1、Designation: E359 10E359 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 numb
2、er in parentheses 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 requir
3、ed on commercial soda ash (sodium carbonate).1.2 The analytical procedures appear in the following sections:SectionsTotal Alkalinity, Titrimetric 8 15Sodium Bicarbonate, Titrimetric 16 23Sodium Bicarbonate, Titrimetric 17 24Loss on Heating, Gravimetric 24 30Loss on Heating, Gravimetric 26 32Moisture
4、, Calculation 31 35Moisture, Calculation 34 38Sodium Chloride, Titrimetric 36 42Sodium Chloride, Titrimetric 40 46Sodium Sulfate, Gravimetric 43 49Sodium Sulfate, Gravimetric 48 54Iron, Photometric 50 58Iron, Photometric 56 64Sieve Analysis 59 65Sieve Analysis 66 721.3 The values stated in SI units
5、are to be regarded as standard. No other units of measurement are included in this standard.1.4 In determining the conformance of the test results using this method to applicable specifications, results shall be roundedoff in accordance with the rounding-off method of Practice E29.1.5 Review the cur
6、rent Materials Safety Data Sheets (MSDS)(SDS) for detailed information concerning toxicity, first aidprocedures, handling and safety precautions.1.6 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 stan
7、dard to establish appropriate safety safety, health and healthenvironmental practices and determine theapplicability of regulatory limitations prior to use. Specific hazards statements are given in Section 6.1.7 This international standard was developed in accordance with internationally recognized
8、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. Referenced Documents2.1 ASTM Standards:2C429 Test Method for Sieve An
9、alysis of Raw Materials for Glass ManufactureD1193 Specification for Reagent WaterD6809 Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related MaterialsE11 Specification for Woven Wire Test Sieve Cloth and Test SievesE29 Practice for Using Significant Digits
10、 in Test Data to Determine Conformance with Specifications1 These test methods are under the jurisdiction of ASTM Committee D16 on Aromatic Hydrocarbons Aromatic, Industrial, Specialty and Related Chemicals and are thedirect responsibility of Subcommittee D16.16 on Industrial and Specialty Product S
11、tandards.Current edition approved March 1, 2010June 15, 2017. Published April 2010August 2017. Originally approved in 1968. Last previous edition approved in 20052010 asE359 00 (2005)E359 10.1. DOI: 10.1520/E0359-10.10.1520/E0359-17.2 For referencedASTM standards, visit theASTM website, www.astm.org
12、, 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.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes
13、 have been made to the previous version. Becauseit 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 versionof the standard as published by ASTM is to be considered the official
14、 document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1E60 Practice for Analysis of Metals, Ores, and Related Materials by SpectrophotometryE70 Test Method for pH of
15、Aqueous Solutions With the Glass ElectrodeE145 Specification for Gravity-Convection and Forced-Ventilation OvensE180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial and Specialty Chemicals(Withdrawn 2009)3E200 Practice for Preparation, Standardization, a
16、nd Storage of Standard and Reagent Solutions for Chemical AnalysisE300 Practice for Sampling Industrial Chemicals2.2 Other Documents:OSHA Regulations, 29 CFR paragraphs 19100.1000 and 1910.120043. Significance and Use3.1 Soda ash is used in a number of manufacturing processes. The procedures listed
17、in 1.2 are suitable for specificationacceptance and manufacturing control of commercial soda ash.4. Apparatus4.1 Photometers and Photometric PracticePhotometers and photometric practice used in these test methods shall conform toPractice E60.4.2 pH MeterspH meters and their use shall conform to Test
18、 Method E70.4.3 BuretA calibrated 50-mL buret, or any standard 50-mL buret calibrated by either the National Institute of Standards andTechnology or by the user. Alternatively, a 100-mL calibrated buret with a 50-mL bulb at the top and a 50-mL stem below maybe used.5. Purity of Reagents and Water5.1
19、 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, wheresuch specifications are available.5 Other grades may b
