ASTM D4856-11(2016)
(Test Method)Standard Test Method for Determination of Sulfuric Acid Mist in Workplace Atmospheres Collected on Mixed Cellulose Ester Filters (Ion Chromatographic Analysis)
Standard Test Method for Determination of Sulfuric Acid Mist in Workplace Atmospheres Collected on Mixed Cellulose Ester Filters (Ion Chromatographic Analysis)
SIGNIFICANCE AND USE
5.1 Sulfuric acid is used in the manufacture of fertilizer, explosives, dyestuffs, other acids, parchment paper, glue, lead acid batteries, textiles, etc., and in the pickling of metals.
5.2 This test method has been found to be satisfactory in the measurement of sulfuric acid for comparison with relevant occupational exposure limits.
SCOPE
1.1 This ion chromatographic test method describes the determination of sulfuric acid mist in air samples collected from workplace atmospheres on a mixed cellulose ester (MCE) filter.
Note 1: Other filter types such as quartz fiber, polytetrafluoroethylene (PTFE), and polyvinyl chloride (PVC) filters are also suitable.
1.2 The lower detection limit of this test method is 0.001 mg/sample or 0.017 mg/m3 of sulfuric acid (H2SO4) mist in 60 L of air sampled at 1 L/min.
1.3 This test method is subject to interference from soluble and partially soluble sulfate salts. Other sulfur-containing compounds can be oxidized to sulfate and also interfere.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 No detailed instrument operating instructions are provided because of differences among various makes and models of ion chromatography (IC) systems. Instead, the analyst shall follow the instructions provided by the manufacturer of the particular instrument, analytical column, and suppressors used.
1.6 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. For specific precautionary statements, see Section 9.
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D4856 − 11 (Reapproved 2016)
Standard Test Method for
Determination of Sulfuric Acid Mist in Workplace
Atmospheres Collected on Mixed Cellulose Ester Filters (Ion
Chromatographic Analysis)
This standard is issued under the fixed designation D4856; 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 2. Referenced Documents
1.1 This ion chromatographic test method describes the 2.1 ASTM Standards:
determination of sulfuric acid mist in air samples collected D1193Specification for Reagent Water
fromworkplaceatmospheresonamixedcelluloseester(MCE) D1356Terminology Relating to Sampling and Analysis of
filter. Atmospheres
D1914PracticeforConversionUnitsandFactorsRelatingto
NOTE 1—Other filter types such as quartz fiber, polytetrafluoroethylene
Sampling and Analysis of Atmospheres
(PTFE), and polyvinyl chloride (PVC) filters are also suitable.
D4327Test Method forAnions in Water by Suppressed Ion
1.2 The lower detection limit of this test method is 0.001
Chromatography
mg/sampleor0.017mg/m ofsulfuricacid(H SO )mistin60
2 4
E200Practice for Preparation, Standardization, and Storage
L of air sampled at 1 L/min.
of Standard and Reagent Solutions for ChemicalAnalysis
1.3 This test method is subject to interference from soluble
2.2 ISO and European Standards:
and partially soluble sulfate salts. Other sulfur-containing
ISO648Laboratory glassware—One Mark pipettes
compounds can be oxidized to sulfate and also interfere.
ISO7708Air quality—Particle size fraction definitions for
health-related sampling
1.4 The values stated in SI units are to be regarded as
ISO 1042Laboratory glassware—One-mark volumetric
standard. No other units of measurement are included in this
flasks
standard.
EN482 Workplace atmospheres—General requirements for
1.5 No detailed instrument operating instructions are pro-
the performance of procedures for the measurement of
videdbecauseofdifferencesamongvariousmakesandmodels
chemical agents
of ion chromatography (IC) systems. Instead, the analyst shall
EN1540Workplace atmospheres—Terminology
follow the instructions provided by the manufacturer of the
EN13890Workplace atmospheres—Procedures for measur-
particularinstrument,analyticalcolumn,andsuppressorsused.
ing metals and metalloids in airborne particles—
1.6 This standard does not purport to address all of the
Requirements and test methods
safety concerns, if any, associated with its use. It is the
3. Terminology
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
3.1 Definitions—For definitions of terms used in this test
bility of regulatory limitations prior to use. For specific
method, refer to Terminology D1356 and EN1540.
precautionary statements, see Section 9.
