ASTM D5932-08
(Test Method)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) Anthracene Method) (MAMA) in the Workplace
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) Anthracene Method) (MAMA) in the Workplace
SIGNIFICANCE AND USE
p>TDI is used mostly in the preparation of rigid and semi-rigid foams and adhesives.
Isocyanate use has been growing for the last 20 years and the industrial need is still growing.
Diisocyanates and polyisocyanates are irritants to skin, eyes, and mucous membranes. They are recognized to cause respiratory allergic sensitization, asthmatic bronchitis, and acute respiratory intoxication (6-9).
The American Conference of Governmental Industrial Hygienists (ACGIH) has adopted a Threshold Limit Value–Time Weighted Average (TLV—TWA) of 0.036 mg/m3 with a Short-Term Exposure Limit (STEL) of 0.14 mg/m3 for 2,4-TDI (10). The Occupational Safety and Health Administration of the U.S. Department of Labor (OSHA) has a permissible exposure limit of 0.02 ppm(V) or 0.14 mg/m3 of TDI as a ceiling limit and 0.005 ppm (V) or 0.036 mg/m3 as a time-weighted average (11).
Monitoring of respiratory and other problems related to diisocyanates and polyisocyanates is aided through the utilization of this test method, due to its sensitivity and low volume requirements (15 L). Its short sampling times are compatible with the duration of many industrial processes and its low quantification limit also suits the concentrations often found in the working area.
The segregating sampling device pertaining to this proposed test method physically separates gas and aerosol allowing isocyanate concentrations in both physical states to be obtained, thus helping in the selection of ventilation systems and personal protection.
This test method is used to measure gaseous concentrations of 2,4- and 2,6-TDI in air for workplace and ambient atmospheres.
SCOPE
1.1 This test method covers the determination of gaseous 2,4-toluene diisocyanate (2,4-TDI) and 2,6-toluene diisocyanate (2,6-TDI) in air samples collected from workplace and ambient atmospheres.
1.2 Differential air sampling is performed with a segregating device. , The gaseous fraction is collected on a glass fiber filter (GFF) impregnated with 9-(N-methylaminomethyl) anthracene (MAMA).
1.3 The analysis of the gaseous fraction is performed with a high performance liquid chromatograph (HPLC) equipped with ultraviolet (UV) and fluorescence detectors.
1.4 The analysis of the aerosol fraction is performed separately as described in Ref (1).
1.5 The range of application of this test method, utilizing UV and a fluorescence detector, is validated for 0.029 to 1.16 μg of monomer 2,4- and 2,6-TDI/2.0 mL of desorption solution, which corresponds to concentrations of 0.002 to 0.077 mg/m3 of TDI based on a 15-L air sample. This corresponds to 0.28 to 11 ppb(V) and brackets the established TLV value of 5 ppb(v).
1.6 A field blank sampling system is used to check the possibility of contamination during the entire sampling and analysis.
1.7 The values stated in SI units are to be regarded as the standard.
1.8 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: D5932 − 08
StandardTest 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) Anthracene Method) (MAMA) in the
1
Workplace
This standard is issued under the fixed designation D5932; 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 corresponds to 0.28 to 11 ppb(V) and brackets the established
TLV value of 5 ppb(v).
1.1 This test method covers the determination of gaseous
2,4-toluene diisocyanate (2,4-TDI) and 2,6-toluene diisocya- 1.6 A field blank sampling system is used to check the
nate (2,6-TDI) in air samples collected from workplace and possibility of contamination during the entire sampling and
ambient atmospheres. analysis.
1.2 Differential air sampling is performed with a segregat- 1.7 The values stated in SI units are to be regarded as the
2,3
ing device. The gaseous fraction is collected on a glass fiber standard.
filter (GFF) impregnated with 9-(N-methylaminomethyl) an-
1.8 This standard does not purport to address all of the
thracene (MAMA).
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
1.3 The analysis of the gaseous fraction is performed with a
priate safety and health practices and determine the applica-
high performance liquid chromatograph (HPLC) equipped
bility of regulatory limitations prior to use.
with ultraviolet (UV) and fluorescence detectors.
1.4 The analysis of the aerosol fraction is performed sepa-
2. Referenced Documents
4
rately as described in Ref (1).
5
2.1 ASTM Standards:
1.5 The range of application of this test method, utilizing
D1193 Specification for Reagent Water
UV and a fluorescence detector, is validated for 0.029 to 1.16
D1356 Terminology Relating to Sampling and Analysis of
µg of monomer 2,4- and 2,6-TDI/2.0 mL of desorption
Atmospheres
solution, which corresponds to concentrations of 0.002 to
D1357 Practice for Planning the Sampling of the Ambient
3
0.077 mg/m of TDI based on a 15-L air sample. This
Atmosphere
2.2 Other Documents:
6
Sampling Guide for Air Contaminants in the Workplace
1
This test method is under the jurisdiction of ASTM Committee D22 on Air
Quality and is the direct responsibility of Subcommittee D22.04 on Workplace Air
3. Terminology
Quality.
Current edition approved April 1, 2008. Published June 2008. Originally
3.1 For definitions of terms used in this test method, refer to
approved in 1996. Last previous edition approved in 2002 as D5932 - 96(2002).
Terminology D1356.
DOI: 10.1520/D5932-08.
2
The sampling device for isocyanates is covered by a patent held by Jacques
4. Summary of Test Method
Lesage et al, IRSST, 505 De Maisonneuve Blvd West, Montreal, Quebec, Canada.
