ASTM D5578-94(1999)e1

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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e1
Designation: D 5578 – 94 (Reapproved 1999)
Standard Test Method for
Determination of Ethylene Oxide in Workplace Atmospheres
(HBr Derivatization Method)
This standard is issued under the fixed designation D 5578; 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 (e) indicates an editorial change since the last revision or reapproval.
e NOTE—Editorial corrections were made throughout in December 1999.
1. Scope Occupational Safety and Health Administration, U.S. De-
partment of Labor, Title 29, Code of Federal Regulations,
1.1 This test method covers a method of collecting and
Part 1910, Subpart Z, Section 1910.1047.
analyzing samples to determine the amount of ethylene oxide
(ETO) present in workplace atmospheres.
3. Terminology
1.2 This test method can be used to provide a time-weighted
3.1 For definitions of terms used in this test method, refer to
average (TWA) over the concentration range from 0.2 to 30
Terminology D 1356, and Practice E 355.
ppm (v).
1.3 This test method can be used to determine 15-min
4. Summary of Test Method
excursions (STEL) ranging from 10 to 500 ppm (v).
4.1 A known volume of air is pumped through a glass tube
1.4 The values stated in SI units are to be regarded as the
packed with carbon molecular sieve, surface area 400 m /g
standard.
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
4.2 The tube contains two reactive sections for sample
responsibility of the user of this standard to establish appro-
collection. The backup section collects vapors that pass
priate safety and health practices and determine the applica-
through the front section and is used to determine if the
bility of regulatory limitations prior to use. See Section 9 for
collection capacity of the front section has been exceeded.
specific safety hazards.
4.3 The resultant derivative, 2-bromoethanol, is desorbed
with a mixture of acetonitrile/toluene and analyzed using a gas
2. Referenced Documents
chromatograph equipped with an electron capture detector.
2.1 ASTM Standards:
4.4 Desorption efficiency is determined by spiking tubes
D 1356 Terminology Relating to Sampling and Analysis of
2 with known amounts of 2-bromoethanol and analyzing with the
Atmospheres
same procedure used for air samples.
D 3686 Practice for Sampling Atmospheres to Collect Or-
4.5 Quantitation is achieved by comparing peak areas from
ganic Compound Vapors (Activated Charcoal Tube Ad-
2 sample solutions with areas from standard solutions.
sorption Method)
D 3687 Practice for Analysis of Organic Compound Vapors
5. Significance and Use
Collected by the Activated Charcoal Tube Adsorption
5.1 Ethylene oxide is a major industrial chemical with
Method
production volume ranked in the top 25 chemicals produced in
E 355 Practice for Gas Chromatography Terms and Rela-
3 the United States. It is used in the manufacture of a great
tionships
variety of products as well as being a sterilizing agent and
2.2 Other Standard:
fumigant.
5.2 This test method provides a means of determining
exposure levels of ETO in the working environment at the
This test method is under the jurisdiction of ASTM Committee D-22 on
presently recommended exposure guidelines.
Sampling and Analysis of Atmospheres and is the direct responsibility of Subcom-
mittee D22.04 on Workplace Atmospheres.
Current edition approved June 15, 1994. Published August 1994.
2 4
Annual Book of ASTM Standards, Vol 11.03. Available from Superintendent of Documents, U.S. Government Printing
Annual Book of ASTM Standards, Vol 14.02.
Office, Washington, DC 20402.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 5578
5.2.1 OSHA Permissible Exposure Limit (PEL) 1 ppm, 7.7.1 Gas Chromatograph, with an electron capture detector
15-min excursion limit 5 ppm (CFR, Part 1910, Subpart Z, and a suitable readout device.
Section 1910.1047). 7.7.2 Chromatographic Column, packed or capillary col-
5.2.2 ACGIH Threshold Limit Value (TLV) 1 ppm (1.8 umns in accordance with 7.7.2.1 and 7.7.2.2 have been found
mg/m ), suspected human carcinogen. suitable for this analysis.
7.7.2.1 Packed, 3.7 m by 3 mm (12 ft by ⁄8 in.), stainless
6. Interferences steel, packed with 10 % diethylene glycol succinate on diato-
maceous earth, flux-calcined, silanized, 80/100 mesh.
