ASTM E410-17a Standard Test Method for Moisture and Residue in Liquid Chlorine.pdf

1、Designation: E410 17aStandard Test Method forMoisture and Residue in Liquid Chlorine1This standard is issued under the fixed designation E410; 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.1. Scope*1.1 This test method covers the determination of moistureand residue in liquid chlorine. Lower limits of detection of 10g/g based on a 150-mL sample

3、are achievable.1.2 This test method describes operations and special appa-ratus for sampling liquid chlorine from cylinders. Samplingother commercial facilities such as tank cars, barges, andstorage tanks require special techniques of manipulation infilling sample cylinders for testing. If condition

4、s and facilitiesare favorable, the analysis apparatus may be connected directlyto these larger storage and transportation units and on-the-spottests may be completed.1.3 The analytical methods are empirical and are gravimet-ric. They are applicable to the determination of the residue andmoisture con

5、tent of commercial grades of liquid chlorine(condensed gaseous product).1.4 Residue is defined as being those substances whichremain in the sample flask after sample volatilization under theconditions of the test. Moisture is defined as the volatilesubstances evolved during volatilization and purgin

6、g of thesample-residue flask and absorbed on the desiccant containedin the absorption tubes under the conditions of the test. Someof the volatile chlorinated hydrocarbons may also be evolvedfrom the sample residue flask during purge and absorbed, thuscontributing to the apparent moisture analysis va

7、lue.1.5 This test method may be used for determining themoisture content only of gaseous chlorine if suitable andappropriate modifications are made for sample measurementand calculation.1.6 Review the current Safety Data Sheet (SDS) for detailedinformation concerning toxicity, first aid procedures,

8、and safetyprecautions.1.7 The values stated in inch-pound units are to be regardedas the standard. No other units of measurement are included inthis standard.1.8 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user

9、of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. Specific hazardsstatements are given in Section 7.1.9 This international standard was developed in accor-dance with internationally recognized principles on

10、 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 Documents2.1 ASTM Standards:2D6809 Guide for Quality Control and Qual

11、ity AssuranceProcedures for Aromatic Hydrocarbons and Related Ma-terialsE180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals (Withdrawn 2009)32.2 Federal Standards:4CFR 173 Title 49 Transportation; Shippers General Re-quirements f

12、or Shipments and Packagings, including Sec-tions:173.304 Charging of Cylinders with Liquefied CompressedGas173.314 Requirements for Compressed Gases in Tank Cars73.315 Compressed Gases in Cargo Tanks and Portable TankContainers3. Summary of Test Method3.1 Acommon liquid sample of chlorine is recomme

13、nded toprovide the best results when determining both residue andmoisture simultaneously.1This test method is under the jurisdiction of ASTM Committee D16 onAromatic, Industrial, Specialty and Related Chemicals and is the direct responsi-bility of Subcommittee D16.16 on Industrial and Specialty Prod

14、uct Standards.Current edition approved July 1, 2017. Published July 2017. Originally approvedin 1970. Last previous edition approved in 2017 as E410 17. DOI: 10.1520/E0410-17a.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. Fo

15、r 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.4Available from U.S. Government Printing Office, Superintendent ofDocuments, 732 N. Capitol St., NW,

16、Washington, DC 20401-0001, http:/www.access.gpo.gov.*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 StatesThis international standard was developed in accordance with internati

17、onally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.13.2 Liquid product sample is transferred from the sa

18、mecylinder into a precalibrated, 250-mL sample-residue flask andpermitted to volatilize completely under prevailing environ-mental conditions. The volatilized product (chlorine gas) ispassed through anhydrous magnesium perchlorate desiccantfor absorption of moisture. It is recommended that the exhau

19、stgas be discharged into a caustic scrubber containing anappropriate amount of 20 % caustic solution to neutralize allthe chlorine. This reaction is exothermic and care should betaken to avoid excess heating by choosing a sufficiently largevolume of caustic solution to serve as a heat sink.3.3 After

20、 complete volatilization of the sample from theflask, residual chlorine and moisture are expelled from anyresidue by purging with dry air through the absorption systemwhere moisture is recovered and determined gravimetrically.3.4 Residue remaining in the flask is determined by carefulanalytical weig