Interested parties are invited to submit information regarding the identification of
4.1 A known volume of air is drawn through a segregating
acceptable alternatives to this patented item to the Committee on Standards,ASTM
sampling device.
International Headquarters, 100 Barr Harbor Dr., PO Box C700, West
Conshohocken, PA 19428. Your comments will receive careful consideration at a
4.2 Gaseous and aerosol fraction are sampled simultane-
meeting of the committee responsible, which you may attend. This sampling device
2
ouslywithatwofilterloadedcassette. Theaerosoliscollected
is currently commercially available under license from SKC Omega Specialty
Division, Eighty-Four, PA.
3
The American Society for Testing and Materials takes no position respecting
5
the validity of any patent rights asserted in connection with any item mentioned in For referenced ASTM standards, visit the ASTM website, www.astm.org, or
this standard. Users of this standard are expressly advised that determination of the contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
validity of any such patent rights, and the risk of infringement of such rights, are Standards volume information, refer to the standard’s Document Summary page on
entirely their own responsibility. the ASTM website.
4 6
The boldface numbers in parentheses refer to the list of references at the end of Available from Institut de Recherche en Santé et en Sécurité du Travail du
this test method. Québec, Laboratory Services and Expertise Department, Montreal, IRSST, 2005.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D5932 − 08
on the first filter made of polytetrafluoroethylene (PTFE), the allowing isocyanateconcentra
...
This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation:D5932–96 (Reapproved 2002) Designation:D5932–08
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) Anthracene Method) (MAMA) in the
1
Workplace
This standard is issued under the fixed designation D 5932; 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
1.1 This test method covers the determination of gaseous 2,4-toluene diisocyanate (2,4-TDI) and 2,6-toluene diisocyanate
(2,6-TDI) in air samples collected from workplace and ambient atmospheres.
,
2 3
1.2 Differential air sampling is performed with a segregating device. The gaseous fraction is collected on a glass fiber filter
(GFF) impregnated with 9-(N-methylaminomethyl) anthracene (MAMA).
1.3 The analysis of the gaseous fraction is performed with a high performance liquid chromatograph (HPLC) equipped with
ultraviolet (UV) and fluorescence detectors.
4
1.4 The analysis of the aerosol fraction is performed separately as described in Ref (1).
1.5 The range of application of this test method, utilizing UV and a fluorescence detector, is validated for 0.029 to 4.21.16 µg
of monomer 2,4- and 2,6-TDI/2.0 mL of desorption solution, which corresponds to concentrations of 0.0010.002 to 0.280.077
3
mg/m of TDI based on a 15-L air sample. This corresponds to 0.15 to 40 ppb(V) and brackets the established TLV value of 5
ppb(v).
1.6The average correlation coefficient is 0.9999 and 0.9999 for the UV detector, for 2,6 and 2,4-TDI, respectively. For the
fluorescence detector, the average correlation coefficient is 0.9803 and 0.9999 for 2,6 and 2,4-TDI, respectively.These values were
obtained from seven standard solutions distributed along the calibration curve, each standard being injected six times, with the
curve having been done twice by different operators.
1.7The quantification limit for 2,6-TDI monomers is 0.007 µg/2 mL of desorption solution, which corresponds to 0.0005 mg/m
3 for 15-L sampled air volume for the UV detector. For the fluorescence detector, the quantification limit is 0.003 µg/2 mL of
3
desorption solution, which correspond to 0.0002 mg/m for a volume of 15 L collected in air. These values are equal to ten times
the standard deviation obtained from ten measurements carried out on a standard solution whose concentration of 0.02 µg/2 mL
is close to the expected detection limit.
1.8The quantification limit for 2,4-TDI monomers is 0.015 µg/2 mL of desorption solution, which corresponds to 0.001 mg/m
3 for 15-L sampled air volume for the UV detector. For the fluorescence detector, the quantification limit is 0.012 µg/2 mL of
3
desorption solution, which corresponds to 0.0008 mg/m for a volume of 15 Lof collected air. These values are equal to ten times
the standard deviation obtained from ten measurements carried out on a standard solution whose concentration 0.02 µg/2 mL is
close to the expected detection limit.
1.92,4- and 2,6-TDI isomers can be separated using a reversed phase C18 column for HPLC. The UV and fluorescence detector
response factor (RF) ratio characterize each isomer.
1.10A field blank sampling system is used to check the possibility of contamination during the entire analytical process.
1
This test method is under the jurisdiction ofASTM Committee D22 on Sampling andAnalysis ofAtmospheres and is the direct responsibility of Subcommittee D22.04
on Workplace Atmospheres.
Current edition approved April 10, 1996. Published June 1996.
1
This test method is under the jurisdiction of ASTM Committee D22 on Air Quality and is the direct responsibility of Subcommittee D22.04 on Workplace Air Quality
.
Current edition approved April 1, 2008. Published June 2008. Originally approved in 1996. Last previous edition approved in 2002 as D5932 - 96(2002).
2
The sampling device for isocyanates is covered by a patent held by Jacques Lesage et al, IRSST, 505 De Maisonneuve Blvd West, Montreal, Quebec, Canada. Interested
parties are invited to submit information regarding the identification of acceptable alternatives to this patented item to the Committee on Standards, ASTM International
Headquarters, 100 Barr Harbor Dr., PO Box C700, West Conshohocken, PA 19428. Your comments will receive careful consideration at a meeting of the committee
responsible, which you may a
...
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