ASTM_D_3697_-_12.pdf

Designation:D369712Standard Test Method forAntimony in Water1This standard is issued under the fixed designation D3697;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 indicates the year of last reapproval.Asuperscript epsilon()indicates an editorial change since the last revision or reapproval.1.Scope*1.1 This test method covers the determination of dissolvedand total recoverable antimony in water by atomic absorptionspectroscopy.21.2 This test method is applicable in the range from 1 to 15g/L of antimony.The range may be extended by less scaleexpansion or by dilution of the sample.1.3 The precision and bias data were obtained on reagentwater,tap water,salt water,and two untreated wastewaters.The information on precision and bias may not apply to otherwaters.1.4 The values stated in either SI units or inch-pound unitsare to be regarded separately as standard.The values stated ineach system are mathematical conversions and may not beexact equivalents;therefore,each system shall be used inde-pendently of the other.1.5 This standard does not purport to address all of thesafety concerns,if any,associated with its use.It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:3D1129 Terminology Relating to WaterD1193 Specification for Reagent WaterD2777 Practice for Determination of Precision and Bias ofApplicable Test Methods of Committee D19 on WaterD3370 Practices for Sampling Water from Closed ConduitsD4691 Practice for Measuring Elements in Water by FlameAtomic Absorption SpectrophotometryD4841 Practice for Estimation of Holding Time for WaterSamples Containing Organic and Inorganic ConstituentsD5847 Practice for Writing Quality Control Specificationsfor Standard Test Methods for Water Analysis3.Terminology3.1 Definitions:For definitions of terms used in this testmethod,refer to Terminology D1129.3.2 Definitions of Terms Specific to This Standard:3.2.1 total recoverable antimony,nan arbitrary analyticalterm relating to forms of antimony that are determinable by thedigestion method which is included in the procedure;someorganic compounds may not be completely recovered.3.2.2 laboratory control sample,na solution with a certi-fied concentration of the antimony.4.Summary of Test Method4.1Organic antimony-containing compounds are decom-posed by adding sulfuric and nitric acids and repeatedlyevaporating the sample to fumes of sulfur trioxide.Theantimony so produced,together with inorganic antimonyoriginally present,is subsequently reacted with potassiumiodide and stannous chloride,and finally with sodium borohy-dride to form stibine.The stibine is removed from solution byaeration and swept by a flow of nitrogen into a hydrogen flamewhere it is determined by atomic absorption at 217.6 nm.5.Significance and Use5.1Because of the association with lead and arsenic inindustry,it is often difficult to assess the toxicity of antimonyand its compounds.In humans,complaints referable to thenervous system have been reported.In assessing human cases,however,the possibility of lead or arsenic poisoning mustalways be borne in mind.Locally,antimony compounds areirritating to the skin and mucous membranes.6.Interference6.1Since the stibine is freed from the original samplematrix,interferences in the flame are minimized.6.2 Selenium and arsenic,which also form hydrides,do notinterfere at concentrations of 100 g/L.Higher concentrationswere not tested.1This test method is under the jurisdiction of ASTM Committee D19 on Waterand is the direct responsibility of Subcommittee D19.05 on Inorganic Constituentsin Water.Current edition approved Sept.1,2012.Published September 2012.Originallyapproved in 1978.Last previous edition approved in 2007 as D3697 07.DOI:10.1520/D3697-12.2Platte,J.A.,and Marcy,V.M.,“ANew Tool for the Water Chemist,”IndustrialWater Engineering,IWEGA,May 1965.3For referenced ASTM standards,visit the ASTM website,www.astm.org,orcontact ASTM Customer Service at serviceastm.org.For Annual Book of ASTMStandards volume information,refer to the standards Document Summary page onthe ASTM website.*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 States1 7.Apparatus7.1 Atomic Absorption Spectrophotometer,for use at 217.6nm with a scale expansion of approximately 3.Ageneral guidefor the use of flame atomic absorption applications is given inPractice D4691.NOTE1The manufacturers instructions should be followed for allinstrumental parameters.7.1.1 Antimony Electrodeless Discharge Lamp.7.2 Recorder or Digital Readout Any multirange variablespeed recorder or digital readout accessory,or both,that iscompatible with the atomic absorption spectrop