ASTM E359-17 Standard Test Methods for Analysis of Soda Ash (Sodium Carbonate).pdf

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1、Designation: E359 17Standard Test Methods forAnalysis of Soda Ash (Sodium Carbonate)1This standard is issued under the fixed designation E359; 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 p

2、arentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the U.S. Department of Defense.1. Scope*1.1 These test methods cover the analyses usually requiredon co

3、mmercial soda ash (sodium carbonate).1.2 The analytical procedures appear in the following sec-tions:SectionsTotal Alkalinity, Titrimetric 815Sodium Bicarbonate, Titrimetric 1724Loss on Heating, Gravimetric 2632Moisture, Calculation 3438Sodium Chloride, Titrimetric 4046Sodium Sulfate, Gravimetric 48

4、54Iron, Photometric 5664Sieve Analysis 66721.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 In determining the conformance of the test results usingthis method to applicable specifications, results shall berounded off in

5、accordance with the rounding-off method ofPractice E29.1.5 Review the current Safety Data Sheets (SDS) for de-tailed information concerning toxicity, first aid procedures,handling and safety precautions.1.6 This standard does not purport to address all of thesafety concerns, if any, associated with

6、its use. It is theresponsibility of the user of this standard to establish appro-priate safety, health and environmental practices and deter-mine the applicability of regulatory limitations prior to use.Specific hazards statements are given in Section 6.1.7 This international standard was developed

7、in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents

8、2.1 ASTM Standards:2C429 Test Method for Sieve Analysis of Raw Materials forGlass ManufactureD1193 Specification for Reagent WaterD6809 Guide for Quality Control and Quality AssuranceProcedures for Aromatic Hydrocarbons and Related Ma-terialsE11 Specification for Woven Wire Test Sieve Cloth and Test

9、SievesE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE60 Practice for Analysis of Metals, Ores, and RelatedMaterials by SpectrophotometryE70 Test Method for pH of Aqueous Solutions With theGlass ElectrodeE145 Specification for Gravity-Convection and

10、 Forced-Ventilation OvensE180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals (Withdrawn 2009)3E200 Practice for Preparation, Standardization, and Storageof Standard and Reagent Solutions for Chemical AnalysisE300 Practice for Sam

11、pling Industrial Chemicals2.2 Other Documents:OSHA Regulations, 29 CFR paragraphs 19100.1000 and1910.120043. Significance and Use3.1 Soda ash is used in a number of manufacturing pro-cesses. The procedures listed in 1.2 are suitable for specifica-tion acceptance and manufacturing control of commerci

12、al sodaash.1These test methods are under the jurisdiction of ASTM Committee D16 onAromatic, Industrial, Specialty and Related Chemicals and are the direct responsi-bility of Subcommittee D16.16 on Industrial and Specialty Product Standards.Current edition approved June 15, 2017. Published August 201

13、7. Originallyapproved in 1968. Last previous edition approved in 2010 as E359 10. DOI:10.1520/E0359-17.2For 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

14、 Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.4Available from U.S. Government Printing Office, Superintendent ofDocuments, 732 N. Capitol St., NW, Washington, DC 20401-0001, http:/www.access.gpo.gov.*A Summary of Changes

15、 section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decisi

16、on on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.14. Apparatus4.1 Photometers and Photometric PracticePhotometersand photometric practice used in these test methods shallconfo

17、rm to Practice E60.4.2 pH MeterspH meters and their use shall conform toTest Method E70.4.3 BuretA calibrated 50-mL buret, or any standard50-mL buret calibrated by either the National Institute ofStandards and Technology or by the user. Alternatively, a100-mL calibrated buret with a 50-mL bulb at th

18、e top and a50-mL stem below may be used.5. Purity of Reagents and Water5.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Che

19、mical Society,where such specifications are available.5Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.5.2 Unless otherwise indicated, references to water shall beunderstood

20、to mean Type II or Type III reagent water conform-ing to Specification D1193.6. Hazards6.1 Soda ash is a primary skin irritant. Dusts or mists aremoderately irritating to the mucous membrane of the nose andeyes. The irritation is temporary and symptoms usually disap-pear shortly after contact is end

