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Determination of lead and tin by stripping voltammetry ... - Metrohm

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Application Bulle<strong>tin</strong> 176/4 e<strong>Determination</strong> <strong>of</strong> <strong>lead</strong> <strong>and</strong> <strong>tin</strong> <strong>by</strong> anodic <strong>stripping</strong> <strong>voltammetry</strong>Page 10/10The voltammogram is recorded with the followingparameters:Working electrodeHMDEStirrer speed2000 rpmModeDPdrop size 4Purge time300 sDeposition potential-800 mVDeposition time90 sEquilibration time10 sPulse amplitude50 mVStart potential-800 mVEnd potential-500 mVVoltage step4 mVVoltage step time0.1 sSweep rate40 mV/sPeak potential (Sn)-640 mVThe concentration is determined <strong>by</strong> st<strong>and</strong>ard addition.Example<strong>Determination</strong> <strong>of</strong> Sn(II)I (nA)2015105Sample VolumeResultsLiteratureSt<strong>and</strong>ard addition curve: SnII2 4 6 8 10 12 14rho(eff) (µg/L)5 mL15.6 µg/L Sn(II)• Lejeune,R. Thunus,J. Thunus,L.Polarographic determination <strong>of</strong> Sn(II) in samplescontaining Sn(IV) such as in 99m-technitium radiopharmaceuticalkitsAnal. Chim. Acta 332, (1996) 67-71Substance: SnII VR(**)I (nA)2015105-800 -750 -700 -650 -600 -550U (mV)AppendixFull Report <strong>of</strong> a determination <strong>of</strong> Sn(II) acc. to method 3 with the 746 VA Trace Analyzer================== METROHM 746 VA TRACE ANALYZER (5.746.0101) ==================Determ. : 09111121 User: Date: 1997-09-11Modified : 2000-12-08 16:52:16 Run : 0 Time: 11:21:01Sample table: ---------------------------------------------------------------------------------Pos. Ident.1/S1 Ident.2/S2 Ident.3/S3 Method.call Sample size/S0sample SnII 5 mL--------------------------------------------------------------------------------Method : AB176_3Title : Det. <strong>of</strong> Sn(II) besides Sn(IV). AB176 method 3Remark1 :Remark2 :--------------------------------------------------------------------------------Substance : SnIICommentsMass conc.: 15.64 ug/L Mass : 78.21 ng ------------------MC.dev. : 0.632 ug/L (4.04%) Add.mass : 25 ngCal.dev. : - V0.sample: 5 mLVR U/mV I/nA I.mean Std.dev. I.delta Comments--- ----- ------ ------ ------- ------- ------------------00 -630 11.50 11.40 0.166401 -629 11.5002 -629 11.21

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