ASTM D6406-99(2004)

Standard Test Method for Analysis of Sugar in Vegetable Tanning Materials

SIGNIFICANCE AND USE
This test method is used to determine the quantity of sugar present in vegetable tanning materials or vegetable tannin extracts. The amount of the reducing sugars, total sugars, and non-reducing sugars in a sample of material or extract can be determined by this method.
Because of the possibility of errors in this test method it is 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 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: 31-Mar-2004
• ICS: 59.140.10 - Processes and auxiliary materials
• Technical Committee: D31 - Leather
• Drafting Committee: D31.01 - Vegetable Leather

Relations

• Replaces: ASTM D6406-99 - Standard Test Method for Analysis of Sugar in Vegetable Tanning Materials
• Effective Date: 01-Apr-2004
• Replaced By: ASTM D6406-99(2009) - Standard Test Method for Analysis of Sugar in Vegetable Tanning Materials
• Effective Date: 01-Apr-2009
• Referred By: ASTM D4899-99(2020) - Standard Practice for Analysis of Vegetable Tanning Materials—General
• Effective Date: 01-Apr-2004

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D6406–99(Reapproved2004)
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
tanninperlitre)ofthetanningmaterialisanalyzedforreducing
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,
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
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
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-
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
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
(K HPO ), dried in an oven at 100°C for 16 h then stored in a
3. Terminology
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 ofASTM Committee D31 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 MethodA30 of the Official
Methods of the American Leather Chemists Association. 6.8 Phenolphthalein Solution, 0.5 g dissolved in 100 mL of
Current edition approved April 1, 2004. Published May 2004. Originally
95 % ethanol.
approved in 1999. Last previous edition approved in 1999 as D 6406 – 99.
6.9 Tartaric Acid, powdered.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
6.10 Copper Sulfate Solution, prepared by dissolving
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
69.278 g of CuSO •5H O in 1 Lof distilled water and filtering
4 2
the ASTM website.
through asbestos.
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.
D6406–99 (2004)
6.11 Alkaline Tartrate Solution, prepared by dissolving 346 7. Test Specimen
g of Rochelle salt (sodium potassium tartrate tetrahydrate) and
7.1 The specimen for the sugar analysis shall consist of 400
100 g of sodium hydroxide in 1 L of distilled water. After
mL of a solution of the tanning material of analytical strength
standing for two days the solution shall be filtered through
(4.006 0.25 g tannin per L).
asbestos.
8. Procedure
6.12 Alcohol, 95 % ethyl alcohol.
6.13 Ether, diethyl ether. 8.1 Sample the tanning material using Practice D 6404, and
prepare the analytical solution as described in Practices
6.14 Filter Paper , 21.5 cm diameter, pleated to contain 32
D 4901, D 4905, D 6405,or D 6408.
evenly divided creases.
8.2 Detannization of Analytical Solution:
6.15 Funnel,100-125mmtopdiameter,60°anglebowl,and
8.2.1 Add to 400 mL of the analytical solution 50 mL of a
150 mm stem length.
saturated lead acetate solution. Shake the mixture well and
6.16 Watch Glasses, a suitable size (approximately 150 mm
allow to stand for 5 to 10 min.
diameter) to be used as a cover for the funnel and filter paper.
6.17 Graduated Cylinder, standard laboratory grade with
NOTE 1—It is important that the mixture of liquor and lead acetate
500 mL capacity. solution be very well shaken. Good results are obtained by placing the
solution mixture in shake bottles and running in the shake machine for 10
6.18 Pipets, capable of measuring and transferring 100 mL,
min (as described in Test Method D 6401) to ensure complete detanniza-
50 mL, and 7.5 mL.
tion of the liquor. The mixture filters better after complete detannization.
