ASTM E538-17a Standard Test Methods for Mercury in Caustic Soda (Sodium Hydroxide) and Caustic Potash (Potassium Hydroxide).pdf
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1、Designation: E538 17aStandard Test Methods forMercury in Caustic Soda (Sodium Hydroxide) and CausticPotash (Potassium Hydroxide)1This standard is issued under the fixed designation E538; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revisi
2、on, the year of last revision. A number 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 routine determination ofmercury in caustic soda and caustic potash liquo
3、rs and anhy-drous caustic soda in the solid, flake, ground, and bead form bythe flameless atomic absorption method.1.2 Two test methods are described as follows: Test MethodA employs a direct analysis of the sample using an alkalinereducing agent with a lower limit of detection of 0.1 ppb(ng/g). Tes
4、t Method A was developed using caustic soda andcaustic potash. Test Method B requires a preliminary neutral-ization of the sample followed by a permanganate oxidationbefore it can be analyzed by an acidic reducing agent with alower limit of detection of this test method of 0.01 ppm (g/g).Test Method
5、 B was developed using caustic soda.1.3 Review the current Safety Data Sheets (SDS) for de-tailed information concerning toxicity, first-aid procedures, andsafety precautions.1.4 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1
6、.5 This standard 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 hazard
7、sstatements are given in Sections 7 and 18.1.6 This international standard was developed 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 Wo
8、rld Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD6809 Guide for Quality Control and Quality AssuranceProcedures for Aromatic Hydrocarbons and Related Ma-terialsE180 Practice for Determining the Precisio
9、n of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals (Withdrawn 2009)3TEST METHOD AALKALINE REDUCING AGENT3. Summary of Test Method3.1 All forms of mercury are reduced to metallic mercurywhich is aerated from the solution and determined by coldvapor atomic absorption anal
10、ysis.4. Significance and Use4.1 Mercury is a toxic material and is also deleterious ifpresent in caustic soda and caustic potash used in certainmanufacturing processes. It must therefore be controlled as apossible pollutant. These test methods provide a procedure formeasuring mercury in liquid and s
11、olid caustic soda and causticpotash.5. Apparatus5.1 Atomic Absorption Spectrophotometer, equipped withmounting to hold an absorption cell and a fast response (0.5-s)recorder.5.2 Mercury Hollow Cathode Lamp, primary line 253.7 nm.5.3 Absorption Cell, 10-cm path length with quartz win-dows.5.4 Gas Was
12、hing Bottle, 125-mL, with extra-coarse frittedbubbler. The bottle has a calibration line drawn at the 60-mLmark.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 D16.15 on In
13、dustrial and Specialty General Standards.Current edition approved July 1, 2017. Published July 2017. Originally approvedin 1975. Last previous edition approved in 2017 as E538 17. DOI: 10.1520/E0538-17a.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Ser
14、vice at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.*A Summary of Changes section appears at the end of this standardCopyright
15、 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 Decision on Principles for theDevelopment of International
16、Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.15.5 Gas Washing Bottle, 125-mL, without frit.5.6 Stopcock, three-way, with TFE-fluorocarbon plug.5.7 Needle Valve.5.8 Drying Tube.5.9 Vacuum Trap.5.10 Flowmeter, capable of measu
17、ring and maintaining aflow rate of 1.5 standard ft3/h.NOTE 1The procedure as described in this test method employs aPerkin-Elmer Model 303 atomic absorption spectrophotometer.Any otherequivalent atomic absorption spectrophotometer may be used as well asthe many commercial instruments specifically de
18、signed for measurementof mercury by flameless atomic absorption now available. However,variation in instrument geometry, cell length, sensitivity, and mode ofresponse measurement may require appropriate modifications of theoperating parameters.6. Reagents6.1 Purity of ReagentsUnless otherwise indica
19、ted, it isintended that all reagents shall conform to the specifications ofthe Committee onAnalytical Reagents of theAmerican Chemi-cal Society, where such specifications are available.4Othergrades may be used, provided it is first ascertained that thereagent is of sufficiently high purity to permit
20、 its use withoutlessening the accuracy of the determination.6.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean Type II or III reagentwater conforming to Specification D1193.6.3 Anhydrous Magnesium Perchlorate.6.4 Sodium Hydroxide 50 %Membrane grade caustic
21、soda50 %.6.5 Aqua RegiaCarefully add 10-mL of concentratedHNO3(sp gr 1.42) to 30 mL of concentrated HCl (sp gr 1.19)in a 100-mLbeaker. Let the mixture stand for 5 min before use.This mixture is unstable and should not be stored. (WarningUse goggles when preparing this solution.)6.6 Cadmium Chloride
22、Solution (10 g/100 mL)Dissolve10 g of cadmium chloride in 50 mL of water and then add 50mL of 50 % membrane grade caustic soda. Cadmium hydrox-ide will precipitate upon the addition of the caustic soda. Thissolution must be well shaken before use. (WarningUsegoggles when preparing this solution.)6.7
23、 Stannous Chloride Solution (10 g/100 mL)Dissolve10 g of stannous chloride (SnCl22H2O) in 100 mL of water.Prepare fresh once a week.6.8 Mercuric Nitrate Stock Solution (0.05 M) (1 mL= 10 mgHg)Dissolve 17.1 g of mercuric nitrate (Hg(NO3)2H2O) in100 mL of water containing 2 mL of concentrated HNO3in a
24、1-L volumetric flask. Dilute to volume with water and mixwell.6.9 Mercury Standard Solution (1 mL = 50 g Hg)Pipet5.0 mL of 0.05 M mercuric nitrate stock solution into a 1-Lvolumetric flask, acidify with 5 mL of H2SO4(1+4), and diluteto volume with water. Mix well.6.10 Mercury Standard Solution (1 mL
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