1、Designation: E534 13E534 18Standard Test Methods forChemical Analysis of Sodium Chloride1This standard is issued under the fixed designation E534; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number
2、in parentheses 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 usually required for sodium chloride.1.2 The analytical procedures appear in the following sec
3、tions:SectionSample Preparation 5 to 9Moisture 10 to 16Moisture 10 to 17Water Insolubles 17 to 24Water Insolubles 18 to 26Calcium and Magnesium 25 to 31Calcium and Magnesium 27 to 34Sulfate 32 to 38Sulfate 35 to 42Reporting of Analyses 39 to 41Reporting of Analyses 43 to 451.3 The values stated in S
4、I units are to be regarded as standard. No other units of measurement are included in this standard.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety safety,
5、health, and healthenvironmental practices and determine theapplicability of regulatory limitations prior to use.1.5 Review the current material safety data sheets (MSDS)(SDS) for detailed information concerning toxicity, first-aidprocedures, handling, and safety precautions.1.6 This international st
6、andard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Re
7、ferenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD6809 Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related MaterialsE180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial and Specialty
8、Chemicals(Withdrawn 2009)3E200 Practice for Preparation, Standardization, and Storage of Standard and Reagent Solutions for Chemical Analysis3. Significance and Use3.1 Sodium chloride occurs in nature. It is a necessary article of diet as well as the source for production of many sodiumcompounds and
9、 chlorine. The methods listed in 1.2 provide procedures for analyzing sodium chloride to determine if it is suitablefor its intended use.1 These test methods are under the jurisdiction ofASTM Committee D16 on Aromatic HydrocarbonsAromatic, Industrial, Specialty and Related Chemicals and are underthe
10、 direct responsibility of Subcommittee D16.16 on Industrial and Specialty Product Standards.Current edition approved June 1, 2013Feb. 1, 2018. Published September 2013April 2018. Originally approved in 1975. Last previous edition approved in 20082013 asE534 08.E534 13. DOI: 10.1520/E0534-13.10.1520/
11、E0534-18.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 The last approved version of this historical stand
12、ard is referenced on www.astm.org.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recom
13、mends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C70
14、0, West Conshohocken, PA 19428-2959. United States14. Reagents4.1 Purity of ReagentsUnless otherwise indicated, it is intended that all reagents should conform to the specifications of theCommittee on Analytical Reagents of the American Chemical Society, where such specifications are available.44.2
15、Purity of WaterUnless otherwise indicated, references to water shall be understood to mean Type II or III reagent waterconforming to Specification D1193.SAMPLE PREPARATION5. Scope5.1 This test method covers preparation of a sample that will be as representative as possible of the entire bulk quantit
16、y. Theresults of any analysis pertain only to the sample used.5. Scope5.1 This test method covers preparation of a sample that will be 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 B
17、lender.Blender.6.3 Oven.6.4 Riffle Sampler.6.5 Scale.7. Reagents7.1 Hydrochloric Acid, Standard (1 meq/mL HCl)Prepare and standardize in accordance with Practice E200.8. 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 1
18、10C for 2 h.8.3 Grind the sample to 8 mesh in the coarse grinder.8.4 Mix ground sample well and weigh out a 25.0-g representative portion for rock salt or 50.0 g for solar salt.8.5 Place 200 mL of water in the high-speed blender and start at low speed.8.6 Slowly add the salt sample to the high-speed
19、 blender and blend for 5 min.8.7 Test for water insolubles as described in Sections 1718 2426.8.8 Save filtrate from water insolubles test and dilute in a volumetric flask to 1 L with water as a stock solution for subsequentanalyses.9. Evaporated and Purified Salt Stock Solutions9.1 Mix and split th
