Voltammetric Determination of Iron - Metrohm

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Application Bulletin 317/1 eVoltammetric Determination of IronPage 12/13797 VA Computrace method printout for Method 2 «Determination of iron in samples < 200 µg/L»--------------------------------------------------------------------------------Method parameters--------------------------------------------------------------------------------Method: AB317_2 Det of Fe below 200 ppb.mthTitle: Determination of Fe (TEA method)Remark1: 10 mL sample + 2 mL electrolyteRemark2: Electrolyte (0.05M TEA, 0.1M KBrO3, 0.3M NaOH)CalibrationTechniqueAddition: Standard addition: Batch: ManualSample ID : sampleSample amount (mL): 10.000Cell volume (mL): 12.000Voltammetric parameters--------------------------------------------------------------------------------Mode: DP - Differential PulseHighest current range: 10 mALowest current range: 100 nAElectrode: HMDEDrop size (1..9) : 4Stirrer speed (rpm) : 2000Initial electr. conditioning : YesStandard deviation : 0.50 %No. of additions : 2No. of replications : 2Measure blank: NoAddition purge time (s) : 60Initial purge time (s) : 300Conditioning cyclesStart potential (V) : -1.200End potential (V) : -0.100No. of cycles : 0Hydrodynamic (measurement) : NoCleaning potential (V) : -0.100Cleaning time (s) : 0.000Deposition potential (V) : 0.000Deposition time (s) : 0.000SweepEquilibration time (s) : 5.000Start potential (V) : -0.700End potential (V) : -1.250Voltage step (V) : 0.006Voltage step time (s) : 0.500Sweep rate (V/s) : 0.012Pulse amplitude (V) : 0.050Pulse time (s) : 0.040Cell off after measurement : YesPeak evaluation--------------------------------------------------------------------------------Regression technique: Linear RegressionPeak evaluation: HeightMinimum peak width (V.steps) : 5Minimum peak height (A): 1.000e-010Reverse peaks: NoSmooth factor : 4Eliminate spikes: YesSubstances--------------------------------------------------------------------------------Fe : -0.96 V +/- 0.050 VStandard solution : 1 10.000 mg/LAddition volume (mL) : 0.025default : Final result (Fe) =Conc * (12.1 / 10) * (1e+006 / 1) + 0 - 0
Application Bulletin 317/1 eVoltammetric Determination of IronPage 13/13746 Trace Analyzer method printout for Method 2 «Determination of iron in samples < 200 µg/L»================== METROHM 746 VA TRACE ANALYZER (5.746.0101) ==================Method: ab317_1 .mthOPERATION SEQUENCETitle : Determination of Iron in Water AB317 Part 1--------------------------------------------------------------------------------Instructions t/s Main parameters Auxiliary parameters------------- ----- ------------------------- -------------------------1 DOS/M V.added 2.000 mL2 REM Triethanolamine electrolyte3 SMPL/M V.fraction mL V.total L4 PURGE5 STIR 300.0 Rot.speed 2000 /min6 (ADD7 PURGE8 STIR 60.0 Rot.speed 2000 /min9 0PURGE10 (REP11 SEGMENT Segm.name DP12 REP)113 ADD>M Soln.name FeStd V.add 0.100 mL14 ADD)215 ENDMethod: ab317_1SEGMENTDP--------------------------------------------------------------------------------Instructions t/s Main parameters Auxiliary parameters------------- ----- ------------------------- -------------------------1 STIR 5.0 Rot.speed 2000 /min2 DME3 DPMODE U.ampl -50 mV t.meas 20.0 mst.step 0.50 s t.pulse 40.0 ms4 0STIR 5.05 SWEEP 43.5 U.start -700 mV U.step 6 mVU.end -1200 mV Sweep rate 12 mV/s6 0MEAS U.standby mV7 ENDMethod: ab317_1DOCUMENTATION--------------------------------------------------------------------------------Auto form feed noAuto error printing noCOPY Reports, CurvesTO Destination-------------------------------------------------- --------------------Report FullPrinterCurve Smth Sbst:Fe VR:**PrinterCurve Cal Sbst:FePrintersample preparation:10 mL sample+ 2 mL Triethanoamine electrolyteMethod: ab317_1SUBSTANCESFe - DP--------------------------------------------------------------------------------RecognitionDisplay / Plot------------------------- ---------------------------U.verify -1000 mV I.scale autoU.tol (+/-) 50 mV U.div 50.00 mV/cmU.width min 10 mV U.begin -700 mVU.width max 400 mV U.end -1200 mVI.threshold 100 pABaselineEvaluation------------------------- ---------------------------Type linear Mode VAScope whole Quantity I.peakdU.front auto Sign. digits 4S.front autodU.rear autoS.rear autoCalibration 2009-05-06 15:41:30 Coefficients--------------------------------- -------------------------Technique std.add. Y.reg -6.428e-08Curve type linear Slope -0.0004544Nonlin.Mean dev. 2.202e-09Additions------------------------------------------------------------Soln.name FeStd----------Mass conc. 10 mg/L g/L g/L g/LRange min 0 g/L g/L g/L g/LRange max g/L g/L g/L g/LM.conc./cm g/L g/L g/L g/LMethod: ab317_1CALCULATIONmax. 15 lines--------------------------------------------------------------------------------Quantity Formula (R##, C##, A##) Res.unit Sig.dig.------------ ---------------------------------------- -------- --------Fe R1000=MC:Fe #g/L 5
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Voltammetric Determination of Iron - Metrohm

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