3.2 Definitions of Terms Specific to This Standard:
1.7 This international standard was developed in accor-
3.2.1 eluent—ionic mobile phase used to transport the
dance with internationally recognized principles on standard-
sample through the exchange columns.
ization established in the Decision on Principles for the
3.2.2 resolution—ability of a column to separate constitu-
Development of International Standards, Guides and Recom-
ents under specified test conditions.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
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
This test method is under the jurisdiction of ASTM Committee D22 on Air Standards volume information, refer to the standard’s Document Summary page on
Quality and is the direct responsibility of Subcommittee D22.04 on WorkplaceAir the ASTM website.
Quality. Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
Current edition approved Oct. 1, 2016. Published October 2016. Originally 4th Floor, New York, NY 10036, http://www.ansi.org.
approved in 1988. Last previous edition approved in 2011 as D4856–11. DOI: Available from European Committee for Standardization (CEN), Avenue
10.1520/D4856-11R16. Marnix 17, B-1000, Brussels, Belgium, http://www.cen.eu.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4856 − 11 (2016)
4. Summary of Test Method 7.2.6 Conductivity Detector, a low-volume, flow-through,
temperature-compensated, electrical conductivity cell.
4.1 A known volume of air is drawn through mixed cellu-
7.2.7 Recorder, Integrator, or Computer, a device for the
lose ester membrane filter-mounted in an appropriate air
purpose of measuring peak height or area, compatible with the
sampler. Examples are, but not limited to: inhalable samplers,
detector output, and capable of recording detector response as
25-mm 3-piece, and 37-mm 3-piece cassettes supported by a
a function of time.
back-up pad or screen.
7.2.8 Eluent Reservoir, a container suitable for storing a
4.2 The sulfuric acid collected on the filter is desorbed with
prepared eluent solution.
D1193 Type 1 water. An aliquot of the desorbed sample
7.2.9 Eluent Generation System, for continuous production
solutionisinjectedintoanionchromatographtodeterminethe
of eluent, suitable for use with the selected separator column,
sulfate ion concentration.
as an alternative to using a manually-prepared eluent.
7.2.10 Ultrasonic Bath, preferably with a timer, suitable for
5. Significance and Use
use in the ultrasonic extraction.
5.1 Sulfuric acid is used in the manufacture of fertilizer,
7.3 Laboratory Supplies:
explosives, dyestuffs, other acids, parchment paper, glue, lead
7.3.1 One-mark Volumetric Flasks, capacities between 10
acid batteries, textiles, etc., and in the pickling of metals.
mL and 2000 mL.
5.2 Thistestmethodhasbeenfoundtobesatisfactoryinthe
7.3.2 One-mark Pipets, complying with the requirements of
measurement of sulfuric acid for comparison with relevant
ISO648.
occupational exposure limits.
7.3.3 Disposable Screw-cap Polyethylene Vessels,of15-mL
capacity.
6. Interferences
7.3.4 Disposable Filters, polytetrafluorethylene (PTFE),
6.1 Soluble or partially soluble sulfate salts, for example,
pore size 0.25 µm, for use in ion chromatography.
sodium or calcium sulfate, will be measured as sulfuric acid.
7.3.5 Disposable 2-mL or 5-mL Syringes, with Luer lock
Other sulfur-containing compounds can be oxidized to sulfate
connector, for use with disposable filters, or for sample
and also interfere.
injections without an autosampler.
7.3.6 Autosampler Vials, suitable for the autosampler used.
7. Apparatus
7.3.7 Pipet Tips, plastic, disposable, of assorted sizes, as
7.1 Sampling Equipment:
needed.
7.1.1 Airsamplerdesignedtocollecttheappropriateaerosol
7.3.8 Labware,preferablyplastic(beakers,flasks,graduated
size fraction needed. Examples are: inhalable sampler, 3-piece
cylinders, etc.), of assorted sizes, as needed.
37-mm or 25-mm filter cassette constructed of styrene acrylo-
7.3.9 Tweezers, manufactured from plastic or tipped with
nitrile to hold the filter that is supported by a cellulose pad.
PTFE, for loading and unloading filters into samplers.
7.1.2 A MCE filter.
8. Reagents
NOTE 2—This method may also be used with other appropriate filters
such PTFE, Glass Fiber, PVC, and others.
8.1 Reagent-grade chemicals shall be used in all tests.
7.1.3 Apersonal sampling pump capable of maintaining the Unlessotherwiseindicate
...
