1、Designation:E53408E53413 Standard Test Methods for Chemical Analysis of Sodium Chloride 1 This standard is issued under the xed designation E534; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision.Anumber in
2、 parentheses indicates the year of last reapproval.A superscript 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 se
3、ctions: Section Sample Preparation 5 to 9 Moisture 10 to 16 Water Insolubles 17 to 24 Calcium and Magnesium 25 to 31 Sulfate 32 to 38 Reporting ofAnalyses 39 to 41 Section Sample Preparation 5 to 9 Moisture 10 to 16 Water Insolubles 17 to 24 Calcium and Magnesium 25 to 31 Sulfate 32 to 38 Reporting
4、ofAnalyses 39 to 41 1.3 The values stated in SI 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 responsibility of the user of this s
5、tandard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 1.5 Review the current material safety data sheets (MSDS) for detailed information concerning toxicity, rst-aid procedures, handling, and safety precautions. 2. Refere
6、nced Documents 2.1 ASTM Standards: 2 D1193Specication for Reagent Water E180Practice for Determining the Precision ofASTM Methods forAnalysis andTesting of Industrial and Specialty Chemicals (Withdrawn 2009) 3 E200Practice for Preparation, Standardization, and Storage of Standard and Reagent Solutio
7、ns for Chemical Analysis 3. Signicance and Use 3.1 Sodiumchlorideoccursinnatureinalmostunlimitedquantities.nature.Itisanecessaryarticleofdietaswellasthesource for production of many sodium compounds and chlorine. The methods listed in 1.2 provide procedures for analyzing sodium chloride to determine
8、 if it is suitable for its intended use. 1 These test methods are under the jurisdiction of ASTM Committee E15 on Industrial and Specialty Chemicalsand are under the direct responsibility of Subcommittee E15.02 on Product Standards. Current edition approved Dec. 15, 2008June 1, 2013. Published Janua
9、ry 2009September 2013. Originally approved in 1975. Last previous edition approved in 20032008 as E53498E53408.(2003). DOI: 10.1520/E0534-08.10.1520/E0534-13. 2 ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatserviceastm.org.ForAnnualBookofASTMStandards volu
10、me information, refer to the standards Document Summary page on the ASTM website. 3 The last approved version of this historical standard is referenced on www.astm.org. This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have
11、 been made to the previous version. Because it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version of the standard as published by ASTM is to be considered the official do
12、cument. *ASummary of Changes section appears at the end of this standard Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959. United States 14. Reagents 4.1 Purity of ReagentsUnless otherwise indicated, it is intended that all reagents should conform to
13、the specications of the Committee on Analytical Reagents of the American Chemical Society, where such specications are available. 4 4.2 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean Type II or III reagent water conforming to Specication D1193. SAMPLE PREP
14、ARATION 5. Scope 5.1 This test method covers preparation of a sample that will be as representative as possible of the entire bulk quantity. The results of any analysis pertain only to the sample used. 6. Apparatus 6.1 Coarse Grinder. 6.2 High-Speed Blender. 6.3 Oven. 6.4 Riffle Sampler. 6.5 Scale.
15、7. Reagents 7.1 Hydrochloric Acid, Standard (1 meq/mL HCl)Prepare and standardize in accordance with Practice E200. 8. Rock and Solar Salt Stock Solutions 8.1 Mix and split sample to 500g, using the riffle sampler. 8.2 If sample appears wet, dry at 110C for 2h. 8.3 Grind the sample to 8 mesh in the
16、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 blender and blend for 5 min. 8.7 Test for wate
17、r insolubles as described in Sections 17 24. 8.8 Save ltrate from water insolubles test and dilute in a volumetric ask to 1 Lwith water as a stock solution for subsequent analyses. 9. Evaporated and Puried Salt Stock Solutions 9.1 Mix and split the sample to 100 g for evaporated salt, or 200 g for p
18、uried evaporated salt. 9.2 Transfer to a 1-L volumetric ask. 9.3 Add 800 mL of water and allow the salt to dissolve. 9.4 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 subsequ
19、ent analyses. MOISTURE 10. Scope 10.1 Thistestmethoddeterminesfreemoistureinthesaltoveraconcentrationrangefrom0.00to0.04%.Itdoesnotdetermine occluded moisture trapped within the salt crystals. The procedure is based on weight loss after a sample is heated to volatize moisture. 4 Reagent Chemicals, A
