No.

231/2 e

Application Bulletin
Of interest to:

General analytical laboratories, Waters,
Environmental protection, Trace analysis

B 1, 2, 9, 16

Voltammetric determination of zinc, cadmium, lead,
copper, thallium, nickel, and cobalt in water samples
according to DIN 38406 Part 16
Summary
The prepared standard method in DIN 38406 Part 16, describes the determination
of Zn, Cd, Pb, Cu, TI, Ni and Co in drinking, ground, surface and precipitating (e.g.
rain) waters. Because the presence of organic substances in the water samples
can strongly interfere with the voltammetric determination, a pretreatment with UV
digestion using hydrogen peroxide is necessary. This digestion ensures the elimination of all organic substances without introduction of blank values.
These methods can, of course, also be applied for trace analysis in other materials,
e.g. trace analysis in the production of semiconductor chips with a silicium basis.
Zn, Cd, Pb, Cu and TI are determined on the HMDE by means of anodic stripping
voltammetry (ASV), Ni and Co by means of adsorptive stripping voltammetry
(AdSV).

Apparatus and accessories
• 746 VA Trace Analyzer with 747 VA Stand or
• 757 VA Computrace

Sample preparation
• Immediately upon taking the water sample, filter it through a microfilter (0.45
µm). The filtrates and filters with residues are treated separately. Acidify the filtrates, per litre, with 1 mL conc. HNO3 or HCI. The pH value of the acidified filtrates should lie between 1.7 and 2.0. If this is not the case, more acid must be
added.

Organic matter often interferes with voltammetric determinations and therefore
sample solutions usually have to be digested.

• If samples contain higher contents of humic acids. 231/2 e Voltammetric determination of Zn. filter residues and samples with organic matter (foods. • Low polluted waste waters can be digested with the 705 UV Digester. powdery residue forms.0 µg/L 0. The blank value of this digestion is relatively small. 50 mg/L 50 mg/L 50 mg/L 50 mg/L 50 mg/L 10 µg/L 10 µg/L • Samples with higher concentrations must be diluted. For methods 1 and 2 the sweep must be reversed from positive to negative potentials. please refer to Application Bulletin No.0 µg/L 0. • The blank values of the digestions and the chemicals must be taken into consideration.1 µg/L Concentration max.) must be digested. .1 µg/L 0.1 µg/L 0. these must be digested immediately to avoid formation of precipitation. The quartz tubes are irradiated for 1h at 90°C. Co Page 2 • Tap water. Pb.g. Ni.100 µL hydrogen peroxide w(H2O2) = 30% to 10 mL acidified samples (pH = 2). .1 µg/L 1. • Filters. open wet digestion with H2SO4 and H2O2 • Preparation of sample for the analysis of semiconductor chips: Place a drop of hydrofluoric acid w(HF) = 40% on chip and fume off by heating. • Metals with high concentrations (>50 mg/L) can also be determined on the DME or SMDE without enrichment. e. • If Fe must also be determined. the digested samples can be transferred directly to the polarographic vessel.High-pressure asher . . A white.According to Application Bulletin113. Prepare a blank value with the same reagents Remarks • These metals can be determined in the following ranges: Element Zn Cd Pb Cu Tl Ni Co Determination limits 1.Microwave digestion Both techniques oxidise the samples in a closed digestion vessel by means of a mixture of concentrated mineral acids. pharmaceutics etc. Tl. mineral waters and drinking waters can usually be analysed without pre-treatment. Cd. After cooling to room temperature. Add 50 . for trace analysis for the production of semiconductor chips.1 µg/L 0. • The analysis of the digested filters and that of the filtrates is identical. Dissolve this with a drop of nitric acid w(HNO3) = 65% and rinse into a polarographic vessel. 74.Application Bulletin No. surface waters.

