ASTM E224-2008 781 Standard Test Methods for Analysis of Hydrochloric Acid《盐酸分析的标准试验方法》.pdf
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1、Designation: E 224 08Standard Test Methods forAnalysis of Hydrochloric Acid1This standard is issued under the fixed designation E 224; 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 parenthes
2、es indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope*1.1 These test methods cover the analysis of hydrochloricacid.1.2 The value
3、s stated in SI units are to be regarded asstandard. The values given in parentheses are for informationonly.1.3 The analytical procedures appear in the following order:SectionsTotal Acidity 8 to 16Baum Gravity 17 to 26Sulfated Ash 27 to 34Iron 35to44Color 45 to 52Total Sulfur 53 to 591.4 This standa
4、rd does not 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. Specific hazardsstatements ar
5、e given in Section 5 and 30.1, 39.7, and 48.4.2. Referenced Documents2.1 ASTM Standards:2D 1193 Specification for Reagent WaterD 1209 Test Method for Color of Clear Liquids (Platinum-Cobalt Scale)E1 Specification for ASTM Liquid-in-Glass ThermometersE60 Practice for Analysis of Metals, Ores, and Rel
6、atedMaterials by Molecular Absorption SpectrometryE 100 Specification for ASTM HydrometersE 180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty ChemicalsE 200 Practice for Preparation, Standardization, and Stor-age of Standard and Reagent S
7、olutions for ChemicalAnalysis3. Significance and Use3.1 These test methods provide for the classification ofvarious grades of hydrochloric acid and for the determinationof various impurities. Acid strength and impurity levels areimportant factors in many uses of hydrochloric acid.4. Purity of Reagen
8、ts4.1 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 Chemical Society,where such specifications are available.3Other grades m
9、ay beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.4.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean Type II or Type IIIreagent water conforming to
10、 Specification D 1193.5. Hazards5.1 Hydrochloric acid is a corrosive acid and is dangerous ifimproperly handled. Avoid any skin contact.5.2 Clean up all spills immediately by covering the spillwith vermiculite or some other inert absorbent material andsweeping into a pan. Dispose of the absorbent by
11、 flooding withwater and discarding in a suitable container. Flush the area withwater.6. Photometers and Photometric Practice6.1 Photometers and the photometric practice prescribed inthese test methods shall conform to Practice E60.1These test methods are under the jurisdiction of ASTM Committee E15
12、onIndustrial and Specialty Chemicals and are the direct responsibility of Subcommit-tee E15.02 on Product Standards.Current edition approved April 1, 2008. Published May 2008. Originallyapproved in 1965. Last previous edition approved in 2002 as E 224 96(2002).2For referenced ASTM standards, visit t
13、he ASTM website, www.astm.org, orcontact ASTM Customer Service 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,
14、 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 Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.1*A Summary of C
15、hanges section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.7. Sampling7.1 Sampling of hydrochloric acid is not within the scope ofthese test methods.7.2 The sample to be analyzed shall be consid
16、ered to be thatsample in a single bottle submitted to the analytical laboratory.7.3 The size of the sample shall be sufficient to perform allanalyses without the reuse of any portion of the sample.TOTAL ACIDITY8. Scope8.1 This test method covers the determination of the totalacidity of 27 to 37 % ma
17、ss (m/m) hydrochloric acid.9. Summary of Test Method9.1 Aweighed sample of acid is diluted in water and titratedwith standardized 0.5 meq/mL (N) sodium hydroxide solution,using phenolphthalein as the indicator.10. Interferences10.1 Acids other than hydrochloric and compounds thatconsume sodium hydro
18、xide will affect the accuracy of this testmethod.11. Apparatus11.1 Buret, 50-mL, Class A.11.2 Weighing Bottle, glass-stoppered, 50-mL.12. Reagents12.1 Phenolphthalein Indicator, Solution (10 g/L)Dissolve1gofphenolphthalein in 100 mL of ethanol (95 %),methanol, or isopropanol.412.2 Sodium Hydroxide,
19、Standard Solution (0.5 meq/mL(N)See Practice E 200. Correct for differences in tempera-ture in accordance with the following formula:N 5 Ns1 0.00014 s 2 t! (1)where:N = normality meq/mL (N) of NaOH solution at tem-perature t,Ns= normality meq/mL (N) of NaOH solution at tem-perature s during standard
20、ization,s = temperature of NaOH solution during standardiza-tion, C, andt = temperature of NaOH solution during analysis,C.13. Procedure13.1 Transfer approximately 30 mL of water to a 50-mLglass-stoppered weighing bottle, stopper, and weigh to thenearest 0.1 mg. Rapidly add a convenient size sample,
21、 depend-ing upon the acid strength as given in Table 1, stopperimmediately, and reweigh. Transfer the sample to a 400-mLbeaker containing approximately 50 mL of water and add 3 to5 drops of phenolphthalein indicator solution. Record thetemperature of the 0.5 meq/mL (N) NaOH solution, and thentitrate
22、 the sample to a pink end point. Record the titration to thenearest 0.02 mL.14. Calculation14.1 Correct the buret reading for calibration errors, andrecord as V the corrected delivered volume at the recordedtemperature.14.2 Calculate the total acidity as % mass (m/m) of hydro-chloric acid as follows
23、:Hydrochloric acid, % mass m/m!5SVN 3 0.03646WD3 100 (2)where:V = corrected mL of NaOH solution required for titra-tion of the sample,N = normality meq/mL (N) of the NaOH solution, andW = sample used, g.15. Report15.1 Report the % mass (m/m) of hydrochloric acid to thenearest 0.01 % mass (m/m).16. P
24、recision and Bias16.1 The following criteria should be used for judging theacceptability of results (see Note 1):16.1.1 Repeatability (Single Analyst)The coefficient ofvariation for a single determination has been estimated to be0.133 % mass (m/m) relative at 50 df. The 95 % limit for thedifference
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