1、Designation: D6406 99 (Reapproved 2014)Standard Test Method forAnalysis of Sugar in Vegetable Tanning Materials1This standard is issued under the fixed designation D6406; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of
2、last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers determining the sugars presentin vegetable tanning materials.1.2 The values stated in SI units
3、 are to be regarded as thestandard. The inch-pound units given in parentheses are forinformation only.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and he
4、alth practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D4901 Practice for Preparation of Solution of Liquid Veg-etable Tannin ExtractsD4905 Practice for Preparation of Solution of Solid, Pastyand Powdered Vegetable Tannin Ext
5、ractsD6401 Test Method for Determining Non-Tannins and Tan-nin in Extracts of Vegetable Tanning MaterialsD6403 Test Method for Determining Moisture in Raw andSpent MaterialsD6404 Practice for Sampling Vegetable Materials Contain-ing TanninD6405 Practice for Extraction of Tannins from Raw andSpent Ma
6、terialsD6408 Test Method for Analysis of Tannery Liquors2.2 ALCA Methods:A30 Sugar in Tanning Materials33. Terminology3.1 Definitions:3.1.1 dextrosed-glucose.3.1.2 glucosea simple sugar with formula C6H12O6, andknown to exist in d-, l-, and racemic forms. The termcommonly refers to the sweet, colorl
7、ess, water-soluble dextro-rotatory form that occurs widely in nature and is the usual formin which carbohydrate is assimilated by animals. The termglucose can also refer to a light-colored syrup made from cornstarch.3.1.3 sugarany of various water-soluble compounds thatvary widely in sweetness and c
8、omprise the oligosaccharidesincluding sucrose.4. Summary of Test Method4.1 An analytical strength solution (that is, 4.00 6 0.25 gtannin per litre) of the tanning material is analyzed for reducingsugars and total sugars by the Munson and Walker procedure.5. Significance and Use5.1 This test method i
9、s used to determine the quantity ofsugar present in vegetable tanning materials or vegetabletannin extracts. The amount of the reducing sugars, totalsugars, and non-reducing sugars in a sample of material orextract can be determined by this method.5.2 Because of the possibility of errors in this tes
10、t method itis essential that the method be followed exactly in order toobtain reproducible results both among specimens within alaboratory and for analyses between laboratories.6. Apparatus and Reagents6.1 Saturated Solution of Normal Lead Acetate.6.2 Dipotassium Hydrogen Phosphate, Anhydrous(K2HPO4
11、), dried in an oven at 100C for 16 h then stored in atightly stoppered bottle.6.3 Toluene, assay 99.5 %.6.4 Fehlings Solutions, A and B.6.5 Hydrochloric Acid, concentrated (sp.gr. 1.18).6.6 Kerosene, commercial grade.6.7 Saturated Solution of Sodium Hydroxide.1This test method is under the jurisdict
12、ion of ASTM Committee D31 on Leatherand is the direct responsibility of Subcommittee D31.01 on Vegetable Leather. Thismethod has been adapted from and is a replacement for Method A30 of the OfficialMethods of the American Leather Chemists Association.Current edition approved Nov. 1, 2014. Published
13、December 2014. Originallyapproved in 1999. Last previous edition approved in 2009 as D6406 99 (2009).DOI: 10.1520/D6406-99R14.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information,
14、 refer to the standards Document Summary page onthe ASTM website.3Official Methods of the American Leather Chemists Association. Availablefrom the American Leather Chemists Association, University of Cincinnati, P.O.Box 210014, Cincinnati, OH 45221-0014.Copyright ASTM International, 100 Barr Harbor
15、Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States16.8 Phenolphthalein Solution, 0.5 g dissolved in 100 mL of95 % ethanol.6.9 Tartaric Acid, powdered.6.10 Copper Sulfate Solution, prepared by dissolving69.278 g of CuSO45H2O in 1 L of distilled water and filteringthrough asbestos.6.1
16、1 Alkaline Tartrate Solution, prepared by dissolving 346g of Rochelle salt (sodium potassium tartrate tetrahydrate) and100 g of sodium hydroxide in 1 L of distilled water. Afterstanding for two days the solution shall be filtered throughasbestos.6.12 Alcohol, 95 % ethyl alcohol.6.13 Ether, diethyl e
17、ther.6.14 Filter Paper4, 21.5 cm diameter, pleated to contain 32evenly divided creases.6.15 Funnel, 100-125 mm top diameter, 60 angle bowl, and150 mm stem length.6.16 Watch Glasses, a suitable size (approximately 150 mmdiameter) to be used as a cover for the funnel and filter paper.6.17 Graduated Cy