1 mg/L 2+ β(Pb ) = 0. Pb. Only ultrapure water should be used. w(NaOH) = 30 % • Acetic acid.9 g KCl + 25 mL NaOH + 14. 315 (1983) 118-120 • Metrohm Application Bulletin No. Anal.W.5 mol/L 55.014 mol/L. β(Cu ) = 1 g/L (commercially available) 2+ Ready-to-use solutions: • KCl-sodium acetate solution: c(KCl) = 1.und Routinebestimmung von Zn. anal. (1984) 2141-2157 und AB 74 • Axel Meyer. Cd. Van den Berg Determining trace concentration of copper in water by cathodic film stripping voltammetry with adsorptive collection Anal. Goedde. suprapur. Chem. c(CH3COONa) = 0. β(Cd ) = 1 g/L (commercially available) 2+ • Pb stock solution. E16 Deutsche Einheitsverfahren. β(Pb ) = 1 g/L (commercially available) 2+ • Cu stock solution. Z. Thallium. Nürnberg Kontroll. Pb. Stöppler. Cd.Application Bulletin No. Kupfer. M.5 mol/L. Anal. M. • Standard solutions: β(Zn ) = 10 mg/L 2+ β(Cd ) = 0. Tl. Z. Nickel. Cadmium. Blei.5 mg/L Diluted solutions are prepared using c(HNO3) = 0. H. Cu. 231/2 e Voltammetric determination of Zn. Co Page 3 Literature • DIN 38406 Teil 16 Verfahren zur Bestimmung von Zink. 2+ . Pb and Cu Reagents All of the used reagents must be of purest quality possible (analytical grade or suprapur). suprapur • Zn stock solution. 113 Method 1 Determination of Zn. 318 (1984) 321-326 • Braun.2 mL CH3COOH filled up to 500 mL with high purity water. • Sodium hydroxide solution. Rolf Neeb Determination of cobalt and nickel by adsorption voltammetry in supporting electrolytes containing triethanolamine and dimethylglyoxime Fresenius. Metzger Umweltanalytische Nickel-Bestimmung durch Adsorptionsvoltammetrie mit der Quecksilberfilmelektrode Fresenius. Ni und Co mit differentieller Pulsvoltammetrie in Materialien der deutschen Umweltbank Fresenius. suprapur. Lett. β(Zn ) = 1 g/L (commercially available) 2+ • Cd stock solution. 318 (1984) 321-326 • G. Chem. Z. Ni. M.5 mg/L 2+ β(Cu ) = 2. Cobalt mittels Voltammetrie. Chem. • Ostapczuk. 17 A. Cd. w(CH3COOH) = 100 % • KCl.

05 V 0.10 V The concentration is determined by standard addition. 50 mV. Tl. If the sample contains no chloride.06 V/s . The voltammogram is recorded with the following parameters: Working electrode Drop Size Stirrer/RDE Measurement mode Purge time Pulse amplitude Deposition potential Deposition time Equilibration time Start potential End potential Voltage step Voltage step time Sweep rate Peak potential (Zn) Peak potential (Cd) Peak potential (Pb) Peak potential (Cu) HMDE 4 2000 rpm DP 300 s 0. c(NH3) = 1 mol/L 55.38 V .6 can be used instead of KCl-sodium acetate solution. • If the Tl concentration is more than 50% of the Pb concentration it is not recommended to use method 1 for determination of Pb. Cd.5 mL w(CH3COOH) = 100 % + 37 mL w(NH3) = 25 % filled up to 500 mL.6: c(CH3COOH) = 2 mol/L.0. NH4 acetate buffer pH 4.1.1 s 0.0. Co Page 4 Analysis Measuring solution: 10 mL (diluted) sample + 1 mL KCl-sodium acetate solution If necessary. • Seeing that the difference of the half wave potentials of TI and Pb is only approx.05 V).006 V 0. the TI content is then determined according to method 2. 231/2 e Voltammetric determination of Zn. adjust the pH of the solution should to 4. Cd. In this case.05 V . An alternative is a post-electrolysis where a large quantity of the Tl deposited on the electrode is removed before the determination of Pb.0. Pb and Cu.15 V 0. Pb. following the analysis of Zn.2. which are easier to evaluate. it is preferable to use this buffer instead of the KCI/Na acetate solution.15 V 90 s 10 s .1. • Zn is often present in tap water in higher concentrations as the other metals. .Application Bulletin No. Zn should be determined separately with shorter enrichment time or after being diluted to a greater extent. Cu achieves peaks with more positive potential (Peak potential Cu: +0.0. Remarks • Ammonium acetate buffer pH 4. TI and Pb are determined together in acetate solutions. For this reason.6 ± 0.56 V . If the concentration of Tl is less than 50% of the concentration of Pb the error for the Pb determination is less than 10%. Ni.98 V .