20、merican Chemical Society Specications ,American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National Form
21、ulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD. E53413 211. Apparatus 11.1 Analytical Balance. 11.2 Desiccator. 11.3 Oven. 12. Procedure, Rock and Solar Salt 12.1 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
22、.3 Cool in a desiccator and weigh. 13. Procedure, Evaporated and Puried Evaporated Salt 13.1 Weigh 20 g of salt to the nearest 0.001 g into a previously dried 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. Calculation 1
23、4.1 Calculate the percentage of moisture as follows: moisture,massm/m!%5 A B 3100 (1) where: A = loss of mass on drying, g, and B = mass of sample, g. 15. Report 15.1 Report the moisture content to the nearest 0.001%. 16. Precision and Bias 16.1 The following criteria should be used in judging the a
24、cceptability of results (Note 1): 16.1.1 Repeatability (Single Analyst)The standard deviation for a single determination has been estimated to be the percent absolute values shown in Table 1 at the indicated degrees of freedom. The 95% limit for the difference between two such runs is the percent ab
25、solute values in Table 1. 16.1.2 Laboratory precision (Within-Laboratory, Between-Days Variability)The standard deviation of results (each the averageofduplicates),obtainedbythesameanalystondifferentdays,hasbeenestimatedtobethepercentabsolutevaluesshown inTable1attheindicateddegreesoffreedom.The95%l
26、imitforthedifferencebetweentwosuchaveragesisthepercentabsolute values in Table 1. 16.1.3 Reproducibility (Multilaboratory)The standard deviation of results (each the average of duplicates), obtained by analysts in different laboratories, has been estimated to be percent absolute values shown in Tabl
27、e 1. The 95% limit for the difference between two such averages is the percent absolute values in Table 1. NOTE 1The preceding precision statements are based on an interlaboratory study performed around 1975 on ve samples of sodium chloride TABLE 1 Precision for Moisture Method Repeatability Laborat
28、ory Precision Reproducibility Level, % Standard Deviation, % Degrees of Freedom 95% Limit, % Standard Deviation, % Degrees of Freedom 95% Limit, % Standard Deviation, % Degrees of Freedom 95% Limit, % 0.003 to 0.004 0.0014 36 0.004 0.00223 18 0.006 0.00322 8 0.009 0.025 to 0.035 0.0071 60 0.02 0.004
29、28 30 0.01 0.0138 9 0.04 TABLE 1 Precision for Moisture Method Repeatability Laboratory Precision Reproducibility Level, % Standard Deviation, % Degrees of Freedom 95% Limit, % Standard Deviation, % Degrees of Freedom 95% Limit, % Standard Deviation, % Degrees of Freedom 95% Limit, % 0.003 to 0.004
30、0.0014 36 0.004 0.00223 18 0.006 0.00322 8 0.009 0.025 to 0.035 0.0071 60 0.02 0.00428 30 0.01 0.0138 9 0.04 E53413 3containing covering the ranges of moisture in Table 1. One analyst in each of ten laboratories performed duplicate determinations and repeated them on a second day. 5 Practice E180 wa
31、s used in developing these precision estimates. 16.2 BiasThe bias of this test method has not been determined due to the unavailability of suitable reference materials. WATER INSOLUBLES 17. Scope 17.1 This gravimetric method determines only the amount of insolubles present in sodium chloride which w
32、ill not dissolve in water. 18. Apparatus 18.1 Analytical Balance. 18.2 Desiccator. 18.3 Magnetic Stirrer with Stirring Bar. 18.4 Parabella Filter Funnel Assembly, 6 1000-mL, or its equivalent with 0.3-m glass ber lter disk. 19. Reagents 19.1 Silver Nitrate, Standard Solution, 0.1 meq/mLAgNO 3 Prepar
33、e and standardize in accordance with Practice E200. 20. Procedure, Rock and Solar Salts 20.1 Transfer a sample prepared in accordance with 8.1 to 8.6 to a 1-LErlenmeyer ask, washing out the blender with 100 mL of water. Add 300 mL of water to give a total of 600 mL of water added. 20.2 Stir on a mag
34、netic stirrer for 1 h.Adjust the stirrer speed to give maximum agitation without danger of losing any sample due to splashing. Place a beaker or watch glass over top of the ask while stirring. 20.3 Filter the solution by vacuum through a previously dried (110C for 1 h) and accurately weighed lter di
35、sk using the Parabellafunnel.Transferallinsolublestothepaperandwashfreeofchlorideswithwateruntiltheltrateshowsnoturbiditywhen tested with 0.1 meq/mLAgNO 3 solution. 20.4 Dilute ltrate and washings to 1 L with water in volumetric ask. 20.5 Dry the lter disk at 110C for 1 h. 20.6 Cool in a desiccator
