ASTM D5578-04(2010)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D5578 − 04(Reapproved 2010)
Standard Test Method for
Determination of Ethylene Oxide in Workplace Atmospheres
(HBr Derivatization Method)
This standard is issued under the fixed designation D5578; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2.2 Other Standard:
Occupational Safety and Health Administration, U.S. De-
1.1 This test method covers a method of collecting and
partmentofLabor,Title29, Code of Federal Regulations,
analyzing samples to determine the amount of ethylene oxide
Part 1910, Subpart Z, Section 1910.1047.
(ETO) present in workplace atmospheres.
1.2 Thistestmethodcanbeusedtoprovideatime-weighted
3. Terminology
average(TWA)overtheconcentrationrangefrom0.2to4ppm
3.1 For definitions of terms used in this test method, refer to
(v).
Terminology D1356, and Practice E355.
1.3 This test method can be used to determine 15-min
excursions (STEL) ranging from 1 to 25 ppm (v).
4. Summary of Test Method
1.4 The values stated in SI units are to be regarded as the 4.1 A known volume of air is pumped through a glass tube
standard.
packed with carbon molecular sieve, surface area 400 m /g
impregnated with hydrogen bromide (HBr) where ETO is
1.5 This standard does not purport to address all of the
adsorbed and converted to 2-bromoethanol.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 4.2 The tube contains two reactive sections for sample
priate safety and health practices and determine the applica- collection. The backup section collects vapors that pass
bility of regulatory limitations prior to use. See Section 9 for
through the front section and is used to determine if the
specific safety hazards. collection capacity of the front section has been exceeded.
4.3 The resultant derivative, 2-bromoethanol, is desorbed
2. Referenced Documents
with a mixture of acetonitrile/toluene and analyzed using a gas
chromatograph equipped with an electron capture detector.
2.1 ASTM Standards:
D1356 Terminology Relating to Sampling and Analysis of
4.4 Desorption efficiency is determined by spiking tubes
Atmospheres
withknownamountsof2-bromoethanolandanalyzingwiththe
D3686 Practice for Sampling Atmospheres to Collect Or-
same procedure used for air samples.
ganic Compound Vapors (Activated Charcoal Tube Ad-
4.5 Quantitation is achieved by comparing peak areas from
sorption Method)
sample solutions with areas from standard solutions.
D3687 Practice for Analysis of Organic Compound Vapors
Collected by the Activated Charcoal Tube Adsorption
5. Significance and Use
Method
E355 Practice for Gas Chromatography Terms and Relation- 5.1 Ethylene oxide is a major industrial chemical with
ships production volume ranked in the top 25 chemicals produced in
the United States. It is used in the manufacture of a great
variety of products as well as being a sterilizing agent and
fumigant.
This test method is under the jurisdiction of ASTM Committee D22 on Air
Qualityand is the direct responsibility of Subcommittee D22.04 on Workplace Air
5.2 This test method provides a means of determining
Quality.
exposure levels of ETO in the working environment at the
Current edition approved April 1, 2010. Published June 2010. Originally
presently recommended exposure guidelines.
approved in 1994. Last previous edition approved in 2004 as D5578 - 04. DOI:
10.1520/D5578-04R10.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on Available from Superintendent of Documents, U.S. Government Printing
the ASTM website. Office, Washington, DC 20402.
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D5578 − 04 (2010)
5.2.1 OSHA Permissible Exposure Limit (PEL) 1 ppm, 7.6 Gas-Tight Syringe, 2 µL, with low dead-volume needle.
15-min excursion limit 5 ppm (CFR, Part 1910, Subpart Z,
7.7 Gas Chromatograph (GC):
Section 1910.1047).
7.7.1 Gas Chromatograph,withanelectroncapturedetector
5.2.2 ACGIH Threshold Limit Value (TLV) 1 ppm (1.8
and a suitable readout device.
3 4
mg/m ), suspected human carcinogen.
7.7.2 Chromatographic Column, packed or capillary col-
umns in accordance with 7.7.2.1 and 7.7.2.2 have been found
6. Interferences
suitable for this analysis.
