ASTM D4382-18
(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
5.1 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. 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/L.3
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 μg/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.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 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.
1.6 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
- Status
- Published
- Publication Date
- 31-Jan-2018
- Technical Committee
- D19 - Water
- Drafting Committee
- D19.05 - Inorganic Constituents in Water
Relations
- Effective Date
- 01-Feb-2018
- Effective Date
- 01-Dec-2023
- Effective Date
- 01-Dec-2023
- Effective Date
- 01-Dec-2023
- Effective Date
- 01-May-2020
- Effective Date
- 01-May-2020
- Effective Date
- 01-Jul-2018
- Effective Date
- 01-Feb-2018
- Effective Date
- 01-Jun-2017
- Effective Date
- 01-Jun-2017
- Effective Date
- 01-Jun-2017
- Effective Date
- 01-Jul-2015
- Effective Date
- 01-Jun-2015
- Effective Date
- 15-Mar-2015
- Effective Date
- 01-Feb-2015
Overview
ASTM D4382-18 is the internationally recognized standard test method for the determination of barium in water using atomic absorption spectrophotometry with a graphite furnace. Developed by ASTM International, this method specifies procedures for measuring both dissolved and total recoverable barium in various types of waters, including drinking water, wastewater, surface water, and effluent samples. The standard supports laboratories and environmental monitoring agencies in adhering to regulatory requirements regarding allowable barium concentrations, ensuring public health and environmental safety.
Barium, while naturally abundant, is typically found in trace amounts in drinking water. Higher concentrations pose significant health risks, such as disorders affecting the heart, blood vessels, and nervous system. For this reason, regulatory frameworks, including drinking water standards, set the maximum contaminant level for barium at 2 mg/L. ASTM D4382-18 enables accurate, sensitive, and reliable measurement of barium levels to support compliance with these limits.
Key Topics
- Measurement Range: This method is designed for the detection of barium concentrations from approximately 33.5 to 132 μg/L, with flexibility to adapt the range by altering sample size or instrument settings.
- Matrix Applicability: Applicable to diverse water matrices, including wastewater, lake water, filtered tap water, and well water. Analysts should confirm suitability for additional matrices.
- Types of Barium Assessed:
- Dissolved barium - determined after filtration through a 0.45-micron membrane.
- Total recoverable barium - measured following acid digestion and filtration.
- Analytical Technique: Utilizes atomic absorption spectrophotometry with a graphite furnace for improved sensitivity at low concentrations, making it suitable for trace analysis.
- Interference and Quality Control: The method incorporates procedures for detecting and correcting interferences. Quality control steps involve calibration, calibration verification, laboratory control samples, method blanks, matrix spikes, and duplicate measurements.
Applications
- Drinking Water Monitoring: Ensuring compliance with maximum contaminant levels for barium as defined by regulatory agencies.
- Environmental Protection: Monitoring surface water, effluent, and wastewater discharges for barium contamination to prevent ecological and public health risks.
- Industrial Wastewater Analysis: Supporting industries in the chemical, mining, or oil and gas sectors to assess and control barium in process effluents and comply with environmental regulations.
- Water Treatment Facilities: Evaluation of incoming and treated water to maintain quality assurance and optimize treatment processes.
The method’s sensitivity enables laboratories to detect even trace barium concentrations, making it highly effective for routine water quality assessment and regulatory reporting.
Related Standards
Several ASTM standards complement and support ASTM D4382-18, offering harmonized approaches for elemental analysis in water:
- ASTM D858 - Test Methods for Manganese in Water
- ASTM D1068 - Test Methods for Iron in Water
- ASTM D1193 - Specification for Reagent Water
- ASTM D1976 - Test Method for Elements in Water by ICP Atomic Emission Spectroscopy
- ASTM D3919 - Practice for Graphite Furnace Atomic Absorption Spectrophotometry
- ASTM D4691 - Practice for Flame Atomic Absorption in Water
- ASTM D5673 - Test Method for Elements in Water by ICP-Mass Spectrometry
- ASTM D2777, D5847 - Practices for test method precision, bias, and quality control
- ASTM D1129 - Terminology relating to water analysis
ASTM D4382-18 is essential for laboratories and professionals involved in water quality monitoring, providing a reliable and standardized approach for detecting and quantifying barium using advanced spectrophotometric techniques. Implementing this method supports regulatory compliance, environmental stewardship, and public health protection.
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Frequently Asked Questions
ASTM D4382-18 is a standard published by ASTM International. Its full title is "Standard Test Method for Barium in Water, Atomic Absorption Spectrophotometry, Graphite Furnace". This standard covers: SIGNIFICANCE AND USE 5.1 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. 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/L.3 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 μg/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. 1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. 1.5 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. 1.6 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.
