ASTM D4856-23
(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.
Note 2: In some countries the occupational exposure limit value (OELV) for sulfuric acid is related to the thoracic aerosol fraction; in such cases it is recommended to use a sampler for the thoracic aerosol fraction (ISO 20581).6
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific precautionary statements, see Section 9.
1.7 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.
General Information
- Status
- Published
- Publication Date
- 31-Aug-2023
- Technical Committee
- D22 - Air Quality
- Drafting Committee
- D22.04 - Workplace Air Quality
Relations
- Effective Date
- 01-Sep-2023
Overview
ASTM D4856-23 is the international standard test method for determining sulfuric acid mist in workplace atmospheres using ion chromatographic analysis of samples collected on mixed cellulose ester (MCE) filters. Developed by ASTM International, this standard provides an essential tool for occupational hygiene, industrial safety, and regulatory compliance by enabling accurate measurement of airborne sulfuric acid mist-a common byproduct in various industrial processes.
Monitoring sulfuric acid mist concentrations is critical because sulfuric acid is widely used in the manufacture of fertilizers, batteries, explosives, dyes, other acids, and during metal pickling. Proper implementation of ASTM D4856-23 helps workplaces manage employee exposure and remain compliant with occupational exposure limits (OELs).
Key Topics
- Sampling Method: Air samples are collected through MCE filters using suitable aerosol fraction samplers. Alternative filters such as quartz fiber, PTFE, and PVC are permitted.
- Analytical Technique: The standard employs ion chromatography to detect and quantify sulfate ions, which indicate the presence of sulfuric acid mist.
- Detection Limits: The method can detect sulfuric acid concentrations as low as 0.001 mg per sample or 0.017 mg/m³ in 60 liters of air.
- Interferences: Results may be impacted by other soluble sulfate salts or sulfur-containing compounds convertible to sulfate.
- Quality Assurance: Analysts use calibration standards and analytical curves, regularly verifying instrument performance according to manufacturer guidelines.
- Safety and Handling: Strict safety and sample handling protocols are mandated, including use of appropriate PPE and sample chain-of-custody documentation.
Applications
ASTM D4856-23 is utilized throughout industries where sulfuric acid is present or generated, including:
- Fertilizer Production: Monitoring worker exposure where sulfuric acid is a key raw material.
- Lead Acid Battery Manufacturing: Ensuring a safe workplace by assessing inhalable mist levels.
- Metal Processing and Pickling: Tracking acid mist to protect personnel during etching and cleaning processes.
- Chemical Manufacturing: Supporting hygiene and environmental monitoring where sulfuric acid is handled.
- Textile and Dye Production: Maintaining safe air quality in facilities where acid usage is routine.
- Occupational Health and Safety Compliance: Providing employers, industrial hygienists, and safety managers with accurate data for OEL adherence and risk management.
Related Standards
For comprehensive air monitoring and analytical rigor, ASTM D4856-23 references and aligns with several other standards:
- ASTM D1193 - Specification for Reagent Water
- ASTM D1356 - Terminology Relating to Sampling and Analysis of Atmospheres
- ASTM D4327 - Test Method for Anions in Water by Suppressed Ion Chromatography
- ASTM D4840 - Guide for Sample Chain-of-Custody Procedures
- ASTM D5337 - Practice for Setting and Verifying the Flow Rate of Personal Sampling Pumps
- ASTM D8358 - Guide for Assessment and Inclusion of Wall Deposits in Single-Stage Samplers
- ISO 20581 - Workplace Atmospheres: Performance of Procedures for Measurement of Chemical Agents
- ISO 21438-1 - Determination of Inorganic Acids by Ion Chromatography
Practical Value
Implementing ASTM D4856-23 enables organizations to:
- Protect Worker Health: Identify and control exposure to hazardous sulfuric acid mist.
- Demonstrate Compliance: Support occupational exposure monitoring and regulatory reporting.
- Enhance Process Safety: Quickly respond to changes in sulfuric acid emissions, minimizing health risks.