6.1 Derivatives and other compounds that have identical or
7.7.2.1 Packed, 3.7 m by 3 mm (12 ft by ⁄8 in.), stainless
nearly the same GC column retention time as 2-bromoethanol
steel, packed with 10 % diethylene glycol succinate on diato-
during the gas chromatographic analysis will interfere.
maceous earth, flux-calcined, silanized, 80/100 mesh.
7.7.2.2 Capillary, 30-m by 0.53-mm inside diameter fused
6.2 Interferences can sometimes be resolved by altering gas
silica capillary column with polyethylene glycol phase.
chromatographic operating conditions. The identity of sus-
pected 2-bromoethanol, or the presence of 2-bromoethanol
8. Reagents
masked by a chromatographic interference, or both, can be
verified by gas chromatography/mass spectrometry. 8.1 Purity of Reagents—Unless otherwise indicated, it is
intended that all reagents conform to the specifications of the
7. Apparatus
Committee on Analytical Reagents of the American Chemical
Society where such specifications are available. Other grades
7.1 Carbon Molecular Sieve, surface area 400 m /g, HBr
may be used, provided it is first ascertained that the reagent is
sampling tube.
of sufficiently high purity to permit its use without lessening
7.1.1 Preparation of Collection Medium—Add 20 mL of
the accuracy of the determination.
HBr(24 %)to70gofcarbonmolecularsieve,surfacearea400
m /g,inaglassjar.Capthejarandmixthecontentsthoroughly
8.2 Acetonitrile, pesticide grade.
for 5 min by rotating.Allow to equilibrate and dry overnight or
8.3 2-Bromoethanol, commercially available at 98 % purity
for 12 h.
or better.
7.1.2 Tube Preparation—Insert a plug of silanized glass
8.4 Desorbing Solution, 1+1 (v/v) mixture of acetonitrile
wool into a 10-cm by 6-mm outside diameter (4-mm inside
and toluene.
diameter) glass tube. Pack the front section of the tube with
400 mg of the reactive adsorbent (7.1.1), using gentle tapping
8.5 Sodium Carbonate (Na CO ).
2 3
orvibrationtopromoteuniformpacking.Insertanotherplugof
8.6 Toluene, pesticide grade.
silanized wool and pack 200 mg of the adsorbent in the backup
section. Hold the backup section in place by firmly inserting an
9. Hazards
additional glass wool plug. The tubes may be flame-sealed or
9.1 Minimize exposure to all reagents and solvents by
sealed with polyethylene caps. Provide a numerical identifica-
performingallsampleandstandardpreparationsaswellastube
tion for each lot of tubes.
desorption in a well-ventilated hood.
7.1.3 Tube Holder, capable of preventing breakage and
protecting worker during sampling.
9.2 Avoid inhalation and skin contact with all reagents and
7.1.4 High-Density Polyethylene or Polypropylene Caps,
solvents.
tight-fitting, for resealing used tubes.
9.3 Use suitable protective holders when collecting samples
7.2 Pump and Tubing:
and handle used tubes carefully to prevent injury.
7.2.1 Sampling Pumps, having stable low flow rates
(610 % of set flow rate) within the range from 20 to 100 10. Calibration
mL/min for up to 8 h.
10.1 Sample Pump Calibration:
7.2.2 Rubber or Plastic Tubing, 6-mm inside diameter, for
10.1.1 Calibrate the sample pump flow in accordance with
connecting collection tube to pump. All tubing must be
Practice D3686, with the ETO sampling tube positioned
downstream (between tube and pump) of collection tube to
vertically and in line during calibration of the pump.
prevent contamination or loss of sample.
10.1.2 Calibrate the flow rate of the pump at 20 mL/min for
7.3 Vials, glass with PTFE-lined caps, 10 mL, for desorbing TWAsampling and 100 mL/min for STELsampling depending
samples and storing standards. on the duration of the sample and the volume of sample
needed.
7.4 Pipettes, 5 mL, for adding desorbing solution to
samples. 10.2 Gas Chromatograph Calibration:
7.5 Syringes, 10, 50, and 100-µL syringes, for preparing
standards.
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
listed by the American Chemical Society, see Annual Standards for Laboratory
Threshold Limit Values for Che
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