20、e sample to 100 g for evaporated salt, or 200 g for purified evaporated salt.9.2 Transfer to a 1-L volumetric flask.9.3 Add 800 mL of water and allow the salt to dissolve.4 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the
21、testing of reagents not listed bythe American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.TABLE 1 Precision for Moisture MethodRepea
22、tability Laboratory Precision ReproducibilityLevel, % StandardDeviation, % Degrees ofFreedom 95 % Limit, % StandardDeviation, % Degrees ofFreedom 95 % Limit, % StandardDeviation, % Degrees ofFreedom 95 % 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
23、 0.00428 30 0.01 0.0138 9 0.04E534 1829.4 Add 2 mL of concentrated HCl to dissolve any water insoluble calcium salts, particularly calcium carbonate.9.5 Dilute to volume with water and use as a stock solution for subsequent analyses.MOISTURE10. Scope10.1 This test method determines free moisture in
24、the salt over a concentration range from 0.00 to 0.04 %. It does not determineoccluded moisture trapped within the salt crystals. The procedure is based on weight loss after a sample is heated to volatizemoisture.10. Scope10.1 This test method determines free moisture in the salt over a concentratio
25、n range from 0.00 to 0.04 %. It does not determineoccluded moisture trapped within the salt crystals. The procedure is based on weight loss after a sample is heated to volatizemoisture.11. Apparatus11.1 Analytical Balance.Balance capable of weighing to 60.001 g.11.2 Desiccator.11.3 Oven.12. Procedur
26、e, Rock and Solar Salt12.1 Weigh 100 g of salt to the nearest 0.05 g into a previously 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 a previously dri
27、ed and weighed glass weighing bottle and 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!%5AB 3100 (1)where:A = loss of mass on drying, g, andB = mass of sample, g.15. Report15.1
28、Report the moisture content to the nearest 0.001 %.16. Precision and Bias516.1 The following criteria should be used in judging Ten laboratories analyzed five samples in duplicate on two different days.Practice E180the acceptability of results ( was followed for the design and analysis of the data;N
29、ote 1): the details are given isASTM Research Report RR:E15-1052.16.1.1 Intermediate Precision, formerly called Repeatability (Single Analyst)The standard deviation for a single determina-tion has been estimated to be the percent absolute values shown in Table 1 at the indicated degrees of freedom.
30、The 95 % limitfor the difference between two such runs is the percent absolute values in Table 1.E534 18316.1.2 Laboratory precisionPrecision (Within-Laboratory, Between-Days Variability)The standard deviation of results (eachthe average of duplicates), obtained by the same analyst on different days
31、, has been estimated to be the percent absolute valuesshown in Table 1 at the indicated degrees of freedom. The 95 % limit for the difference between two such averages is the percentabsolute values in Table 1.16.1.3 Reproducibility (Multilaboratory)The standard deviation of results (each the average
32、 of duplicates), obtained byanalysts in different laboratories, has been estimated to be percent absolute values shown in Table 1. The 95 % limit for thedifference between two such averages is the percent absolute values in Table 1.NOTE 1The preceding precision statements are based on an interlabora
33、tory study performed around 1975 on five samples of sodium chloridecontaining covering the ranges of moisture in Table 1. One analyst in each of ten laboratories performed duplicate determinations and repeated them ona second day.5 Practice E180 was used in developing these precision estimates.16.2
34、BiasThe bias of this test method has not been determined due to the unavailability of suitable reference materials.17. Quality Guidelines17.1 Laboratories shall have a quality control system in place.17.1.1 Confirm the performance of the test instrument or test method by analyzing a quality control
35、sample following theguidelines of standard statistical quality control practices.17.1.2 Aquality control sample is a stable material isolated from the production process and representative of the sample beinganalyzed.17.1.3 When QA/QC protocols are already established in the testing facility, these
