Determination of lead and tin by stripping voltammetry ... - Metrohm
Determination of lead and tin by stripping voltammetry ... - Metrohm Determination of lead and tin by stripping voltammetry ... - Metrohm
Application Bulletin 176/4 eDetermination of lead and tin by anodic stripping voltammetryPage 4/4AppendixFull Report of a determination of Pb in presence of Sn (200 fold excess) acc. to method 1a with the757 VA Computrace==================== METROHM 757 VA COMPUTRACE (5.757.0010) ====================Determ. : 06161543_Pb(excessSn200).dthDate : 1999-06-16 Time: 14:43:09Modified : 2000-12-05 11:37:32 User: Cell volume: 10.050 ml--------------------------------------------------------------------------------IdentSample volumePb(excessSn200)5.000 ml--------------------------------------------------------------------------------Method : AB176_1.mthTitle : Determination of Pb. AB176 method 1aRemark1 : 5ml sample + 5ml electrolyte + 50µl cetyltrimethylammoniumbromideRemark2 : el.: 0.1mol/l trisodiumcitrate + 0.1mol/l oxalic acid + 0.2mol/l HCl--------------------------------------------------------------------------------Substance : PbCommentsMass conc.: 5.211 ug/l ------------------MC.dev. : 0.844 ug/l ( 16.19%)Mass : 52.366 ngAdd.mass : 50.000 ngVR V nA i.mean Std.Dev. i.delta Comments---- ----- ------ ------ ------- ------- ------------------1-1 -0.423 11.57 10.80 1.0961-2 -0.423 10.022-1 -0.423 21.18 20.44 1.040 9.642-2 -0.423 19.713-1 -0.423 30.37 31.01 0.907 10.573-2 -0.423 31.66Substance Calibr. Y.reg/offset Slope Nonlin. Mean deviat.--------- -------- ------------ ---------- ---------- ------------Pb std.add. 1.060e-008 2.058e-003 9.879e-010Final results +/- Res. dev. % Comments--------------------------------- ------------------ ------------------Pb = 10.473 µg/l 1.696 16.190Method parameters of a determination of Pb in presence of Sn (200 fold excess) acc. to method 1a with the746 VA Trace Analyzer================== METROHM 746 VA TRACE ANALYZER (5.746.0101) ==================Method: AB176_1a.mthOPERATION SEQUENCETitle : Det.of Pb beneath Sn with CTAB. AB176 part 1a--------------------------------------------------------------------------------Instructions t/s Main parameters Auxiliary parameters------------- ----- ------------------------- -------------------------1 DOS/M V.added 5.050 mL2 REM 5mL sample + 5 mL electrolyte + 50 µL meth. blue3 SMPL/M V.fraction mL V.total L4 PURGE5 STIR 300.0 Rot.speed 2000 /min6 (ADD7 PURGE8 STIR 30.0 Rot.speed 2000 /min9 0PURGE10 (REP11 SEGMENT Segm.name asv12 REP)113 PURGE14 STIR Rot.speed 2000 /min15 ADD>M Soln.name Pb-std V.add 0.100 mL16 ADD)217 ENDMethod: AB176_1aSEGMENTasv--------------------------------------------------------------------------------Instructions t/s Main parameters Auxiliary parameters------------- ----- ------------------------- -------------------------1 STIR 5.0 Rot.speed 2000 /min2 HMDE Drop size 4 Meas.cell normal3 DPMODE U.ampl 50 mV t.meas 20.0 mst.step 0.20 s t.pulse 40.0 ms4 MEAS 90.0 U.meas -480 mV5 0STIR 20.06 SWEEP 14.8 U.start -530 mV U.step 4 mVU.end -250 mV Sweep rate 20 mV/s7 0MEAS U.standby mV8 ENDMethod: AB176_1aCALCULATIONmax. 15 lines--------------------------------------------------------------------------------Quantity Formula (R##, C##, A##) Res.unit Sig.dig.------------ ---------------------------------------- -------- --------Pb R1000=MC:Pb #g/L 5
