ASTM: D4658: Sulfide in Water

Summary
Analytes
Revision
Data and Sites

Official Method Name

Standard Test Method for Sulfide Ion in Water

Current Revision

1992

Media

WATER

Instrumentation

Ion Selective Electrode

Method Subcategory

Inorganic

Method Source

ASTM

Citation

Annual Book of ASTM Standards, Section 11, Water and Environmental Technology, Volume 11.02, Water (I)

Brief Method Summary

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.

Scope and Application

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. 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.

Applicable Concentration Range

0.04 - 4000 mg/L

Interferences

Samples are treated prior to analysis with sulfide antioxidant buffer (SAOB). This buffer fixes the solution pH at a highly alkaline level and contains ascorbic acid to retard air oxidation of sulfide ion in solution. This ensures that the sulfide present occurs chiefly as S = ion rather than as complexed HS- or H2S that are present at lower pH values.

Quality Control Requirements

Sample Handling

Collect samples in accordance with Practices D 3370. Samples should be taken with a minimum of aeration to avoid air oxidation of sulfide or loss of volatile hydrogen sulfide from the sample. Preserve samples by adding 0.2 mL (4 drops) of 2 M zinc acetate (equivalent to 128 mg/L S^2- ) and 0.05 mL (1 drop) of 6 M sodium hydroxide to a 100-mL bottle. Fill the bottle completely with the sample and stopper it. There should be no air bubbles trapped under the stopper. If the concentration of sulfide is greater than approximately 100 mg/L, the amounts of both reagents should be increased. Sulfide in samples that have been "preserved" with zinc acetate can be determined without special treatment, since SAOB contains EDTA to redissolve the zinc and free the sulfide. The entire sample is used for analysis, and since the results will be given in milligrams sulfide per litre, the sample volume must be known.

Maximum Holding Time

Relative Cost

Unknown

Sample Preparation Methods

This method has 1 analyte associated with it.

Analyte	Detection Level	Bias	Precision	Pct False Positive	Pct False Negative	Spiking Level
Sulfide(18496-25-8) Sulfide	0.040 mg/L	N/A	1.50 % RSD (ML)

Precision Descriptor Notes:	On each of three days, operators in each of six laboratories standardized a sodium sulfide stock solution as described in Section 10. Full calibration, using four standards prepared by dilution of the standardized stock solution, was carried out five times on each day by each operator, and the potential values were recorded. The five replicates at each level were averaged and standard deviations were calculated. By averaging the standard deviation values in segments of the concentration range, Table 1 was developed. Since the sodium sulfide stock solutions varied from day to day, this approach was chosen to provide the most useful information. The data show the average standard deviation in millivolts (from which concentration variations may be calculated) that an average user may expect at the concentrations indicated.
Detection Level Note:	None.

Precision Descriptor Notes:

On each of three days, operators in each of six laboratories standardized a sodium sulfide stock solution as described in Section 10. Full calibration, using four standards prepared by dilution of the standardized stock solution, was carried out five times on each day by each operator, and the potential values were recorded. The five replicates at each level were averaged and standard deviations were calculated. By averaging the standard deviation values in segments of the concentration range, Table 1 was developed. Since the sodium sulfide stock solutions varied from day to day, this approach was chosen to provide the most useful information. The data show the average standard deviation in millivolts (from which concentration variations may be calculated) that an average user may expect at the concentrations indicated.

Detection Level Note:

None.

Revision	PDF/Link
1992

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ASTM: D4658: Sulfide in Water

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