SIGNIFICANCE AND USE 5.1 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. 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/L.3 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 μg/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. 1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. 1.5 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. 1.6 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.
ASTM D4382-18 is classified under the following ICS (International Classification for Standards) categories: 13.060.50 - Examination of water for chemical substances. The ICS classification helps identify the subject area and facilitates finding related standards.
ASTM D4382-18 has the following relationships with other standards: It is inter standard links to ASTM D4382-12, ASTM D2972-15(2023), ASTM D3859-15(2023), ASTM D3558-15(2023), ASTM D1976-20, ASTM D1129-13(2020)e2, ASTM D1976-18, ASTM D3866-18, ASTM D3373-17, ASTM D1687-17, ASTM D3557-17, ASTM D5673-15, ASTM D3559-15, ASTM D3859-15, ASTM D3558-15. Understanding these relationships helps ensure you are using the most current and applicable version of the standard.
ASTM D4382-18 is available in PDF format for immediate download after purchase. The document can be added to your cart and obtained through the secure checkout process. Digital delivery ensures instant access to the complete standard document.
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: D4382 − 18
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.
1. Scope* D1068 Test Methods for Iron in Water
D1129 Terminology Relating to Water
1.1 This test method covers the determination of dissolved
D1193 Specification for Reagent Water
and total recoverable barium in most waters and wastewaters.
D1687 Test Methods for Chromium in Water
1.2 Thistestmethodwasevaluatedintherangefrom33.5to
D1688 Test Methods for Copper in Water
132 µg/L of barium. The range can be increased or decreased
D1886 Test Methods for Nickel in Water
by varying the volume of sample injected or the instrumental
D1976 Test Method for Elements in Water by Inductively-
settings. High concentrations may be diluted but preferably
Coupled Argon Plasma Atomic Emission Spectroscopy
should be analyzed by direct aspiration atomic absorption
D2777 Practice for Determination of Precision and Bias of
spectrophotometry.
Applicable Test Methods of Committee D19 on Water
1.3 This test method has been used successfully with waste D2972 Test Methods for Arsenic in Water
D3373 Test Method for Vanadium in Water
treatment plant effluent water, lake water, filtered tap water,
and well water. It is the responsibility of the analyst to D3557 Test Methods for Cadmium in Water
D3558 Test Methods for Cobalt in Water
determine the suitability of the test method for other matrices.
D3559 Test Methods for Lead in Water
1.4 The values stated in SI units are to be regarded as
D3859 Test Methods for Selenium in Water
standard. No other units of measurement are included in this
D3866 Test Methods for Silver in Water
standard.
D3919 Practice for Measuring Trace Elements in Water by
1.5 This standard does not purport to address all of the
Graphite Furnace Atomic Absorption Spectrophotometry
safety concerns, if any, associated with its use. It is the
D4691 Practice for Measuring Elements in Water by Flame
responsibility of the user of this standard to establish appro-
Atomic Absorption Spectrophotometry
priate safety, health, and environmental practices and deter-
D4841 Practice for Estimation of Holding Time for Water
mine the applicability of regulatory limitations prior to use.
Samples Containing Organic and Inorganic Constituents
1.6 This international standard was developed in accor-
D5673 Test Method for Elements in Water by Inductively
dance with internationally recognized principles on standard-
Coupled Plasma—Mass Spectrometry
ization established in the Decision on Principles for the
D5810 Guide for Spiking into Aqueous Samples
Development of International Standards, Guides and Recom-
D5847 Practice for Writing Quality Control Specifications
mendations issued by the World Trade Organization Technical
for Standard Test Methods for Water Analysis
Barriers to Trade (TBT) Committee.
3. Terminology
2. Referenced Documents
3.1 Definitions:
2.1 ASTM Standards:
3.1.1 For definitions of terms used in this standard, refer to
D858 Test Methods for Manganese in Water
Terminology D1129.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 total recoverable barium, n—a descriptive term relat-
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 ingtotherecoverableformsofbariumthataredeterminableby
in Water.
the digestion method which is included in this test method.
