ASTM_E_1754_-_08.pdf

Designation:E175408Standard Test Method forDetermination of Low Levels of Water in Liquid Chlorine ByInfrared Spectrophotometry1This standard is issued under the fixed designation E1754;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 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 the contentof water in liquid chlorine in the concentration range of 0.5 to15 mg/kg(ppm).1.2 The values stated in SI units are to be regarded asstandard.The values given in parentheses are for informationonly.1.3 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.See Section 7 forspecific hazards statements.1.4 Review the current Material Safety Data Sheets(MSDS)for detailed information concerning toxicity,first aidprocedures,and safety precautions.2.Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterE806 Test Method for Carbon Tetrachloride and Chloroformin Liquid Chlorine by Direct Injection(Gas Chromato-graphic Procedure)2.2 Federal Standards:349 CFR 173 Code of Federal Regulations Title 49 Trans-portation:Shippers General Requirements for Shipmentsand Packaging,including Sections:173.304 Charging of Cylinders with Liquefied CompressedGas173.314 Requirements for Compressed Gases in Tank Cars173.315 Compressed Gases in Cargo Tanks and PortableTank Containers3.Summary of Test Method3.1 A sample of liquid chlorine is introduced into a specialinfrared cell and maintained as a liquid under its own pressure.A spectrometer scans from 400 to 4400 wavenumbers of theinfrared transmission spectrum of liquid chlorine.This spec-trum is then ratioed to one obtained of the nitrogen-filledinfrared cell previously.The ratioed spectrum is converted toabsorbance,and the net absorbance of the water band at 1596wavenumbers,relative to a reference at 1663 wavenumbers,isdetermined.The amount of water corresponding to this netabsorbance is determined from a calibration curve preparedfrom the infrared absorbances of standards that contain knownconcentrations of water in liquid chlorine.4.Significance and Use4.1 Trace amounts of water may be detrimental to the use ofchlorine in some applications.The amount of water in thechlorine must be known to prevent problems during its use.5.Apparatus5.1 Infrared Spectrometer,capable of measurements in the1600 wavenumber region.An FTIR with 4 wavenumberresolution is the instrument of choice,but dispersive instru-ments may also be used to achieve similar results.5.2 Special Infrared Cell(see Fig.1),neither cell size norpathlength are critical to the analysis,but sensitivity and limitof detection are dependent on pathlength.The concentrationrange reported in the scope is achievable with a 60-mmpathlength cell constructed with:5.2.1 Hastelloy C and 316 Stainless Steel Stock,suitable formachining.5.2.2 Silver Chloride Windows,0.5 by 2.5 cm.1This test method is under the jurisdiction of ASTM Committee E15 onIndustrial and Specialty Chemicals and is the direct responsibility of SubcommitteeE15.02 on Product Standards.Current edition approved April 1,2008.Published May 2008.Originallyapproved in 1995.Last previous edition approved in 2001 as E1754 95(2001)1.DOI:10.1520/E1754-08.2For referenced ASTM standards,visit the 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.3Available from Superintendent of Documents,Government Printing Office,Washington,DC 20402.*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 States1 FIG.1(a)Pipe AdapterNOTE1Drawing not to scale.FIG.1 Infrared CellE1754 082 FIG.1(b)Air Cap DetailFIG.1(c)Body DetailFIG.1(d)Gasket DetailFIG.1(e)Insert DetailFIG.1(f)Flange Detail5.2.3 Perfluoroelastomer Sheet,0.030 in.thickness.E1754 083 5.3 Ball Valves,Monel14in.valve with pipe and14in.tubeends.5.4 Needle Valves,nickel or Monel 6.35 mm(14in.)valvewith pipe and 6.35 mm(14in.)tube ends.5.5 Sample Cylinder Assembly(see Fig.2),consisting of:5.5.1 Sample Cylinder,nickel,Monel,or tantalum;400 to1000 mL capacity,double-ended,with valves at each end,specially cleaned.Cylinders with both valves at one end andwith a dip tube on one valve have been found to be satisfactory.Another option is to construct special cylinders containing aseptum fitting on one end.NOTE1A procedure for cleaning cylinders and valves,for use withliquid chlorine,is given in Test Method E806,Appen