ASTM D6017-1997(2003) Standard Test Method for Determination of Magnesium Sulfate (Epsom Salt) in Leather《测定皮革中硫酸镁含量的标准试验方法》.pdf

1、Designation: D 6017 97 (Reapproved 2003)Standard Test Method forDetermination of Magnesium Sulfate (Epsom Salt) inLeather1This standard is issued under the fixed designation D 6017; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, t

2、he 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.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 This test method covers q

3、uantitatively determining themagnesium sulfate (epsom salt) in leather.1.2 The values given 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 use. It is theresponsibility of the user of this standard to

4、establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:D 3790 Test Method for Volatile Matter (Moisture) ofLeather by Oven Drying22.2 Federal Standards:Federal Test Standard No. 311, Method

5、6541 MagnesiumSulfate (Epsom Salt)33. Significance and Use3.1 This test method distinguishes magnesium sulfate fromother water soluble non-tanning salts found in leather.4. Apparatus4.1 Platinum Crucible.4.2 Filtering Crucible.4.3 Suction Flask.4.4 Muffle Furnace.5. Reagents5.1 Hydrochloric Acid, sp

6、ecific gravity 1.19.5.2 Nitric Acid, specific gravity 1.42.5.3 Ammonium Chloride.5.4 Ammonium Hydroxide, 1 to 1 and 1 to 9 parts by volumewith distilled water.5.5 Ammonium Nitrate Solution, 10 g dissolved in distilledwater and made up to 100 mL.5.6 Ammonium Oxalate, saturated solution.5.7 Ferric Chl

7、oride Solution, 10 g dissolved in distilledwater and made up to 100 mL.5.8 Methyl Orange Indicator, 0.05 %.5.9 Sodium Ammonium Hydrogen Phosphate, saturated so-lution.6. Procedure6.1 Unless otherwise specified in the material specification,determine the moisture content of the composite sample fromw

8、hich the test specimen is drawn, in accordance with TestMethod D 3790. Determine the weight of the compositespecimens for moisture content at the same time and under thesame ambient conditions as the specimens weighed for chemi-cal tests.6.2 Place the specimen in a tared porcelain crucible, 5 gweigh

9、ed to the nearest 0.001 g, and record the value as W2.Place the weighed specimen in a cold muffle furnace orprecarbonize over a burner prior to placing in a hot furnace.Gradually raise the temperature of the furnace to 600 6 25Cand maintain at this temperature for 60 min. Remove thecrucible and cont

10、ents, cool in a desiccator, and weigh. Replacein the furnace at 600 6 25C for 30 min and repeat the coolingand weighing procedure until a constant weight is obtained (60.01 g). If it is difficult to obtain a constant weight, leach theresidue with hot distilled water and filter through an ashlessfilt

11、er paper. Place the filter paper in the crucible and ash. Addthe filtrate to the crucible and evaporate. The crucible shall thenbe put back in the muffle furnace and heated, cooled, andweighed as above until a constant weight (6 0.01 g) has beenobtained.1This test method is under the jurisdiction of

12、 ASTM Committee D31 on Leatherand is the direct responsibility of Subcommittee D31.06 on ChemicalAnalysis. Thistest method was developed from Federal Test Method Standard No. 311,Method 6541 in cooperation with the U.S. Army Natick Research Development add 1 mL of ammonium hydroxide(1:1) and heat th

13、e solution to boiling. Add 10 mL of saturatedammonium oxalate solution slowly while stirring, then coverthe beaker and set aside over a steam bath for at least 2 h.Transfer the solution and precipitate to a 250 mL volumetricflask, cool to room temperature, dilute to the mark, and mixwell. Filter sol

14、ution through a dry quantitative filter paper.6.5 Transfer an aliquot of 50 mL to a beaker, dilute to about150 mL with distilled water, add a few drops of methyl orangeindicator, and add hydrochloric acid until slightly acid. Add aslight excess of saturated sodium ammonium hydrogen phos-phate over t

15、hat necessary to precipitate the magnesium (usually5 mL is sufficient). While stirring vigorously, make the solutionslightly ammoniacal by the dropwise addition of ammoniumhydroxide (1:1) and set aside for 15 min. Add 5 mL ofammonium hydroxide (1:1) while stirring and set the solutionaside overnight

16、 at room temperature.6.6 Filter the solution through a filtering crucible, transferthe precipitate to the platinum crucible, and wash free from thechlorides with ammonium hydroxide (1:9) solution. Moistenthe precipitate with a few drops of 10 % ammonium nitratesolution, dry cautiously, ignite for1ht

17、oaconstant weight (60.001 g) at 1000 to 1100C, cool in a desiccator to roomtemperature, immediately weigh the value, and record as W1.7. Calculation7.1 Calculate the magnesium sulfate (epsom salt,MgSO47H2) in the specimen as follows:magnesium sulfate MgSO47H2O!,%moisture2free basis! (1)5W13 2.2147 3

18、 5 3 100W23100 2 M!100!where:W1= weight of the ignited precipitate (Mg2P2O7), g,W2= weight of the specimen, g, andM = moisture content of leather.NOTE 1See Test Method D 3790.8. Report8.1 The magnesium sulfate in the specimen is the average ofthe results obtained from the specimens tested and report

19、ed tothe nearest 0.1 %. Report individual results utilized in obtain-ing the average.9. Precision and Bias9.1 This test method is adopted from Federal Test StandardNo. 311, Method 6541 where it has long been in use and wasapproved for publication before the inclusion of precision andbias statements

20、was mandated. The user is cautioned to verifyby the use of reference materials, if available, that the precisionand bias (or reproducibility) of this test method is adequate forthe contemplated use.10. Keywords10.1 epsom salt; leather; magnesium sulfate; soluble saltsASTM International takes no posi

21、tion respecting 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 responsibili

22、ty.This standard 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 AST

23、M International 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

24、shown below.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).D 6017 97 (2003)2