36、protocols are acceptable when they confirmthe validity of test results.17.1.4 When there are no QA/QC protocols established in the testing facility, use the guidelines described in Guide D6809 orsimilar statistical quality control practices.WATER INSOLUBLES17. Scope17.1 This gravimetric method deter
37、mines only the amount of insolubles present in sodium chloride which will not dissolve inwater.18. Scope18.1 This gravimetric method determines only the amount of insolubles present in sodium chloride which will not dissolve inwater.19. Apparatus19.1 Analytical Balance.19.2 Desiccator.19.3 Magnetic
38、Stirrer with Stirring Bar.19.4 Parabella Filter Funnel Assembly, 1000-mL, or its equivalent with 0.3-m glass fiber filter disk.20. Reagents20.1 Silver Nitrate, Standard Solution, 0.1 meq/mL AgNO3Prepare and standardize in accordance with Practice E200.21. Procedure, Rock and Solar Salts21.1 Transfer
39、 a sample prepared in accordance with 8.1 to 8.6 to a 1-L Erlenmeyer flask, washing out the blender with 100 mLof water. Add 300 mL of water to give a total of 600 mL of water added.21.2 Stir on a magnetic stirrer for 1 h. Adjust the stirrer speed to give maximum agitation without danger of losing a
40、ny sampledue to splashing. Place a beaker or watch glass over top of the flask while stirring.21.3 Filter the solution by vacuum through a previously dried (110C for 1 h) and accurately weighed filter disk using theParabella funnel.Transfer all insolubles to the paper and wash free of chlorides with
41、 water until the filtrate shows no turbidity whentested with 0.1 meq/mL AgNO3 solution.21.4 Dilute filtrate and washings to 1 L with water in volumetric flask.21.5 Dry the filter disk at 110C for 1 h.5 Supporting data have been filed at ASTM International Headquarters and may be obtained by requesti
42、ng Research Report RR:E15-1052. Contact ASTM CustomerService at serviceastm.org.E534 18421.6 Cool in a desiccator and weigh the disk on an analytical balance.21.7 Save the filtrate for subsequent analyses.22. Procedure, Evaporated and Purified Evaporated Salts22.1 Place a well mixed sample in a 2-L
43、beaker. Use 100-g sample for evaporated or 200 g for purified evaporated salt.22.2 Add 750 mL of water.22.3 Mix with a mechanical stirrer until solution is complete.22.4 Filter the solution by vacuum through a previously dried (110C for 1 h) and accurately weighed filter disk using theParabella funn
44、el.Transfer all insolubles to the paper and wash free of chlorides with water until the filtrate shows no turbidity whentested with 0.1 meq/mL AgNO3 solution.22.5 Dry the filter disk at 110C for 1 h.22.6 Cool in a desiccator and weigh on an analytical balance.22.7 Dilute the filtration and washings
45、to 1 L with water in a volumetric flask and reserve for subsequent analyses.23. Calculation23.1 Calculate the percentage of water insolubles as follows:insolubles,%mass m/m!5AB 3100 (2)where:A = increase in mass of filter disk, g, andB = sample mass, g.24. Report24.1 Report the percentage of water i
46、nsolubles to the nearest percentage shown as follows:Range, % Report to, %0.002 to 0.005 0.0010.01 to 0.04 0.010.15 to 0.35 0.0125. Precision and Bias525.1 The following criteria should be used in judging Ten laboratories analyzed six samples in duplicate on two different days.Practice E180the accep
47、tability of results ( was followed for the design and analysis of the data;Note 2): the details are given isASTM Research Report RR:E15-1052.25.1.1 Intermediate Precision, formerly called Repeatability (Single Analyst)The coefficient of variation for a singledetermination has been estimated to be th
48、e percent relative values shown in Table 2 at the indicated degrees of freedom. The 95 %limit for the difference between two such runs is percent relative values shown in Table 2.25.1.2 Laboratory Precision (Within-Laboratory, Between-Days Variability)The coefficient of variation of results (each th
49、eaverage of duplicates), obtained by the same analyst on different days, has been estimated to be 23.5 % relative at 57 df. The 95 %limit for the difference between two such averages is 66 % relative.25.1.3 Reproducibility (Multilaboratory)The coefficient of variation of results (each the average of duplicates), obtained byanalysts in different laboratories, has been estimated to be percent relative values shown in Table 2 at the indicated degrees offreedom. The 95 % limit for the difference between two such averages is percent relative values shown