Current edition approved Feb. 1, 2018. Published May 2018. Originally
approved in 1984. Last previous edition approved in 2012 as D4382 – 12. DOI:
4. Summary of Test Method
10.1520/D4382-18.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
4.1 Barium is determined by an atomic absorption spectro-
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
photometer used in conjunction with a graphite furnace. A
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. sample is placed in a graphite tube, evaporated to dryness,
*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
D4382 − 18
charred (pyrolyzed or ashed), and atomized. The absorption 7.3 Graphite Furnace, capable of reaching temperatures
signal produced during atomization may be recorded and sufficient to atomize the element of interest.
compared with values obtained from standards that have been
7.4 Graphite Tubes, compatible with furnace device. To
carried through the same process. This facilitates interpolation
eliminatetheformationofcarbides,pyrolyticallycoatedgraph-
of the level of barium in the solution being analyzed. Since the
ite tubes are recommended.
graphite furnace uses the sample much more efficiently than
7.5 Data Storage and Reduction Devices—Computer and
flame atomization, the detection of low concentrations in small
microprocessor controlled devices, or a strip chart recorder,
sample volumes is possible.
shall be utilized for data collection, storage, reduction, and
NOTE 1—The same graphite furnace procedure may be applicable to
problem recognition (drift, incomplete atomization, changes in
determination of arsenic (see Test Methods D2972), cadmium (see Test
sensitivity, etc.).
Methods D3557), chromium (see Test Methods D1687), cobalt (see Test
Methods D3558), copper (see Test Methods D1688), iron (see Test
7.6 Automatic Sampling accessory should be used, if avail-
Methods D1068), lead (see Test Methods D3559), manganese (see Test
able.
Methods D858), nickel (see Test Methods D1886), selenium (see Test
Methods D3859), silver (see Test Methods D3866), and vanadium (see
8. Reagents and Materials
Test Method D3373).
8.1 Purity of Reagents—Reagent grade chemicals shall be
4.2 Dissolved barium is determined on a sample filtered
used in all tests. Unless otherwise indicated, it is intended that
through a 0.45-µm membrane filter.The definition of dissolved
all reagents shall conform to the specifications of the Commit-
barium is arbitrary since very fine crystals of barium sulfate
tee onAnalytical Reagents of theAmerican Chemical Society,
may pass through the membrane filter.
where such specifications are available. Other grades may be
4.3 Total recoverable barium is determined following acid
used, provided it is first ascertained that the reagent is of
digestion and filtration. Because chlorides interfere with fur-
sufficiently high purity to permit its use without lessening the
nace procedures for some metals, the use of hydrochloric acid
accuracy of the determination.
in any digestion or solubilization step is to be avoided. If
8.2 Purity of Water—Unless otherwise indicated, references
suspended material is not present, this digestion and filtration
towatershallbeunderstoodtomeanreagentwaterconforming
may be omitted. The holding time for the samples may be
to Specification D1193, Type I. Other reagent water types may
calculated in accordance with Practice D4841.
be used, provided it is first ascertained that the water is of
4.4 ICP-MS or ICP-AES may also be appropriate but at a
sufficiently high purity to permit its use without adversely
higher instrument cost. See Test Methods D5673 and D1976.
affecting the bias and precision of the test method. Type II
water was specified at the time of round-robin testing of this
5. Significance and Use
test method.
5.1 Barium ranks about sixth in order of abundance in
8.3 Barium Solution, Stock (1.0 mL = 1000 µg barium)—
nature; however, it is normally found in only trace quantities in
Dissolve1.779gofbariumchloride(BaCl ·2H O)in50mLof
2 2
drinking water. Consumption, inhalation, or absorption of 500
concentrated hydrochloric acid (HCl) (sp gr 1.19) and about
to 600 mg is considered fatal to human beings. Lower levels
700 mLof water. Dilute to 1 Lwith water.Apurchased barium
may result in disorders of the heart, blood vessels, and nerves.
stock solution of appropriate known purity is also acceptable.
The drinking water standards set the maximum contaminant
8.4 Barium Solution, Intermediate (1.0 mL = 10 µg
level for barium as 2 mg/L.
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
8.7 Argon, standard, welders grade, commercially available.
obtained by using a less sensitive wavelength.
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-
Reagent Chemicals, American Chemical Society Specifications, American
ing calcium are not recommended.
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.
D4382 − 18
8.8 Filter Paper—Purchase suitable filter paper. Typically 11. Calculation
the filter papers have a pore size of 0.45-µm membrane.
11.1 Determine the concentration of barium in each sample
Material such as fine-textured, acid-washed, ashless paper, or
by referring to the Sample Analysis Procedure section of
glass fiber paper are acceptable. The user must first ascertain
Practice D3919.
that the filter paper is of sufficient purity to use without
adversely affecting the bias and precision of the test method. 12. Precision and Bias
12.1 Based on data from six participating laboratories, the
9. Standardization
overall precision of the test method and recoveries from a
seriesofstandardscontainingknownamountsofbarium,areas
9.1 Initially, set the instrument in accordance with the
given in Table 1.
manufacturer’s specifications. Follow the general instructions
as provided in Practice D3919.