- Use Standardized Methods: Ensure reliable, reproducible results accepted by regulators and international stakeholders.
Keywords: sulfuric acid mist, workplace air monitoring, ion chromatography, ASTM D4856-23, exposure assessment, air sampling, occupational hygiene, industrial safety.
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Frequently Asked Questions
ASTM D4856-23 is a standard published by ASTM International. Its full title is "Standard Test Method for Determination of Sulfuric Acid Mist in Workplace Atmospheres Collected on Mixed Cellulose Ester Filters (Ion Chromatographic Analysis)". This standard covers: 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. Note 2: In some countries the occupational exposure limit value (OELV) for sulfuric acid is related to the thoracic aerosol fraction; in such cases it is recommended to use a sampler for the thoracic aerosol fraction (ISO 20581).6 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific precautionary statements, see Section 9. 1.7 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.
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. Note 2: In some countries the occupational exposure limit value (OELV) for sulfuric acid is related to the thoracic aerosol fraction; in such cases it is recommended to use a sampler for the thoracic aerosol fraction (ISO 20581).6 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific precautionary statements, see Section 9. 1.7 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.
ASTM D4856-23 is classified under the following ICS (International Classification for Standards) categories: 13.040.30 - Workplace atmospheres. The ICS classification helps identify the subject area and facilitates finding related standards.
ASTM D4856-23 has the following relationships with other standards: It is inter standard links to ASTM D4856-11(2016). Understanding these relationships helps ensure you are using the most current and applicable version of the standard.
ASTM D4856-23 is available in PDF format for immediate download after purchase. The document can be added to your cart and obtained through the secure checkout process. Digital delivery ensures instant access to the complete standard document.
Standards Content (Sample)
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 − 23
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 mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
1.1 This ion chromatographic test method describes the
determination of sulfuric acid mist in air samples collected
2. Referenced Documents
from workplace atmospheres on a mixed cellulose ester (MCE)
2.1 ASTM Standards:
filter.
D1193 Specification for Reagent Water
NOTE 1—Other filter types such as quartz fiber, polytetrafluoroethylene
D1356 Terminology Relating to Sampling and Analysis of
(PTFE), and polyvinyl chloride (PVC) filters are also suitable.
Atmospheres
1.2 The lower detection limit of this test method is
D1914 Practice for Conversion Units and Factors Relating to
0.001 mg ⁄sample or 0.017 mg ⁄m of sulfuric acid (H SO )
2 4 Sampling and Analysis of Atmospheres
mist in 60 L of air sampled at 1 L/min.
D4327 Test Method for Anions in Water by Suppressed Ion
Chromatography
1.3 This test method is subject to interference from soluble
D4840 Guide for Sample Chain-of-Custody Procedures
and partially soluble sulfate salts. Other sulfur-containing
D5337 Practice for Setting and Verifying the Flow Rate of
compounds can be oxidized to sulfate and also interfere.
Personal Sampling Pumps
1.4 The values stated in SI units are to be regarded as
D8358 Guide for Assessment and Inclusion of Wall Deposits
standard. No other units of measurement are included in this
in the Analysis of Single-Stage Samplers for Airborne
standard.
Particulate Matter
1.5 No detailed instrument operating instructions are pro-
E200 Practice for Preparation, Standardization, and Storage
vided because of differences among various makes and models
of Standard and Reagent Solutions for Chemical Analysis
of ion chromatography (IC) systems. Instead, the analyst shall
E288 Specification for Laboratory Glass Volumetric Flasks
follow the instructions provided by the manufacturer of the
E1154 Specification for Piston or Plunger Operated Volu-
particular instrument, analytical column, and suppressors used.
metric Apparatus and Operator Qualification
2.2 ISO and European Standards:
1.6 This standard does not purport to address all of the
ISO 648 Laboratory glassware — Single-volume pipettes
safety concerns, if any, associated with its use. It is the
ISO 7708 Air quality — Particle size fraction definitions for
responsibility of the user of this standard to establish appro-
health-related sampling
priate safety, health, and environmental practices and deter-
ISO 18158 Workplace air — Terminology
mine the applicability of regulatory limitations prior to use.