20、e used, provided it is first ascertained that the reagent is of sufficiently highpurity to permit its use without lessening the accuracy of the determination.5.2 Unless otherwise indicated, references to water shall be understood to mean Type II or Type III reagent water conformingto Specification D
21、1193.6. Hazards6.1 Soda ash is a primary skin irritant. Dusts or mists are moderately irritating to the mucous membrane of the nose and eyes.The irritation is temporary and symptoms usually disappear shortly after contact is ended.6.2 Consult current OSHA regulations, suppliers Safety Data Sheets, a
22、nd local regulations for all materials used in this testmethod.7. Sampling7.1 The general principles for sampling solids are covered in Practice E300. The following aspects of soda ash sampling mustbe considered:7.2 General:7.2.1 The selection of a representative sample is a necessary prerequisite f
23、or any accurate analysis, and this is particularlyimportant with the alkalies, since they are susceptible to rapid contamination by moisture and carbon dioxide upon exposure toair. Also, some of them are not uniform in particle size and tend to segregate on handling.7.2.2 The characteristics of soda
24、 ash that make proper sampling difficult at times are its tendency to absorb moisture and carbondioxide from the air through any commercial container in which it is generally shipped, and the susceptibility of dense ash in bulkto segregate in relation to particle size as the result of normal transit
25、 vibrations.7.2.3 Details of good sampling depend on: (1) the type of shipment, whether in containers or in bulk; (2) the type of product,whether light or dense soda ash; and (3) the type of analysis desired, whether chemical or physical.7.3 Bulk Shipments:3 The last approved version of this histori
26、cal standard is referenced on www.astm.org.4 Available from U.S. Government Printing Office, Superintendent of Documents, 732 N. Capitol St., NW, Washington, DC 20401-0001, http:/www.access.gpo.gov.5 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington,
27、DC. For suggestions on the 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.E359 1727.3.1 A
28、lthough bulk shipments are normally in transit a relatively short time, there is likely to be some absorption of moistureand carbon dioxide in exposed surface areas. If physical tests such as screen analysis are to be included, it is particularly importantto avoid segregation that occurs on surface
29、areas.7.3.2 To sample boxcar shipments, brush aside the surface layer to a depth of 12 in. (305 mm) and take portions systematicallyfrom the newly exposed area to the bottom of the car by means of a sample thief.7.3.3 Hopper cars and trucks are more difficult to sample adequately. Samples can be tak
30、en through the hatches with a samplethief, as for boxcar sampling. Preferably, samples should be taken during the unloading operation at the point of discharge to thebin, or from any open section of the conveyor.7.4 Bag Shipments:7.4.1 Packaged soda ash that has been in storage for some time can be
31、sampled satisfactorily only by emptying the wholepackage and mixing thoroughly before taking the sample. Even such a portion is likely to represent only the package sampledrather than the stock of packages as a whole. The reason is that a bag or other container taken from an outer layer of the stora
32、gepile is subject to more air contact and consequently more moisture and carbon dioxide absorption than are packages buried fartherback 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 center of the package
33、. This may be done by removing the top 6 or 8 in. (150 or 200 mm) of soda ash from the package, thenremoving the sample from the center of the remaining portion. Such a sample carefully taken will generally be found representativeexcept in cases of long storage or unusually damp storage conditions.7
34、.5 Sample Preparation:7.5.1 Thoroughly mix the total sample taken. Then quarter or 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 other suitable container that will not contam
35、inate the sample and that can besealed to prevent exposure of the sample to moisture or carbon dioxide.TOTAL ALKALINITY8. Scope8.1 This test method covers the titrimetric determination of the total alkalinity of soda ash. This alkalinity is normally expressedas percent sodium oxide (Na2O).8. Scope8.