21、ed.6.2 Consult current OSHA regulations, suppliers SafetyData Sheets, and local regulations for all materials used in thistest method.7. Sampling7.1 The general principles for sampling solids are coveredin Practice E300. The following aspects of soda ash samplingmust be considered:7.2 General:7.2.1

22、The selection of a representative sample is a necessaryprerequisite for any accurate analysis, and this is particularlyimportant with the alkalies, since they are susceptible to rapidcontamination by moisture and carbon dioxide upon exposureto air. Also, some of them are not uniform in particle size

23、 andtend to segregate on handling.7.2.2 The characteristics of soda ash that make propersampling difficult at times are its tendency to absorb moistureand carbon dioxide from the air through any commercialcontainer in which it is generally shipped, and the susceptibil-ity of dense ash in bulk to seg

24、regate in relation to particle sizeas the result of normal transit vibrations.7.2.3 Details of good sampling depend on: (1) the type ofshipment, whether in containers or in bulk; (2) the type ofproduct, whether light or dense soda ash; and (3) the type ofanalysis desired, whether chemical or physica

25、l.7.3 Bulk Shipments:7.3.1 Although bulk shipments are normally in transit arelatively short time, there is likely to be some absorption ofmoisture and carbon dioxide in exposed surface areas. Ifphysical tests such as screen analysis are to be included, it isparticularly important to avoid segregati

26、on that occurs onsurface areas.7.3.2 To sample boxcar shipments, brush aside the surfacelayer to a depth of 12 in. (305 mm) and take portionssystematically from the newly exposed area to the bottom ofthe car by means of a sample thief.7.3.3 Hopper cars and trucks are more difficult to sampleadequate

27、ly. Samples can be taken through the hatches with asample thief, as for boxcar sampling. Preferably, samplesshould be taken during the unloading operation at the point ofdischarge to the bin, or from any open section of the conveyor.7.4 Bag Shipments:7.4.1 Packaged soda ash that has been in storage

28、for sometime can be sampled satisfactorily only by emptying the wholepackage and mixing thoroughly before taking the sample. Evensuch a portion is likely to represent only the package sampledrather than the stock of packages as a whole. The reason is thata bag or other container taken from an outer

29、layer of the storagepile is subject to more air contact and consequently moremoisture and carbon dioxide absorption than are packagesburied farther back in the stock.7.4.2 To get an idea of the quality of the soda ash as packed,it is the usual practice to take the sample from somewhere nearthe cente

30、r of the package. This may be done by removing thetop 6 or 8 in. (150 or 200 mm) of soda ash from the package,then removing the sample from the center of the remainingportion. Such a sample carefully taken will generally be foundrepresentative except in cases of long storage or unusuallydamp storage

31、 conditions.7.5 Sample Preparation:7.5.1 Thoroughly mix the total sample taken. Then quarteror riffle the entire sample to obtain the required size sample foranalysis. Minimize exposure to moisture and carbon dioxide.7.5.2 Store the sample for analysis in a glass or othersuitable container that will

32、 not contaminate the sample and thatcan be sealed to prevent exposure of the sample to moisture orcarbon dioxide.TOTAL ALKALINITY8. Scope8.1 This test method covers the titrimetric determination ofthe total alkalinity of soda ash. This alkalinity is normallyexpressed as percent sodium oxide (Na2O).5

33、Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopei

34、aand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.E359 1729. Summary of Test Method9.1 Total alkalinity is determined by titration with standardhydrochloric (or sulfuric) acid using methyl orange or modifiedmethyl orange indicator solution.10. Interferences10.1 Alkali

35、es other than soda ash (sodium carbonate) andcompounds that consume acid will affect the accuracy of thistest method.11. Reagents11.1 Hydrochloric (or Sulfuric) Acid (1.0 meq/mL)Prepare in accordance with Practice E200 (record temperatureof solution when standardized).11.2 Modified Methyl Orange Ind

36、icator Solution or MethylOrange Indicator SolutionSee Practice E200.11.3 Water, carbon dioxide-free (freshly boiled and cooled).12. Procedure12.1 Weigh, to the nearest 0.1 mg, 4.4 6 0.1g(Note 1)ofthe sample and transfer to a 500-mL conical flask.Add 100 mLof water and swirl to dissolve the sample.NO

