Add to 100 mL of the clarified (de-tanned) and
asbestos on the bottom and dress off the mat with the finer
de-leaded filtrate solution obtained from 8.2.3 33.3 mL of
asbestos particles.
distilled water. If the reduction is not to be made at once also
6.24.6 Wash the mat with boiling Fehling’s solution.
add eight to ten drops of toluene. Shake this mixture well and
6.24.7 Wash the mat with nitric acid diluted 1 to 3.
stopper with a plug of cotton. Keep the prepared solution in a
6.24.8 Wash and rinse the mat with hot distilled water.
cool place and make the reduction within 24 h. When ready for
6.24.9 Crucibles so prepared can be used for a long time.
reduction, filter the solution if toluene has been added. Deter-
6.25 Suction Flask and Crucible Holder, with connections
mine reducing sugars by the Munson and Walker procedure in
to a vacuum.
8.4 using duplicate 50 mL aliquots.
6.26 Balance, analytical balance which will weigh up to 100
8.4 Munson and Walker Method for Sugar Analysis:
g with an accuracy of 6 0.1 mg (6 0.0001 g).
8.4.1 Measure a 50 mL aliquot by pipet into a 400 mL
6.27 Drying Oven, a forced-air convection oven (or
beaker containing a mixture of 25 mL of the alkaline tartrate
mechanical-convection draft oven) capable of maintaining a
solution and 25 mL of the copper sulfate solution and cover the
temperature of 100 6 2.0°C.
beaker. Heat this mixture to 100°C, as indicated by a thermom-
6.28 Thermometer, accurate to 6 0.2°C used to check and
eter, in exactly 4 min and continue boiling for exactly 2 min.
monitor the oven set point.
8.4.1.1 Regulate the rate of heating before the determination
6.29 Dessicator, any convenient form or size, using any
is started by adjusting the burner or hotplate so that 50 mL of
normal desiccant.
water, 25 mL of the tartrate solution, and 25 mL of the copper
sulfate solution in a 400 mL beaker will be heated to 100°C in
The sole source of supply of S&S No. 610 filter paper known to the committee
exactly 4 min.
at this time is Schleicher & Schuell, 10 Optical Avenue, P.O. Box 2012, Keene, NH
8.4.2 Filter the solution, without dilution, immediately
03431. If you are aware of alternative suppliers, please provide this information to
through a tared crucible. Wash the residue thoroughly with hot
ASTM Headquarters. Your comments will receive careful consideration at a meeting
of the responsible technical committee, which you may attend. water, then with alcohol, and finally with ether. Prepare the
D 6406
tared crucibles ahead of time by oven drying and weighing as add five to ten drops of kerosene to the mixture. Then remove
described in Test Method D 6403. the flask from the heat source, loosely stopper when moder-
8.4.3 Dry the crucible and contents for 30 min in the oven,
ately cool, and allow to stand until ready for reduction, usually
cool in a dessicator, and weigh.
overnight.
8.5 Determination of Total Sugars:
8.5.2 When ready for reduction, cool the hydrolyzed solu-
8.5.1 To a 500 mL Erlenmeyer flask add 150 mL aliquot of
tion in ice-water for 20 to 30 min and add two drops of
the clarified (de-tanned) and deleaded filtrate solution obtained
phenolphthalein solution as an indicator. Neutralize the cooled
from 8.2.3 and 7.5 mL of concentrated hydrochloric acid.
solution carefully with a saturated solution of sodium hydrox-
Connect a reflux condenser to the Erlenmeyer flask and boil the
ide. Then add concentrated hydrochloric acid, drop by drop,
mixture under refluxing conditions for exactly1hto hydrolyze
until the red or pink color of the indicator is just discharged.
