ASTM D4658-08
(Test Method)Standard Test Method for Sulfide Ion in Water
Standard Test Method for Sulfide Ion in Water
SIGNIFICANCE AND USE
Sulfide ion is found in ground waters and wastewater, causing odor and corrosion problems. If acidified, these waters can release hydrogen sulfide, which is extremely toxic even at low levels. This test method provides a means for interference-free measurement of free sulfide ion.
Note 1—Sulfide forms complexes with hydrogen ions (HS1− and H2S). In addition, sulfide ion forms soluble complexes with elemental sulfur (S22−, S32−, S42−, etc.), tin, antimony, and arsenic ions.
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 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 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. Sulfide samples, when acidified, can release highly toxic hydrogen sulfide gas. For a specific precautionary statement, see Note 2.
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Designation: D 4658 – 08
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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope D5847 Practice for Writing Quality Control Specifications
for Standard Test Methods for Water Analysis
1.1 This test method uses an ion-selective electrode to
determinesulfideioninwater.Thetestmethodisapplicablein
3. Terminology
the range from 0.04 to 4000 mg/L of sulfide.
3.1 Definitions: For definitions of terms used in this test
1.2 Precision data presented in this test method were ob-
method, refer to Terminology D1129.
tainedusingreagentwateronly.Itistheuser’sresponsibilityto
3.2 Definitions of Terms Specific to This Standard:
ensure the validity of this test method for untested types of
3.2.1 For definitions of terms specific to this test method,
water.
refer to Terminology D4127.
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
4. Summary of Test Method
standard.
4.1 Sulfide ion is measured potentiometrically using a
1.4 This standard does not purport to address all of the
sulfide ion-selective electrode in conjunction with a double-
safety concerns, if any, associated with its use. It is the
junction sleeve type reference electrode. Potentials are read
responsibility of the user of this standard to establish appro-
usingapHmeterhavinganexpandedmillivoltscalecapableof
priate safety and health practices and determine the applica-
beingreadtothenearest0.1mV,oraspecificionmeterhaving
bility of regulatory limitations prior to use. Sulfide samples,
a direct concentration scale for sulfide ion.
when acidified, can release highly toxic hydrogen sulfide gas.
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
highly alkaline level and contains ascorbic acid to retard air
2. Referenced Documents
2
oxidationofsulfideioninsolution.Thisensuresthatthesulfide
2.1 ASTM Standards:
2−
present occurs chiefly as S ion rather than as complexed
D1129 Terminology Relating to Water
1−
HS or H S that are present at lower pH values.
2
D1193 Specification for Reagent Water
D2777 Practice for Determination of Precision and Bias of
5. Significance and Use
Applicable Test Methods of Committee D19 on Water
5.1 Sulfide ion is found in ground waters and wastewater,
D3370 PracticesforSamplingWaterfromClosedConduits
causing odor and corrosion problems. If acidified, these waters
D4127 Terminology Used with Ion-Selective Electrodes
can release hydrogen sulfide, which is extremely toxic even at
D5810 Guide for Spiking into Aqueous Samples
lowlevels.Thistestmethodprovidesameansforinterference-
free measurement of free sulfide ion.
1−
NOTE 1—Sulfideformscomplexeswithhydrogenions(HS andH S).
1
2
This test method is under the jurisdiction ofASTM Committee D19 on Water
In addition, sulfide ion forms soluble complexes with elemental sulfur
andarethedirectresponsibilityofSubcommitteeD19.05onInorganicConstituents
2− 2− 2−
(S ,S ,S , etc.), tin, antimony, and arsenic ions.
in Water. 2 3 4
Current edition approved Aug. 15, 2008. Published August 2008. Originally
6. Apparatus
approved in 1987. Last previous edition approved in 2003 as D4658–03.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
6.1 pH Meter, with expanded millivolt scale, or a specific
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
ion meter having a direct concentration scale for sulfide ion.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. 6.2 Sulfide Ion-Selective Electrode.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
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D4658–08
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 a
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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:D4658–03 Designation: D 4658 – 08
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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope *
1.1 Thistestmethodusesanion-selectiveelectrodetodeterminesulfideioninwater.Thetestmethodisapplicableintherange
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
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 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.Sulfidesamples,whenacidified,canreleasehighlytoxichydrogensulfidegas.Foraspecificprecautionary
statement, see Note 2.
2. Referenced Documents
2
2.1 ASTM Standards:
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
D2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D-19D19 on Water
D3370 Practices for Sampling Water from Closed Conduits
D4127 Terminology Used with Ion-Selective Electrodes
D5810 Guide for Spiking into Aqueous Samples
D5847 Practice for the Writing Quality Control Specifications for Standard Test Methods for Water Analysis
3. Terminology
3.1 Definitions: For definitions of terms used in this test method, refer to Terminology D1129.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 For definitions of terms specific to this test method, refer to Terminology D4127.
4. Summary of Test Method
4.1 Sulfide ion is measured potentiometrically using a sulfide ion-selective electrode in conjunction with a double-junction
sleeve type reference electrode. Potentials are read 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 a direct concentration scale for sulfide ion.
4.2 Samples are treated prior to analysis with sulfide antioxidant buffer (SAOB). This buffer fixes the solution pH at a highly
alkalinelevelandcontainsascorbicacidtoretardairoxidationofsulfideioninsolution.Thisensuresthatthesulfidepresentoccurs
2− 1−
chiefly as S ion rather than as complexed HS or H S that are present at lower pH values.
2
5. Significance and Use
5.1 Sulfide ion is found in ground waters and wastewater, causing odor and corrosion problems. If acidified, these waters can
release hydrogen sulfide, which is extremely toxic even at low levels. This test method provides a means for interference-free
measurement of free sulfide ion.
1
This test method is under the jurisdiction of ASTM Committee D19 on Water and are the direct responsibility of Subcommittee D19.05 on Inorganic Constituents in
Water.
Current edition approved Jan. 10, 2003.Aug. 15, 2008. Published January 2003.August 2008. Originally approved in 1987. Last previous edition approved in 19962003
as D4658–92 (1996).D4658–03.
2
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@astm.org.For Annual Book of ASTM Standards
, Vol 11.01.volume information, refer to the standard’s Document Summary page on the ASTM website.
*A Summary of Changes section appears at the end of this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
D4658–08
1− 2−
NOTE 1—Sulfide forms complexes with hydrogen ions (HS and H S). In addition, sulfide ion forms soluble complexes with elemental sulfur (S ,
2 2
2− 2−
S ,S , etc.), tin, antimony, and arsenic ions.
3 4
6. Apparatus
6.1 pH Meter, with expanded millivolt scale, or a specific ion meter having a direct concentration scale for sulfide ion.
6.2 Sulfide Ion-Selective Electrode .
6.3 Reference Electrode, double-junction sleeve type with 1.0 M potassium nitrate solution, pH adjusted to 13.5 with 1.0 M
sodium hydroxide in the outer sleeve.
7. Reagents
7.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests.
...
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