21、hing, the weight gain calculated as residuecontent of the sample. Moisture is computed from the sum ofthe gain in weight of the two absorption tubes containing thedesiccant. Any gain in weight of the second absorber tubeshould be nominal with respect to that of the first tube in theseries.3.5 The mo

22、isture content of a chlorine gas stream isdetermined gravimetrically as above, by passing a meteredsample through the moisture absorption system only.4. Significance and Use4.1 This test method provides for the determination ofmoisture and residue in liquid chlorine. The concentrationlevels of these

23、 impurities are important factors in manycommercial uses of liquid chlorine.5. Apparatus5.1 The arrangement and assembly of apparatus for collec-tion and measurement of the analytical sample and volatiliza-tion is shown in Fig. 1.5.2 Sample-Residue Flask (H), Erlenmeyer-type, 250-mLcapacity, equippe

24、d with a 35/20 JSground-ball joint.5Apermanent calibration mark shall be inscribed on the flask atthe 150-mL volume level for sample measurement.5.3 Adapter (G), equipped with a 35/20 JSground-socketjoint attached and sealed as shown in Fig. 1. In addition,appropriate 12/5 JSjoints shall be sealed t

25、o the adapter. A balljoint, sealed and closed off at the end, shall be provided forattachment to the inlet tube after collection of liquid sample inthe sample-residue flask. This shall be held in position with anappropriate clamp during volatilization, then removed andreplaced with appropriate conne

26、ctions from the metered dry-airsupply at the time of aeration and purge of the sample-residueflask.5.4 A second assembly consisting of a sample-residue flaskand adapter shall be used to facilitate collection and disposal ofsample purge from the cylinder sample line prior to withdrawalof the analytic

27、al sample for test.5.5 RegulatorAn appropriate needle valve type shall beattached to the cylinder outlet to control and regulate the flowof liquid chlorine from the sample cylinder. Connection (F )between the outlet from this valve and the adapter (G) shall beby a short length of appropriately sized

28、 TFE-fluorocarbontubing equipped with a 12/5 JSground-ball joint.5.6 Rubber Tubing, length and size sufficient to exhaustchlorine vapors to the caustic soda absorber or hood systemduring sample collection and volatilization. A ground-glass12/5 JSsocket joint shall be fitted to one end of the rubbert

29、ubing to make appropriate connection to the adapter duringsample collection and transferred to the exhaust connectionfrom the second moisture absorption U-tube for gas dischargeto disposal during volatilization of the sample.5The recommended sample-residue flask, equipped with a 35/20 JSground-ballj

30、oint and the adapter equipped with a 35/20 JSground-socket joint and associated12/5 JSground joints shown in Fig. 1, can be purchased from a reputable glass vendoror can be fabricated by a glass blower.FIG. 1 Apparatus for Collection and Volatilization of Liquid ChlorineE410 17a25.7 Watch Glass, sma

31、ll size, used to close the sample-residue flask during analytical weighing before and aftersample volatilization to prevent loss of residue or absorption ofmoisture from the atmosphere.5.8 Moisture Absorption Tubes (I) (Fig. 1)SchwartzU-tube design, 100 mm length top of arms to center, modifiedand e

32、quipped with ground-glass 12/5 JSsocket and ball jointssealed to the inlets and outlets. Two such absorber tubes shallbe connected in a series arrangement.5.9 Flow Meter, capable of metering air at 4.5 L/min andequipped with appropriate ground glass connection.5.10 Caustic Scrubber, for chlorine dis

33、posal.6. Reagents6.1 Purity of ReagentsUnless otherwise indicated, it isintended that all reagents should conform to the specificationsof the Committee on Analytical Reagents of the AmericanChemical Society, where such specifications are available.66.2 Pulverized Dry Ice and a Small Amount ofTrichlo

34、roethylene, contained in a glass crystallizing dish (190by 100 mm), for use in cooling the sample-residue flask duringsample purge, collection and measurement.6.3 Granular Form of Anhydrous Magnesium PerchlorateReagent Grade.6.4 Caustic Solution20 % by mass, sodium hydroxide inwater. Dissolve 200 g

