1、Designation: D3373 12D3373 17Standard Test Method forVanadium in Water1This standard is issued under the fixed designation D3373; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses in
2、dicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the U.S. Department of Defense.1. Scope*1.1 This test method covers the determination of dissolved and total recover
3、able vanadium in most waters and wastewater bygraphite furnace atomic absorption spectrophotometry.1.2 The optimum range of this test method is 10 to 200 g/L of vanadium based on a 20-L sample size. Concentrations higherthan 200 g/L200 g/L may be determined by proper dilution of sample. A detection
4、level as low as 4 g/L of vanadium has beenreported.1.3 This test method has been used successfully with reagent water, lake water, tap water, river water, condensate from amedium Btu coal gasification process, and well water. It is the users responsibility to ensure the validity of this test method
5、forwaters of untested 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 responsibilityof the user
6、of this standard to establish appropriate safety and health practices and determine the applicability or regulatorylimitations prior to use.1.6 Former Test Method A (Catalytic) was discontinued. Refer to Appendix X1 for historical information.1.7 This international standard was developed in accordan
7、ce with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Stand
8、ards:2D1066 Practice for Sampling SteamD1129 Terminology Relating to WaterD1193 Specification for Reagent WaterD1976 Test Method for Elements in Water by Inductively-Coupled Argon Plasma Atomic Emission SpectroscopyD2777 Practice for Determination of Precision and Bias of Applicable Test Methods of
9、Committee D19 on WaterD3370 Practices for Sampling Water from Closed ConduitsD3919 Practice for Measuring Trace Elements in Water by Graphite Furnace Atomic Absorption SpectrophotometryD4841 Practice for Estimation of Holding Time for Water Samples Containing Organic and Inorganic ConstituentsD5673
10、Test Method for Elements in Water by Inductively Coupled PlasmaMass SpectrometryD5810 Guide for Spiking into Aqueous SamplesD5847 Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis3. Terminology3.1 Definitions: For definitions of terms used in this test
11、method refer to Terminology D1129.3.1.1 For definitions of terms used in this standard, refer to Terminology D1129.3.2 Definitions of Terms Specific to This Standard:1 This test method is under the jurisdiction ofASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.05 on
12、Inorganic Constituents in Water.Current edition approved Sept. 1, 2012June 1, 2017. Published September 2012June 2017. Originally approved in 1975. Last previous edition approved in 20072012 asD3373 03 (2007)D3373 12.1. DOI: 10.1520/D3373-12.10.1520/D3373-17.2 For referencedASTM standards, visit the
13、ASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an
14、indication of what changes have been made to the previous version. Becauseit 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 versionof the standard as published by ASTM is to
15、be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.2.1 continuing calibration blank, na solution containing no analytes (of interest)
16、which is used to verify blank response andfreedom from carryover.3.2.2 continuing calibration verification, na solution (or set of solutions) of known concentration used to verify freedom fromexcessive instrumental drift; the concentration is to cover the range of calibration curve.3.2.3 total recov
17、erable vanadium, ndissolved vanadium plus that solubilized by acid digestion of particulates and organics inthe sample.a descriptive term relating to the metal forms of vanadium recovered in the acid-digestion procedure specified in thistest standard.4. Summary of Test Method4.1 Vanadium is determin
18、ed by an atomic absorption spectrophotometer utilizing a graphite furnace for sample atomization.4.2 A sample volume of several microlitres, depending upon the concentration of the analyte, is transferred to a graphite tubehoused within an electrical furnace and the system is heated in an inert or r
19、educing atmosphere. The sample is evaporated todryness, charred (pyrolyzed or ashed) and atomized.4.3 Ground state atoms, produced in atomization, absorb the light of their spectrum emanating from a source and passingthrough the sample vapor. The amount of light absorbed is proportional to the conce
