ASTM D3558-15(2023)
(Test Method)Standard Test Methods for Cobalt in Water
Standard Test Methods for Cobalt in Water
SIGNIFICANCE AND USE
4.1 Most waters rarely contain more than trace concentrations of cobalt from natural sources. Although trace amounts of cobalt seem to be essential to the nutrition of some animals, large amounts have pronounced toxic effects on both plant and animal life.
SCOPE
1.1 These test methods cover the determination of dissolved and total recoverable cobalt in water and wastewater 2 by atomic absorption spectrophotometry. Three test methods are included as follows:
Concentration Range
Sections
Test Method A—Atomic Absorption, Direct
0.1 mg/L to 10 mg/L
7 to 16
Test Method B—Atomic Absorption, Chelation-Extraction
10 μg/L to 1000 μg/L
17 to 26
Test Method C—Atomic Absorption, Graphite Furnace
5 μg/L to 100 μg/L
27 to 36
1.2 Test Method A has been used successfully with reagent water, potable water, river water, and wastewater. Test Method B has been used successfully with reagent water, potable water, river water, sea water and brine. Test Method C was successfully evaluated in reagent water, artificial seawater, river water, tap water, and a synthetic brine. It is the analyst's responsibility to ensure the validity of these test methods for other matrices.
1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses are mathematical conversions to inch-pound units that are provided for information only and are not considered 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see 11.8.1, 21.12, and 23.10.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
Relations
Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D3558 − 15 (Reapproved 2023)
Standard Test Methods for
Cobalt in Water
This standard is issued under the fixed designation D3558; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
2.1 ASTM Standards:
1.1 These test methods cover the determination of dissolved
D858 Test Methods for Manganese in Water
and total recoverable cobalt in water and wastewater by
D1066 Practice for Sampling Steam
atomic absorption spectrophotometry. Three test methods are
D1068 Test Methods for Iron in Water
included as follows:
D1129 Terminology Relating to Water
Concentration Range Sections
Test Method A—Atomic Absorption, 0.1 mg ⁄L to 10 mg ⁄L 7 to 16 D1193 Specification for Reagent Water
Direct
D1687 Test Methods for Chromium in Water
Test Method B—Atomic Absorption, 10 μg ⁄L to 1000 μg ⁄L 17 to 26
D1688 Test Methods for Copper in Water
Chelation-Extraction
D1691 Test Methods for Zinc in Water
Test Method C—Atomic Absorption, 5 μg ⁄L to 100 μg/L 27 to 36
Graphite Furnace
D1886 Test Methods for Nickel in Water
D2777 Practice for Determination of Precision and Bias of
1.2 Test Method A has been used successfully with reagent
Applicable Test Methods of Committee D19 on Water
water, potable water, river water, and wastewater. Test Method
D3370 Practices for Sampling Water from Flowing Process
B has been used successfully with reagent water, potable water,
Streams
river water, sea water and brine. Test Method C was success-
D3557 Test Methods for Cadmium in Water
fully evaluated in reagent water, artificial seawater, river water,
D3559 Test Methods for Lead in Water
tap water, and a synthetic brine. It is the analyst’s responsibility
D3919 Practice for Measuring Trace Elements in Water by
to ensure the validity of these test methods for other matrices.
Graphite Furnace Atomic Absorption Spectrophotometry
1.3 The values stated in SI units are to be regarded as
D4841 Practice for Estimation of Holding Time for Water
standard. The values given in parentheses are mathematical
Samples Containing Organic and Inorganic Constituents
conversions to inch-pound units that are provided for informa-
D5673 Test Method for Elements in Water by Inductively
tion only and are not considered standard.
Coupled Plasma—Mass Spectrometry
1.4 This standard does not purport to address all of the D5810 Guide for Spiking into Aqueous Samples
safety concerns, if any, associated with its use. It is the D5847 Practice for Writing Quality Control Specifications
responsibility of the user of this standard to establish appro- for Standard Test Methods for Water Analysis
priate safety, health, and environmental practices and deter-
3. Terminology
mine the applicability of regulatory limitations prior to use.
For specific hazard statements, see 11.8.1, 21.12, and 23.10.
3.1 Definitions:
1.5 This international standard was developed in accor- 3.1.1 For definitions of terms used in these test methods,
refer to Terminology D1129.
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the 3.2 Definitions of Terms Specific to This Standard:
Development of International Standards, Guides and Recom- 3.2.1 total recoverable cobalt, n—a descriptive term relating
mendations issued by the World Trade Organization Technical to the cobalt forms recovered in the acid-digestion procedure
Barriers to Trade (TBT) Committee. specified in these test methods.
4. Significance and Use
4.1 Most waters rarely contain more than trace concentra-
These test methods are under the jurisdiction of ASTM Committee D19 on
tions of cobalt from natural sources. Although trace amounts of
Water and are the direct responsibility of Subcommittee D19.05 on Inorganic
Constituents in Water.
