ASTM D5932-2008(2013) 9375 Standard Test Method for Determination of 2 4-Toluene Diisocyanate (2 4-TDI) and 2 6-Toluene Diisocyanate (2 6-TDI) in Air (with 9-(N-Methylaminomethyl) .pdf
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1、Designation: D5932 08 (Reapproved 2013)Standard Test Method forDetermination of 2,4-Toluene Diisocyanate (2,4-TDI) and 2,6-Toluene Diisocyanate (2,6-TDI) in Air (with 9-(N-Methylaminomethyl) Anthracene Method) (MAMA) in theWorkplace1This standard is issued under the fixed designation D5932; the numb
2、er 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. Scope1
3、.1 This test method covers the determination of gaseous2,4-toluene diisocyanate (2,4-TDI) and 2,6-toluene diisocya-nate (2,6-TDI) in air samples collected from workplace andambient atmospheres.1.2 Differential air sampling is performed with a segregat-ing device.2,3The gaseous fraction is collected
4、on a glass fiberfilter (GFF) impregnated with 9-(N-methylaminomethyl) an-thracene (MAMA).1.3 The analysis of the gaseous fraction is performed with ahigh performance liquid chromatograph (HPLC) equippedwith ultraviolet (UV) and fluorescence detectors.1.4 The analysis of the aerosol fraction is perfo
5、rmed sepa-rately as described in Ref (1).41.5 The range of application of this test method, utilizingUV and a fluorescence detector, is validated for 0.029 to 1.16g of monomer 2,4- and 2,6-TDI/2.0 mL of desorptionsolution, which corresponds to concentrations of 0.002 to0.077 mg/m3of TDI based on a 1
6、5-L air sample. Thiscorresponds to 0.28 to 11 ppb(V) and brackets the establishedTLV value of 5 ppb(v).1.6 A field blank sampling system is used to check thepossibility of contamination during the entire sampling andanalysis.1.7 The values stated in SI units are to be regarded as thestandard.1.8 Thi
7、s 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.2. Referenced Document
8、s2.1 ASTM Standards:5D1193 Specification for Reagent WaterD1356 Terminology Relating to Sampling and Analysis ofAtmospheresD1357 Practice for Planning the Sampling of the AmbientAtmosphere2.2 Other Documents:Sampling Guide for Air Contaminants in the Workplace63. Terminology3.1 For definitions of te
9、rms used in this test method, refer toTerminology D1356.4. Summary of Test Method4.1 A known volume of air is drawn through a segregatingsampling device.4.2 Gaseous and aerosol fraction are sampled simultane-ously with a two filter loaded cassette.2The aerosol is collected1This test method is under
10、the jurisdiction of ASTM Committee D22 on AirQuality and is the direct responsibility of Subcommittee D22.04 on Workplace AirQuality.Current edition approved April 1, 2013. Published April 2013. Originallyapproved in 1996. Last previous edition approved in 2008 as D5932 - 08. DOI:10.1520/D5932-08R13
11、.2The sampling device for isocyanates is covered by a patent held by JacquesLesage et al, IRSST, 505 De Maisonneuve Blvd West, Montreal, Quebec, Canada.Interested parties are invited to submit information regarding the identification ofacceptable alternatives to this patented item to the Committee o
12、n Standards, ASTMInternational Headquarters, 100 Barr Harbor Dr., PO Box C700, WestConshohocken, PA 19428. Your comments will receive careful consideration at ameeting of the committee responsible, which you may attend. This sampling deviceis currently commercially available under license from SKC O
13、mega SpecialtyDivision, Eighty-Four, PA.3The American Society for Testing and Materials takes no position respectingthe validity of any patent rights asserted in connection with any item mentioned inthis standard. Users of this standard are expressly advised that determination of thevalidity of any
14、such patent rights, and the risk of infringement of such rights, areentirely their own responsibility.4The boldface numbers in parentheses refer to the list of references at the end ofthis test method.5For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Servi
15、ce at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.6Available from Institut de Recherche en Sant et en Scurit du Travail duQubec, Laboratory Services and Expertise Department, Montreal, IRSST, 2005.Copyright AST
16、M International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1on the first filter made of polytetrafluoroethylene (PTFE), thegaseous counterpart being adsorbed on the second filter madeof glass fiber (GFF) impregnated with MAMA.4.3 The analysis of the monomer a
17、nd oligomer in theaerosol fraction is performed separately in accordance with theprocedure described in Ref (1,2).4.4 The diisocyanate present as a gas reacts with thesecondary amine function of the MAMA impregnated on theGFF to form a urea derivative (3,4), as shown below.4.5 Desorption is done wit
18、h dimethylformamide 67 % con-taining 33 % mobile phase (70 % acetonitrile, 30 % buffer).4.6 The resulting solution is analyzed by HPLC with twodetectors in series: UV (254 nm) and fluorescence (254-nmexcitation and 412-nm emission) (5).4.7 2,4- and 2,6-TDI urea derivatives are separated usingreverse
19、d phase HPLC column.4.8 A complete calibration curve, covering the range ofapplication of the test method, was obtained to determine thelinearity of the method (see 1.5).4.9 Concentration of urea derivative contained in thesamples is calculated by using an external standard of theappropriate urea de
20、rivative.5. Significance and Use5.1 TDI is used mostly in the preparation of rigid andsemi-rigid foams and adhesives.5.2 Isocyanate use has been growing for the last 20 yearsand the industrial need is still growing.5.3 Diisocyanates and polyisocyanates are irritants to skin,eyes, and mucous membrane
21、s. They are recognized to causerespiratory allergic sensitization, asthmatic bronchitis, andacute respiratory intoxication (6-9).5.4 The American Conference of Governmental IndustrialHygienists (ACGIH) has adopted a Threshold Limit Valu-eTime Weighted Average (TLVTWA) of 0.036 mg/m3witha Short-Term
22、Exposure Limit (STEL) of 0.14 mg/m3for2,4-TDI (10). The Occupational Safety and Health Adminis-tration of the U.S. Department of Labor (OSHA) has apermissible exposure limit of 0.02 ppm(V) or 0.14 mg/m3ofTDI as a ceiling limit and 0.005 ppm (V) or 0.036 mg/m3as atime-weighted average (11).5.5 Monito
23、ring of respiratory and other problems related todiisocyanates and polyisocyanates is aided through the utiliza-tion of this test method, due to its sensitivity and low volumerequirements (15 L). Its short sampling times are compatiblewith the duration of many industrial processes and its lowquantif
24、ication limit also suits the concentrations often found inthe working area.5.6 The segregating sampling device pertaining to thisproposed test method physically separates gas and aerosolallowing isocyanate concentrations in both physical states to beobtained, thus helping in the selection of ventila
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