ASTM D4658-92(1996)
(Test Method)Standard Test Method for Sulfide Ion in Water
Standard Test Method for Sulfide Ion in Water
SCOPE
1.1 This test method uses an ion-selective electrode to determine sulfide ion in water. The test method is applicable in the range from 0.04 to 4000 mg/L of sulfide.
1.2 Precision data presented in this test method were obtained using reagent water only. It is the user's responsibility to ensure the validity of this test method for untested types of water.
1.3 This standard does not purport to address all of the safety problems, 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 limits prior to use. Sulfide samples, when acidified, can release highly toxic hydrogen sulfide (H2S) gas. For a specific precautionary statement, see Note 2.
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or
withdrawn.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: D 4658 – 92 (Reapproved 1996)
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Sulfide Ion in Water
This standard is issued under the fixed designation D 4658; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 4.2 Samples are treated prior to analysis with sulfide anti-
oxidant buffer (SAOB). This buffer fixes the solution pH at a
1.1 This test method uses an ion-selective electrode to
highly alkaline level and contains ascorbic acid to retard air
determine sulfide ion in water. The test method is applicable in
oxidation of sulfide ion in solution. This ensures that the sulfide
the range from 0.04 to 4000 mg/L of sulfide.
present occurs chiefly as S ion rather than as complexed
1.2 Precision data presented in this test method were ob-
−
HS or H S that are present at lower pH values.
tained using reagent water only. It is the user’s responsibility to
ensure the validity of this test method for untested types of
5. Significance and Use
water.
5.1 Sulfide ion is found in ground waters and wastewater,
1.3 This standard does not purport to address all of the
causing odor and corrosion problems. If acidified, these waters
safety concerns, if any, associated with its use. It is the
can release hydrogen sulfide, which is extremely toxic even at
responsibility of the user of this standard to establish appro-
low levels. This test method provides a means for interference-
priate safety and health practices and determine the applica-
free measurement of free sulfide ion.
bility of regulatory limitations prior to use. Sulfide samples,
when acidified, can release highly toxic hydrogen sulfide gas. −
NOTE 1—Sulfide forms complexes with hydrogen ions (HS and H S).
For a specific precautionary statement, see Note 2.
In addition, sulfide ion forms soluble complexes with elemental sulfur
5 5 5
(S ,S ,S , etc.), tin, antimony, and arsenic ions.
2 3 4
2. Referenced Documents
6. Apparatus
2.1 ASTM Standards:
D 1129 Terminology Relating to Water
6.1 pH Meter, with expanded millivolt scale, or a specific
D 1193 Specification for Reagent Water
ion meter having a direct concentration scale for sulfide ion.
D 2777 Practice for Determination of Precision and Bias of
6.2 Sulfide Ion-Selective Electrode.
Applicable Test Methods of Committee D-19 on Water
6.3 Reference Electrode, double-junction sleeve type
D 3370 Practices for Sampling Water from Closed Con-
with 1.0 M potassium nitrate solution, pH adjusted to 13.5 with
duits
1.0 M sodium hydroxide in the outer sleeve.
D 4127 Terminology Used with Ion-Selective Electrodes
7. Reagents
3. Terminology
7.1 Purity of Reagents—Reagent grade chemicals shall be
3.1 Definitions: For definitions of terms used in this test
used in all tests. Unless otherwise indicated, it is intended that
method, refer to Terminology D 1129.
all reagents shall conform to the specifications of the Commit-
3.2 Definitions of Terms Specific to This Standard:
tee on Analytical Reagents of the American Chemical Society.
3.2.1 For definitions of terms specific to this test method,
Other grades may be used, provided it is first ascertained that
refer to Terminology D 4127.
the reagent is of sufficiently high purity to permit its use
4. Summary of Test Method
without lessening the accuracy of the determination.
4.1 Sulfide ion is measured potentiometrically using a 7.2 Purity of Water—Unless otherwise indicated, references
sulfide ion-selective electrode in conjunction with a double- to water shall be understood to mean reagent water conforming
junction sleeve type reference electrode. Potentials are read to Specification D 1193, Type III.
7.3 Cadmium Nitrate Solution (0.1 M)—Place 12.84 g of
using a pH meter having an expanded millivolt scale capable of
being read to the nearest 0.1 mV, or a specific ion meter having cadmium oxide into a 125-mL beaker. Add 12 to 14 mL of
concentrated nitric acid (sp gr 1.42), stir with a glass stirring
a direct concentration scale for sulfide ion.
1 3
This test method is under the jurisdiction of ASTM Committee D-19 on Water Reagent Chemicals, American Chemical Society Specifications, American
and are the direct responsibility of Subcommittee D 19.05 on Inorganic Constituents Chemical Society, Washington, DC. For suggestions on the testing of reagents not
in Water. listed by the American Chemical Society, see Analar Standards for Laboratory
Current edition approved May 15, 1992. Published September 1992. Originally Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
published as D 4658 – 87. Last previous edition D 4658 – 87. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 11.01. MD.
NOTICE:¬This¬standard¬has¬either¬been¬superseded¬and¬replaced¬by¬a¬new¬version¬or
discontinued.¬Contact¬ASTM¬International¬(www.astm.org)¬for¬the¬latest¬information.¬
D 4658
rod, and add about 10 mL of water. Stir thoroughly, add an tion, 45 mL of SAOB (use a graduated cylinder), and dilute to
additional 40 to 50 mL of water, washing off the glass stirring 100 mL with water.
rod with part of the water. Transfer to a 1-L volumetric flask 9.1.2 Standard B—1.00 mL of sodium sulfide stock solu-
and dilute to 1000 mL with water. tion, 50 mL of SAOB (use a graduated cylinder), and dilute to
7.4 Lead Perchlorate Solution (0.1 M)—Commercially 100 mL with water.
available. Alternatively, it can be prepared using lead perchlo- 9.1.3 Standard C—2.00 mL of calibration standard A,50
rate and water. Dissolve 46.02 g of the salt in water using a 1-L mL of SAOB (use a graduated cylinder), and dilute to 100 mL
volumetric flask and dilute to 1000 mL with water. with water.
7.5 Sodium Sulfide Solution, Stock—Prepare sodium sulfide 9.1.4 Standard D—1.00 mL of calibration standard A,50
stock solution from sodium sulfide hydrate (Na ·9H O). mL of SAOB (use a graduated cylinder), and dilute to 100 mL
2 2
with water.
NOTE 2—Warning: All sulfide solution preparation and measurement
9.2 The concentrations of the calibration standards, in
must be performed in a hood to avoid breathing noxious fumes.
milligrams per litre, are calculated from the concentration, S,of
7.5.1 Precise standards cannot be prepared by weighing the
the sodium sulfide stock solution as determined by titration:
salt because of the large and variable water of hydration.
A 5 0.05S
Instead, prepare a saturated sodium sulfide solution by adding
B 5 0.01S
approximately 100 g of the Na S·9H O to approximately 100
2 2
C 5 0.001S
mL of water, shake well, stopper securely, and allow it to stand,
D 5 0.0005S
at least overnight.
9.3 Prepare a calibration curve by immersing the electrode
7.5.2 To prepare the sodium sulfide stock solution, pipet 1
pair in each of the calibration standards, beginning with the
mL of the saturated solution described above into 50 mL of
most dilute, and record the stable electrode potential millivolt
SAOB (7.6), and dilute to 100 mL with water.
reading developed in each. Construct
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