ASTM D4856-99(2004)
(Test Method)Standard Test Method for Determination of Sulfuric Acid Mist in the Workplace Atmosphere (Ion Chromatographic)
Standard Test Method for Determination of Sulfuric Acid Mist in the Workplace Atmosphere (Ion Chromatographic)
SIGNIFICANCE AND USE
Sulfuric acid is used in the manufacture of fertilizer, explosives, dyestuffs, other acids, parchment paper, glue, and the pickling of metal.
This test method has been found satisfactory for measuring sulfuric acid at levels required by federal occupational health regulations.
SCOPE
1.1 This ion chromatographic test method describes the determination of sulfuric acid mist in air samples collected from workplace atmospheres in a three-piece cassette filter.
1.2 The lower detection limit of this test method is 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 relatively free from interference. The only known interference is soluble or partially soluble sulfate salts.
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 .
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D4856–99 (Reapproved 2004)
Standard Test Method for
Determination of Sulfuric Acid Mist in the Workplace
Atmosphere (Ion Chromatographic)
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 E200 Practice for Preparation, Standardization, and Storage
of Standard and Reagent Solutions for Chemical Analysis
1.1 This ion chromatographic test method describes the
determination of sulfuric acid mist in air samples collected
3. Terminology
from workplace atmospheres in a three-piece cassette filter.
3.1 Definitions—For definitions of terms used in this test
1.2 The lower detection limit of this test method is 0.017
method, refer to Terminology D1356.
mg/m of sulfuric acid (H SO ) mist in 60 Lof air sampled at
2 4
3.2 Definitions of Terms Specific to This Standard:
1 L/min.
3.2.1 eluent—ionic mobile phase used to transport the
1.3 Thistestmethodisrelativelyfreefrominterference.The
sample through the exchange columns.
only known interference is soluble or partially soluble sulfate
3.2.2 resolution—ability of a column to separate constitu-
salts.
ents under specified test conditions.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4. Summary of Test Method
responsibility of the user of this standard to establish appro-
4.1 Aknownvolumeofairisdrawnthroughacassettefilter
priate safety and health practices and determine the applica-
holder containing a 37-mm mixed cellulose ester membrane
bility of regulatory limitations prior to use. For specific
filterof0.8-µmporesize.Thefilterisheldina3-piececassette
precautionary statements, see Section 9.
supported by a cellulose back-up pad.
4.2 The filter is desorbed with Specification D1193 Type 1
2. Referenced Documents
water and an aliquot of the desorbed sample is injected into an
2.1 ASTM Standards:
ion chromatograph. The sample is pumped through two differ-
D1193 Specification for Reagent Water
ent ion exchange columns into a conductivity detector. Those
D1356 Terminology Relating to Sampling and Analysis of
columns are a precolumn and separator column which are
Atmospheres
packed with low-capacity anion exchanger. Ions are separated
D1357 Practice for Planning the Sampling of the Ambient
based on their affinity for the exchange sites of the resin. A
Atmosphere
method for anion suppression is used to reduce background
D1605 Practices for SamplingAtmospheres forAnalysis of
3 conductivity of the eluent.
Gases and Vapors
D1914 Practice for Conversion Units and Factors Relating
5. Significance and Use
to Sampling and Analysis of Atmospheres
5.1 Sulfuric acid is used in the manufacture of fertilizer,
D4327 Test Method for Anions in Water by Chemically
explosives, dyestuffs, other acids, parchment paper, glue, and
Suppressed Ion Chromatography
the pickling of metal.
5.2 This test method has been found satisfactory for mea-
suring sulfuric acid at levels required by federal occupational
This test method is under the jurisdiction of ASTM Committee D22 on
SamplingAnalysis ofAtmospheres and is the direct responsibility of Subcommittee
health regulations.
D22.04 on Workplace Atmospheres.
CurrenteditionapprovedOctober1,2004.PublishedDecember2004.Originally
6. Interferences
´1
approved in 1988. Last previous edition approved in 1999 as D4856-99 . DOI:
6.1 Soluble or partially soluble sulfate salts, for example,
10.1520/D4856-99R04.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
sodium or calcium sulfate, will constitute a positive bias.
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. Precision (CV =0.082) was obtained from NIOSH Contract No. CDC-99-
T
3 3
Withdrawn. 74-45 on a range of 0.561−2.577 mg/M using cellulose ester filters.
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D4856–99 (2004)
7. Apparatus (spgr1.84)to600mLofwater.Coolthesolutionanddiluteto
4 L with water. Some anion suppressor membranes use the
7.1 Sampling Equipment:
effluent from the detector. See manufacturer’s guidance for
7.1.1 A3-piece 37-mm filter cassette constructed of styrene
appropriate use.
acrylonitrile is used to hold the filter that is supported by a
8.6 Anion Working Solutions—Prepare a blank and a mini-
cellulosic pad. The cassette has polyethylene end plugs that fit
mum of three different working solutions containing the
into an inlet and outlet sampling orifice.
following concentrations of sulfate. The sulfate solutions are
7.1.2 The filter that is used in this procedure is a 37-mm
prepared by diluting the stock solution.
diametercelluloseestermembranefilterofa0.8-mmporesize.
8.6.1 High sulfate stock concentration (100 mg/L) is pre-
7.1.3 A portable sampling pump capable of a 1 L/min
pared by the dilution of 100 mLof the sulfate stock solution to
sampling rate with a filter cassette containing a backing pad
1 000 mL in a volumetric flask with water.
and cellulose ester membrane filter previously described.
8.6.2 Intermediate sulfate stock concentration (10 mg/L) is
7.2 Ion Chromatograph—capableofdelivering2to5mLof
prepared by the dilution of 100 mL of the high stock sulfate
eluent per minute at a pressure of from 200 to 700 psi [1.3 to
concentration to 1 000 mL in a volumetric flask with water.
4.8 MPa].
8.6.3 Low sulfate stock concentration (1 mg/L) is prepared
7.2.1 Precolumn—a column placed before the separator
by diluting 100 mL of the intermediate stock sulfate concen-
column to protect it from being fouled by particulate matter.
tration to 1 000 mL in a volumetric flask with water.
7.2.2 Separator Column—a column packed with pellicular
anion exchange resin that is suitable for resolving the sulfate
9. Precautions
anion.
9.1 Safety Precautions—Extreme care must be taken when
7.2.3 Suppressor Column or Membrane—a column packed
preparing solutions from concentrated sulfuric acid. Th
...
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