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: D4856 − 11 (Reapproved 2016)
Standard Test Method for
Determination of Sulfuric Acid Mist in Workplace
Atmospheres Collected on Mixed Cellulose Ester Filters (Ion
Chromatographic Analysis)
This standard is issued under the fixed designation D4856; 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. Referenced Documents
1.1 This ion chromatographic test method describes the 2.1 ASTM Standards:
determination of sulfuric acid mist in air samples collected D1193 Specification for Reagent Water
from workplace atmospheres on a mixed cellulose ester (MCE) D1356 Terminology Relating to Sampling and Analysis of
filter. Atmospheres
D1914 Practice for Conversion Units and Factors Relating to
NOTE 1—Other filter types such as quartz fiber, polytetrafluoroethylene
Sampling and Analysis of Atmospheres
(PTFE), and polyvinyl chloride (PVC) filters are also suitable.
D4327 Test Method for Anions in Water by Suppressed Ion
1.2 The lower detection limit of this test method is 0.001
Chromatography
mg/sample or 0.017 mg/m of sulfuric acid (H SO ) mist in 60
2 4
E200 Practice for Preparation, Standardization, and Storage
L of air sampled at 1 L/min.
of Standard and Reagent Solutions for Chemical Analysis
1.3 This test method is subject to interference from soluble
2.2 ISO and European Standards:
and partially soluble sulfate salts. Other sulfur-containing
ISO 648 Laboratory glassware—One Mark pipettes
compounds can be oxidized to sulfate and also interfere.
ISO 7708 Air quality—Particle size fraction definitions for
health-related sampling
1.4 The values stated in SI units are to be regarded as
ISO 1042 Laboratory glassware—One-mark volumetric
standard. No other units of measurement are included in this
flasks
standard.
EN 482 Workplace atmospheres—General requirements for
1.5 No detailed instrument operating instructions are pro-
the performance of procedures for the measurement of
vided because of differences among various makes and models
chemical agents
of ion chromatography (IC) systems. Instead, the analyst shall
EN 1540 Workplace atmospheres—Terminology
follow the instructions provided by the manufacturer of the
EN 13890 Workplace atmospheres—Procedures for measur-
particular instrument, analytical column, and suppressors used.
ing metals and metalloids in airborne particles—
1.6 This standard does not purport to address all of the
Requirements and test methods
safety concerns, if any, associated with its use. It is the
3. Terminology
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
3.1 Definitions—For definitions of terms used in this test
bility of regulatory limitations prior to use. For specific
method, refer to Terminology D1356 and EN 1540.
precautionary statements, see Section 9.
3.2 Definitions of Terms Specific to This Standard:
1.7 This international standard was developed in accor-
3.2.1 eluent—ionic mobile phase used to transport the
dance with internationally recognized principles on standard-
sample through the exchange columns.
ization established in the Decision on Principles for the
3.2.2 resolution—ability of a column to separate constitu-
Development of International Standards, Guides and Recom-
ents under specified test conditions.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
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
This test method is under the jurisdiction of ASTM Committee D22 on Air Standards volume information, refer to the standard’s Document Summary page on
Quality and is the direct responsibility of Subcommittee D22.04 on Workplace Air the ASTM website.
Quality. Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
Current edition approved Oct. 1, 2016. Published October 2016. Originally 4th Floor, New York, NY 10036, http://www.ansi.org.
approved in 1988. Last previous edition approved in 2011 as D4856 – 11. DOI: Available from European Committee for Standardization (CEN), Avenue
10.1520/D4856-11R16. Marnix 17, B-1000, Brussels, Belgium, http://www.cen.eu.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4856 − 11 (2016)
4. Summary of Test Method 7.2.6 Conductivity Detector, a low-volume, flow-through,
temperature-compensated, electrical conductivity cell.
4.1 A known volume of air is drawn through mixed cellu-
7.2.7 Recorder, Integrator, or Computer, a device for the
lose ester membrane filter-mounted in an appropriate air
purpose of measuring peak height or area, compatible with the
sampler. Examples are, but not limited to: inhalable samplers,
detector output, and capable of recording detector response as
25-mm 3-piece, and 37-mm 3-piece cassettes supported by a
5 a function of time.
back-up pad or screen.
7.2.8 Eluent Reservoir, a container suitable for storing a
4.2 The sulfuric acid collected on the filter is desorbed with
prepared eluent solution.