Current edition approved Dec. 1, 2023. Published December 2023. Originally
approved in 1977. Last previous edition approved in 2015 as D3558 – 15. DOI: For referenced ASTM standards, visit the ASTM website, www.astm.org, or
10.1520/D3558-15R23. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Platte, J. A., and March, V. M., “A New Tool for the Water Chemist,” Industrial Standards volume information, refer to the standard’s Document Summary page on
Water Engineering, May 1965. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3558 − 15 (2023)
cobalt seem to be essential to the nutrition of some animals, following hydrochloric-nitric acid digestion and filtration. The
large amounts have pronounced toxic effects on both plant and same digestion procedure may be used to determine total
animal life. recoverable nickel (Test Methods D1886), chromium (Test
Methods D1687), cadmium (Test Methods D3557), copper
5. Purity of Reagents
(Test Methods D1688), iron (Test Methods D1068), lead (Test
5.1 Reagent grade chemicals shall be used in all tests. Methods D3559), manganese (Test Methods D858), zinc (Test
Methods D1691).
Unless otherwise indicated, it is intended that all reagents shall
conform to the specifications of the Committee on Analytical
9. Interferences
Reagents of the American Chemical Society where such
9.1 Nitrate reportedly interferes at 1 mg/L by suppressing
specifications are available. Other grades may be used, pro-
the absorption of the cobalt. This interference can be elimi-
vided it is first ascertained that the reagent is of sufficiently
nated by adding 18 000 mg/L of ammonium chloride to
high purity to permit its use without lessening the accuracy of
blanks, standards, and samples.
the determination.
9.2 Other metals usually do not interfere in the determina-
5.2 Unless otherwise indicated, reference to water shall be
understood to mean reagent water conforming to Specification tion of cobalt by increasing or decreasing the amount of
absorbed radiation. The most common interference is caused
D1193, Type I. Other reagent water types may be used,
provided it is first ascertained that the water is of sufficiently by a chemical reaction in the flame that prevents conversion of
the cobalt to the atomic state.
high purity to permit its use without lessening the bias and
precision of the determination. Type II water specified at the
9.3 Sodium, potassium, and sulfate, magnesium (4500 mg/
time of the round-robin testing of this test method.
L), iron (4000 mg/L), and nickel, lead, copper, zinc, cadmium,
and chromium (10 mg/L each) do not interfere.
6. Sampling
9.4 Background correction or a chelation-extraction proce-
6.1 Collect the samples in accordance with Practices D3370
dure (see Test Method B) may be necessary to determine low
and Practice D1066, as applicable.
levels of cobalt in some water.
6.2 Preserve samples with HNO (sp gr 1.42) to a pH of 2 or
NOTE 2—Instrument manufacturers’ instructions for use of the specific
less immediately at the time of collection, normally about
correction technique should be followed.
2 mL ⁄L. If only dissolved cobalt is to be determined, filter the
sample through a 0.45 μm membrane filter before acidification. 10. Apparatus
The holding time for samples may be calculated in accordance
10.1 Atomic Absorption Spectrophotometer, for use at
with Practice D4841.
240.7 nm.
NOTE 1—Alternatively, the pH may be adjusted in the laboratory if the
NOTE 3—The manufacturer’s instructions should be followed for all
sample is returned within 14 days. However, acid must be added at least
instrumental parameters. A wavelength other than 240.7 nm may be used
24 hours before analysis to dissolve any metals that adsorb to the container
if it has been determined to be equally suitable.
walls. This could reduce hazards of working with acids in the field when
appropriate. 10.2 Cobalt Hollow-Cathode Lamps—Multielement
hollow-cathode lamps.
TEST METHOD A—ATOMIC ABSORPTION, DIRECT
10.3 Pressure-Reducing Valves—The supplies of fuel and
7. Scope
oxidant shall be maintained at pressures somewhat higher than
the controlled operating pressure of the instrument by suitable
7.1 This test method covers the determination of dissolved
valves.
and total recoverable cobalt in most waters and waste waters.
It is the user’s responsibility to ensure the validity of this test
11. Reagents and Materials
method in a particular matrix.
11.1 Cobalt Solution, Stock (1 mL = 1.0 mg Co)—
7.2 This test method is applicable in the range from
Commercially purchase or dissolve 4.0372 g of cobaltous
0.1 mg ⁄L to 10 mg ⁄L of cobalt. The range may be extended to
chloride (CoCl ·6H O) in reagent water and dilute to 1 L. A
2 2
concentrations greater than 10 mg/L by dilution of the sample.
purchased cobalt stock solution of appropriate known purity is
also acceptable.
