1、Designation: E410 17E410 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 numb
2、er in parentheses 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 moisture and residue in liquid chlorine. Lower limits of detection of 10 g/gbased on a 150-mL
3、 sample are achievable.1.2 This test method describes operations and special apparatus for sampling liquid chlorine from cylinders. Sampling othercommercial facilities such as tank cars, barges, and storage tanks require special techniques of manipulation in filling samplecylinders for testing. If c
4、onditions and facilities are favorable, the analysis apparatus may be connected directly to these largerstorage and transportation units and on-the-spot tests may be completed.1.3 The analytical methods are empirical and are gravimetric. They are applicable to the determination of the residue andmoi
5、sture content of commercial grades of liquid chlorine (condensed gaseous product).1.4 Residue is defined as being those substances which remain in the sample flask after sample volatilization under theconditions of the test. Moisture is defined as the volatile substances evolved during volatilizatio
6、n and purging of the sample-residueflask and absorbed on the desiccant contained in the absorption tubes under the conditions of the test. Some of the volatilechlorinated hydrocarbons may also be evolved from the sample residue flask during purge and absorbed, thus contributing to theapparent moistu
7、re analysis value.1.5 This test method may be used for determining the moisture content only of gaseous chlorine if suitable and appropriatemodifications are made for sample measurement and calculation.1.6 Review the current Safety Data Sheet (SDS) for detailed information concerning toxicity, first
8、 aid procedures, and safetyprecautions.1.7 The values stated in inch-pound units are to be regarded as the standard. No other units of measurement are included in thisstandard.1.8 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the respons
9、ibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. Specific hazards statements are given in Section 7.1.9 This international standard was developed in accordance with internationally recogniz
10、ed 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:2D6809 Guide for Quality Co
11、ntrol and Quality Assurance Procedures for Aromatic Hydrocarbons and Related MaterialsE180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial and Specialty Chemicals(Withdrawn 2009)32.2 Federal Standards:4CFR 173 Title 49 Transportation; Shippers General Re
12、quirements for Shipments and Packagings, including Sections:173.304 Charging of Cylinders with Liquefied Compressed Gas1 This test method is under the jurisdiction of ASTM Committee D16 on Aromatic Hydrocarbons Aromatic, Industrial, Specialty and Related Chemicals and is the directresponsibility of
13、Subcommittee D16.16 on Industrial and Specialty Product Standards.Current edition approved March 1, 2017July 1, 2017. Published March 2017July 2017. Originally approved in 1970. Last previous edition approved in 20082017 asE410 08.E410 17. DOI: 10.1520/E0410-17.10.1520/E0410-17a.2 For referencedASTM
14、 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.3 The last approved version of this historical standard is referenced on www.astm
15、.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.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 m
16、ade 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 document.*A
17、 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 States1173.314 Requirements for Compressed Gases in Tank Cars73.315 Compressed Gases in Cargo Tanks and Portable Tank Containers3.
18、 Summary of Test Method3.1 A common liquid sample of chlorine is recommended to provide the best results when determining both residue andmoisture simultaneously.3.2 Liquid product sample is transferred from the same cylinder into a precalibrated, 250-mLsample-residue flask and permittedto volatiliz
19、e completely under prevailing environmental conditions. The volatilized product (chlorine gas) is passed throughanhydrous magnesium perchlorate desiccant for absorption of moisture. It is recommended that the exhaust gas be discharged intoa caustic scrubber containing an appropriate amount of 20 % c
20、austic solution to neutralize all the chlorine. This reaction isexothermic and care should be taken to avoid excess heating by choosing a sufficiently large volume of caustic solution to serveas a heat sink.3.3 After complete volatilization of the sample from the flask, residual chlorine and moistur
21、e are expelled from any residue bypurging with dry air through the absorption system where moisture is recovered and determined gravimetrically.3.4 Residue remaining in the flask is determined by careful analytical weighing, the weight gain calculated as residue contentof the sample. Moisture is com
22、puted from the sum of the gain in weight of the two absorption tubes containing the desiccant.Anygain in weight of the second absorber tube should be nominal with respect to that of the first tube in the series.3.5 The moisture content of a chlorine gas stream is determined gravimetrically as above,
23、 by passing a metered sample throughthe moisture absorption system only.4. Significance and Use4.1 This test method provides for the determination of moisture and residue in liquid chlorine. The concentration levels of theseimpurities are important factors in many commercial uses of liquid chlorine.
