1、Designation: E506 17E506 17aStandard Test Method forMercury in Liquid Chlorine1This standard is issued under the fixed designation E506; 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 parenth
2、eses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This test method2 covers the determination of mercury in liquid chlorine with a lower limit of detection of 0.1 g/L.1.2 Review the current Safety Data
3、Sheet (SDS) for detailed information concerning toxicity, first-aid procedures, and safetyprecautions.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
4、, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. Specific precautionary statements are given in Sections 7, 6.3, 6.4, 6.5, and Note 2.1.4
5、 Review the current Safety Data Sheet (SDS) for detailed information concerning toxicity, first-aid procedures, and safetyprecautions.1.5 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for
6、 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:3D1193 Specification for Reagent WaterD6809 Guide for Quality Control and Quality Assurance Procedures f
7、or Aromatic Hydrocarbons and Related MaterialsE180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial and Specialty Chemicals(Withdrawn 2009)4E200 Practice for Preparation, Standardization, and Storage of Standard and Reagent Solutions for Chemical Analysis
8、3. Summary of Test Method3.1 Liquid chlorine samples are taken in chilled glass flasks, then allowed to evaporate slowly to dryness. The mercury is leftin the residue. The residue is dissolved in dilute nitric acid and diluted to volume. The addition of nitric acid prevents any lossof mercury from t
9、he aqueous solution on standing. For analysis, an aliquot of the acidic aqueous solution is boiled with excesspermanganate to remove interfering materials. The mercuric ions are then reduced to metallic mercury with stannous chloride. Thesolution is aerated and the mercury, now in the air stream, is
10、 determined using an atomic absorption spectrophotometer.4. Significance and Use4.1 This test method was developed primarily for the determination of traces of mercury in chlorine produced by themercury-cell process.1 This test method is under the jurisdiction of ASTM Committee D16 on Aromatic Hydro
11、carbons Aromatic, Industrial, Specialty and Related Chemicals and is the directresponsibility of Subcommittee D16.16 on Industrial and Specialty Product Standards.Current edition approved March 1, 2017July 1, 2017. Published March 2017July 2017. Originally approved in 1973. Last previous edition app
12、roved in 20082017 asE506 08.E506 17. DOI: 10.1520/E0506-17.10.1520/E0506-17a.2 Analytical Methods for Atomic Absorption Spectrophotometry, Perkin-Elmer Ltd., September 1968.“Determination of Mercury in Effluents and Process Streams from a Mercury-Cell Chlorine Plant (AtomicAbsorption Flameless Metho
13、d)” CAS-AM-70.13, June 23, 1970,Analytical Laboratory, Dow Chemical of Canada, Ltd., Sarnia, Ontario, Canada.“Determination of Mercury in Liquid Chlorine,” CSAL-M72.4, Feb. 25, 1972, Analytical Laboratory, Dow Chemical of Canada, Ltd., Sarnia, Ontario, Canada.Chlorine Institute Reference No. MIR-104
14、.3 For referencedASTM standards, visit theASTM website, www.astm.org, 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.4 The last approved version of this historical standard is r
15、eferenced on www.astm.org.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends th
16、at 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 document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West
17、Conshohocken, PA 19428-2959. United States15. Apparatus5.1 Atomic Absorption Spectrophotometer, equipped with mounting to hold 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 windows.5.4 Ga
18、s Washing Bottle, 125 mL, with extra-coarse fritted bubbler. The bottle has a calibration line drawn at the 60-mL mark.5.5 Stopcock, 3-way, with plug of TFE-fluorocarbon.5.6 Gas Washing Bottle, 125-mL without frit.5.7 Drying Tube.5.8 Flow Meter, capable of measuring and maintaining a flow of 42.5 L/
19、h.5.9 Large Dewar Flasks, two, with sufficient capacity to hold a 500-mL flask and a large volume of dry ice cooling mixture.5.10 Flexible Tygon or equivalent Connection.5.11 Stainless Steel Compression Nut.5.12 Two-Hole Rubber Stopper.5.13 Fluorocarbon Tubing.NOTE 1The procedure, as described in th
20、is test method, was developed using a Perkin-Elmer Model 303 atomic absorption spectrophotometerequipped with a 10-cm absorption cell. Any other equivalent atomic absorption spectrophotometer may be used as well as one of the many commercialinstruments specifically designed for measurement of mercur
