ASTM D4658-03

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Designation: D 4658 – 03
Standard Test Method for
1
Sulfide Ion in Water
This standard is issued under the fixed designation D4658; 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.
1. Scope* 3. Terminology
1.1 This test method uses an ion-selective electrode to 3.1 Definitions: For definitions of terms used in this test
determine sulfide ion in water.The test method is applicable in method, refer to Terminology D1129.
the range from 0.04 to 4000 mg/L of sulfide. 3.2 Definitions of Terms Specific to This Standard:
1.2 Precision data presented in this test method were ob- 3.2.1 For definitions of terms specific to this test method,
tainedusingreagentwateronly.Itistheuser’sresponsibilityto refer to Terminology D4127.
ensure the validity of this test method for untested types of
4. Summary of Test Method
water.
4.1 Sulfide ion is measured potentiometrically using a
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the sulfide ion-selective electrode in conjunction with a double-
junction sleeve type reference electrode. Potentials are read
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- usingapHmeterhavinganexpandedmillivoltscalecapableof
beingreadtothenearest0.1mV,oraspecificionmeterhaving
bility of regulatory limitations prior to use. Sulfide samples,
when acidified, can release highly toxic hydrogen sulfide gas. a direct concentration scale for sulfide ion.
4.2 Samples are treated prior to analysis with sulfide anti-
For a specific precautionary statement, see Note 2.
oxidant buffer (SAOB). This buffer fixes the solution pH at a
2. Referenced Documents
highly alkaline level and contains ascorbic acid to retard air
2.1 ASTM Standards: oxidationofsulfideioninsolution.Thisensuresthatthesulfide
2 2−
D1129 Terminology Relating to Water present occurs chiefly as S ion rather than as complexed
1−
2
D1193 Specification for Reagent Water HS or H S that are present at lower pH values.
2
D2777 Practice for Determination of Precision and Bias of
2 5. Significance and Use
Applicable Test Methods of Committee D-19 on Water
5.1 Sulfide ion is found in ground waters and wastewater,
D3370 Practices for Sampling Water from Closed Con-
2
duits causing odor and corrosion problems. If acidified, these waters
2
can release hydrogen sulfide, which is extremely toxic even at
D4127 Terminology Used with Ion-Selective Electrodes
2
D5810 Guide for Spiking into Aqueous Samples lowlevels.Thistestmethodprovidesameansforinterference-
free measurement of free sulfide ion.
D5847 Practice for the Writing Quality Control Specifica-
2
tions for Standard Test Methods for Water Analysis
1−
NOTE 1—Sulfide forms complexes with hydrogen ions (HS and
H S). In addition, sulfide ion forms soluble complexes with elemental
2
2− 2− 2−
sulfur (S ,S ,S , etc.), tin, antimony, and arsenic ions.
2 3 4
1
This test method is under the jurisdiction of ASTM Committee D19 on Water
6. Apparatus
andarethedirectresponsibilityofSubcommitteeD19.05onInorganicConstituents
in Water.
6.1 pH Meter, with expanded millivolt scale, or a specific
Current edition approved Jan. 10, 2003. Published January 2003. Originally
ion meter having a direct concentration scale for sulfide ion.
approved in 1987. Last previous edition approved in 1996 as D4658–92 (1996).
2
Annual Book of ASTM Standards, Vol 11.01. 6.2 Sulfide Ion-Selective Electrode.
*A Summary of Changes section appears at the end of this standard.
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D4658–03
NOTE 3—Freshly prepared SAOB, when stored in a tightly stoppered
6.3 Reference Electrode, double-junction sleeve type with
bottle, has a shelf life of approximately two weeks, if opened frequently.
1.0 M potassium nitrate solution, pH adjusted to 13.5 with 1.0
When oxidized, the solution turns dark brown and should be discarded.
M sodium hydroxide in the outer sleeve.
7.7 Zinc Acetate Solution (2.0 M)—Dissolve 43.90 g of
7. Reagents
zinc acetate [Zn(C H O ) ·2H O] in water, using a 100 mL
2 3 2 2 2
7.1 Purity of Reagents—Reagent grade chemicals shall be
volumetric flask, and dilute to 100 mL with water.
used in all tests. Unless otherwise indicated, it is intended that
8. Sampling and Storage
all reagents shall conform to the specifications of the Commit-
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teeonAnalyticalReagentsoftheAmericanChemicalSociety.
8.1 Collect samples in accordance with Practices D3370.
Other grades may be used
...