8. Summary of Test Method
11.2 Cobalt Solution, Standard (1 mL = 0.1 mg Co)—Dilute
8.1 Cobalt is determined by atomic absorption spectropho-
100.0 mL of the stock cobalt solution to 1 L with water.
tometry. Dissolved cobalt is determined by aspirating a portion
11.3 Filter Paper—Purchase suitable filter paper. Typically
of the filtered sample directly with no pretreatment. Total
the filter papers have a pore size of 0.45 μm membrane.
recoverable cobalt is determined by aspirating the sample
Material such as fine-textured, acid-washed, ashless paper, or
glass fiber paper are acceptable. The user must first ascertain
ACS Reagent Chemicals, Specifications and Procedures for Reagents and
that the filter paper is of sufficient purity to use without
Standard-Grade Reference Materials, American Chemical Society, Washington,
DC. For suggestions on the testing of reagents not listed by the American Chemical adversely affecting the bias and precision of the test method.
Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
11.4 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
copeial Convention, Inc. (USPC), Rockville, MD. chloric acid (HCl).
D3558 − 15 (2023)
NOTE 4—If a high reagent blank is obtained, distill the HCl or use NOTE 7—For samples with high levels of suspended matter, the amount
spectrograde acid. When HCl is distilled, an azeotrophic mixture is of reduction in volume is left to the discretion of the analyst.
obtained (approximately 6 N HCl is formed). Therefore, whenever NOTE 8—Many laboratories have found block digestion systems a
concentrated HCl is specified for the preparation of a reagent or in the useful way to digest samples for trace metals analysis. Systems typically
procedure, use double the volume specified if distilled acid is used. consist of either a metal or graphite block with wells to hold digestion
tubes. The block temperature controller must be able to maintain unifor-
11.5 Nitric Acid (sp gr 1.42)—Concentrated nitric acid
mity of temperature across all positions of the block. For trace metals
(HNO ).
analysis, the digestion tubes should be constructed of polypropylene and
have a volume accuracy of at least 0.5 %. All lots of tubes should come
NOTE 5—If a high reagent blank is obtained, distill the HNO or use a
with a certificate of analysis to demonstrate suitability for their intended
spectrograde acid.
purpose.
11.6 Nitric Acid (1 + 499)—Add 1 volume of HNO (sp gr
13.4 Cool and filter the samples through a suitable filter
1.42) to 499 volumes of water.
(11.3), such as fine-texture, acid-washed, ashless paper, into
11.7 Oxidant:
100 mL volumetric flasks. Wash the filter paper two or three
11.7.1 Air, which has been passed through a suitable filter to
times with water and bring to volume.
remove oil, water, and other foreign substances is the usual
13.5 Atomize each filtered and acidified sample and deter-
oxidant.
mine its absorbance or concentration. Atomize HNO (1 + 499)
11.8 Fuel:
between samples.
11.8.1 Acetylene—Standard, commercially available acety-
14. Calculation
lene is the usual fuel. Acetone, always present in acetylene
cylinders can affect analytical results. The cylinder should be
14.1 Calculate the concentration of cobalt in the sample, in
replaced at 345 kPa (50 psi). (“Purified” grade acetylene
milligrams per litre, using an analytical curve or, alternatively,
containing a special proprietary solvent rather than acetone
read directly in concentration (see 12.4).
should not be used with poly(vinyl chloride) tubing as weak-
ening of the tubing walls can cause a potentially hazardous 15. Precision and Bias
situation.)
15.1 The single-operator and overall precision of this test
method within its designated range for eleven laboratories,
12. Standardization
which include a total of sixteen operators (at 1.0 mg ⁄L,
12.1 Prepare 100 mL each of a blank and at least four
4.0 mg ⁄L, and 8.0 mg ⁄L) analyzing each sample on three
standard solutions to bracket the expected cobalt concentration
different days varies with the quantity being tested in accor-
range of the samples to be analyzed by diluting the standard
dance with Fig. 1 and Fig. 2.
cobalt solution (see 11.2) with HNO (1 + 499). Analyze at
15.2 Recoveries of known amounts of cobalt in a series of
least four working standards containing concentrations of
prepared standards for the same laboratories were as shown in
cobalt that bracket the expected sample concentration, prior to
Table 1.
analysis of samples, to calibrate the instrument. Prepare the
standards each time the test is to be performed or as determined 15.3 These precision and bias data may not apply to waters
of different matrices. The waters used in evaluations were
by Practice D4841.
reagent water, potable water, river water, and wastewater. It is
12.2 When determining total recoverable cobalt, add 0.5 mL
the user’s responsibility to ensure the validity of this test
of HNO (sp gr 1.42) (11.5) and proceed as directed in 13.2
method for waters of untested matrices.
through 13.4. When determining dissolved cobalt, proceed
15.4 This section on precision and bias conforms to Practice
with 12.3.
D2777 – 77 which was in place at the time of collaborative
12.3 Aspirate the blank and the standards and record the
testing. Under the allowances made in 1.4 of Practice
instrument readings. Aspirate HNO (1 + 499) between stan-
D2777 – 13, these precision and bias data do meet existing
dards.
requirements of interlaboratory studies of Committee D19 test
...
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