ASTM D3373-03(2007)e1
(Test Method)Standard Test Method for Vanadium in Water
Standard Test Method for Vanadium in Water
SIGNIFICANCE AND USE
Vanadium can be found in waste that result from chemical cleaning of components in which the metal is alloyed.
National Pollutant Discharge Elimination Systems permits or other standards, or both, require monitoring pollutants in waste discharged onto the water shed of, or into, navigable waters, and those disposed of in such a manner that eventual contamination of underground water could result.
This test method affords an accurate and sensitive means of determining compliance or noncompliance, or both, with those permits.
SCOPE
1.1 This test method covers the determination of dissolved and total recoverable vanadium in most waters and wastewater by graphite furnace atomic absorption spectrophotometry.
1.2 The optimum range of this test method is 10 to 200 μg/L of vanadium based on a 20-L sample size. Concentrations higher than 200 g/L may be determined by proper dilution of sample. A detection level as low as 4 μg/L of vanadium has been reported.
1.3 This test method has been used successfully with reagent water, lake water, tap water, river water, condensate from a medium Btu coal gasification process, and well water. It is the user's responsibility to ensure the validity of this test method for waters of untested 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 or regulatory limitations prior to use.
1.4 Former Test Method A (Catalytic) was discontinued. Refer to Appendix X1 for historical information.
General Information
Relations
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
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Designation: D3373 − 03(Reapproved 2007)
Standard Test Method for
Vanadium in Water
This standard is issued under the fixed designation D3373; 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.
This standard has been approved for use by agencies of the Department of Defense.
´ NOTE—Sections 7.5 and 13.5 were updated editorially in September 2007
1. Scope D1193 Specification for Reagent Water
D2777 Practice for Determination of Precision and Bias of
1.1 This test method covers the determination of dissolved
Applicable Test Methods of Committee D19 on Water
and total recoverable vanadium in most waters and wastewater
D3370 Practices for Sampling Water from Closed Conduits
by graphite furnace atomic absorption spectrophotometry.
D3919 Practice for Measuring Trace Elements in Water by
1.2 Theoptimumrangeofthistestmethodis10to200µg/L
Graphite Furnace Atomic Absorption Spectrophotometry
of vanadium based on a 20-µL sample size. Concentrations
D4841 Practice for Estimation of Holding Time for Water
higher than 200µ g/L may be determined by proper dilution of
Samples Containing Organic and Inorganic Constituents
sample. A detection level as low as 4 µg/L of vanadium has
D5810 Guide for Spiking into Aqueous Samples
been reported.
D5847 Practice for Writing Quality Control Specifications
1.3 This test method has been used successfully with
for Standard Test Methods for Water Analysis
reagent water, lake water, tap water, river water, condensate
from a medium Btu coal gasification process, and well water.
3. Terminology
It is the user’s responsibility to ensure the validity of this test
3.1 Definitions: For definitions of terms used in this test
method for waters of untested matrices.
method refer to Terminology D1129.
1.4 This standard does not purport to address all of the
3.2 Definitions of Terms Specific to This Standard:
safety concerns, if any, associated with its use. It is the
3.2.1 total recoverable vanadium—dissolvedvanadiumplus
responsibility of the user of this standard to establish appro-
that solubilized by acid digestion of particulates and organics
priate safety and health practices and determine the applica-
in the sample.
bility or regulatory limitations prior to use.
1.5 Former Test Method A (Catalytic) was discontinued.
4. Summary of Test Method
Refer to Appendix X1 for historical information.
4.1 Vanadium is determined by an atomic absorption spec-
2. Referenced Documents
trophotometer utilizing a graphite furnace for sample atomiza-
2.1 ASTM Standards:
tion.
D1066 Practice for Sampling Steam
4.2 Asamplevolumeofseveralmicrolitres,dependingupon
D1129 Terminology Relating to Water
the concentration of the analyte, is transferred to a graphite
D1192 Guide for Equipment for Sampling Water and Steam
3 tube housed within an electrical furnace and the system is
in Closed Conduits (Withdrawn 2003)
heated in an inert or reducing atmosphere. The sample is
evaporated to dryness, charred (pyrolyzed or ashed) and
atomized.
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
4.3 Groundstateatoms,producedinatomization,absorbthe
in Water.
light of their spectrum emanating from a source and passing
Current edition approved Aug. 1, 2007. Published September 2007. Originally
approved in 1975. Last previous edition approved in 2003 as D3373 – 03. DOI: through the sample vapor. The amount of light absorbed is
10.1520/D3373-03R07E01.
proportional to the concentration of the analyte in the sample.
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
4.4 Since the graphite furnace uses the sample much more
Standards volume information, refer to the standard’s Document Summary page on
efficiently than does flame atomization, the detection of low
the ASTM website.
concentrations of the elements of interest in small volumes is
The last approved version of this historical standard is referenced on
www.astm.org. possible.
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959. United States
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D3373 − 03 (2007)
4.5 Finally, the absorption signal produced during atomiza- where such specifications are available. Other grades may be
tion is recorded and compared to those of standards, taken used, provided it is first ascertained that the reagent is of
through the same process, by means of an analytical curve. sufficiently high purity to permit its use without lessening the
accuracy of the determination.
