ASTM D4382-02(2007)e1
(Test Method)Standard Test Method for Barium in Water, Atomic Absorption Spectrophotometry, Graphite Furnace
Standard Test Method for Barium in Water, Atomic Absorption Spectrophotometry, Graphite Furnace
SIGNIFICANCE AND USE
Barium ranks about sixth in order of abundance in nature; however, it is normally found in only trace quantities in drinking water. Consumption, inhalation, or absorption of 500 to 600 mg is considered fatal to human beings.3 Lower levels may result in disorders of the heart, blood vessels, and nerves. The drinking water standards set the maximum contaminant level for barium as 2 mg barium/L.
SCOPE
1.1 This test method covers the determination of dissolved and total recoverable barium in most waters and wastewaters.
1.2 This test method was evaluated in the range from 33.5 to 132 g/L of barium. The range can be increased or decreased by varying the volume of sample injected or the instrumental settings. High concentrations may be diluted but preferably should be analyzed by direct aspiration atomic absorption spectrophotometry.
1.3 This test method has been used successfully with waste treatment plant effluent water, lake water, filtered tap water, and well water. It is the responsibility of the analyst to determine the suitability of the test method for other matrices.
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.
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Designation: D4382 − 02(Reapproved 2007)
Standard Test Method for
Barium in Water, Atomic Absorption Spectrophotometry,
Graphite Furnace
This standard is issued under the fixed designation D4382; 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.
´ NOTE—Section 12.5 was updated editorially in September 2007.
1. Scope D2972 Test Methods for Arsenic in Water
D3373 Test Method for Vanadium in Water
1.1 This test method covers the determination of dissolved
D3557 Test Methods for Cadmium in Water
and total recoverable barium in most waters and wastewaters.
D3558 Test Methods for Cobalt in Water
1.2 Thistestmethodwasevaluatedintherangefrom33.5to
D3559 Test Methods for Lead in Water
132 µg/L of barium. The range can be increased or decreased
D3859 Test Methods for Selenium in Water
by varying the volume of sample injected or the instrumental
D3866 Test Methods for Silver in Water
settings. High concentrations may be diluted but preferably
D3919 Practice for Measuring Trace Elements in Water by
should be analyzed by direct aspiration atomic absorption
Graphite Furnace Atomic Absorption Spectrophotometry
spectrophotometry.
D4691 Practice for Measuring Elements in Water by Flame
1.3 This test method has been used successfully with waste Atomic Absorption Spectrophotometry
D4841 Practice for Estimation of Holding Time for Water
treatment plant effluent water, lake water, filtered tap water,
and well water. It is the responsibility of the analyst to Samples Containing Organic and Inorganic Constituents
D5810 Guide for Spiking into Aqueous Samples
determine the suitability of the test method for other matrices.
D5847 Practice for Writing Quality Control Specifications
1.4 This standard does not purport to address all of the
for Standard Test Methods for Water Analysis
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
3. Terminology
priate safety and health practices and determine the applica-
3.1 Definitions:
bility of regulatory limitations prior to use.
3.1.1 For definitions of terms used in this test method, refer
to Terminology D1129.
2. Referenced Documents
3.2 Definitions of Terms Specific to This Standard:
2.1 ASTM Standards:
3.2.1 total recoverable barium—an arbitrary analytical term
D858 Test Methods for Manganese in Water
relating to the recoverable forms of barium that are determin-
D1068 Test Methods for Iron in Water
able by the digestion method which is included in this test
D1129 Terminology Relating to Water
method.
D1193 Specification for Reagent Water
D1687 Test Methods for Chromium in Water
4. Summary of Test Method
D1688 Test Methods for Copper in Water
4.1 Barium is determined by an atomic absorption spectro-
D1886 Test Methods for Nickel in Water
photometer used in conjunction with a graphite furnace. A
D2777 Practice for Determination of Precision and Bias of
sample is placed in a graphite tube, evaporated to dryness,
Applicable Test Methods of Committee D19 on Water
charred (pyrolyzed or ashed), and atomized. The absorption
signal produced during atomization may be recorded and
1 compared with values obtained from standards that have been
This test method is under the jurisdiction of ASTM Committee D19 on Water
and is the direct responsibility of Subcommittee D19.05 on Inorganic Constituents carried through the same process. This facilitates interpolation
in Water.
of the level of barium in the solution being analyzed. Since the
Current edition approved Aug. 1, 2007. Published September 2007. Originally
graphite furnace uses the sample much more efficiently than
approved in 1984. Last previous edition approved in 2002 as D4382 – 95. DOI:
flame atomization, the detection of low concentrations in small
10.1520/D4382-02R07E01.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
sample volumes is possible.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on NOTE 1—The same graphite furnace procedure may be applicable to
the ASTM website. determination of arsenic (see Test Methods D2972), cadmium (see Test
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D4382 − 02 (2007)
Methods D3557), chromium (see Test Methods D1687), cobalt (see Test
7.6 Automatic Sampling accessory should be used, if avail-
Methods D3558), copper (see Test Methods D1688), iron (see Test
able.