the sugars. If the solution foams at the start, which is unusual,
A
TABLE 1 Munson and Walker’s Table
(Expressed in Milligrams)
Cuprous Cuprous Cuprous
Copper Dextrose Copper Dextrose Copper Dextrose
oxide oxide oxide
(Cu) (d-glucose) (Cu) (d-glucose) (Cu) (d-glucose)
(Cu O) (Cu O) (Cu O)
2 2 2
10 8.9 4.0 55 48.9 23.5 100 88.8 43.3
11 9.8 4.5 56 49.7 23.9 101 89.7 43.8
12 10.7 4.9 57 50.6 24.3 102 90.6 44.2
13 11.5 5.3 58 51.5 24.8 103 91.5 44.7
14 12.4 5.7 59 52.4 25.2 104 92.4 45.1
15 13.3 6.2 60 53.3 25.6 105 93.3 45.5
16 14.2 6.6 61 54.2 26.1 106 94.2 46.0
17 15.1 7.0 62 55.1 26.5 107 95.0 46.4
18 16.0 7.5 63 56.0 27.0 108 95.9 46.9
19 16.9 7.9 64 56.8 27.4 109 96.8 47.3
20 17.8 8.3 65 57.7 27.8 110 97.7 47.8
21 18.7 8.7 66 58.6 28.3 111 98.6 48.2
22 19.5 9.2 67 59.5 28.7 112 99.5 48.7
23 20.4 9.6 68 60.4 29.2 113 100.4 49.1
24 21.3 10.0 69 61.3 29.6 114 101.3 49.6
25 22.2 10.5 70 62.2 30.0 115 102.2 50.0
26 23.1 10.9 71 63.1 30.5 116 103.0 50.5
27 24.0 11.3 72 64.0 30.9 117 103.9 50.9
28 24.9 11.8 73 64.8 31.4 118 104.8 51.4
29 25.8 12.2 74 65.7 31.8 119 105.7 51.8
30 26.6 12.6 75 66.6 32.2 120 106.6 52.3
31 27.5 13.1 76 67.5 32.7 121 107.5 52.7
32 28.4 13.5 77 68.4 33.1 122 108.4 53.2
33 29.3 13.9 78 69.3 33.6 123 109.3 53.6
34 30.2 14.3 79 70.2 34.0 124 110.1 54.1
35 31.1 14.8 80 71.1 34.4 125 111.0 54.5
36 32.0 15.2 81 71.9 34.9 126 111.9 55.0
37 32.9 15.6 82 72.8 35.3 127 112.8 55.4
38 33.8 16.1 83 73.7 35.8 128 113.7 55.9
39 34.6 16.5 84 74.6 36.2 129 114.6 56.3
40 35.5 16.9 85 75.5 36.7 130 115.5 56.8
41 36.4 17.4 86 76.4 37.1 131 116.4 57.2
42 37.3 17.8 87 77.3 37.5 132 117.3 57.7
43 38.2 18.2 88 78.2 38.0 133 118.1 58.1
44 39.1 18.7 89 79.1 38.4 134 119.0 58.6
45 40.0 19.1 90 79.9 38.9 135 119.9 59.0
46 40.9 19.6 91 80.8 39.3 136 120.8 59.5
47 41.7 20.0 92 81.7 39.8 137 121.7 60.0
48 42.6 20.4 93 82.6 40.2 138 122.6 60.4
49 43.5 20.9 94 83.5 40.6 139 123.5 60.9
50 44.4 21.3 95 84.4 41.1 140 124.4 61.3
51 45.3 21.7 96 85.3 41.5 141 125.2 61.8
52 46.2 22.2 97 86.2 42.0 142 126.1 62.2
53 47.1 22.6 98 87.1 42.4 143 127.0 62.7
54 48.0 23.0 99 87.9 42.9 144 127.9 63.1
145 128.8 63.6 192 170.5 85.3 239 212.3 107.5
146 129.7 64.0 193 171.4 85.7 240 213.2 108.0
147 130.6 64.5 194 172.3 86.2 241 214.1 108.4
148 131.5 65.0 195 173.2 86.7 242 215.0 108.9
149 132.4 65.4 196 174.1 87.1 243 215.8 109.4
150 133.2 65.9 197 175.0 87.6 244 216.7 109.0
151 134.1 66.3 198 175.9 88.1 245 217.6 110.4
152 135.0 66.8 199 176.8 88.5 246 218.5 110.8
153 135.9 67.2 200 177.7 89.0 247 219.4 111.3
D 6406
TABLE 1 Continued
(Expressed in Milligrams)
Cuprous Cuprous Cuprous
Copper Dextrose Copper Dextrose Copper Dextrose
oxide oxide oxide
(Cu) (d-glucose) (Cu) (d-glucose) (Cu) (d-glucose)
(Cu O) (Cu O) (Cu O)
2 2 2
154 136.8 67.7 201 178.5 89.5 248 220.2 111.8
155 137.7 68.2 202 179.4 89.8 249 221.2 112.3
156 138.6 68.6 203 180.3 90.4 250 222.1 112.8
157 139.5 69.1 204 181.2 90.9 251 223.0 113.2
158 140.3 69.5 205 182.1 91.4 252 223.8 113.7
159 141.2 70.0 206 183.0 91.8 253 224.7 114.2
160 142.2 70.4 207 183.9 92.3 254 225.6 114.7
161 143.0 70.9 208 184.8 92.8 255 226.5 115.2
162 143.9 71.4 209 185.6 93.2 256 227.4 115.7
163 144.8 71.8 210 186.5 93.7 257 228.3 116.1
164 145.7 72.3 211 187.4 94.2 258 229.2 116.6
165 146.6 72.8 212 188.3 94.6 259 230.1 117.1
166 147.5 73.2 213 189.2 95.1 260 231.0 117.6
167 148.3 73.7 214 190.1 9
...