ASTM D6561-06
(Test Method)Standard Test Method for Determination of Aerosol Monomeric and Oligomeric Hexamethylene Diisocyanate (HDl) in Air with (Methoxy-2-phenyl-1) Piperazine (MOPIP) in the Workplace
Standard Test Method for Determination of Aerosol Monomeric and Oligomeric Hexamethylene Diisocyanate (HDl) in Air with (Methoxy-2-phenyl-1) Piperazine (MOPIP) in the Workplace
SIGNIFICANCE AND USE
HDI is mostly used in the preparation of paints. For the last ten years, the use of isocyanates and their industrial needs have been in constant growth.
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 (3-6).
The American Conference of Governmental Industrial Hygienists (ACGIH) has adopted a threshold limit value - time weighted average (TLV - TWA) of 0.005 ppm (V) or 0.034 mg/m3 for monomeric HDI (7). The Occupational Safety & Health Administration of the U.S. Department of Labor (OSHA) has not listed a permissible exposure limit (PEL) for HDI (8).
Due to its low LOD and low required volume (15 L), this test method is well suited for monitoring of respiratory and other problems related to diisocyanates and polyisocyanates. Its short sampling times are compatible with the duration of many industrial processes, and its low detection limit with the concentrations often found in the working area.
SCOPE
1.1 This test method covers the determination of aerosol hexamethylene diisocyanate (HDI) in air samples collected from workplace and ambient atmospheres. The method described in this test method collects separate fractions. One fraction will be dominated by vapor, and the other fraction will be dominated by aerosol. It is not known at the present time whether this represents a perfect separation of vapor and aerosol, and in any case, there are not separate exposure standards for vapor and aerosol. Therefore, in comparing the results for isocyanate against a standard, results from the two fractions should be combined to give a single total value. The reason for splitting the sample into two fractions is to increase analytic sensitivity for the vapor fraction and also to give the hygienist or ventilation engineer some information concerning the likely state of the isocyanate species. The analyses of the two fractions are different, and are provided in separate, linked, standards to avoid confusion. This test method is principally used to determine short term exposure (15 min) of HDI in workplace environments for personal monitoring or in ambient air. The analysis of the vapor fraction is performed separately, as described in Test Method D 6562.
1.2 Differential air sampling is performed with a segregating device. The aerosol fraction is collected on a polytetrafluoroethylene (PTFE) filter.
1.3 Immediately after sampling, the PTFE filter is transferred into a jar containing a (methoxy-2 phenyl-1) piperazine (MOPIP) solution in toluene.
1.4 The analysis of the aerosol fraction is performed by using a high performance liquid chromatograph (HPLC) equipped with an ultraviolet (UV) detector. The range of application of the test method has been validated from 0.052 to 1.04 g of monomeric HDI/mL, which corresponds, based on a 15 L air sample, to concentrations from 0.004 to 0.070 mg/m3 of HDI. Those concentrations correspond to a range of aerosol phase concentrations from 0.5 ppb (V) to 10 ppb (V) and cover the established threshold limit valve (TLV) value of 5 ppb (V).
1.5 The quantification limit for the monomeric HDI is 0.041 g per mL, which corresponds to 0.003 mg/m3 for a 15 L sampled air volume. This value is equivalent to ten times the standard deviation obtained from ten measurements carried out on a standard solution in contact with the PTFE filter whose concentration of 0.1 g/mL is close to the expected detection limit.
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. See Section 9 for additional hazards.
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Standards Content (Sample)
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Designation:D6561–06
Standard Test Method for
Determination of Aerosol Monomeric and Oligomeric
Hexamethylene Diisocyanate (HDl) in Air with (Methoxy-
1
2–phenyl-1) Piperazine (MOPIP) in the Workplace
This standard is issued under the fixed designation D6561; 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 equipped with an ultraviolet (UV) detector. The range of
application of the test method has been validated from 0.052 to
1.1 This test method covers the determination of aerosol
1.04 µg of monomeric HDI/mL, which corresponds, based on
hexamethylene diisocyanate (HDI) in air samples collected
3
a15Lairsample,toconcentrationsfrom0.004to0.070mg/m
from workplace and ambient atmospheres. The method de-
of HDI. Those concentrations correspond to a range of aerosol
scribed in this test method collects separate fractions. One
phase concentrations from 0.5 ppb (V) to 10 ppb (V) and cover
fraction will be dominated by vapor, and the other fraction will
the established threshold limit valve (TLV) value of 5 ppb (V).
be dominated by aerosol. It is not known at the present time
1.5 ThequantificationlimitforthemonomericHDIis0.041
whether this represents a perfect separation of vapor and
3
µg per mL, which corresponds to 0.003 mg/m fora15L
aerosol, and in any case, there are not separate exposure
sampled air volume. This value is equivalent to ten times the
standards for vapor and aerosol. Therefore, in comparing the
standard deviation obtained from ten measurements carried out
results for isocyanate against a standard, results from the two
on a standard solution in contact with the PTFE filter whose
fractions should be combined to give a single total value. The
concentration of 0.1 µg/mL is close to the expected detection
reason for splitting the sample into two fractions is to increase
limit.
analytic sensitivity for the vapor fraction and also to give the
1.6 This standard does not purport to address all of the
hygienist or ventilation engineer some information concerning
safety concerns, if any, associated with its use. It is the
the likely state of the isocyanate species. The analyses of the
responsibility of the user of this standard to establish appro-
twofractionsaredifferent,andareprovidedinseparate,linked,
priate safety and health practices and determine the applica-
standards to avoid confusion. This test method is principally
bility of regulatory limitations prior to use. See Section 9 for
used to determine short term exposure (15 min) of HDI in
additional hazards.
workplace environments for personal monitoring or in ambient
air. The analysis of the vapor fraction is performed separately,
2. Referenced Documents
as described in Test Method D6562.
3
2.1 ASTM Standards:
1.2 Differential air sampling is performed with a segregat-
2 D1193 Specification for Reagent Water
ing device. The aerosol fraction is collected on a polytetra-
D1356 Terminology Relating to Sampling and Analysis of
fluoroethylene (PTFE) filter.
Atmospheres
1.3 Immediately after sampling, the PTFE filter is trans-
D1357 Practice for Planning the Sampling of the Ambient
ferred into a jar containing a (methoxy-2 phenyl-1) piperazine
Atmosphere
(MOPIP) solution in toluene.
D5337 Practice for Flow Rate Calibration of Personal
1.4 The analysis of the aerosol fraction is performed by
Sampling Pumps
using a high performance liquid chromatograph (HPLC)
D6562 Test Method for Determination of Gaseous Hexam-
ethylene Diisocyanate (HDI) in Air with 9-(N-
1
This test method is under the jurisdiction of ASTM Committee D22 on Air
methylaminomethyl) Anthracene Method (MAMA) in the
Quality and is the direct responsibility of Subcommittee D22.04 on Workplace
Workplace
Atmospheres.
Current edition approved Oct. 1, 2006. Published October 2006. Originally
approved in 2000. Last previous edition approved in 2000 as D6561 - 00. DOI:
10.1520/D6561-06.
2
The sampling device for isocyanates is covered by a patent held by Jacques
3
Lesage et al, IRSST, 505 De Maisonneuve Blvd. West, Montreal, Quebec, Canada. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
If you are aware of an alternative to this patented item, please provide this contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
information to ASTM Headquarters. Your comments will receive careful consider- Standards volume information, refer to the standard’s Document Summary page on
1
ation at a meeting of the responsible technical committee, which you may attend. the ASTM website.
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