00023 5. Peak potential Tl Peak potential Pb Peak potential Cd -0. With this electrolyte it is possible to separate the peaks of Pb and Tl.00 -0.80 -0.00n 1.50u 6.20u 1.50u 2.00u Zn Cu 150n 2.0 . Lead.00u 1.00 E (V) Zn c = +/- Cd c = n/a 0.0 .Application Bulletin No.00n 800n 1.0 n Cd 1.60 -0. to DIN38406/16 tap water 3.68 V Figures Determination of Zinc. Cadmium.20 0.01%) 8.40 0 .2 0 500n Cd Pb -0.61 V -0.00n i (A) i (A) 1.43 V -0.0 0 Cu 0 -1. 231/2 e Voltammetric determination of Zn.00n 500n 0 -200u -100u 0 c / (g/l) 100u 200u 4.6 0 . Ni. Cd.00u -0.50u 100n i (A) i (A) 2. Tl.4 0 E (V ) -0 .80u . But in this case Cd interferes the determination of Pb.60u c / (g/l) 1.015 mg/l (6.00u 1. Pb.258 mg/l 0.00u 0 .50u Pb 5 0 .00u 7.00n 2. and Copper acc. Co Page 5 • Another possibility is the determination of Pb and Tl at a pH>12 (NH3Cl buffer according to method 3 + NaOH).40u 1.

: n/a Add.596 -0.Dev. to DIN38406/16 Remark1 : 10 ml sample + 1 ml acetate buffer (1. in scan Ovl.delta ------.Dev.------0.000 i.757.delta ------.5mol/l KCl + 0.mean -----1.466 -0.215 7.: 6. Cd.5mol/l NaAc) Remark2 : pH 4. in scan Ovl.000 ml -------------------------------------------------------------------------------Ident Sample volume tap water 10.044 0.008 9.483 ug/l i.853 Comments -----------------No peak found No peak found Ovl.000 ug VR ---1-1 1-2 2-1 2-2 3-1 3-2 V uA ----.13 -0.485 ug/l -----------------MC.596 Substance : Pb Mass conc. Pb. Ni. Lead.441 Add. in scan 36.052 0.403 11.345 Std. i. Cadmium. i.191 0.663 Substance : Cd Mass conc.23 Substance : Cu Mass conc. in scan Ovl. i.989 2.222 MC. in scan Ovl.dev.223 µg/l (3.: 234.------0.03 -0.061 -0. 231/2 e Voltammetric determination of Zn.400 15.400 27.237 3.Dev.989 1.989 2.000 VR ---1-1 1-2 2-1 2-2 3-1 3-2 VR ---1-1 1-2 2-1 2-2 3-1 3-2 Comments ------------------ 2.0u c / (g/l) c / (g/l) ==================== METROHM 757 VA COMPUTRACE (5. and Copper acc.0010) ==================== Determ.6 -------------------------------------------------------------------------------Substance : Zn Comments Mass conc.0n 10.024 Comments ------------------ V ---------0.57 Ovl.339 Comments ------------------ 26.086 ug/l ( 6.979 µg/l 0.3e-006 -6. in scan ng nA ---------4.579 ug Add.877 8.583 Ovl.19%) 125n 30. : 14.82%) 6.0n i (A) i (A) 20.362 Mass : 68.400 37.0u 40.0u 10.mass : 10.dth Date : 2001-06-05 Time: 15:47:51 Modified : 2001-06-05 15:48:55 User: Cell volume: 11.626 0. in scan Comments ------------------ .84 0.mass : 50.Application Bulletin No.596 -0.0n 100n 75.------0.dev.------0. Tl.82%) i.01%) Mass : 2.168 4. : 06051547_tap water.596 -0.0u 30.2e-006 0 0 -5.27 Std.0u 0 10.delta ------.mth Title : Determination of Zinc.mean -----15.400 35.042 0.050 8.026 0.024 -0. in scan 2.mean -------- Std.51 -0.0n 50.56 -0.400 26.398 µg/l (5.81 -0.mass : 1.501 -0.211 ug/l ug/l ng ng V nA ----.0u 20.989 2.844 µg/l 0.--------- 4.989 2.: 6.000 ml -------------------------------------------------------------------------------Method : AB231_1_Det of Zn Cd Pb Cu with HMDE.400 15. : 0.00u 0 5.559 Ovl.52 1.: n/a MC.0n -6. in scan Comments ------------------ ( 5.68 Ovl.589 -0.0n 25.989 1.dev.00u -10. Co Page 6 Pb c = +/- Cu c = +/- 6.