ISO 20581 Workplace air — General requirements for the
For specific precautionary statements, see Section 9.
performance of procedures for the measurement of chemi-
1.7 This international standard was developed in accor-
cal agents
dance with internationally recognized principles on standard-
ISO 21438-1 Workplace atmospheres — Determination of
ization established in the Decision on Principles for the
inorganic acids by ion chromatography — Part 1: Non-
Development of International Standards, Guides and Recom-
volatile acids (sulfuric acid and phosphoric acid)
1 2
This test method is under the jurisdiction of ASTM Committee D22 on Air For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Quality and is the direct responsibility of Subcommittee D22.04 on Workplace Air contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Quality. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Sept. 1, 2023. Published October 2023. Originally the ASTM website.
approved in 1988. Last previous edition approved in 2016 as D4856 – 11 (2016). Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
DOI: 10.1520/D4856-23. 4th Floor, New York, NY 10036, http://www.ansi.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4856 − 23
NOTE 3—Some size-selective samplers are designed to collect the
EN 13205 Workplace exposure — Assessment of sampler
targeted fraction of airborne particles on the filter, and any particulate
performance for measurement of airborne particle concen-
matter deposited on the internal surfaces of the sampler (separate from the
trations
filter) is not considered part of the sampled air. Other size-selective
samplers are designed such that all airborne particles which pass through
3. Terminology
the entry orifice(s) are of interest, hence particulate matter deposited on
the inner walls of the sampler does form part of the sample. In such cases
3.1 Definitions—For definitions of terms used in this test
it will be necessary to account for particulate material collected on the
method, refer to Terminology D1356 and ISO 18518.
inner walls of the sampler (in addition to that collected on the filter). Refer
to Guide D8358 for additional information.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 eluent, n—ionic mobile phase used to transport the
7.1.2 Mixed cellulose ester (MCE) filters.
sample through the exchange columns.
NOTE 4—Other filter types such as quartz fiber, polytetrafluoroethylene
3.2.2 resolution, n—ability of a column to separate constitu-
(PTFE), and polyvinyl chloride (PVC) filters are also suitable.
ents under specified test conditions.
7.1.3 A personal sampling pump capable of maintaining the
required sampling rate through the sampler, throughout the
4. Summary of Test Method
sampling period.
4.1 A known volume of air is drawn through mixed cellu-
7.2 Ion Chromatograph:
lose ester membrane filter-mounted in an appropriate air
7.2.1 Pump, capable of delivering a constant flow of 0.1 mL
sampler. Examples are, but not limited to: inhalable samplers,
to 5 mL of eluent per minute at a pressure of from 3.4 MPa to
25 mm 3 piece and 37 mm 3-piece cassettes, with filters
5 34 MPa (500 psi to 5000 psi).
supported by a back-up pad or screen.
7.2.2 Injection Valve, a low dead volume, non-metallic
4.2 The sulfuric acid collected on the filter is desorbed with
valve fitted with a sample loop having a volume of up to
Specification D1193 Type 1 water or eluent. An aliquot of the
500 μL, for injecting the samples into the eluent stream. An
desorbed sample solution is injected into an ion chromatograph
autosampler can be attached for automation.
to determine the sulfate ion concentration.
7.2.3 Guard Column, a column placed before the separator
column to protect it from being fouled by particulate matter.
5. Significance and Use
7.2.4 Separator Column, a column packed with anion ex-
5.1 Sulfuric acid is used in the manufacture of fertilizer,
change resin that is suitable for resolving the sulfate anion.
explosives, dyestuffs, other acids, parchment paper, glue, lead
7.2.5 Suppressor Module, a module to reduce the total
acid batteries, textiles, etc., and in the pickling of metals.
conductivity of the eluent, suitable for use with the separator
column and capable of converting the eluent and separated
5.2 This test method has been found to be satisfactory in the
anions to their respective acid forms.
measurement of sulfuric acid for comparison with relevant
7.2.6 Conductivity Detector, a low-volume, flow-through,
occupational exposure limits.
temperature-compensated, electrical conductivity cell.