Application Bulletin 176/4 eDetermination of lead and tin by anodic stripping voltammetryPage 5/5Full Report of a determination of Pb and Sn simultaneously acc. to method 1b with the 757 VA Computrace==================== METROHM 757 VA COMPUTRACE (5.757.0010) ====================Determ. : 06151514_Sn_Pb.dthDate : 1999-06-15 Time: 14:14:57Modified : 2000-12-05 13:48:06 User: Cell volume: 10.050 ml--------------------------------------------------------------------------------IdentSample volumesample5.000 ml--------------------------------------------------------------------------------Method : AB176_1.mthTitle : Determination of Sn and Pb. AB174 method 1aRemark1 : 5ml sample + 5ml electrolyte + 50µl cetyltrimethylammoniumbromideRemark2 : el.: 0.1mol/l trisodiumcitrate + 0.1mol/l oxalic acid + 0.2mol/l HCl--------------------------------------------------------------------------------Substance : SnCommentsMass conc.: 10.580 ug/l ------------------MC.dev. : 0.617 ug/l ( 5.83%)Mass : 106.331 ngAdd.mass : 100.000 ngVR V nA i.mean Std.Dev. i.delta Comments---- ----- ------ ------ ------- ------- ------------------1-1 -0.554 4.42 4.52 0.1451-2 -0.554 4.622-1 -0.554 8.59 8.71 0.167 4.192-2 -0.554 8.833-1 -0.550 12.84 12.71 0.184 4.003-2 -0.550 12.58Substance : PbCommentsMass conc.: 11.138 ug/l ------------------MC.dev. : 0.938 ug/l ( 8.42%)Mass : 111.936 ngAdd.mass : 100.000 ngVR V nA i.mean Std.Dev. i.delta Comments---- ----- ------ ------ ------- ------- ------------------1-1 -0.427 23.24 24.03 1.1261-2 -0.427 24.832-1 -0.423 45.69 46.13 0.615 22.092-2 -0.423 46.563-1 -0.423 66.87 65.76 1.564 19.643-2 -0.423 64.66Substance Calibr. Y.reg/offset Slope Nonlin. Mean deviat.--------- -------- ------------ ---------- ---------- ------------Sn std.add. 4.523e-009 4.282e-004 1.360e-010Pb std.add. 2.442e-008 2.201e-003 9.876e-010Final results +/- Res. dev. % Comments--------------------------------- ------------------ ------------------Sn = 21.266 µg/l 1.240 5.829Pb = 22.387 µg/l 1.885 8.419Method parameters of a determination of Pb and Sn simultaneously acc. to method 1b with the746 VA Trace Analyzer================== METROHM 746 VA TRACE ANALYZER (5.746.0101) ==================Method: AB176_1b.mthOPERATION SEQUENCETitle : Det.of Sn and Pb with CTAB. AB176 part 1b--------------------------------------------------------------------------------Instructions t/s Main parameters Auxiliary parameters------------- ----- ------------------------- -------------------------1 DOS/M V.added 5.050 mL2 REM 5mL sample + 5 mL electrolyte + 50 µL meth. blue3 SMPL/M V.fraction mL V.total L4 PURGE5 STIR 300.0 Rot.speed 2000 /min6 (ADD7 PURGE8 STIR 30.0 Rot.speed 2000 /min9 0PURGE10 (REP11 SEGMENT Segm.name asvSn12 REP)113 PURGE14 STIR Rot.speed 2000 /min15 ADD>M Soln.name Pb-std V.add 0.100 mL16 ADD>M Soln.name Sn-std V.add 0.100 mL17 ADD)218 ENDMethod: AB176_1bSEGMENTasvSn--------------------------------------------------------------------------------Instructions t/s Main parameters Auxiliary parameters------------- ----- ------------------------- -------------------------1 STIR 5.0 Rot.speed 2000 /min2 HMDE Drop size 4 Meas.cell normal3 DPMODE U.ampl 50 mV t.meas 20.0 mst.step 0.20 s t.pulse 40.0 ms4 MEAS 90.0 U.meas -700 mV