24、5. Apparatus5.1 The arrangement and assembly of apparatus for collection and measurement of the analytical sample and volatilization isshown in Fig. 1.5.2 Sample-Residue Flask (H), Erlenmeyer-type, 250-mL capacity, equipped with a 35/20 JS ground-ball joint.5 A permanentcalibration mark shall be ins
25、cribed on the flask at the 150-mL volume level for sample measurement.5.3 Adapter (G), equipped with a 35/20 JS ground-socket joint attached and sealed as shown in Fig. 1. In addition, appropriate12/5 JS joints shall be sealed to the adapter. A ball joint, sealed and closed off at the end, shall be
26、provided for attachment to theinlet tube after collection of liquid sample in the sample-residue flask. This shall be held in position with an appropriate clampduring volatilization, then removed and replaced with appropriate connections from the metered dry-air supply at the time ofaeration and pur
27、ge of the sample-residue flask.5 The recommended sample-residue flask, equipped with a 35/20 JS ground-ball joint and the adapter equipped with a 35/20 JS ground-socket joint and associated 12/5 JSground joints shown in Fig. 1, can be purchased from a reputable glass vendor or can be fabricated by a
28、 glass blower.FIG. 1 Apparatus for Collection and Volatilization of Liquid ChlorineE410 17a25.4 A second assembly consisting of a sample-residue flask and adapter shall be used to facilitate collection and disposal ofsample purge from the cylinder sample line prior to withdrawal of the analytical sa
29、mple for test.5.5 RegulatorAn appropriate needle valve type shall be attached to the cylinder outlet to control and regulate the flow of liquidchlorine from the sample cylinder. Connection (F ) between the outlet from this valve and the adapter (G) shall be by a short lengthof appropriately sized TF
30、E-fluorocarbon tubing equipped with a 12/5 JS ground-ball joint.5.6 Rubber Tubing, length and size sufficient to exhaust chlorine vapors to the caustic soda absorber or hood system duringsample collection and volatilization. A ground-glass 12/5 JS socket joint shall be fitted to one end of the rubbe
31、r tubing to makeappropriate connection to the adapter during sample collection and transferred to the exhaust connection from the second moistureabsorption U-tube for gas discharge to disposal during volatilization of the sample.5.7 Watch Glass, small size, used to close the sample-residue flask dur
32、ing analytical weighing before and after samplevolatilization to prevent loss of residue or absorption of moisture from the atmosphere.5.8 Moisture Absorption Tubes (I) (Fig. 1)Schwartz U-tube design, 100 mm length top of arms to center, modified andequipped with ground-glass 12/5 JS socket and ball
33、 joints sealed to the inlets and outlets. Two such absorber tubes shall beconnected in a series arrangement.5.9 Flow Meter, capable of metering air at 4.5 L/min and equipped with appropriate ground glass connection.5.10 Caustic Scrubber, for chlorine disposal.6. Reagents6.1 Purity of ReagentsUnless
34、otherwise indicated, it is intended that all reagents should conform to the specifications of theCommittee on Analytical Reagents of the American Chemical Society, where such specifications are available.66.2 Pulverized Dry Ice and a Small Amount of Trichloroethylene, contained in a glass crystalliz
35、ing dish (190 by 100 mm), foruse in cooling the sample-residue flask during sample purge, collection and measurement.6.3 Granular Form of Anhydrous Magnesium PerchlorateReagent Grade.6.4 Caustic Solution20 % by mass, sodium hydroxide in water. Dissolve 200 g of sodium hydroxide (NaOH) in water anddi
36、lute to 1 L. Store in a tight polyethylene container.7. Hazards7.1 Chlorine is a corrosive and toxic material. A well ventilated fume hood should be used to house the test equipment whenthis product is analyzed in the laboratory.7.2 The analysis should be attempted only by persons who are thoroughly