NOTE 2—In some countries the occupational exposure limit value
7.2.7 Recorder, Integrator, or Computer, a device for the
(OELV) for sulfuric acid is related to the thoracic aerosol fraction; in such
purpose of measuring peak height or area, compatible with the
cases it is recommended to use a sampler for the thoracic aerosol fraction
detector output, and capable of recording detector response as
(ISO 20581).
a function of time.
6. Interferences
7.2.8 Eluent Reservoir, a container suitable for storing a
prepared eluent solution.
6.1 Soluble or partially soluble sulfate salts, for example,
7.2.9 Eluent Generation System, for continuous production
sodium or calcium sulfate, will be measured as sulfuric acid.
of eluent, suitable for use with the selected separator column,
Other sulfur-containing compounds can be oxidized to sulfate
as an alternative to using a manually-prepared eluent.
and also interfere.
7.2.10 Ultrasonic Bath, preferably with a timer, suitable for
7. Apparatus
use in the ultrasonic extraction.
7.1 Sampling Equipment:
7.3 Laboratory Supplies:
7.1.1 Air sampler designed to collect the appropriate aerosol
7.3.1 One-mark Volumetric Flasks, capacities between
size fraction needed (ISO 7708). Examples are: inhalable
10 mL and 2000 mL.
sampler, 3-piece 37 mm or 25 mm filter cassette constructed of
7.3.2 One-mark Pipets, complying with the requirements of
styrene acrylonitrile to hold the filter that is supported by a
ISO 648; or Piston-Operated Volumetric Pipettors and
cellulose pad.
Dispensers, complying with the requirements of Specification
E1154.
7.3.3 Disposable Screw-cap Polyethylene Vessels, of 15 mL
Available from European Committee for Standardization (CEN), Avenue
capacity.
Marnix 17, B-1000, Brussels, Belgium, http://www.cen.eu.
7.3.4 Disposable Filters, polytetrafluorethylene (PTFE),
Precision (CV = 0.082) was obtained (NIOSH Contract No. CDC-99-74-45)
T
3 3
over a range of 0.561 mg ⁄M to 2.577 mg ⁄M using mixed cellulose ester filters.
pore size 0.45 μm, for use in ion chromatography.
Breuer, D.; Heckmann, P.; Gusbeth, K.; Schwab, G.; Blaskowitz, M.; Moritz,
7.3.5 Disposable 2 mL or 5 mL Syringes, with Luer lock
A.“Sulfuri
...
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 (Reapproved 2016) D4856 − 23
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 0.0010.001 mg mg/sample or 0.017 ⁄sample or 0.017 mg mg/m⁄m of sulfuric
acid (H SO ) mist in 60 L 60 L of air sampled at 1 L/min.
2 4
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 healthsafety, health, and environmental practices and determine
the applicability of regulatory limitations prior to use. For specific precautionary statements, see Section 9.
1.7 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.
2. Referenced Documents
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D1356 Terminology Relating to Sampling and Analysis of Atmospheres
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 Oct. 1, 2016Sept. 1, 2023. Published October 2016October 2023. Originally approved in 1988. Last previous edition approved in 20112016 as
D4856 – 11.D4856 – 11 (2016). DOI: 10.1520/D4856-11R16.10.1520/D4856-23.