Methods D1068), lead (see Test Methods D3559), manganese (see Test
Methods D858), nickel (see Test Methods D1886), selenium (see Test
8. Reagents and Materials
Methods D3859), silver (see Test Methods D3866), and vanadium (see
8.1 Purity of Reagents—Reagent grade chemicals shall be
Test Method D3373).
used in all tests. Unless otherwise indicated, it is intended that
4.2 Dissolved barium is determined on a sample filtered
all reagents shall conform to the specifications of the Commit-
through a 0.45-µm membrane filter.The definition of dissolved
tee onAnalytical Reagents of theAmerican Chemical Society,
barium is arbitrary since very fine crystals of barium sulfate
where such specifications are available. Other grades may be
may pass through the membrane filter.
used, provided it is first ascertained that the reagent is of
4.3 Total recoverable barium is determined following acid
sufficiently high purity to permit its use without lessening the
digestion and filtration. Because chlorides interfere with fur-
accuracy of the determination.
nace procedures for some metals, the use of hydrochloric acid
8.2 Purity of Water—Unless otherwise indicated, references
in any digestion or solubilization step is to be avoided. If
towatershallbeunderstoodtomeanreagentwaterconforming
suspended material is not present, this digestion and filtration
to Specification D1193, Type I. Other reagent water types may
may be omitted. The holding time for the samples may be
be used, provided it is first ascertained that the water is of
calculated in accordance with Practice D4841.
sufficiently high purity to permit its use without adversely
affecting the bias and precision of the test method. Type II
5. Significance and Use
water was specified at the time of round-robin testing of this
5.1 Barium ranks about sixth in order of abundance in
test method.
nature; however, it is normally found in only trace quantities in
8.3 Barium Solution, Stock (1.0 mL = 1000 µg barium)—
drinking water. Consumption, inhalation, or absorption of 500
Dissolve1.779gofbariumchloride(BaCl ·2H O)in50mLof
2 2
to 600 mg is considered fatal to human beings. Lower levels
concentrated hydrochloric acid (HCl) (sp gr 1.19) and about
may result in disorders of the heart, blood vessels, and nerves.
700 mL of water. Dilute to 1 L with water. A purchased stock
The drinking water standards set the maximum contaminant
solution of appropriate purity is also acceptable.
level for barium as 2 mg barium/L.
8.4 Barium Solution, Intermediate (1.0 mL = 10 µg
barium)—Dilute 10.0 mLof barium solution, stock (8.3) and 1
6. Interferences
mL of HNO (sp gr 1.42) to 1 L with water.
6.1 For a complete discussion on general interferences with
8.5 Barium Solution, Standard (1.0 mL = 0.10 µg barium)—
furnace procedures, refer to Practice D3919.
Dilute 10.0 mLof barium intermediate solution (8.4) and 1 mL
of HNO (sp gr 1.42) to 1 L with water. This standard is used
7. Apparatus
to prepare working standards at the time of the analysis.
7.1 Atomic Absorption Spectrophotometer , for use at 553.6
8.6 Nitric Acid (sp gr 1.42)—Concentrated nitric acid
nm with background correction. A general guide for flame
(HNO ).
atomic absorption applications is given in Practice D4691.
NOTE 4—If the reagent blank concentration is greater than the method
NOTE 2—Awavelength other than 553.6 nm may be used if it has been
detection limit, distill the HNO or use a spectrograde acid.
determined to be suitable.At high concentration, greater linearity may be
obtained by using a less sensitive wavelength.
8.7 Argon, standard, welders grade, commercially available.
NOTE 3—The manufacturer’s instructions should be followed for all
Nitrogen and hydrogen may also be used, if recommended by
instrumental parameters.
the instrument manufacturer.
7.2 Barium Light Source—Barium hollow-cathode lamp. A
single-element lamp is preferred. Multielement lamps contain- 9. Standardization
ing calcium are not recommended.
9.1 Initially, set the instrument in accordance with the
7.3 Graphite Furnace, capable of reaching temperatures manufacturer’s specifications. Follow the general instructions
sufficient to atomize the element of interest. as provided in Practice D3919.
7.4 Graphite Tubes, compatible with furnace device. To
10. Procedure
eliminatetheformationofcarbides,pyrolyticallycoatedgraph-
10.1 Clean all glassware to be used for preparation of
ite tubes are recommended.
standard solutions or in the digestion step, or both, by rinsing
7.5 Data Storage and Reduction Devices—Computer and
first with HNO (1 + 1) and then with water. Alternatively,
microprocessor controlled devices, or a strip chart recorder,
soaking the glassware overnight in (1 + 1) HNO is useful for
shall be utilized for data collection, storage, reduction, and
low levels.
problem recognition (drift, incomplete atomization, changes in
sensitivity, etc.).
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
listed by the American Chemical Society, see Annual Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Standards Method for the Examination of Water and Wastewater, 15th Edition, and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
American Public Health Assn., 1015 15th St., NW, Washington, DC 20005. MD.
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D4382 − 02 (2007)
10.2 Measure 100 mL of each standard and well-mixed 12.2 Because of the large number of metals analyzed in this
sample into
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