6.1 Derivatives and other compounds that have identical or
7.7.2.2 Capillary, 30-m by 0.53-mm inside diameter fused
nearly the same retention time as 2-bromoethanol during the
silica capillary column with polyethylene glycol phase.
gas chromatographic analysis will interfere.
6.2 Interferences can sometimes be resolved by altering gas
8. Reagents
chromatographic operating conditions. The presence of
8.1 Purity of Reagents—Unless otherwise indicated, it is
2-bromoethanol under a chromatographic peak can be verified
intended that all reagents conform to the specifications of the
using a mass spectrometer.
Committee on Analytical Reagents of the American Chemical
Society where such specifications are available. Other grades
7. Apparatus
may be used, provided it is first ascertained that the reagent is
7.1 Carbon Molecular Sieve, surface area 400 m /g, HBr
of sufficiently high purity to permit its use without lessening
sampling tube.
the accuracy of the determination.
7.1.1 Preparation of Collection Medium—Add 20 mL of
8.2 Acetonitrile, pesticide grade.
HBr (24 %) to 70 g of carbon molecular sieve, surface area 400
8.3 2-Bromoethanol, commercially available at 98 % purity
m /g, in a glass jar. Cap the jar and mix the contents thoroughly
or better.
for 5 min by rotating. Allow to equilibrate and dry overnight or
8.4 Desorbing Solution, 1+1 (v/v) mixture of acetonitrile
for 12 h.
and toluene.
7.1.2 Tube Preparation— Insert a plug of silanized glass
8.5 Sodium Carbonate (Na CO ).
2 3
wool into a 10-cm by 6-mm outside diameter (4-mm inside
8.6 Toluene, pesticide grade.
diameter) glass tube. Pack the front section of the tube with
400 mg of the reactive adsorbent (7.1.1), using gentle tapping
9. Hazards
or vibration to promote uniform packing. Insert another plug of
9.1 Minimize exposure to all reagents and solvents by
silanized wool and pack 200 mg of the adsorbent in the backup
performing all sample and standard preparations as well as tube
section. Hold the backup section in place by firmly inserting an
desorption in a well-ventilated hood.
additional glass wool plug. The tubes may be flame-sealed or
9.2 Avoid inhalation and skin contact with all reagents and
sealed with polyethylene caps. Provide a numerical identifica-
solvents.
tion for each lot of tubes.
9.3 Use suitable protective holders when collecting samples
7.1.3 Tube Holder, capable of preventing breakage and
and handle used tubes carefully to prevent injury.
protecting worker during sampling.
7.1.4 High-Density Polyethylene or Polypropylene Caps,
10. Calibration
tight-fitting, for resealing used tubes.
10.1 Sample Pump Calibration:
7.2 Pump and Tubing:
10.1.1 Calibrate the sample pump flow in accordance with
7.2.1 Sampling Pumps, having stable low flow rates
Practice D 3686, with the ETO sampling tube positioned
(610 % of set flow rate) within the range from 20 to 100
vertically and in line during calibration of the pump.
mL/min for up to 8 h.
10.1.2 Calibrate the flow rate of the pump at 20 mL/min for
7.2.2 Rubber or Plastic Tubing, 6-mm inside diameter, for
TWA sampling and 100 mL/min for STEL sampling depending
connecting collection tube to pump. All tubing must be
on the duration of the sample and the volume of sample
downstream (between tube and pump) of collection tube to
needed.
prevent contamination or loss of sample.
10.2 Gas Chromatograph Calibration:
7.3 Vials, glass with TFE-fluorocarbon lined caps, 10 mL,
10.2.1 Prepare a 2-bromoethanol stock solution (1 μg/μL)
for desorbing samples and storing standards.
by adding 57 μL of 2-bromoethanol to 100 mL of toluene. If
7.4 Pipettes, 5 mL, for adding desorbing solution to
refrigerated, this solution is stable for at least one month.
samples.
10.2.2 To a series of four 10-mL vials containing 5.0 mL of
7.5 Syringes, 10, 50, and 100-μL syringes, for preparing
desorbing solution, add 0.0, 50, 100, and 200 μL of stock
standards.
solution, thus, providing calibration standards equivalent to
7.6 Gas-Tight Syri
...