6.19 Beakers, 400 mL, low form.
Complete detannization also results in less danger of residual quantities of
6.20 Erlenmeyer Flasks, 500 mL capacity.
unreacted lead which may exceed the capacity of the potassium phosphate
6.21 Reflux Condensers, to connect to the top of the to remove and which could then interfere in the final copper precipitation
step.
Erlenmeyer flasks.
6.22 Heat Source, either a Bunsen burner or a hotplate.
8.2.2 Then filter the mixture through a folded filter paper
6.23 Volumetric Flasks, 200 mL capacity.
and return the filtrate to the filter until it is clear. Continue
filtration until 360 to 380 mL of the clear filtrate has been
6.24 Filtering Crucibles, either porcelain crucibles of Fine
porosity or Gooch-asbestos crucibles prepared as follows: collected; this may take an hour or more to accomplish. Cover
the funnel during the filtration.
6.24.1 Digestfinelydividedlongfiberedasbestoswithnitric
8.2.3 Measure the volume of the collected filtrate in a
acid (diluted 1 to 3) for 2 to 3 days.
graduated cylinder. Remove the excess lead from this filtrate
6.24.2 Wash the asbestos free from acid.
by adding dried dipotassium hydrogen phosphate (K HPO)at
2 4
6.24.3 Digest the asbestos with 10 % sodium hydroxide
the rate of 2.5 g (6 0.1 g) phosphate per 100 mLof the filtrate.
solution for two to three days.
After addition of the phosphate shake the mixture well for 4 to
6.24.4 Wash the asbestos free from alkali.
5 min and then filter through a folded filter paper. Allow time
6.24.5 PreparetheGoochcruciblebymakingabottomlayer
for the solution to drain completely from the lead phosphate.
of 6.4 mm ( ⁄4 in.) thickness using the coarser particles of
Cover the funnel during the filtration.
asbestos on the bottom and dress off the mat with the finer
8.3 Determination of Reducing Sugars:
asbestos particles.
8.3.1 Add to 100 mL of the clarified (de-tanned) and
6.24.6 Wash the mat with boiling Fehling’s solution.
de-leaded filtrate solution obtained from 8.2.3 33.3 mL of
6.24.7 Wash the mat with nitric acid diluted 1 to 3.
distilled water. If the reduction is not to be made at once also
6.24.8 Wash and rinse the mat with hot distilled water.
add eight to ten drops of toluene. Shake this mixture well and
6.24.9 Crucibles so prepared can be used for a long time.
stopper with a plug of cotton. Keep the prepared solution in a
6.25 Suction Flask and Crucible Holder, with connections
cool place and make the reduction within 24 h.When ready for
to a vacuum.
reduction, filter the solution if toluene has been added. Deter-
6.26 Balance,analyticalbalancewhichwillweighupto100
mine reducing sugars by the Munson and Walker procedure in
g with an accuracy of 6 0.1 mg (6 0.0001 g).
8.4 using duplicate 50 mL aliquots.
6.27 Drying Oven, a forced-air convection oven (or 8.4 Munson and Walker Method for Sugar Analysis:
mechanical-convection draft oven) capable of maintaining a 8.4.1 Measure a 50 mL aliquot by pipet into a 400 mL
temperature of 100 6 2.0°C. beaker containing a mixture of 25 mL of the alkaline tartrate
solutionand25mLofthecoppersulfatesolutionandcoverthe
6.28 Thermometer, accurate to 6 0.2°C used to check and
monitor the oven set point. beaker. Heat this mixture to 100°C, as indicated by a thermom-
eter, in exactly 4 min and continue boiling for exactly 2 min.
6.29 Dessicator, any convenient form or size, using any
8.4.1.1 Regulatetherateofheatingbeforethedetermination
normal desiccant.
is started by adjusting the burner or hotplate so that 50 mL of
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 OpticalAvenue, 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
ASTMHeadquarters.Yourcommentswillreceivecarefulconsiderationatameeting
of the responsible technical committee, which you may attend. water, then with alcohol, and finally with ether. Prepare the
D6406–99 (2004)
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-
ConnectarefluxcondensertotheErlenmeyerflaskandboilthe
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
D6406–99 (2004)
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
...