37、 familiar with the handling of chlorine, and even anexperienced person should not work alone. The operator must be provided with adequate eye protection and respirator. Splashesof liquid chlorine destroy clothing and if such clothing is next to the skin, will produce irritations and burns.7.3 When s
38、ampling 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 for disposal of excess chlorine in an environmentally safe and acceptablemanner. If chlorine cannot be d
39、isposed of in a chlorine consuming process, a chlorine absorption system should be provided. Whenthe analysis and sampling regimen requires an initial purging of chlorine from a container, the purged chlorine should be similarlyhandled. Purging to the atmosphere should be avoided.7.5 In the event ch
40、lorine is inhaled, first aid should be summoned immediately and oxygen administered without delay.8. Sampling Tank Cars, Barges, Large Cylinders, and Storage Facilities8.1 Sampling from tank cars, barges, storage tanks, and large cylinders present unique problems. Each facility, however, mustbe capa
41、ble of delivering liquid-sample (not gas) for test.8.2 Since location of these larger facilities may not be at the immediate site of analysis, sample collection in a suitable secondarycontainer is recommended to facilitate its safe transport to the laboratory for tests.8.3 It is recommended that sam
42、ples be collected from these facilities in small-size sample cylinders with cylinders and valvesfabricated of tantalum or nickel and capable of being negotiated in the laboratory fume hood. Technical literature available fromproducers and distributors of liquid chlorine should be consulted for instr
43、uctions in filling small size cylinders properly from bulkstorage.6 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see Analar Standards for Laboratory Chemi
44、cals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.E410 17a38.4 Do not allow the sample cylinder to become liquid full.Agood rule is that the weight of the chlorine in the cylinder shouldnot be more
45、 that 125 % of the weight of the water that the cylinder could contain in accordance with 49 CFR 173.9. Preparation of Apparatus9.1 Thoroughly clean the absorption tubes, sample-residue flasks, and adapters free of grease and lubricants, particularly at theground surfaces of the joints. After thorou
46、gh cleansing, dry the apparatus thermally in an oven at 105C. When cooled, charge theabsorption tubes with desiccant.9.2 Charge each tube within about 20 mm of the top in each leg with a granular form of anhydrous magnesium perchlorate,minimizing the use of dusty product. Place loosely packed glass
47、wool on the surfaces of the desiccant in both legs of the absorbertube to avoid carry-over of chemical dust during sample volatilization and air purge operations. Place the unlubricated stoppersfirmly in the ground necks of the tubes and adjust to the “off” position preparatory to conditioning with
48、chlorine gas, air purge,and weighing.9.3 Connect the moisture absorption tubes in a series by means of appropriately sized spring clamps in an upright operatingposition supported on a ring stand. Attach the ground joint and rubber tubing to the outlet of the second absorber for exhaustingchlorine ga
49、s to the caustic scrubber.9.4 Attach a source of chlorine gas to the inlet of the first absorber tube, open the ground stoppers on both tubes to permit thefree flow of gas through them and purge for 1 h at a rate of 2 to 3 bubbles of chlorine gas/s when the exhaust end of the rubbertube is held momentarily beneath the surface of water.9.5 After purging with chlorine (see Section 10), attach the dry air supply to the first absorber in the series and aerate for exactly5 min at a rate of 4.5 L/min.9.6 After aeration, carefully close the ground stoppers, dismantle the tub