20、ntration of the analyte in the sample.4.4 Since the graphite furnace uses the sample much more efficiently than does flame atomization, the detection of lowconcentrations of the elements of interest in small volumes is possible.4.5 Finally, the absorption signal produced during atomization is record
21、ed and compared to those of standards, taken throughthe same process, by means of an analytical curve.4.6 A general guide for graphite furnace applications is given in Practice D3919.4.7 Dissolved vanadium is determined after filtration and addition of HNO3 to a pH of 2.4.8 Total recoverable vanadiu
22、m is determined following acid digestion and filtration.5. Significance and Use5.1 Vanadium can be found in waste that result from chemical cleaning of components in which the metal is alloyed.5.2 National Pollutant Discharge Elimination Systems permits or other standards, or both, require monitorin
23、g pollutants in wastedischarged onto the water shed of, or into, navigable waters, and those disposed of in such a manner that eventual contaminationof underground water could result.5.3 This test method affords an accurate and sensitive means of determining compliance or noncompliance, or both, wit
24、h thosepermits.5.4 ICP-MS or ICP-AES may also be appropriate but at a higher instrument cost. See Test Methods D5673 and D1976.6. Interferences6.1 For a complete discussion on general interferences with furnace procedures, the analyst is referred to Practice D3919.7. Apparatus7.1 Atomic Absorption S
25、pectrophotometer, for use at 318.4 nm with background correction.NOTE 1The manufacturers instructions should be followed for all instrumental parameters.7.2 Vanadium Hollow Cathode Lamp.7.3 Graphite Furnace capable of reaching temperature sufficient to atomize the element of interest.7.4 Graphite Tu
26、bes, pyrolytically coated, compatible with furnace device are recommended.7.5 Pipettes, microlitre with disposable tips, ranging in size from 1 to 100 L.7.6 Strip Chart RecorderData Storage and Reduction Devices, Computer- and Microprocessor-Controlled Devices, or StripChart Recorders A recorder is
27、strongly recommended. The tracings can be used as permanent records and are of diagnostic valuein the identification and analysis of instrument problems shall be utilized for collection, storage, reduction, and problem recognition(such as drift, incomplete atomization, changechanges in sensitivity,
28、etc.). A fast response recorder (0.2 s or less for full-scaledeflection) is recommended Strip chart recorders shall have a full scale deflection time of 0.2 s or less to ensure accuracy.Electronic peak-measuring devices have also been found useful.7.7 Automatic Sampling Accessory is recommended, if
29、available.8. Reagents and Materials8.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents shall conform to the specifications of Committee on Analytical Reagents of the American Chemical Society, where suchD3373 172specif
30、ications are available.3 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purityto permit its use without lessening the accuracy of the determination.8.2 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean reag
31、ent water conforming toSpecification D1193, Type I. Other reagent water types may be used provided it is first ascertained that the water is of sufficientlyhigh purity to permit its use without adversely affecting the precision and bias of the test method.8.3 Nitric Acid (sp gr 1.42)Concentrated nit
32、ric acid (HNO3).8.4 Vanadium Solution, Stock (1.0 mL = 100 g vanadium). Dissolve 0.2296 g of ammonium metavanadate (NH4VO3) in waterand dilute to 1000 mL. A purchased vanadium stock solution of appropriate known purity is also acceptable.8.5 Vanadium Solution, Intermediate (1.0 mL = 1.0 g vanadium)D
33、ilute 5 mL of vanadium stock solution to 500 mL withwater.8.6 Vanadium Solution, Standard (1.0 mL = 0.100 g vanadium)Dilute 10.0 mLof vanadium intermediate solution to 100 mLwith water.8.7 Nitrogen Gasstandard, welders grade, commercially available.NOTE 2It is probable that argon or some other inert
34、 gas can be used in place of nitrogen. It is the analysts responsibility to verify suitability.8.8 Filter PaperPurchase suitable filter paper.Typically the filter papers have a pore size of 0.45-m membrane. Material suchas fine-textured, acid-washed, ashless paper, or glass fiber paper are acceptabl
35、e. The user must first ascertain that the filter paperis of sufficient purity to use without adversely affecting the bias and precision of the test method.9. Sampling9.1 Collect the sample in accordance with Practices D1066 and D3370, as applicable. The holding time for the sample may becalculated i