35、of sodium hydroxide (NaOH) in waterand dilute to 1 L. Store in a tight polyethylene container.7. Hazards7.1 Chlorine is a corrosive and toxic material. A wellventilated fume hood should be used to house the test equip-ment when this product is analyzed in the laboratory.7.2 The analysis should be at

36、tempted only by persons whoare thoroughly familiar with the handling of chlorine, and evenan experienced person should not work alone. The operatormust be provided with adequate eye protection and respirator.Splashes of liquid chlorine destroy clothing and if suchclothing is next to the skin, will p

37、roduce irritations and burns.7.3 When sampling and working with chlorine out of doors,people downwind from such operation should be warned of thepossible release of chlorine vapors.7.4 It is recommended that means should be available fordisposal of excess chlorine in an environmentally safe andaccep

38、table manner. If chlorine cannot be disposed of in achlorine consuming process, a chlorine absorption systemshould be provided. When the analysis and sampling regimenrequires an initial purging of chlorine from a container, thepurged chlorine should be similarly handled. Purging to theatmosphere sho

39、uld be avoided.7.5 In the event chlorine is inhaled, first aid should besummoned immediately and oxygen administered withoutdelay.8. Sampling Tank Cars, Barges, Large Cylinders, andStorage Facilities8.1 Sampling from tank cars, barges, storage tanks, andlarge cylinders present unique problems. Each

40、facility,however, must be capable of delivering liquid-sample (not gas)for test.8.2 Since location of these larger facilities may not be at theimmediate site of analysis, sample collection in a suitablesecondary container is recommended to facilitate its safetransport to the laboratory for tests.8.3

41、 It is recommended that samples be collected from thesefacilities in small-size sample cylinders with cylinders andvalves fabricated of tantalum or nickel and capable of beingnegotiated in the laboratory fume hood. Technical literatureavailable from producers and distributors of liquid chlorineshoul

42、d be consulted for instructions in filling small sizecylinders properly from bulk storage.8.4 Do not allow the sample cylinder to become liquid full.A good rule is that the weight of the chlorine in the cylindershould not be more that 125 % of the weight of the water thatthe cylinder could contain i

43、n accordance with 49 CFR 173.9. Preparation of Apparatus9.1 Thoroughly clean the absorption tubes, sample-residueflasks, and adapters free of grease and lubricants, particularly atthe ground surfaces of the joints.After thorough cleansing, drythe apparatus thermally in an oven at 105C. When cooled,c

44、harge the absorption tubes with desiccant.9.2 Charge each tube within about 20 mm of the top in eachleg with a granular form of anhydrous magnesium perchlorate,minimizing the use of dusty product. Place loosely packedglass wool on the surfaces of the desiccant in both legs of theabsorber tube to avo

45、id carry-over of chemical dust duringsample volatilization and air purge operations. Place theunlubricated stoppers firmly in the ground necks of the tubesand adjust to the “off” position preparatory to conditioningwith chlorine gas, air purge, and weighing.9.3 Connect the moisture absorption tubes

46、in a series bymeans of appropriately sized spring clamps in an uprightoperating position supported on a ring stand.Attach the groundjoint and rubber tubing to the outlet of the second absorber forexhausting chlorine gas to the caustic scrubber.9.4 Attach a source of chlorine gas to the inlet of the

47、firstabsorber tube, open the ground stoppers on both tubes topermit the free flow of gas through them and purge for1hata rate of 2 to 3 bubbles of chlorine gas/s when the exhaust endof the rubber tube is held momentarily beneath the surface ofwater.9.5 After purging with chlorine (see Section 10), a

48、ttach thedry air supply to the first absorber in the series and aerate forexactly 5 min at a rate of 4.5 L/min.6Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society

49、, 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.E410 17a39.6 After aeration, carefully close the ground stoppers,dismantle the tubes from the assembly, and condition in theenvironment of the balance for 10 min prior to analyticalweighing of each tube. After weighing, the tubes may bereassembled for the next analysis.9.7 Conditioning of the absorber tubes with chlorine isrequired after an initial fresh charge of de