1、Designation: E 534 08Standard Test Methods forChemical Analysis of Sodium Chloride1This standard is issued under the fixed designation E 534; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in pa
2、rentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 These test methods cover the chemical analyses usuallyrequired for sodium chloride.1.2 The analytical procedures appear in the following sec-tions
3、:SectionSample Preparation 5 to 9Moisture 10 to 16Water Insolubles 17 to 24Calcium and Magnesium 25 to 31Sulfate 32 to 38Reporting of Analyses 39 to 411.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 This standard does no
4、t 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 health practices and determine the applica-bility of regulatory limitations prior to use.1.5 Review the current material safety d
5、ata sheets (MSDS)for detailed information concerning toxicity, first-aid proce-dures, handling, and safety precautions.2. Referenced Documents2.1 ASTM Standards:2D 1193 Specification for Reagent WaterE 180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial a
6、nd Spe-cialty ChemicalsE 200 Practice for Preparation, Standardization, and Stor-age of Standard and Reagent Solutions for ChemicalAnalysis3. Significance and Use3.1 Sodium chloride occurs in nature in almost unlimitedquantities. It is a necessary article of diet as well as the sourcefor production
7、of many sodium compounds and chlorine. Themethods listed in 1.2 provide procedures for analyzing sodiumchloride to determine if it is suitable for its intended use.4. Reagents4.1 Purity of ReagentsUnless otherwise indicated, it isintended that all reagents should conform to the specificationsof the
8、Committee on Analytical Reagents of the AmericanChemical Society, where such specifications are available.34.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean Type II or III reagentwater conforming to Specification D 1193.SAMPLE PREPARATION5. Scope5.1 This t
9、est method covers preparation of a sample that willbe as representative as possible of the entire bulk quantity. Theresults of any analysis pertain only to the sample used.6. Apparatus6.1 Coarse Grinder.6.2 High-Speed Blender.6.3 Oven.6.4 Riffle Sampler.6.5 Scale.7. Reagents7.1 Hydrochloric Acid, St
10、andard (1 meq/mL HCl)Prepareand standardize in accordance with Practice E 200.8. Rock and Solar Salt Stock Solutions8.1 Mix and split sample to 500 g, using the riffle sampler.8.2 If sample appears wet, dry at 110C for 2 h.8.3 Grind the sample to 8 mesh in the coarse grinder.8.4 Mix ground sample we
11、ll and weigh out a 25.0-grepresentative portion for rock salt or 50.0 g for solar salt.8.5 Place 200 mL of water in the high-speed blender andstart at low speed.1These test methods are under the jurisdiction of ASTM Committee E15 onIndustrial and Specialty Chemicals and are under the direct responsi
12、bility ofSubcommittee E15.02 on Product Standards.Current edition approved Dec. 15, 2008. Published January 2009. Originallyapproved in 1975. Last previous edition approved in 2003 as E 534 98(2003).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service
13、 at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by t
14、he American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.1*A Summary of Changes section appears at the end of this standard.Copyright A
15、STM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.8.6 Slowly add the salt sample to the high-speed blenderand blend for 5 min.8.7 Test for water insolubles as described in Sections 17-24.8.8 Save filtrate from water insolubles test and dilute in a
16、volumetric flask to 1 L with water as a stock solution forsubsequent analyses.9. Evaporated and Purified Salt Stock Solutions9.1 Mix and split the sample to 100 g for evaporated salt, or200 g for purified evaporated salt.9.2 Transfer to a 1-L volumetric flask.9.3 Add 800 mL of water and allow the sa
17、lt to dissolve.9.4 Add 2 mL of concentrated HCl to dissolve any waterinsoluble calcium salts, particularly calcium carbonate.9.5 Dilute to volume with water and use as a stock solutionfor subsequent analyses.MOISTURE10. Scope10.1 This test method determines free moisture in the saltover a concentrat
18、ion range from 0.00 to 0.04 %. It does notdetermine occluded moisture trapped within the salt crystals.The procedure is based on weight loss after a sample is heatedto volatize moisture.11. Apparatus11.1 Analytical Balance.11.2 Desiccator.11.3 Oven.12. Procedure, Rock and Solar Salt12.1 Weigh 100 g
19、of salt to the nearest 0.05 g into apreviously dried and tared moisture dish.12.2 Dry at 110C for 2 h.12.3 Cool in a desiccator and weigh.13. Procedure, Evaporated and Purified Evaporated Salt13.1 Weigh 20 g of salt to the nearest 0.001 g into apreviously dried and weighed glass weighing bottle and