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4856 − 23
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
D4840 Guide for Sample Chain-of-Custody Procedures
D5337 Practice for Setting and Verifying the Flow Rate of Personal Sampling Pumps
D8358 Guide for Assessment and Inclusion of Wall Deposits in the Analysis of Single-Stage Samplers for Airborne Particulate
Matter
E200 Practice for Preparation, Standardization, and Storage of Standard and Reagent Solutions for Chemical Analysis
E288 Specification for Laboratory Glass Volumetric Flasks
E1154 Specification for Piston or Plunger Operated Volumetric Apparatus and Operator Qualification
2.2 ISO and European Standards:
ISO 648ISO 648 Laboratory glassware—One Mark glassware — Single-volume pipettes
ISO 7708 Air quality—Particlequality — Particle size fraction definitions for health-related sampling
ISO 1042ISO 18158 Laboratory glassware—One-mark volumetric flasksWorkplace air — Terminology
EN 482 ISO 20581 Workplace atmospheres—General air — General requirements for the performance of procedures for the
measurement of chemical agents
EN 1540ISO 21438-1 Workplace atmospheres—Terminologyatmospheres — Determination of inorganic acids by ion chroma-
tography — Part 1: Nonvolatile acids (sulfuric acid and phosphoric acid)
EN 13890EN 13205 Workplace atmospheres—Procedures for measuring metals and metalloids in airborne particles—
Requirements and test methodsexposure — Assessment of sampler performance for measurement of airborne particle
concentrations
3. Terminology
3.1 Definitions—For definitions of terms used in this test method, refer to Terminology D1356 and EN 1540.ISO 18518.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 eluent—eluent, n—ionic mobile phase used to transport the sample through the exchange columns.
3.2.2 resolution—resolution, n—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 25 mm 3 piece and 37 mm
3-piece cassettes, with filters supported by a back-up pad or screen.
4.2 The sulfuric acid collected on the filter is desorbed with Specification D1193 Type 1 water. water or eluent. 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.
NOTE 2—In some countries the occupational exposure limit value (OELV) for sulfuric acid is related to the thoracic aerosol fraction; in such cases it is
recommended to use a sampler for the thoracic aerosol fraction (ISO 20581).
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.
3 3
Precision (CV = 0.082) was obtained (NIOSH Contract No. CDC-99-74-45) over a range of 0.561 − 2.577 0.561 mg mg/M⁄M to 2.577 mg ⁄M using mixed cellulose
T
ester filters.
Breuer, D.; Heckmann, P.; Gusbeth, K.; Schwab, G.; Blaskowitz, M.; Moritz, A.“Sulfuric acid at workplaces - Applicability of the new Indicative Occupational Exposure
Limit Value (IOELV) to thoracic particles.” Journal of Environmental Monitoring, Vol. 14 (2012), pp. 440-445.
D4856 − 23
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. needed (ISO 7708). Examples are: inhalable
sampler, 3-piece 37-mm or 25-mm37 mm or 25 mm filter cassette constructed of styrene acrylonitrile to hold the filter that is
supported by a cellulose pad.
NOTE 3—Some size-selective samplers are designed to collect the targeted fraction of airborne particles on the filter, and any particulate matter deposited
on the internal surfaces of the sampler (separate from the filter) is not considered part of the sampled air. Other size-selective samplers are designed such
that all airborne particles which pass through the entry orifice(s) are of interest, hence particulate matter deposited on the inner walls of the sampler does
form part of the sample. In such cases it will be necessary to account for particulate material collected on the inner walls of the sampler (in addition to
that collected on the filter). Refer to Guide D8358 for additional information.
7.1.2 A MCE filter.Mixed cellulose ester (MCE) filters.
NOTE 4—This method may also be used with other appropriate filters such PTFE, Glass Fiber, PVC, and others.Other filter types such as quartz fiber,
polytetrafluoroethylene (PTFE), and polyvinyl chloride (PVC) filters are also suitable.
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 0.1 mL to 5 mL of eluent per minute at a pressure of from 3.4
to 34 MPa (500 to 5000 psi).3.4 MPa to 34 MPa (500 psi 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, 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 between 10 mL 10 mL and 2000 mL.
D4856 − 23
7.3.2 One-mark Pipets, complying with the requirements of ISO 648.ISO 648; or Piston-Operated Volumetric Pipettors and
Dispensers, complying with the requirements of Specification E1154.
7.3.3 Disposable Screw-cap Polyethylene Vessels, of 15-mL15 mL capacity.
7.3.4 Disposable Filters, polytetrafluorethylene (PTFE), pore size 0.250.45 μm, for use in ion chromatography.
7.3.5 Disposable 2-mL or 5-mL2 mL or 5 mL Syringes, with Luer lock connector, for
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