TABLE 1 Determination of Precision and Bias, Barium Graphite
Furnace Atomic Absorption
10. Procedure
Amount Amount
Bias, Statistically
Added, Found, S , µg/L Bias, µg/L
10.1 Clean all glassware to be used for preparation of T
% Significant
µg/L µg/L
standard solutions or in the digestion step, or both, by rinsing
first with HNO (1 + 1) and then with water. Alternatively,
Reagent Water Type II
soaking the glassware overnight in (1 + 1)
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM 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: D4382 − 12 D4382 − 18
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.
1. 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 μg/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.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.6 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.
2. Referenced Documents
2.1 ASTM Standards:
D858 Test Methods for Manganese in Water
D1068 Test Methods for Iron in Water
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
D1687 Test Methods for Chromium in Water
D1688 Test Methods for Copper in Water
D1886 Test Methods for Nickel in Water
D1976 Test Method for Elements in Water by Inductively-Coupled Argon Plasma Atomic Emission Spectroscopy
D2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
D2972 Test Methods for Arsenic in Water
D3373 Test Method for Vanadium in Water
D3557 Test Methods for Cadmium in Water
D3558 Test Methods for Cobalt in Water
D3559 Test Methods for Lead in Water
D3859 Test Methods for Selenium in Water
D3866 Test Methods for Silver in Water
D3919 Practice for Measuring Trace Elements in Water by Graphite Furnace Atomic Absorption Spectrophotometry
D4691 Practice for Measuring Elements in Water by Flame Atomic Absorption Spectrophotometry
D4841 Practice for Estimation of Holding Time for Water Samples Containing Organic and Inorganic Constituents
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 in Water.
Current edition approved Sept. 1, 2012Feb. 1, 2018. Published September 2012May 2018. Originally approved in 1984. Last previous edition approved in 20022012 as
ɛ1
D4382 – 95 (2007)D4382 – 12. . DOI: 10.1520/D4382-12.10.1520/D4382-18.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 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 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
D4382 − 18
D5673 Test Method for Elements in Water by Inductively Coupled Plasma—Mass Spectrometry
D5810 Guide for Spiking into Aqueous Samples
D5847 Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis
3. Terminology
3.1 Definitions:
3.1.1 For definitions of terms used in this test method, refer to Terminology D1129.
3.1 Definitions:
3.1.1 For definitions of terms used in this standard, refer to Terminology D1129.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 total recoverable barium, n—an arbitrary analytical a descriptive term relating to the recoverable forms of barium that are
determinable by the digestion method which is included in this test method.
4. Summary of Test Method
4.1 Barium is determined by an atomic absorption spectrophotometer used in conjunction with a graphite furnace. A sample is
placed in a graphite tube, evaporated to dryness, charred (pyrolyzed or ashed), and atomized. The absorption signal produced
during atomization may be recorded and compared with values obtained from standards that have been carried through the same
process. This facilitates interpolation of the level of barium in the solution being analyzed. Since the graphite furnace uses the
sample much more efficiently than flame atomization, the detection of low concentrations in small sample volumes is possible.
NOTE 1—The same graphite furnace procedure may be applicable to determination of arsenic (see Test Methods D2972), cadmium (see Test Methods
D3557), chromium (see Test Methods D1687), cobalt (see Test Methods D3558), copper (see Test Methods D1688), iron (see Test Methods D1068), lead
(see Test Methods D3559), manganese (see Test Methods D858), nickel (see Test Methods D1886), selenium (see Test Methods D3859), silver (see Test
Methods D3866), and vanadium (see Test Method D3373).
4.2 Dissolved barium is determined on a sample filtered through a 0.45-μm membrane filter. The definition of dissolved barium
is arbitrary since very fine crystals of barium sulfate may pass through the membrane filter.
4.3 Total recoverable barium is determined following acid digestion and filtration. Because chlorides interfere with furnace
procedures for some metals, the use of hydrochloric acid in any digestion or solubilization step is to be avoided. If suspended
material is not present, this digestion and filtration may be omitted. The holding time for the samples may be calculated in
accordance with Practice D4841.
4.4 ICP-MS or ICP-AES may also be appropriate but at a higher instrument cost. See Test Methods D5673 and D1976.
5. Significance and Use
5.1 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. 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/L. 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/L.