20、cover.13.2 Dry at 110C for 2 h.13.3 Cool in a desiccator, replace cover, and weigh.14. Calculation14.1 Calculate the percentage of moisture as follows:moisture, mass m/m! % 5AB3 100 (1)where:A = loss of mass on drying, g, andB = mass of sample, g.15. Report15.1 Report the moisture content to the nea
21、rest 0.001 %.16. Precision and Bias16.1 The following criteria should be used in judging theacceptability of results (Note 1):16.1.1 Repeatability (Single Analyst)The standard devia-tion for a single determination has been estimated to be thepercent absolute values shown in Table 1 at the indicatedd
22、egrees of freedom. The 95 % limit for the difference betweentwo such runs is the percent absolute values in Table 1.16.1.2 Laboratory precision (Within-Laboratory, Between-Days Variability)The standard deviation of results (each theaverage of duplicates), obtained by the same analyst ondifferent day
23、s, has been estimated to be the percent absolutevalues shown in Table 1 at the indicated degrees of freedom.The 95 % limit for the difference between two such averages isthe percent absolute values in Table 1.16.1.3 Reproducibility (Multilaboratory)The standard de-viation of results (each the averag
24、e of duplicates), obtained byanalysts in different laboratories, has been estimated to bepercent absolute values shown in Table 1. The 95 % limit forthe difference between two such averages is the percentabsolute values in Table 1.NOTE 1The preceding precision statements are based on an interlabo-ra
25、tory study performed around 1975 on five samples of sodium chloridecontaining covering the ranges of moisture in Table 1. One analyst in eachof ten laboratories performed duplicate determinations and repeated themon a second day.4Practice E 180 was used in developing these precisionestimates.16.2 Bi
26、asThe bias of this test method has not beendetermined due to the unavailability of suitable referencematerials.WATER INSOLUBLES17. Scope17.1 This gravimetric method determines only the amountof insolubles present in sodium chloride which will notdissolve in water.18. Apparatus18.1 Analytical Balance
27、.18.2 Desiccator.18.3 Magnetic Stirrer with Stirring Bar.4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: E151052.TABLE 1 Precision for Moisture MethodRepeatability Laboratory Precision ReproducibilityLevel, %StandardDeviation,
28、%Degrees ofFreedom95 % Limit, % StandardDeviation, %Degrees ofFreedom95 % Limit, % StandardDeviation, %Degrees ofFreedom95 % Limit, %0.003 to0.0040.0014 36 0.004 0.00223 18 0.006 0.00322 8 0.0090.025 to0.0350.0071 60 0.02 0.00428 30 0.01 0.0138 9 0.04E53408218.4 Parabella Filter Funnel Assembly,5100
29、0-mL, or itsequivalent with 0.3-m glass fiber filter disk.19. Reagents19.1 Silver Nitrate, Standard Solution, 0.1 meq/mLAgNO3Prepare and standardize in accordance with PracticeE 200.20. Procedure, Rock and Solar Salts20.1 Transfer a sample prepared in accordance with 8.1 to8.6 to a 1-L Erlenmeyer fl
30、ask, washing out the blender with100 mL of water. Add 300 mL of water to give a total of 600mL of water added.20.2 Stir on a magnetic stirrer for 1 h. Adjust the stirrerspeed to give maximum agitation without danger of losing anysample due to splashing. Place a beaker over top of the flaskwhile stir
31、ring.20.3 Filter the solution by vacuum through a previouslydried (110C for 1 h) and accurately weighed filter disk usingthe Parabella funnel. Transfer all insolubles to the paper andwash free of chlorides with water until the filtrate shows noturbidity when tested with 0.1 meq/mL AgNO3solution.20.4
32、 Dilute filtrate and washings to 1 L with water involumetric flask.20.5 Dry the filter disk at 110C for 1 h.20.6 Cool in a desiccator and weigh the disk on an analyti-cal balance.20.7 Save the filtrate for subsequent analyses.21. Procedure, Evaporated and Purified Evaporated Salts21.1 Place a well m
33、ixed sample in a 2-L beaker. Use 100-gsample for evaporated or 200 g for purified evaporated salt.21.2 Add 750 mL of water.21.3 Mix with a mechanical stirrer until solution is com-plete.21.4 Filter the solution by vacuum through a previouslydried (110C for 1 h) and accurately weighed filter disk usi
34、ngthe Parabella funnel. Transfer all insolubles to the paper andwash free of chlorides with water until the filtrate shows noturbidity when tested with 0.1 meq/mL AgNO3solution.21.5 Dry the filter disk at 110C for 1 h.21.6 Cool in a desiccator and weigh on an analyticalbalance.21.7 Dilute the filtra