36、1 This test method covers the titrimetric determination of the total alkalinity of soda ash. This alkalinity is normally expressedas percent sodium oxide (Na2O).9. Summary of Test Method9.1 Total alkalinity is determined by titration with standard hydrochloric (or sulfuric) acid using methyl orange
37、or modifiedmethyl orange indicator solution.10. Interferences10.1 Alkalies other than soda ash (sodium carbonate) and compounds that consume acid will affect the accuracy of this testmethod.11. Reagents11.1 Hydrochloric (or Sulfuric) Acid (1.0 meq/mL)Prepare in accordance with Practice E200 (record
38、temperature of solutionwhen standardized).11.2 Modified Methyl Orange Indicator Solution or Methyl Orange 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 0.1 g (Note 1) of the sample and transfer to
39、 a 500-mL conical flask. Add 100 mL ofwater and swirl to dissolve the sample.NOTE 1Use of the specfiedspecified weight of sample requires a 100-mL buret for 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 indicator
40、solution (Note 2). Titrate this solution with standard 1.0 meq/mL acidto a gray end point (Note 3). Record the volume to the nearest 0.02 mLand temperature of the acid used. Correct the acid normalityE359 173for any difference from the standardization temperature by use of the factor N/C = 0.00035 b
41、etween 20 and 30C. Add thecorrection when the temperature of use is below and subtract when above the temperature of standardization (see Practice E200).NOTE 2If desired, 0.1 % methyl orange indicator solution may be used.NOTE 3The analyst should end the titration at the same shade of color as was u
42、sed for the end point in the standardization of the acid.13. Calculation13.1 Calculate the total alkalinity as percent sodium oxide (Na2O) as follows:sodium oxide,%mass m/m!5A 3B 30.030990!3100W (1)sodium oxide, weight % 5 A 3B 30.030990!3100W (1)where:A = acid required for titration of the sample,
43、mL,B = corrected meq/mL of the acid, andW = sample used, g.13.2 Alternatively, calculate the alkalinity as sodium carbonate as follows:sodium carbonate,%mass m/m!51.71013Na2O,wt % (2)sodium carbonate, weight % 51.71013Na2O,wt % (2)13.3 If actual sodium carbonate content is desired, the sodium bicarb
44、onate content must be determined separately as describedin Sections 1617 and 2324. Then:sodium carbonate actual!,%5A 2B 30.6308! (3)where:A = Na2CO3, % (see 13.2), andB = NaHCO3, % (see 21.1).B = NaHCO3, % (see 22.1).14. Report14.1 Report the percentage of sodium oxide to the nearest 0.01 %.15. Prec
45、ision and Bias15.1 PrecisionThe following criteria should be used for judging the acceptability of results (Note 4):15.1.1 Repeatability (Single Analyst)The standard deviation for a single determination has been estimated to be 0.032 %absolute at 52 DF. The 95 % limit for the difference between two
46、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 on different days, has been estimated to be 0.038 % absolute at 26 DF. The95 % limit for the differenc
47、e between two such averages is 0.11 % absolute.15.1.3 Reproducibility (Multilaboratory)The standard deviation of results (each the average of duplicates), obtained byanalysts in different laboratories, has been estimated to be 0.154 % absolute at 8 DF. The 95 % limit for the difference betweentwo su
48、ch averages is 0.43 % absolute.NOTE 4These precision estimates are based on an interlaboratory study of analyses performed in 1967 on three samples of soda ash covering the rangefrom 58.190 to 58.385 % sodium oxide. Ten laboratories analyzed the three samples, with one analyst in each laboratory per
49、forming duplicatedeterminations and repeating 1 day later.6 Practice E180 was used for developing these precision estimates.15.2 BiasThe bias of this test method has not been determined because of the lack of acceptable reference material.16. Quality Guidelines16.1 Laboratories shall have a quality control system in place.16.1.1 Confirm the performance of the test instrument or test method by analyzing a quality control sample following theguidelines of standard statistical quality control practices.16.1.2 Aquality contr
