ASTM D6562-06
(Test Method)Standard Test Method for Determination of Gaseous Hexamethylene Diisocyanate (HDI) in Air with 9-(N-methylaminomethyl) Anthracene Method (MAMA) in the Workplace
Standard Test Method for Determination of Gaseous Hexamethylene Diisocyanate (HDI) in Air with 9-(N-methylaminomethyl) Anthracene Method (MAMA) 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 (4-7).
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 (8). The Occupational Safety & Health Administration of the U.S. Department of Labor (OSHA) has not listed a permissible exposure limit (PEL) for HDI (9).
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 gaseous 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 aerosol fraction is performed separately, as described in Test Method D 6561.
1.2 Differential air sampling is performed with a segregating device. The vapor 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 range of application of this test method, using UV and fluorescence detectors both connected in serial, has been validated from 0.006 to 1.12 g of monomeric HDI/2.0 mL of desorption solution, which corresponds to concentrations equivalent to 0.0004 to 0.075 mg/m 3 of HDI based on a 15-L air sample. Those concentrations correspond to a range of vapor phase concentrations from 0.06 ppb(V) to 11 ppb(V) and cover the established threshold limit value (TLV) value of 5 ppb(V).
1.5 The quantification limit for the monomeric HDI, using the UV detection, has been established as 0.012 g/2 mL of desorption solution and as 0.008 g/2 mL, using the fluorescence detector. These limits correspond to 0.0008 mg/m3 and 0.0005 mg/m3 respectively for an air sampled volume of 15 L. These values are equal to ten times the standard deviation (SD) obtained from ten measurements carried out on a standard solution in contact with the GFF, whose concentration of 0.02 g/2 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 limi...
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D6562–06
Standard Test Method for
Determination of Gaseous Hexamethylene Diisocyanate
(HDI) in Air with 9-(N-methylaminomethyl) Anthracene
1
Method (MAMA) in the Workplace
This standard is issued under the fixed designation D6562; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope validated from 0.006 to 1.12 µg of monomeric HDI/2.0 mLof
desorption solution, which corresponds to concentrations
1.1 This test method covers the determination of gaseous
3
equivalent to 0.0004 to 0.075 mg/m of HDI based on a 15-L
hexamethylene diisocyanate (HDI) in air samples collected
air sample. Those concentrations correspond to a range of
from workplace and ambient atmospheres. The method de-
vaporphaseconcentrationsfrom0.06ppb(V)to11ppb(V)and
scribed in this test method collects separate fractions. One
cover the established threshold limit value (TLV) value of 5
fractionwillbedominatedbyvapor,andtheotherfractionwill
ppb(V).
be dominated by aerosol. It is not known at the present time
1.5 The quantification limit for the monomeric HDI, using
whether this represents a perfect separation of vapor and
the UV detection, has been established as 0.012 µg/2 mL of
aerosol, and in any case, there are not separate exposure
desorption solution and as 0.008 µg/2 mL, using the fluores-
standards for vapor and aerosol. Therefore, in comparing the
3
cence detector. These limits correspond to 0.0008 mg/m and
results for isocyanate against a standard, results from the two
3
0.0005 mg/m respectively for an air sampled volume of 15 L.
fractions should be combined to give a single total value. The
Thesevaluesareequaltotentimesthestandarddeviation(SD)
reason for splitting the sample into two fractions is to increase
obtained from ten measurements carried out on a standard
analytic sensitivity for the vapor fraction and also to give the
solution in contact with the GFF, whose concentration of 0.02
hygienist or ventilation engineer some information concerning
µg/2 mL is close to the expected detection limit.
the likely state of the isocyanate species. The analyses of the
1.6 This standard does not purport to address all of the
twofractionsaredifferent,andareprovidedinseparate,linked,
safety concerns, if any, associated with its use. It is the
standards to avoid confusion. This test method is principally
responsibility of the user of this standard to establish appro-
used to determine short term exposure (15 min) of HDI in
priate safety and health practices and determine the applica-
workplaceenvironmentsforpersonalmonitoringorinambient
bility of regulatory limitations prior to use. See Section 9 for
air.Theanalysisoftheaerosolfractionisperformedseparately,
additional hazards.
as described in Test Method D6561.
1.2 Differential air sampling is performed with a segregat-
2. Referenced Documents
2
ing device. The vapor fraction is collected on a glass fiber
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2.1 ASTM Standards:
filter (GFF) impregnated with 9-(N-methylaminomethyl) an-
D1193 Specification for Reagent Water
thracene (MAMA).
D1356 Terminology Relating to Sampling and Analysis of
1.3 Theanalysisofthegaseousfractionisperformedwitha
Atmospheres
high performance liquid chromatograph (HPLC) equipped
D1357 Practice for Planning the Sampling of the Ambient
with ultraviolet (UV) and fluorescence detectors.
Atmosphere
1.4 The range of application of this test method, using UV
D5337 Practice for Flow Rate Calibration of Personal
and fluorescence detectors both connected in serial, has been
Sampling Pumps
D6561 Test Method for Determination of Aerosol Mono-
meric and Oligomeric Hexamethylene Diisocyanate (HDl)
1
This test method is under the jurisdiction of ASTM Committee D22 on
inAir with (Methoxy-2−phenyl-1) Piperazine (MOPIP) in
Sampling andAnalysis ofAtmospheres and is the direct responsibility of Subcom-
the Workplace
mittee D22.04 on Workplace Atmospheres.
Current edition approved Oct. 1, 2006. Published October 2006. Originally
2.2 Other Standard:
approved in 2000. Last previous edition approved in 2000 as D6562-00. DOI:
10.1520/D6562-06.
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 toASTM Headquarters. Your comments will receive careful consider- Standards volume information, refer to the standard’s Document Summary page on
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at
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