4.6 A general guide for graphite furnace applications is
given in Practice D3919. 8.2 Purity of Water—Unless otherwise indicated, references
towatershallbeunderstoodtomeanreagentwaterconforming
4.7 Dissolved vanadium is determined after filtration and
to Specification D1193, Type I. Other reagent water types may
addition of HNO toapHof ≤ 2.
be used provided it is first ascertained that the water is of
4.8 Total recoverable vanadium is determined following
sufficiently high purity to permit its use without adversely
acid digestion and filtration.
affecting the precision and bias of the test method.
8.3 Nitric Acid (sp gr 1.42)—Concentrated nitric acid
5. Significance and Use
(HNO ).
5.1 Vanadium can be found in waste that result from
8.4 Vanadium Solution, Stock (1.0 mL = 100 µg vanadium).
chemicalcleaningofcomponentsinwhichthemetalisalloyed.
Dissolve 0.2296 g of ammonium metavanadate (NH VO)in
4 3
5.2 National Pollutant Discharge Elimination Systems per-
water and dilute to 1000 mL.
mits or other standards, or both, require monitoring pollutants
8.5 Vanadium Solution, Intermediate (1.0 mL = 1.0 µg va-
in waste discharged onto the water shed of, or into, navigable
nadium) —Dilute 5 mL of vanadium stock solution to 500 mL
waters, and those disposed of in such a manner that eventual
with water.
contamination of underground water could result.
8.6 Vanadium Solution, Standard (1.0 mL = 0.100 µg
5.3 Thistestmethodaffordsanaccurateandsensitivemeans
vanadium)—Dilute10.0mLofvanadiumintermediatesolution
of determining compliance or noncompliance, or both, with
to 100 mL with water.
those permits.
8.7 Nitrogen Gas—standard, welders grade, commercially
6. Interferences
available.
6.1 For a complete discussion on general interferences with
NOTE 2—It is probable that argon or some other inert gas can be used
furnace procedures, the analyst is referred to Practice D3919.
in place of nitrogen. It is the analyst’s responsibility to verify suitability.
7. Apparatus
9. Sampling
7.1 Atomic Absorption Spectrophotometer , for use at 318.4
9.1 Collect the sample in accordance with Practice D1066,
nm with background correction.
Specification D1192, and Practices D3370, as applicable. The
holding time for the sample may be calculated in accordance
NOTE 1—The manufacturer’s instructions should be followed for all
with Practice D4841.
instrumental parameters.
7.2 Vanadium Hollow Cathode Lamp.
9.2 Preserve samples with nitric acid (HNO , sp gr 1.42) to
a pH of 2 or less immediately at the time of collection,
7.3 Graphite Furnace capable of reaching temperature suf-
normally about 2 mL/L. If only dissolved vanadium is to be
ficient to atomize the element of interest.
determined, filter the sample through a 0.45-µm (No. 325)
7.4 Graphite Tubes, pyrolytically coated, compatible with
membrane filter before acidification.
furnace device are recommended.
7.5 Pipettes, microlitre with disposable tips, ranging in size
10. Standardization
from 1 to 100 µL.
10.1 Initially, set the instrument in accordance with the
7.6 Strip Chart Recorder—A recorder is strongly recom-
manufacturer’s specifications. Follow the general instructions
mended.Thetracingscanbeusedaspermanentrecordsandare as provided in Practice D3919.
of diagnostic value in the identification and analysis of
instrument problems (such as drift, incomplete atomization, 11. Procedure
change in sensitivity, etc.). A fast response recorder (0.2 s or
11.1 Clean all glassware to be used for preparation of
less for full-scale deflection) is recommended to ensure accu-
standard solutions or in the digestion step, or both, by rinsing
racy. Electronic peak-measuring devices have also been found
first with HNO (1 + 1) and then with water. Alternatively,
useful.
soaking the glassware overnight in HNO (1 + 1) is useful for
7.7 Automatic Sampling Accessory is recommended, if low levels.
available.
8. Reagents and Materials
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
8.1 Purity of Reagents—Reagent grade chemicals shall be
listed by the American Chemical Society, see Annual Standards for Laboratory
used in all tests. Unless otherwise indicated, it is intended that
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
all reagents shall conform to the specifications of Committee
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
on Analytical Reagents of the American Chemical Society, MD.
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D3373 − 03 (2007)
TABLE 1 Determination of Precision and Bias for Vanadium
water, river water, well water, and condensate from a medium
Amount Amount Btu coal gasification process.
S , Bias, Statistically
T
Added, Found, % Bias
µg/L µg/L Significant
A A
13.4 These data may not apply to waters of other matrices.
µg V/L µg V/L
Reagent Water Type II
13.5 ThissectiononprecisionandbiasconformstoPractice
25 24 2.6 −1.0 4.0 no
D2777 – 77 which was in place at the time of collaborative
70 73.4 4.8 + 3.4 4.9 no
240 232.7 25.5 −7.3 3.0 no testing.Undertheallowancesmadein1.4ofD2777 – 06,these
Water of Choice
precision and bias data do meet existing requirements of
25 25.9 3.6 + 0.9 3.6 no
interlaboratory studies of Committee D19 test methods.
70 70 7.6 0 0 no
240 247.3 27.7 + 7.3 3.0 no
14. Quality Control
A
Editorially corrected.
14.1 In order to be certain that analytical values obtained
using these test methods are valid and accurate within the
confidencelimitsofthetest,thefollowingQCproceduresmust
11.2 Measure 100.0 mL of each standard and well-mixed
be followed when analyzing vanadium.
sample into a 125-mL beaker or flask. For total recoverable
vanadium, add 5 mLof HNO (sp gr 1.42) to each sample and
14.2 Calibration and Calibration Verification
proceed as d
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