D1193 Type 1 water. An aliquot of the desorbed sample
7.2.9 Eluent Generation System, for continuous production
solution is injected into an ion chromatograph to determine the
of eluent, suitable for use with the selected separator column,
sulfate ion concentration.
as an alternative to using a manually-prepared eluent.
7.2.10 Ultrasonic Bath, preferably with a timer, suitable for
5. Significance and Use
use in the ultrasonic extraction.
5.1 Sulfuric acid is used in the manufacture of fertilizer,
7.3 Laboratory Supplies:
explosives, dyestuffs, other acids, parchment paper, glue, lead
7.3.1 One-mark Volumetric Flasks, capacities between 10
acid batteries, textiles, etc., and in the pickling of metals.
mL and 2000 mL.
5.2 This test method has been found to be satisfactory in the
7.3.2 One-mark Pipets, complying with the requirements of
measurement of sulfuric acid for comparison with relevant
ISO 648.
occupational exposure limits.
7.3.3 Disposable Screw-cap Polyethylene Vessels, of 15-mL
capacity.
6. Interferences
7.3.4 Disposable Filters, polytetrafluorethylene (PTFE),
6.1 Soluble or partially soluble sulfate salts, for example,
pore size 0.25 µm, for use in ion chromatography.
sodium or calcium sulfate, will be measured as sulfuric acid.
7.3.5 Disposable 2-mL or 5-mL Syringes, with Luer lock
Other sulfur-containing compounds can be oxidized to sulfate
connector, for use with disposable filters, or for sample
and also interfere.
injections without an autosampler.
7.3.6 Autosampler Vials, suitable for the autosampler used.
7. Apparatus
7.3.7 Pipet Tips, plastic, disposable, of assorted sizes, as
7.1 Sampling Equipment:
needed.
7.1.1 Air sampler designed to collect the appropriate aerosol
7.3.8 Labware, preferably plastic (beakers, flasks, graduated
size fraction needed. Examples are: inhalable sampler, 3-piece
cylinders, etc.), of assorted sizes, as needed.
37-mm or 25-mm filter cassette constructed of styrene acrylo-
7.3.9 Tweezers, manufactured from plastic or tipped with
nitrile to hold the filter that is supported by a cellulose pad.
PTFE, for loading and unloading filters into samplers.
7.1.2 A MCE filter.
8. Reagents
NOTE 2—This method may also be used with other appropriate filters
such PTFE, Glass Fiber, PVC, and others.
8.1 Reagent-grade chemicals shall be used in all tests.
7.1.3 A personal sampling pump capable of maintaining the Unless otherwise indicated, it is intended that all reagents shall
required sampling ra
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM 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: D4856 − 11 D4856 − 11 (Reapproved 2016)
Standard Test Method for
Determination of Sulfuric Acid Mist in Workplace
Atmospheres Collected on Mixed Cellulose Ester Filters (Ion
Chromatographic Analysis)
This standard is issued under the fixed designation D4856; 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 ion chromatographic test method describes the determination of sulfuric acid mist in air samples collected from
workplace atmospheres on a mixed cellulose ester (MCE) filter.
NOTE 1—Other filter types such as quartz fiber, polytetrafluoroethylene (PTFE), and polyvinyl chloride (PVC) filters are also suitable.
1.2 The lower detection limit of this test method is 0.001 mg/sample or 0.017 mg/m of sulfuric acid (H SO ) mist in 60 L of
2 4
air sampled at 1 L/min.
1.3 This test method is subject to interference from soluble and partially soluble sulfate salts. Other sulfur-containing
compounds can be oxidized to sulfate and also interfere.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 No detailed instrument operating instructions are provided because of differences among various makes and models of ion
chromatography (IC) systems. Instead, the analyst shall follow the instructions provided by the manufacturer of the particular
instrument, analytical column, and suppressors used.
1.6 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. For specific precautionary statements, see Section 9.