36、and weigh the disk on an analytical balance. 20.7 Save the ltrate for subsequent analyses. 21. Procedure, Evaporated and Puried Evaporated Salts 21.1 Place a well mixed sample in a 2-L beaker. Use 100-g sample for evaporated or 200 g for puried evaporated salt. 21.2 Add 750 mL of water. 21.3 Mix wit
37、h a mechanical stirrer until solution is complete. 21.4 Filter the solution by vacuum through a previously dried (110C for 1 h) and accurately weighed lter disk using the Parabellafunnel.Transferallinsolublestothepaperandwashfreeofchlorideswithwateruntiltheltrateshowsnoturbiditywhen tested with 0.1
38、meq/mLAgNO 3 solution. 21.5 Dry the lter disk at 110C for 1 h. 21.6 Cool in a desiccator and weigh on an analytical balance. 21.7 Dilute the ltration and washings to 1 L with water in a volumetric ask and reserve for subsequent analyses. 22. Calculation 22.1 Calculate the percentage of water insolub
39、les as follows: insolubles,%massm/m!5 A B 3100 (2) where: A = increase in mass of lter disk, g, and 5 Supporting data have been led at ASTM International Headquarters and may be obtained by requesting Research Report RR:E15-1052. 6 Fisher Scientic No. 9-730-200 has been found satisfactory. E53413 4B
40、 = sample mass, g. 23. Report 23.1 Report the percentage of water insolubles to the nearest percentage shown as follows: Range, % Report to, % 0.002 to 0.005 0.001 0.01 to 0.04 0.01 0.15 to 0.35 0.01 Range, % Report to, % 0.002 to 0.005 0.001 0.01 to 0.04 0.01 0.15 to 0.35 0.01 24. Precision and Bia
41、s 24.1 The following criteria should be used in judging the acceptability of results (Note 2): 24.1.1 Repeatability (Single Analyst)The coefficient of variation for a single determination has been estimated to be the percent relative values shown in Table 2 at the indicated degrees of freedom. The 9
42、5% limit for the difference between two such runs is percent relative values shown in Table 2. 24.1.2 Laboratory Precision (Within-Laboratory, Between-Days Variability)The coefficient of variation of results (each the averageofduplicates),obtainedbythesameanalystondifferentdays,hasbeenestimatedtobe2
43、3.5%relativeat57df.The95% limit for the difference between two such averages is 66% relative. 24.1.3 Reproducibility (Multilaboratory)The coefficient of variation of results (each the average of duplicates), obtained by analysts in different laboratories, has been estimated to be percent relative va
44、lues shown in Table 2 at the indicated degrees of freedom. The 95% limit for the difference between two such averages is percent relative values shown in Table 2. NOTE2Theprecedingprecisionstatementsarebasedonaninterlaboratorystudyperformedaround1975onsixsamplesofsodiumchloridecovering therangesofwa
45、terinsolublesinTable2.Oneanalystineachoftenlaboratoriesperformedduplicatedeterminationsandrepeatedthemonasecondday. 5 Practice E180 was used in developing these precision estimates. 24.2 BiasThe bias of this test method has not been determined due to the unavailablilityunavailability of suitable ref
46、erence materials. CALCIUM AND MAGNESIUM 25. Scope 25.1 This test method covers the EDTA titrimetric determination of calcium and magnesium and the EDTA titrimetric determination of calcium. The magnesium content is determined by difference. 26. Apparatus 26.1 Magnetic Stirrer with Stirring Bar. 27.
47、Reagents 27.1 Eriochrome Black T Indicator Solution, Hydroxy Naphthol Blue, or its equivalent. 27.2 Murexide (Ammonium Purpurate) Indicator Solution, or its equivalent. TABLE 2 Precision for Water Insolubles Method Repeatability Reproducibility Level, % Coefficient of Variation, % relative Degrees o
48、f Freedom 95% Limit, % relative Coefficient of Variation, % Relative Degrees of Freedom 95% Limit, % relative 0.002 to 0.005 22.0 20 62 91.7 9 257 0.01 to 0.04 21.9 18 61 42.2 8 118 0.15 to 0.35 22.0 20 62 20.5 9 57 TABLE 2 Precision for Water Insolubles Method Repeatability Reproducibility Level, %
49、 Coefficient of Variation, % relative Degrees of Freedom 95% Limit, % relative Coefficient of Variation, % Relative Degrees of Freedom 95% Limit, % relative 0.002 to 0.005 22.0 20 62 91.7 9 257 0.01 to 0.04 21.9 18 61 42.2 8 118 0.15 to 0.35 22.0 20 62 20.5 9 57 E53413 527.3 EDTAStandardSolution(1mL=0.400mgcalcium)Dissolve4.0gofdisodiumdihydrogenethylenediaminetetraacetate (EDTA) in 1 L of water. Standardize this solution against a standard calcium solution prepared by dissolving 1.000 g of CaCO 3 and 2 mLof HCl in wate
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