21、y by flameless atomic absorption. However, variation in instrument geometry, cell length,sensitivity, and mode of response measurement may require appropriate modifications of the operating parameters.6. Reagents6.1 Purity of ReagentsUnless otherwise indicated, it is intended that all reagents shoul
22、d conform to the specifications of theCommittee on Analytical Reagents of the American Chemical Society, where such specifications are available.5 Blanks should berun on all reagents to assure a negligible mercury content.6.2 Purity of WaterUnless otherwise indicated, references to water shall be un
23、derstood to mean Type II or Type III reagentwater conforming to Specification D1193.6.3 Aqua RegiaCarefully add 10 mL of concentrated HNO3 (sp gr 1.42) to 30 mL of concentrated HCl (sp gr 1.19) in a100-mL beaker. Let the mixture stand for 5 min before use. This mixture is unstable and should not be
24、stored. (Warning Usegoggles when preparing or using this solution.)6.4 Nitric Acid (1 + 9)Pipet 25 mL of concentrated HNO3 (sp gr 1.42) into a 250-mL volumetric flask containing about 150mL of water. Dilute to volume with water and mix well. (WarningUse goggles when preparing this solution.)6.5 Sulf
25、uric Acid (1 + 4)Add slowly with stirring 200 mL of concentrated H2SO4 (sp gr 1.84) to 800 mL of water.(WarningUse goggles when preparing this solution.)6.6 Cooling Mixture for Dewar FlasksFill two thirds of the Dewar flask with dichloromethane. Add dry ice slowly, allowingtime for the solution to c
26、ool, until there is no sublimation of dry ice on further addition. Replenish the dry ice when necessary.See the SDS sheet for dichloromethane before using this material.6.7 Hydroxylamine Hydrochloride Solution (100 g/L)See Practice E200. This reagent is dispensed with a dropping bottle.6.8 Mercury S
27、tandard Solution (50 g Hg/mL)As prepared in Practice E200.6.9 Mercury Standard Solution (10 g Hg/mL)Pipet 10 mL of the standard mercury solution containing 50 g Hg/mL intoa 50-mL volumetric flask, acidify with 5 mL of 1 + 4 H2SO4 and dilute to volume with water. Mix well. Prepare fresh daily.6.10 Me
28、rcury Standard Solution (1 g Hg/mL)Pipet 10 mL of the standard mercury solution containing 10 g Hg/mL intoa 100-mL volumetric flask, acidify with 5 mL 1 + 4 H2SO4 and dilute to volume with water. Mix well. Prepare fresh daily.6.11 Potassium Permanganate Solution (40 g/L) (4 %)Weigh 40 g of KMnO4 int
29、o a 1000-mL beaker. Add about 800 mL ofwater and stir with a mechanical stirrer until completely dissolved. Allow the solution to stand overnight and filter. Transfer to a1000-mL volumetric flask, dilute to volume, and store in a brown bottle.5 Reagent Chemicals, American Chemical Society Specificat
30、ions, American Chemical Society, Washington, 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 Conventio
31、n, Inc. (USPC), Rockville, MD.E506 17a26.12 Stannous Chloride (10 %)Dissolve 20 g of stannous chloride (SnCl22H2O) in 40 mL of warm concentrated HCl (sp gr1.19). Add 160 mL of water when all the stannous chloride has dissolved. Allow the solution to stand overnight and filter. Mixand store in a 250-
32、mL reagent bottle. Prepare fresh once a week. A piece of metallic tin in the bottle allows longer term storageif the bottle is well sealed.7. Safety Precautions7.1 Sulfuric acid will cause severe burns if allowed to come in contact with any part of the skin or eyes. All spillages must beimmediately
33、flushed from the skin or eyes with cold water. This acid must always be added slowly to water with adequate stirringsince heat is developed and spattering occurs if the acid is added too quickly.7.2 Aqua regia contains both HNO3 and HCl, which will cause severe burns if allowed to come in contact wi
34、th any part of theskin or eyes. All spillages must be immediately flushed from the skin or eyes with cold water. Vapors produced by aqua regia cancause burns if inhaled. It should be used only in a fume hood or with similar ventilation. This solution is unstable and must notbe placed in a stoppered
35、flask or bottle.7.3 Nitric acid will cause severe burns if allowed to come in contact with any part of the skin or eyes. All spillages must beimmediately flushed from the skin or eyes with cold water.7.4 Chlorine is a corrosive and toxic material. A well-ventilated fume hood should be used to house