6. Interferences
6.1 For a complete discussion on general interferences with furnace procedures, refer to Practice D3919.
7. Apparatus
7.1 Atomic Absorption Spectrophotometer, for use at 553.6 nm with background correction. A general guide for flame atomic
absorption applications is given in Practice D4691.
NOTE 2—A wavelength other than 553.6 nm may be used if it has been determined to be suitable. At high concentration, greater linearity may be
obtained by using a less sensitive wavelength.
NOTE 3—The manufacturer’s instructions should be followed for all instrumental parameters.
7.2 Barium Light Source—Barium hollow-cathode lamp. A single-element lamp is preferred. Multielement lamps containing
calcium are not recommended.
7.3 Graphite Furnace, capable of reaching temperatures sufficient to atomize the element of interest.
7.4 Graphite Tubes, compatible with furnace device. To eliminate the formation of carbides, pyrolytically coated graphite tubes
are recommended.
Standards Method for the Examination of Water and Wastewater, 15th Edition, American Public Health Assn., 1015 15th St., NW, Washington, DC 20005.
D4382 − 18
7.5 Data Storage and Reduction Devices—Computer and microprocessor controlled devices, or a strip chart recorder, shall be
utilized for data collection, storage, reduction, and problem recognition (drift, incomplete atomization, changes in sensitivity, etc.).
7.6 Automatic Sampling accessory should be used, if available.
8. Reagents and Materials
8.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where
such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination.
8.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to
Specification D1193, Type I. Other reagent water types may be used, provided it is first ascertained that the water is of sufficiently
high purity to permit its use without adversely affecting the bias and precision of the test method. Type II water was specified at
the time of round-robin testing of this test method.
8.3 Barium Solution, Stock (1.0 mL = 1000 μg barium)—Dissolve 1.779 g of barium chloride (BaCl ·2H O) in 50 mL of
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concentrated hydrochloric acid (HCl) (sp gr 1.19) and about 700 mL of water. Dilute to 1 L with water. A purchased barium stock
solution of appropriate known purity is also acceptable.
8.4 Barium Solution, Intermediate (1.0 mL = 10 μg barium)—Dilute 10.0 mL of barium solution, stock (8.3) and 1 mL of HNO
(sp gr 1.42) to 1 L with water.
8.5 Barium Solution, Standard (1.0 mL = 0.10 μg barium)—Dilute 10.0 mL of barium intermediate solution (8.4) and 1 mL of
HNO (sp gr 1.42) to 1 L with water. This standard is used to prepare working standards at the time of the analysis.
8.6 Nitric Acid (sp gr 1.42)—Concentrated nitric acid (HNO ).
NOTE 4—If the reagent blank concentration is greater than the method detection limit, distill the HNO or use a spectrograde acid.
8.7 Argon, standard, welders grade, commercially available. Nitrogen and hydrogen may also be used, if recommended by the
instrument manufacturer.
8.8 Filter Paper—Purchase suitable filter paper. Typically the filter papers have a pore size of 0.45-μm membrane. Material such
as fine-textured, acid-washed, ashless paper, or glass fiber paper are acceptable. The user must first ascertain that the filter paper
is of sufficient purity to use without adversely affecting the bias and precision of the test method.
9. Standardization
9.1 Initially, set the instrument in accordance with the manufacturer’s specifications. Follow the general instructions as provided
in Practice D3919.
10. Procedure
10.1 Clean all glassware to be used for preparation of standard solutions or in the digestion step, or both, by rinsing first with
HNO (1 + 1) and then with water. Alternatively, soaking the glassware overnight in (1 + 1) HNO is useful for low levels.
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10.2 Measure 100 mL of each standard and well-mixed sample into a 125-mL beaker or flask.
10.3 For total recoverable barium, add 5 mL HNO (sp gr 1.42) to each standard and sample and proceed as directed in 10.4
– 10.6. If only dissolved barium is to be determined, take an aliquot of sample that has been filtered through a 0.45-μm membrane
filter (8.8) and proceed to 10.6.
10.4 Heat the samples at approximately 95°C (between 65°C and 95°C) on a steam bath or hotplate below boiling in a
well-ventilated fume hood until the volume has been reduced to 15 to 20 mL, making certain that the samples do not boil.
NOTE 5—When analyzing samples of brines or samples containing appreciable amounts of suspended matter or dissolved solids, the amount of
reduction in volume is left to the discretion of the analyst.
NOTE 6—Many laboratories have found block digestion systems a useful way to digest samples for trace metals analysis. Systems typically consist of
either a metal or graphite block with wells to hold digestion tubes. The block temperature controller must be able to maintain un
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