2. Referenced Documents
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D1356 Terminology Relating to Sampling and Analysis of Atmospheres
D1914 Practice for Conversion Units and Factors Relating to Sampling and Analysis of Atmospheres
D4327 Test Method for Anions in Water by Suppressed Ion Chromatography
E200 Practice for Preparation, Standardization, and Storage of Standard and Reagent Solutions for Chemical Analysis
2.2 ISO and European Standards: and European Standards:
ISO 648 Laboratory glassware—One Mark pipettes
ISO 7708 Air quality—Particle size fraction definitions for health-related sampling
ISO 1042 Laboratory glassware—One-mark volumetric flasks
EN 482 Workplace atmospheres—General requirements for the performance of procedures for the measurement of chemical
agents.agents
EN 1540 Workplace atmospheres—Terminology
EN 13890 Workplace atmospheres—Procedures for measuring metals and metalloids in airborne particles—Requirements and
test methods
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 Sept. 15, 2011Oct. 1, 2016. Published September 2011October 2016. Originally approved in 1988. Last previous edition approved in 20042011
as D4856 - 99 (2004).D4856 – 11. DOI: 10.1520/D4856-11.10.1520/D4856-11R16.
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 the ASTM website.
Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http://www.ansi.org.
Available from European Committee for Standardization (CEN), Avenue Marnix 17, B-1000, Brussels, Belgium, http://www.cen.eu.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4856 − 11 (2016)
3. Terminology
3.1 Definitions—For definitions of terms used in this test method, refer to Terminology D1356 and EN 1540.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 eluent—ionic mobile phase used to transport the sample through the exchange columns.
3.2.2 resolution—ability of a column to separate constituents under specified test conditions.
4. Summary of Test Method
4.1 A known volume of air is drawn through mixed cellulose ester membrane filter-mounted in an appropriate air sampler.
Examples are, but not limited to: inhalable samplers, 25-mm 3-piece, and 37-mm 3-piece cassettes supported by a back-up pad
or screen.
4.2 The sulfuric acid collected on the filter is desorbed with D1193 Type 1 water. An aliquot of the desorbed sample solution
is injected into an ion chromatograph to determine the sulfate ion concentration.
5. Significance and Use
5.1 Sulfuric acid is used in the manufacture of fertilizer, explosives, dyestuffs, other acids, parchment paper, glue, lead acid
batteries, textiles, etc., and in the pickling of metals.
5.2 This test method has been found to be satisfactory in the measurement of sulfuric acid for comparison with relevant
occupational exposure limits.
6. Interferences
6.1 Soluble or partially soluble sulfate salts, for example, sodium or calcium sulfate, will be measured as sulfuric acid. Other
sulfur-containing compounds can be oxidized to sulfate and also interfere.
7. Apparatus
7.1 Sampling Equipment:
7.1.1 Air sampler designed to collect the appropriate aerosol size fraction needed. Examples are: inhalable sampler, 3-piece
37-mm or 25-mm filter cassette constructed of styrene acrylonitrile to hold the filter that is supported by a cellulose pad.
7.1.2 A MCE filter.
NOTE 2—This method may also be used with other appropriate filters such PTFE, Glass Fiber, PVC, and others.
7.1.3 A personal sampling pump capable of maintaining the required sampling rate through the sampler throughout the sampling
period.
7.2 Ion Chromatograph:
7.2.1 Pump, capable of delivering a constant flow of 0.1 to 5 mL of eluent per minute at a pressure of from 3.4 to 34 MPa (500
to 5000 psi).
7.2.2 Injection Valve, a low dead volume, non-metallic valve fitted with a sample loop having a volume of up to 500 μl, for
injecting the samples into the eluent stream. An autosampler can be attached for automation.
7.2.3 Guard Column, a column placed before the separator column to protect it from being fouled by particulate matter.
7.2.4 Separator Column, a column packed with anion exchange resin that is suitable for resolving the sulfate anion.
7.2.5 Suppressor Module, a module to reduce the total conductivity of the eluent, suitable for use with the separator column and
capable of converting the eluent and separated anions to their respective acid forms.
7.2.6 Conductivity Detector, a low-volume, flow-through, temperature-compensated, electrical conductivity cell.
7.2.7 Recorder, Integrator, or Computer, a device for the purpose of measuring peak height or area, compatible with the detector
output, and capable of recording detector response as a function of time.
7.2.8 Eluent Reservoir, a container suitable for storing a prepared eluent solution.
7.2.9 Eluent Generation System, for continuous production of eluent, suitable for use with the selected separator column, as an
alternative to using a manually-prepared eluent.
7.2.10 Ultrasonic Bath, preferably with a timer, suitable for use in the ultrasonic extraction.
7.3 Laboratory Supplies:
7.3.1 One-mark Volumetric Flasks, capacities b
...
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