36、all test equipment whenthis product is analyzed in the laboratory.7.5 Liquid chlorine sampling should be performed only by those persons thoroughly familiar with the handling of this materialand the operation of the sampling system. Personnel should be equipped with monogoggles, gloves (if desired),
37、 and a respirator.Sampling should be done in a well-ventilated area or in a fume hood.7.6 The analysis should be attempted only by persons who are thoroughly familiar with the handling of chlorine, and even anexperienced person should not work alone. The operator must be provided with adequate eye p
38、rotection and a respirator. Splashesof liquid chlorine destroy clothing and, if such clothing is next to the skin, will produce irritations and burns.7.7 When sampling and working with chlorine out of doors, people downwind from such operation should be warned of thepossible release of chlorine vapo
39、rs.7.8 It is recommended that means be available for disposal of excess chlorine in an environmentally safe and acceptable manner.If chlorine cannot be disposed of in a chlorine consuming process, the chlorine should be discharged into a caustic scrubbercontaining an appropriate amount of 20 % caust
40、ic solution to neutralize all the chlorine. This reaction is exothermic, and careshould be taken to avoid excess heating by choosing a sufficiently large volume of caustic solution to serve as a heat sink. Whenthe analysis and sampling regimen requires an initial purging of chlorine from a container
41、, the purged chlorine should be similarlyhandled. Purging to the atmosphere should be avoided.7.9 In the event chlorine is inhaled, first aid should be summoned immediately and oxygen administered without delay.7.10 Handle all other reagents as recommended by the supplier.8. Sampling8.1 Soak all 500
42、-mL receiver flasks carefully in 50C aqua regia and rinse with water before use.8.2 Cool two receiver flasks in the dichloromethane-dry ice mixture.8.3 Assemble the sampling apparatus as shown in Fig. 1.8.4 With a respirator ready for immediate use, locate yourself upwind of the receiver flask.8.5 K
43、eeping the receiver flask in the dry ice solution, purge the sampling system allowing 100 to 200 mL of liquid chlorine toflow through the sampling system into the flask. This purges any residual mercury deposits from the lines and sample point.8.6 Stop the flow of liquid chlorine.8.7 Cap the waste l
44、iquid chlorine flask with an open, one-hole stopper and store in a dry ice bath for disposal in anenvironmentally safe and acceptable manner.8.8 Attach the delivery system to a cooled 500-mL receiver flask and fill with liquid chlorine to the 200-mL mark. Othervolumes may be used if desired.8.9 Stop
45、 the flow of liquid chlorine.8.10 Cap the flask with an open, one-hole stopper and store in a dichloromethane-dry ice mixture.NOTE 2Except for properly designed cylinders, never completely stopper a vessel containing liquid chlorine.Avent must always be present to relievethe pressure from evaporatin
46、g liquid chlorine.E506 17a38.11 Remove the sample of liquid chlorine and waste liquid chlorine from the dichloromethane-dry ice mixture and allow themto evaporate to dryness into a chlorine absorption system or some other type of environmentally safe and acceptable manner ofchloride disposal. Discar
47、d the residue from the waste chlorine.8.12 Add 10 mL of HNO3 (1 + 9) to the flask containing the residue from the liquid chlorine sample. Swirl to assure completesolution of the residue.Add 25 mLof water and transfer to a 50-mLvolumetric flask. Dilute to volume with the water used to rinsethe flask
48、and mix well.8.13 Prepare a blank consisting of 10 mL of HNO3 (1 + 9) in a 50-mL volumetric flask, dilute to volume with water, and mixwell.9. Calibration9.1 Care must be taken to avoid contamination of the apparatus with mercury. Soak all glass apparatus (pipets, beakers, and gaswashing bottle) in
49、aqua regia prior to use and rinse thoroughly with water before use.9.2 Connect the apparatus shown in Fig. 2 to the atomic absorption spectrophotometer and adjust the air flow rate to 42.5 L/h.9.3 Adjust the operating conditions in accordance with the manufacturers recommendations for doing mercury analysis andallow the spectrophotometer to warm up for at least 15 min (see Note 1). Listed below are typical conditions for one instrument.Wavelength 253.7 nmSlit width (0.65 nm)Lamp current approximately by 10 mARecorder noise suppression 2, giving approx
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