35、tion and washings to 1 L with water ina volumetric flask and reserve for subsequent analyses.22. Calculation22.1 Calculate the percentage of water insolubles as fol-lows:insolubles, % mass m/m!5AB3 100 (2)where:A = increase in mass of filter disk, g, andB = sample mass, g.23. Report23.1 Report the p
36、ercentage of water insolubles to the nearestpercentage shown as follows:Range, % Report to, %0.002 to 0.005 0.0010.01 to 0.04 0.010.15 to 0.35 0.0124. Precision and Bias24.1 The following criteria should be used in judging theacceptability of results (Note 2):24.1.1 Repeatability (Single Analyst)The
37、 coefficient ofvariation for a single determination has been estimated to bethe percent relative values shown in Table 2 at the indicateddegrees of freedom. The 95 % limit for the difference betweentwo such runs is percent relative values shown in Table 2.24.1.2 Laboratory Precision (Within-Laborato
38、ry, Between-Days Variability)The coefficient of variation of results (eachthe average of duplicates), obtained by the same analyst ondifferent days, has been estimated to be 23.5 % relative at 57df. The 95 % limit for the difference between two suchaverages is 66 % relative.24.1.3 Reproducibility (M
39、ultilaboratory)The coefficientof variation of results (each the average of duplicates), ob-tained by analysts in different laboratories, has been estimatedto be percent relative values shown in Table 2 at the indicateddegrees of freedom. The 95 % limit for the difference betweentwo such averages is
40、percent relative values shown in Table 2.NOTE 2The preceding precision statements are based on an interlabo-ratory study performed around 1975 on six samples of sodium chloridecovering the ranges of water insolubles in Table 2. One analyst in each often laboratories performed duplicate determination
41、s and repeated them ona second day.4Practice E 180 was used in developing these precisionestimates.24.2 BiasThe bias of this test method has not beendetermined due to the unavailablility of suitable referencematerials.5Fisher Scientific No. 9-730-200 has been found satisfactory.TABLE 2 Precision for
42、 Water Insolubles MethodRepeatability ReproducibilityLevel, %Coefficient of Variation,% relativeDegreesofFreedom95 % Limit, % relativeCoefficient of Variation,% RelativeDegreesofFreedom95 % Limit, % relative0.002 to 0.005 22.0 20 62 91.7 9 2570.01 to 0.04 21.9 18 61 42.2 8 1180.15 to 0.35 22.0 20 62
43、 20.5 9 57E534083CALCIUM AND MAGNESIUM25. Scope25.1 This test method covers the EDTA titrimetric determi-nation of calcium and magnesium and the EDTA titrimetricdetermination of calcium. The magnesium content is deter-mined by difference.26. Apparatus26.1 Magnetic Stirrer with Stirring Bar.27. Reage
44、nts27.1 Eriochrome Black T Indicator Solution, HydroxyNaphthol Blue, or its equivalent.27.2 Murexide (Ammonium Purpurate) Indicator Solution,or its equivalent.27.3 EDTA Standard Solution (1 mL = 0.400 mg calcium)Dissolve 4.0 g of disodium dihydrogen ethylene diaminetet-raacetate (EDTA) in 1 L of wat
45、er. Standardize this solutionagainst a standard calcium solution prepared by dissolving1.000 g of CaCO3and 2 mL of HCl in water and diluting to 1L with water in a volumetric flask. Obtain an exact factor forthe EDTA solution. This factor is equal to the milligrams ofcalcium equivalent to 1.00 mL of
46、EDTA solution. See PracticeE 200.factor 5WV(3)where:W = calcium in aliquot, mg, andV = EDTA solution required for titration, mL.27.4 Ammonium ChlorideAmmonium HydroxideSolutionAdd 67.5 g of ammonium chloride (NH4Cl) to 570mL of ammonium hydroxide (NH4OH) contained in a 1-Lvolumetric flask. Reserve t
47、his solution for use as described in27.6 and 27.7.27.5 Potassium Cyanide Solution (50 g/L)Dissolve 50 gof potassium cyanide (KCN) in water and dilute to 1 L withwater. Store in a borosilicate glass bottle. (WarningPotassium cyanide is extremely poisonous.)27.6 Magnesium Sulfate Solution (2.5 g/L)Dis
48、solve 2.5 gof MgSO47H2O in water and dilute to volume with water in a1-L volumetric flask. Determine the volume of EDTA solutionequivalent to 50 mL of MgSO4solution as follows: Pipet 50mL of MgSO4solution into a 400-mL beaker. Add 200 mL ofwater and 2 mL of NH4Cl:NH4OH solution (27.4). Add 1 mLof KC
49、N solution and a sufficient amount of Eriochrome BlackT Indicator solution or its equivalent. Titrate the solution withEDTAsolution while stirring with a magnetic stirrer to the trueblue end point. This gives the volume of EDTA solutionequivalent to 50.0 mL of MgSO4solution.27.7 Buffer SolutionPipet 50 mL of MgSO4solution intothe volumetric flask containing the remaining NH4ClNH4OHsolution (27.4). Add the exact volume of EDTA solutionequivalent to 50 mL of the MgSO4solution. Dilute to 1 L withwater. Store the solution in a polyethylene bottle.27.8
