ASTM D4856-99e1

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D4856–99
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 (e) indicates an editorial change since the last revision or reapproval.
e NOTE—Paragraph 8.5 was corrected editorially in June 1999.
1. Scope Suppressed Ion Chromatography
E200 Practice for Preparation, Standardization, and Stor-
1.1 This ion chromatographic test method describes the
age of Standard and Reagent Solutions for Chemical
determination of sulfuric acid mist in air samples collected
Analysis
from workplace atmospheres in a three-piece cassette filter.
1.2 The lower detection limit of this test method is 0.017
3. Terminology
mg/m of sulfuric acid (H SO ) mist in 60 L of air sampled at
2 4
3.1 Definitions—For definitions of terms used in this test
1 L/min.
method, refer to Terminology D1356.
1.3 Thistestmethodisrelativelyfreefrominterference.The
3.2 Definitions of Terms Specific to This Standard:
only known interference is soluble or partially soluble sulfate
3.2.1 eluent—ionic mobile phase used to transport the
salts.
sample through the exchange columns.
1.4 This standard does not purport to address all of the
3.2.2 resolution—ability of a column to separate constitu-
safety concerns, if any, associated with its use. It is the
ents under specified test conditions.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
4. Summary of Test Method
bility of regulatory limitations prior to use. For specific
4.1 Aknownvolumeofairisdrawnthroughacassettefilter
precautionary statements, see Section 9.
holder containing a 37-mm mixed cellulose ester membrane
filterof0.8-µmporesize.Thefilterisheldina3-piececassette
2. Referenced Documents
supported by a cellulose back-up pad.
2.1 ASTM Standards:
2 4.2 The filter is desorbed with Specification D 1193 Type 1
D1193 Specification for Reagent Water
water and an aliquot of the desorbed sample is injected into an
D1356 Terminology Relating to Sampling and Analysis of
3 ion chromatograph. The sample is pumped through two differ-
Atmospheres
ent ion exchange columns into a conductivity detector. Those
D1357 Practice for Planning the Sampling of the Ambient
3 columns are a precolumn and separator column which are
Atmosphere
packed with low-capacity anion exchanger. Ions are separated
D1605 PracticesforSamplingAtmospheresforAnalysisof
4 based on their affinity for the exchange sites of the resin. A
Gases and Vapors
method for anion suppression is used to reduce background
D1914 Practice for Conversion Units and Factors Relating
3 conductivity of the eluent.
to Sampling and Analysis of Atmospheres
D4327 Test Method for Anions in Water by Chemically
5. Significance and Use
5.1 Sulfuric acid is used in the manufacture of fertilizer,
explosives, dyestuffs, other acids, parchment paper, glue, and
This test method is under the jurisdiction of ASTM Committee D22 on
the pickling of metal.
SamplingAnalysis ofAtmospheres and is the direct responsibility of Subcommittee
D22.04 on Workplace Atmospheres.
Current edition approved March 10, 1999. Published May 1999. Originaly
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published as D4856 - 88. Last previous edition D4856 - 88 (1993) .
2 5
Annual Book of ASTM Standards, Vol 11.01. Annual Book of ASTM Standards, Vol 15.05.
3 6
Annual Book of ASTM Standards, Vol 11.03. Precision (CV =0.082) was obtained from NIOSH Contract No. CDC-99-
T
4 3
Discontinued—See 1991 Annual Book of ASTM Standards, Vol 11.03. 74-45 on a range of 0.561−2.577 mg/M using cellulose ester filters.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D4856–99
−2
5.2 This test method has been found satisfactory for mea- 8.4.1 Sulfate Stock Solution (1.00 mL=1.00 mg SO )
suring sulfuric acid at levels required by federal occupational Dry sodium sulfate (Na SO ) for 1 h at 105°C and cool in
2 4
health regulations. dessicator. Dissolve 1.4790 g of dried salt in water and dilute
to 1 L with water.
8.5 Suppressor Regenerant Solution (for use with suppres-
6. Interferences
sor columns)—Cautiouslyadd111mLofconcentratedH SO
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6.1 Soluble or partially soluble sulfate salts, for example,
(spgr1.84)to600mLofwater.Coolthesolutionanddiluteto
sodium or calcium sulfate, will constitute a positive bias.
4 L with water. Some anion suppressor membranes use the
effluent from the detector. See manufacturer’s guidance for
7. Apparatus
appropriate use.
7.1 Sampling Equipment:
8.6 Anion Working Solutions—Prepare a blank and a mini-
7.1.1 A3-piece 37-mm filter cassette constructed of styrene
mum of three different working solutions containing the
acrylonitrile is used to hold the filter that is supported by a
following concentrations of sulfate. The sulfate solutions are
cellulosic pad. The cassette has polyethylene end plugs that fit
prepared by diluting the stock solution.
into an inlet and outlet sampling orifice.
8.6.1 High sulfate stock concentration (100 mg/L) is pre-
7.1.2 The filter that is used in this procedure is a 37-mm
pared by the dilution of 100 mLof the sulfate stock solution to
diametercelluloseestermembranefilterofa0.8-mmporesize.
1 000 ml in a volumetric flask with water.
7.1.3 A portable sampling pump capable of a 1 L/min
8.6.2 Intermediate sulfate stock concentration (10 mg/L) is
sampling rate with a filter cassette containing a backing pad
prepared by the dilution of 100 ml of the high stock sulfate
and cellulose ester membrane filter previously described.
concentration to 1 000 mL in a volumetric flask with water.
7.2 Ion Chromatograph—capableofdelivering2to5mLof
8.6.3 Low sulfate stock concentration (1 mg/L) is prepared
eluent per minute at a pressure of from 200 to 700 psi (1.3 to by diluting 100 ml of the intermediate stock sulfate concen-
4.8 MPa).
tration to 1 000 mL in a volumetric flask with water.
7.2.1 Precolumn—a column placed before the separator
9. Precautions
colum
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