36、n accordance with Practice D4841.9.2 Preserve samples with nitric acid (HNO3, sp gr 1.42) to a pH of 2 or less immediately at the time of collection, normallyabout 2 mL/L. If only dissolved vanadium is to be determined, filter the sample through a 0.45-m (No. 325) membrane filterbefore acidification
37、.NOTE 3Alternatively, the pH may be adjusted in the laboratory if the sample is returned within 14 days. within 14 days of collection. However, acidmust be added at least 24 hours before analysis to dissolve any metals that adsorb to the container walls. This could reduce hazards of working with aci
38、dsin the field when appropriate.10. Standardization10.1 Initially, set the instrument in accordance with the manufacturers specifications. Follow the general instructions asprovided in Practice D3919.11. Procedure11.1 Clean all glassware to be used for preparation of standard solutions or in the dig
39、estion step, or both, by rinsing first withHNO3 (1 + 1) and then with water. Alternatively, soaking the glassware overnight in HNO3 (1 + 1) is useful for low levels.11.2 Measure 100.0 mLof each standard and well-mixed sample into a 125-mLbeaker or flask. For total recoverable vanadium,add 5 mL of HN
40、O3 (sp gr 1.42) to each sample and proceed as directed in 11.4 through 11.6.11.3 If only dissolved vanadium is to be determined, proceed to 11.6.11.4 Heat the samples at 95C (between 65C and 95C) on a steam bath or hotplate hot plate below boiling in a well-ventilatedfume hood until the volume has b
41、een reduced to 15 to 20 mL making certain that the samples do not boil.NOTE 4When analyzing samples of brines or samples containing appreciable amounts of suspended matter or dissolved solids, the amount ofreduction in volume is left to the discretion of the analyst.NOTE 5Many laboratories have foun
42、d block digestion systems a useful way to digest samples for trace metals analysis. Systems typically consist ofeither a metal or graphite block with wells to hold digestion tubes. The block temperature controller must be able to maintain uniformity of temperatureacross all positions of the block. T
43、he digestion block must be capable of maintaining a temperature between 65C and 95C. For trace metals analysis,the digestion tubes should be constructed of polypropylene and have a volume accuracy of at least 0.5%. 0.5 %. All lots of tubes should come with acertificate of analysis to demonstrate sui
44、tability for their intended purpose.11.5 Cool and filter the sample through a suitable filter (8.8) (such as fine-textured, acid washed, ashless paper) into a 100-mLvolumetric flask. Wash the filter paper 2 or 3 times with water and bring to volume. See Note 6. The acid concentration at this pointsh
45、ould be 5 % HNO3.3 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For Suggestions on the testing of reagents not listed bythe American Chemical Society, see Annual Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the Unit
46、ed States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.D3373 173NOTE 6If suspended material is not present, this filtration may be omitted, however, digested sample must still be diluted to 100 mL.11.6 Inject a measured aliquot of sample into the furn
47、ace device following the directions as provided by the particularinstrument manufacturer. Refer to Practice D3919.12. Calculation12.1 Determine the concentration of vanadium in each sample in accordance with the Samples Analysis Procedure Section ofPractice D3919.13. Precision and Bias413.1 Based on
48、 data from twelve participating laboratories, the overall precision of this test method and recoveries from a seriesof standards containing known amounts of vanadium, were as given in Table 1.13.2 Because of the large number of metals analyzed in this study the requirement for replicate tests have b
49、een waived;therefore, single-operator precision is not available.13.3 Each participating laboratory evaluated this test method in reagent water. Individual laboratories selected one water ofchoice as an additional matrix of interest in which to test recovery. Listed among those choices were: lake water, tap water, riverwater, well water, and condensate from a medium Btu coal gasification process.13.4 These data may not apply to waters of other matrices.13.5 This section on precision and bias conforms to Practice D2777 77 which was in