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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 4/4AppendixFull Report <strong>of</strong> a determination <strong>of</strong> Pb in presence <strong>of</strong> Sn (200 fold excess) acc. to method 1a with the757 VA Computrace==================== METROHM 757 VA COMPUTRACE (5.757.0010) ====================Determ. : 06161543_Pb(excessSn200).dthDate : 1999-06-16 Time: 14:43:09Modified : 2000-12-05 11:37:32 User: Cell volume: 10.050 ml--------------------------------------------------------------------------------IdentSample volumePb(excessSn200)5.000 ml--------------------------------------------------------------------------------Method : AB176_1.mthTitle : <strong>Determination</strong> <strong>of</strong> Pb. AB176 method 1aRemark1 : 5ml sample + 5ml electrolyte + 50µl cetyltrimethylammoniumbromideRemark2 : el.: 0.1mol/l trisodiumcitrate + 0.1mol/l oxalic acid + 0.2mol/l HCl--------------------------------------------------------------------------------Substance : PbCommentsMass conc.: 5.211 ug/l ------------------MC.dev. : 0.844 ug/l ( 16.19%)Mass : 52.366 ngAdd.mass : 50.000 ngVR V nA i.mean Std.Dev. i.delta Comments---- ----- ------ ------ ------- ------- ------------------1-1 -0.423 11.57 10.80 1.0961-2 -0.423 10.022-1 -0.423 21.18 20.44 1.040 9.642-2 -0.423 19.713-1 -0.423 30.37 31.01 0.907 10.573-2 -0.423 31.66Substance Calibr. Y.reg/<strong>of</strong>fset Slope Nonlin. Mean deviat.--------- -------- ------------ ---------- ---------- ------------Pb std.add. 1.060e-008 2.058e-003 9.879e-010Final results +/- Res. dev. % Comments--------------------------------- ------------------ ------------------Pb = 10.473 µg/l 1.696 16.190Method parameters <strong>of</strong> a determination <strong>of</strong> Pb in presence <strong>of</strong> Sn (200 fold excess) acc. to method 1a with the746 VA Trace Analyzer================== METROHM 746 VA TRACE ANALYZER (5.746.0101) ==================Method: AB176_1a.mthOPERATION SEQUENCETitle : Det.<strong>of</strong> Pb beneath Sn with CTAB. AB176 part 1a--------------------------------------------------------------------------------Instructions t/s Main parameters Auxiliary parameters------------- ----- ------------------------- -------------------------1 DOS/M V.added 5.050 mL2 REM 5mL sample + 5 mL electrolyte + 50 µL meth. blue3 SMPL/M V.fraction mL V.total L4 PURGE5 STIR 300.0 Rot.speed 2000 /min6 (ADD7 PURGE8 STIR 30.0 Rot.speed 2000 /min9 0PURGE10 (REP11 SEGMENT Segm.name asv12 REP)113 PURGE14 STIR Rot.speed 2000 /min15 ADD>M Soln.name Pb-std V.add 0.100 mL16 ADD)217 ENDMethod: AB176_1aSEGMENTasv--------------------------------------------------------------------------------Instructions t/s Main parameters Auxiliary parameters------------- ----- ------------------------- -------------------------1 STIR 5.0 Rot.speed 2000 /min2 HMDE Drop size 4 Meas.cell normal3 DPMODE U.ampl 50 mV t.meas 20.0 mst.step 0.20 s t.pulse 40.0 ms4 MEAS 90.0 U.meas -480 mV5 0STIR 20.06 SWEEP 14.8 U.start -530 mV U.step 4 mVU.end -250 mV Sweep rate 20 mV/s7 0MEAS U.st<strong>and</strong><strong>by</strong> mV8 ENDMethod: AB176_1aCALCULATIONmax. 15 lines--------------------------------------------------------------------------------Quantity Formula (R##, C##, A##) Res.unit Sig.dig.------------ ---------------------------------------- -------- --------Pb R1000=MC:Pb #g/L 5
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