37、TE 1Use of the specified weight of sample requires a 100-mL buretfor titration and is recommended. If a 50-mL buret is used, the sampleweight should be halved.12.2 Add 3 drops of modified methyl orange indicatorsolution (Note 2). Titrate this solution with standard 1.0meq/mL acid to a gray end point

38、 (Note 3). Record the volumeto the nearest 0.02 mL and temperature of the acid used.Correct the acid normality for any difference from the stan-dardization temperature by use of the factor N/C = 0.00035between 20 and 30C.Add the correction when the temperatureof use is below and subtract when above

39、the temperature ofstandardization (see Practice E200).NOTE 2If desired, 0.1 % methyl orange indicator solution may beused.NOTE 3The analyst should end the titration at the same shade of coloras was used for the end point in the standardization of the acid.13. Calculation13.1 Calculate the total alka

40、linity as percent sodium oxide(Na2O) as follows:sodium oxide, weight % 5A 3 B 30.030990! 3100W(1)where:A = acid required for titration of the sample, mL,B = corrected meq/mL of the acid, andW = sample used, g.13.2 Alternatively, calculate the alkalinity as sodium car-bonate as follows:sodium carbona

41、te, weight % 5 1.7101 3 Na2O, wt % (2)13.3 If actual sodium carbonate content is desired, thesodium bicarbonate content must be determined separately asdescribed in Sections 17 and 24. Then:sodium carbonate actual!,%5 A 2 B 30.6308! (3)where:A =Na2CO3, % (see 13.2), andB = NaHCO3, % (see 22.1).14. R

42、eport14.1 Report the percentage of sodium oxide to the nearest0.01 %.15. Precision and Bias15.1 PrecisionThe following criteria should be used forjudging the acceptability of results (Note 4):15.1.1 Repeatability (Single Analyst)The standard devia-tion for a single determination has been estimated t

43、o be0.032 % absolute at 52 DF. The 95 % limit for the differencebetween two such runs is 0.09 % absolute.15.1.2 Laboratory Precision (Within-Laboratory, Between-Days Variability)The standard deviation of results (each theaverage of duplicates), obtained by the same analyst ondifferent days, has been

44、 estimated to be 0.038 % absolute at 26DF. The 95 % limit for the difference between two suchaverages is 0.11 % absolute.15.1.3 Reproducibility (Multilaboratory)The standard de-viation of results (each the average of duplicates), obtained byanalysts in different laboratories, has been estimated to b

45、e0.154 % absolute at 8 DF. The 95 % limit for the differencebetween two such averages is 0.43 % absolute.NOTE 4These precision estimates are based on an interlaboratorystudy of analyses performed in 1967 on three samples of soda ashcovering the range from 58.190 to 58.385 % sodium oxide. Ten labora-

46、tories analyzed the three samples, with one analyst in each laboratoryperforming duplicate determinations and repeating 1 day later.6PracticeE180 was used for developing these precision estimates.15.2 BiasThe bias of this test method has not beendetermined because of the lack of acceptable reference

47、 mate-rial.16. Quality Guidelines16.1 Laboratories shall have a quality control system inplace.16.1.1 Confirm the performance of the test instrument ortest method by analyzing a quality control sample followingthe guidelines of standard statistical quality control practices.16.1.2 A quality control

48、sample is a stable material isolatedfrom the production process and representative of the samplebeing analyzed.16.1.3 When QA/QC protocols are already established inthe testing facility, these protocols are acceptable when theyconfirm the validity of test results.16.1.4 When there are no QA/QC proto

49、cols established inthe testing facility, use the guidelines described in GuideD6809 or similar statistical quality control practices.6Supporting data have been filed ASTM Headquarters and may be obtained byrequesting Request Research Report RR:E15-0046. Contact ASTM CustomerService at service astm.org.E359 173SODIUM BICARBONATE17. Scope17.1 This test method describes the titrimetric determinationof sodium bicarbonate in soda ash. The lower limit of deter-mination is 0.02 % sodium bicarbonate.18. Summary of Test Method18.1 Bicarbonate is determined t