18、linder, standard laboratory grade with500 mL capacity.6.18 Pipets, capable of measuring and transferring 100 mL,50 mL, and 7.5 mL.6.19 Beakers, 400 mL, low form.6.20 Erlenmeyer Flasks, 500 mL capacity.6.21 Reflux Condensers, to connect to the top of theErlenmeyer flasks.6.22 Heat Source, either a Bu
19、nsen burner or a hotplate.6.23 Volumetric Flasks, 200 mL capacity.6.24 Filtering Crucibles, either porcelain crucibles of Fineporosity or Gooch-asbestos crucibles prepared as follows:6.24.1 Digest finely divided long fibered asbestos with nitricacid (diluted 1 to 3) for 2 to 3 days.6.24.2 Wash the a
20、sbestos free from acid.6.24.3 Digest the asbestos with 10 % sodium hydroxidesolution for two to three days.6.24.4 Wash the asbestos free from alkali.6.24.5 Prepare the Gooch crucible by making a bottom layerof 6.4 mm (14 in.) thickness using the coarser particles ofasbestos on the bottom and dress o
21、ff the mat with the finerasbestos particles.6.24.6 Wash the mat with boiling Fehlings solution.6.24.7 Wash the mat with nitric acid diluted 1 to 3.6.24.8 Wash and rinse the mat with hot distilled water.6.24.9 Crucibles so prepared can be used for a long time.6.25 Suction Flask and Crucible Holder, w
22、ith connectionsto a vacuum.6.26 Balance, analytical balance which will weigh up to 100g with an accuracy of 6 0.1 mg (6 0.0001 g).6.27 Drying Oven, a forced-air convection oven (ormechanical-convection draft oven) capable of maintaining atemperature of 100 6 2.0C.6.28 Thermometer, accurate to 6 0.2C
23、 used to check andmonitor the oven set point.6.29 Dessicator, any convenient form or size, using anynormal desiccant.7. Test Specimen7.1 The specimen for the sugar analysis shall consist of 400mL of a solution of the tanning material of analytical strength(4.006 0.25 g tannin per L).8. Procedure8.1
24、Sample the tanning material using Practice D6404, andprepare the analytical solution as described in Practices D4901,D4905, D6405,orD6408.8.2 Detannization of Analytical Solution:8.2.1 Add to 400 mL of the analytical solution 50 mL of asaturated lead acetate solution. Shake the mixture well andallow
25、 to stand for 5 to 10 min.NOTE 1It is important that the mixture of liquor and lead acetatesolution be very well shaken. Good results are obtained by placing thesolution mixture in shake bottles and running in the shake machine for 10min (as described in Test Method D6401) to ensure complete detanni
26、za-tion of the liquor. The mixture filters better after complete detannization.Complete detannization also results in less danger of residual quantities ofunreacted lead which may exceed the capacity of the potassium phosphateto remove and which could then interfere in the final copper precipitation
27、step.8.2.2 Then filter the mixture through a folded filter paperand return the filtrate to the filter until it is clear. Continuefiltration until 360 to 380 mL of the clear filtrate has beencollected; this may take an hour or more to accomplish. Coverthe funnel during the filtration.8.2.3 Measure th
28、e volume of the collected filtrate in agraduated cylinder. Remove the excess lead from this filtrateby adding dried dipotassium hydrogen phosphate (K2HPO4)atthe rate of 2.5 g (6 0.1 g) phosphate per 100 mL of the filtrate.After addition of the phosphate shake the mixture well for 4 to5 min and then
29、filter through a folded filter paper. Allow timefor the solution to drain completely from the lead phosphate.Cover the funnel during the filtration.8.3 Determination of Reducing Sugars:8.3.1 Add to 100 mL of the clarified (de-tanned) andde-leaded filtrate solution obtained from 8.2.3 33.3 mL ofdisti
30、lled water. If the reduction is not to be made at once alsoadd eight to ten drops of toluene. Shake this mixture well andstopper with a plug of cotton. Keep the prepared solution in acool place and make the reduction within 24 h. When ready forreduction, filter the solution if toluene has been added
31、. Deter-mine reducing sugars by the Munson and Walker procedure in8.4 using duplicate 50 mL aliquots.8.4 Munson and Walker Method for Sugar Analysis:4The sole source of supply of S glucose analysis; sugar analysis;tannin analysis; vegetable tannin analysisASTM International takes no position respect
32、ing the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This stan
33、dard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM Internatio
34、nal Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.
35、This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 99 (2014)6
