ASTM D5578-2004(2015) Standard Test Method for Determination of Ethylene Oxide in Workplace Atmospheres (HBr Derivatization Method)《用于测定工作场所环境中环氧乙烷的标准试验方法 (HBr衍生法)》.pdf
《ASTM D5578-2004(2015) Standard Test Method for Determination of Ethylene Oxide in Workplace Atmospheres (HBr Derivatization Method)《用于测定工作场所环境中环氧乙烷的标准试验方法 (HBr衍生法)》.pdf》由会员分享,可在线阅读,更多相关《ASTM D5578-2004(2015) Standard Test Method for Determination of Ethylene Oxide in Workplace Atmospheres (HBr Derivatization Method)《用于测定工作场所环境中环氧乙烷的标准试验方法 (HBr衍生法)》.pdf(4页珍藏版)》请在麦多课文档分享上搜索。
1、Designation: D5578 04 (Reapproved 2015)Standard Test Method forDetermination of Ethylene Oxide in Workplace Atmospheres(HBr Derivatization Method)1This standard is issued under the fixed designation D5578; the number immediately following the designation indicates the year oforiginal adoption or, in
2、 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. Scope1.1 This test method covers a method of collecting andanalyzing samples to determine th
3、e amount of ethylene oxide(ETO) present in workplace atmospheres.1.2 This test method can be used to provide a time-weightedaverage (TWA) over the concentration range from 0.2 to 4 ppm(v).1.3 This test method can be used to determine 15-minexcursions (STEL) ranging from 1 to 25 ppm (v).1.4 The value
4、s stated in SI units are to be regarded as thestandard.1.5 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
5、 of regulatory limitations prior to use. See Section 9 forspecific safety hazards.2. Referenced Documents2.1 ASTM Standards:2D1356 Terminology Relating to Sampling and Analysis ofAtmospheresD3686 Practice for Sampling Atmospheres to Collect Or-ganic Compound Vapors (Activated Charcoal Tube Ad-sorpti
6、on Method)D3687 Practice for Analysis of Organic Compound VaporsCollected by the Activated Charcoal Tube AdsorptionMethodE355 Practice for Gas Chromatography Terms and Relation-ships2.2 Other Standard:3Occupational Safety and Health Administration, U.S. De-partment of Labor, Title 29, Code of Federa
7、l Regulations,Part 1910, Subpart Z, Section 1910.10473. Terminology3.1 DefinitionsFor definitions of terms used in this testmethod, refer to Terminology D1356, and Practice E355.4. Summary of Test Method4.1 A known volume of air is pumped through a glass tubepacked with carbon molecular sieve, surfa
8、ce area 400 m2/gimpregnated with hydrogen bromide (HBr) where ETO isadsorbed and converted to 2-bromoethanol.4.2 The tube contains two reactive sections for samplecollection. The backup section collects vapors that passthrough the front section and is used to determine if thecollection capacity of t
9、he front section has been exceeded.4.3 The resultant derivative, 2-bromoethanol, is desorbedwith a mixture of acetonitrile/toluene and analyzed using a gaschromatograph equipped with an electron capture detector.4.4 Desorption efficiency is determined by spiking tubeswith known amounts of 2-bromoeth
10、anol and analyzing with thesame procedure used for air samples.4.5 Quantitation is achieved by comparing peak areas fromsample solutions with areas from standard solutions.5. Significance and Use5.1 Ethylene oxide is a major industrial chemical withproduction volume ranked in the top 25 chemicals pr
11、oduced inthe United States. It is used in the manufacture of a greatvariety of products as well as being a sterilizing agent andfumigant.5.2 This test method provides a means of determiningexposure levels of ETO in the working environment at thepresently recommended exposure guidelines.1This test me
