ASTM D6407-1999(2004) Standard Test Method for Analysis of Iron and Copper in Vegetable Tanning Materials《植物单宁材料中铁和铜的分析的标准试验方法》.pdf
《ASTM D6407-1999(2004) Standard Test Method for Analysis of Iron and Copper in Vegetable Tanning Materials《植物单宁材料中铁和铜的分析的标准试验方法》.pdf》由会员分享,可在线阅读,更多相关《ASTM D6407-1999(2004) Standard Test Method for Analysis of Iron and Copper in Vegetable Tanning Materials《植物单宁材料中铁和铜的分析的标准试验方法》.pdf(4页珍藏版)》请在麦多课文档分享上搜索。
1、Designation: D 6407 99 (Reapproved 2004)Standard Test Method forAnalysis of Iron and Copper in Vegetable Tanning Materials1This standard is issued under the fixed designation D 6407; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision,
2、the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method is intended for use in determining ironand copper content in vegetable tanning materials
3、. This testmethod is applicable to liquid, solid, pasty and powderedextracts, to raw and spent materials, and to tannery liquors.1.2 The values stated in SI units are to be regarded as thestandard.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its us
4、e. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 4901 Practice for Preparation of Solution of Liquid Veg-etable Tannin Ext
5、ractsD 4902 Test Method for Evaporation and Drying of Ana-lytical SolutionsD 4905 Practice for Preparation of Solution of Solid, Pasty,and Powdered Vegetable Tannin ExtractsD 6404 Practice for Sampling of Vegetable Materials Con-taining TanninD 6405 Practice for Extraction of Tannins from Raw andSpe
6、nt Materials2.2 ALCA Methods:A31 Method for Copper and Iron in Tanning Materials33. Summary of Test Method3.1 A specified quantity of the tanning material is analyzedfor iron and copper and content.4. Significance and Use4.1 This test method is used to determine the quantity ofiron and copper presen
7、t in vegetable tanning materials orvegetable tannin extracts prepared using Practices D 4901,D 6404,orD 6405.4.2 Because of the possibility of errors in this test method itis essential that the method be followed exactly in order toobtain reproducible results both among specimens within alaboratory
8、and for analyses between laboratories.5. Apparatus and Reagents5.1 Sulfuric Acid, concentrated (96 %).5.2 Sulfuric Acid Solution, diluted 1:20 with distilled water.5.3 Nitric Acid, fuming.5.4 Hydrochloric Acid, concentrated (36 %).5.5 Hydrochloric Acid Solution, 0.1 N.5.6 Bromine Water, saturated so
9、lution.5.7 Ammonium Hydroxide Solution, concentrated diluted1:1 with distilled water.5.8 Potassium Permanganate Solution, 0.1 N.5.9 Potassium (or Ammonium) Thiocyanate Solution,10gshall be dissolved in distilled water and diluted to 100 mL withdistilled water.5.10 Stock Iron Solution, This may be a
10、purchased ironstandard solution or may be prepared as follows:5.10.1 0.70 g of crystallized ferrous ammonium sulfateFeSO4(NH4)2SO46H2O shall be dissolved in 50 mL ofdistilled water and 20 mL of dilute sulfuric acid (diluted 1:4).5.10.2 This solution shall be titrated with 0.1 N potassiumpermanganate
11、 solution until a faint pink persists for 1 minuteand the iron is completely oxidized.5.10.3 Dilute this solution to 1 L with distilled water. 1 mLof this solution is equivalent to 0.0001 g Fe. This solution shallbe stored in brown bottles and be protected from light.5.10.4 Standard Iron Solution, 1
12、0 mL of the prepared stocksolution, or its equivalent of purchased iron standard solution,shall be diluted to 100 mL with distilled water. 1 mL of thisstandard solution is equivalent to 0.00001 g Fe. The standardsolution shall be freshly prepared for each analysis.5.11 Stock Copper Solution, 3.9283
13、g of copper sulfatecrystals (CuSO45H2O) shall be dissolved in distilled waterand diluted to 1 L with distilled water. 1 mL of this solution isequivalent to 0.001 g Cu.1This test method is under the jurisdiction of ASTM Committee D31 on Leatherand is the direct responsibility of Subcommittee D31.01 o
14、n Vegetable Leather. Thistest method has been adapted from and is a replacement for Method A31 of theOfficial Methods of the American Leather Chemists Association.Current edition approved April 1, 2004. Published May 2004. Originallyapproved in 1999. Last previous edition approved in 1999 as D 6407
15、99.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Official Methods of the American Leather Chemists Associa
16、tion. Availablefrom the American Leather Chemists Association, University of Cincinnati, P.O.Box 210014, Cincinnati, OH 45221-0014.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.11.1 Standard Copper Solution, 10 mL of the stock co
17、ppersolution shall be diluted to 1 L with distilled water and the pHadjusted to between 5.5 and 6.0. 1 mL of this standard solutionis equivalent to 0.00001 g Cu. The standard solution shall befreshly prepared for each analysis.5.12 Xanthate Solution, 1.0 g of potassium ethyl xanthateshall be dissolv
18、ed in distilled water and diluted to 1 L withdistilled water. The solution shall be freshly prepared for eachanalysis.5.13 Matched Nessler Tubes and Supporting Rack.5.14 Balance, analytical balance which will weigh up to 100g with an accuracy of 6 0.1 mg (6 0.0001 g).5.15 Drying Oven, a forced-air c
19、onvection oven (ormechanical-convection draft oven) capable of maintaining atemperature of 100 6 2.0C.5.16 Thermometer, accurate to 6 0.2C used to check andmonitor the oven set point.5.17 Dessicator, any convenient form or size, using anynormal desiccant.5.18 Glazed, Porcelain Dish or Crucible of Su
20、itable Size.5.19 Muffle Furnace, capable of maintaining a temperatureof 600 6 25C.5.20 Hotplate, ordinary lab grade.5.21 Steam Bath, ordinary lab grade.5.22 Volumetric Flasks, 200 and 250 mL capacity.5.23 Beakers, 250 mL.5.24 Filter Paper, quantitative, Whatman grade 40 or 52 orsimilar.5.25 Buret, 1
21、0 mL capacity is sufficient.6. Test Specimen6.1 The sample of material from which the test specimensare taken shall be prepared as described in Practice D 6404 forextracts and tannery liquor and as in the Preparation of Samplesection of Practice D 6405 for raw and spent materials.6.2 The specimen sh
22、all consist of5gofsolid extract or itsequivalent (that is 10 g of liquid extract; 25 to 50 g of tanneryliquor;5gofraworspent materials).7. General Instructions7.1 The distilled water shall be distilled from a glass,tin-lined, or block tin still and shall be stored in glass, tin-lined,or block tin co
23、ntainers.7.2 All apparatus used in this analysis shall be cleaned withhot hydrochloric acid solution (diluted 1 to 1) and rinsed withdistilled water before use.7.3 Blank determinations shall be made to minimize errorsdue to iron or copper either present in the reagents used orpicked up during the an
24、alysis.7.4 Duplicate determinations are recommended wheneverpossible.7.5 In the actual colorimetric determinations described be-low, the indicated volumes of reagents, and of the preparedsolutions of the specimens and of standards, are based on theuse 50 mL tall-form Nessler tubes. Other tube volume
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