12、thod is under the jurisdiction of ASTM Committee D22 on AirQuality and is the direct responsibility of Subcommittee D22.04 on Workplace AirQuality.Current edition approved Oct. 1, 2015. Published October 2015. Originallyapproved in 1994. Last previous edition approved in 2010 as D5578 04 (2010).DOI:
13、 10.1520/D5578-04R15.2For 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 U.S. Government Printing
14、 Office, Superintendent ofDocuments, 732 N. Capitol St., NW, Washington, DC 20401-0001, http:/www.access.gpo.gov.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15.2.1 OSHA Permissible Exposure Limit (PEL) 1 ppm,15-min excursion limit
15、5 ppm (CFR, Part 1910, Subpart Z,Section 1910.1047).35.2.2 ACGIH Threshold Limit Value (TLV) 1 ppm (1.8mg/m3), suspected human carcinogen.46. Interferences6.1 Derivatives and other compounds that have identical ornearly the same GC column retention time as 2-bromoethanolduring the gas chromatographi
16、c analysis will interfere.6.2 Interferences can sometimes be resolved by altering gaschromatographic operating conditions. The identity of sus-pected 2-bromoethanol, or the presence of 2-bromoethanolmasked by a chromatographic interference, or both, can beverified by gas chromatography/mass spectrom
17、etry.7. Apparatus7.1 Carbon Molecular Sieve, surface area 400 m2/g, HBrsampling tube.7.1.1 Preparation of Collection MediumAdd 20 mL ofHBr (24 %) to 70 g of carbon molecular sieve, surface area 400m2/g, in a glass jar. Cap the jar and mix the contents thoroughlyfor 5 min by rotating.Allow to equilib
18、rate and dry overnight orfor 12 h.7.1.2 Tube PreparationInsert a plug of silanized glasswool into a 10-cm by 6-mm outside diameter (4-mm insidediameter) glass tube. Pack the front section of the tube with400 mg of the reactive adsorbent (7.1.1), using gentle tappingor vibration to promote uniform pa
19、cking. Insert another plug ofsilanized wool and pack 200 mg of the adsorbent in the backupsection. Hold the backup section in place by firmly inserting anadditional glass wool plug. The tubes may be flame-sealed orsealed with polyethylene caps. Provide a numerical identifica-tion for each lot of tub
20、es.7.1.3 Tube Holder, capable of preventing breakage andprotecting worker during sampling.7.1.4 High-Density Polyethylene or Polypropylene Caps,tight-fitting, for resealing used tubes.7.2 Pump and Tubing:7.2.1 Sampling Pumps, having stable low flow rates(610 % of set flow rate) within the range from
21、 20 to 100mL/min for up to 8 h.7.2.2 Rubber or Plastic Tubing, 6-mm inside diameter, forconnecting collection tube to pump. All tubing must bedownstream (between tube and pump) of collection tube toprevent contamination or loss of sample.7.3 Vials, glass with PTFE-lined caps, 10 mL, for desorbingsam
22、ples and storing standards.7.4 Pipettes, 5 mL, for adding desorbing solution tosamples.7.5 Syringes, 10, 50, and 100-L syringes, for preparingstandards.7.6 Gas-Tight Syringe, 2 L, with low dead-volume needle.7.7 Gas Chromatograph (GC):7.7.1 Gas Chromatograph, with an electron capture detectorand a s
23、uitable readout device.7.7.2 Chromatographic Column, packed or capillary col-umns in accordance with 7.7.2.1 and 7.7.2.2 have been foundsuitable for this analysis.7.7.2.1 Packed, 3.7 m by 3 mm (12 ft by18 in.), stainlesssteel, packed with 10 % diethylene glycol succinate on diato-maceous earth, flux
24、-calcined, silanized, 80/100 mesh.7.7.2.2 Capillary, 30-m by 0.53-mm inside diameter fusedsilica capillary column with polyethylene glycol phase.8. Reagents8.1 Purity of ReagentsUnless otherwise indicated, it isintended that all reagents conform to the specifications of theCommittee on Analytical Re
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