746. i.258 mg/l Cd = n/a µg/l Pb = 6.add.480e-006 2.193 Fig.349 Comments ------------------ 76.10 s U. ---------- +/.meas -1150 mV Auxiliary parameters ------------------------- U.mth OPERATION SEQUENCE Title : Det.3 Ovl.477e-003 2. std.8 -0.6 Calibr. Cu acc. std.add 0.844 µg/l Cu = 6.0 0PURGE (REP SEGMENT REP)1 PURGE ADD>M ADD)2 END Main parameters ------------------------V.0101) ================== Method: AB231_1 .----SMPL>M DOS>M PURGE STIR 300. dev. std.120 76.354e-003 2. Cu according to method 1 with the 746 VA Trace Analyzer . Co Page 7 MC. 2 Parameters for the determination of Zn.------0.add. -----------2.114 126.0 20.2 Ovl. Cd.398 0.462e-010 Comments ------------------ 5.007 0.meas t.name buffer Rot.0 ms 6 mV 60 mV/s Fig.0 10.015 6. ( 3.120 77. -------std. in scan Ovl.end U.100 mL Method: AB231_1 SEGMENT ZnCdPbCu -------------------------------------------------------------------------------- 1 2 3 Instructions t/s ------------.----STIR 5.8 0.203 69.cell t.278e-010 3.5 -0.612e-010 3.626e-003 Nonlin.132 16.538e-008 1.name ZnCdPbCu Auxiliary parameters ------------------------V.114 129.------0.684 60. to DIN 38406/16 -------------------------------------------------------------------------------- 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 Instructions t/s ------------.Application Bulletin No.3 Main parameters ------------------------Rot.19%) i. 231/2 e Voltammetric determination of Zn.309e-008 2. 1 Determination of Zn.3 -0.total L V. Cd.speed 2000 /min Drop size 4 U.add. % -----------------0.add 1.5 Std.dev.979 µg/l Slope ---------6.pulse normal 20. of Zn. Pb.Dev. Tl.standby U.0 ms 40.name ZnCdPbCu Soln.mass : : : 0. Pb.speed 2000 /min Rot. in scan Y. Mass Add. Cd.fraction mL Soln.223 Mean deviat.step Sweep rate -1150 mV 50 mV mV Meas.687e-010 1.3 -0.add.delta ------.260 51.Res.1 2. Ni.000 mL V.0 (ADD PURGE STIR 10. Cd. Pb and Cu according to method 1 with the 757 VA Computrace ================== METROHM 746 VA TRACE ANALYZER (5.0 HMDE DPMODE 4 5 6 MEAS 0STIR SWEEP 7 8 0MEAS END 90.4 -0.speed 2000 /min Segm.132 16.step 0.328e-003 4. Pb.ampl 50 mV t.665e-008 Final results --------------------------------Zn = 0.mean -----16.822 3.791 250.start U.000 VR ---1-1 1-2 2-1 2-2 3-1 3-2 Substance --------Zn Cd Pb Cu ug/l ng ng V nA ----. in scan 128.reg/offset -----------1.

45 V The concentration is determined by standard addition. • EDTA solution: c(EDTA) = 0. .5 mol/L 55. w(NaOH) = 30 % • Acetic acid. w(CH3COOH) = 100 % • KCl. Pb.0. Only ultrapure water should be used.05 V . c(CH3COONa) = 0. suprapur.93 g Na2-EDTA·2H2O in H2O and fill up to 25 mL.0.p.5 mol/L. Ni.0. • Standard solution: β(Tl ) = 0. β(Tl ) = 1 g/L (commercially available) + Ready-to-use solutions: • KCl-sodium acetate solution: c(KCl) = 1.0.2 mL CH3COOH filled up to 500 mL with high purity water.8 V 180 s 10 s .006 V 0.2 V 0.a. Tl.2.014 mol/L. Co Page 8 Method 2 Determination of Tl Reagents All of the used reagents must be of purest quality possible (analytical grade or suprapur).Application Bulletin No. suprapur • Ethylenediaminetetraacetic acid disodium salt dihydrate. suprapur. 231/2 e Voltammetric determination of Zn. CAS 638192-6 • Tl stock solution. • Sodium hydroxide solution. + Analysis Measuring solution: 10 mL (diluted) sample + 1 mL KCl-sodium acetate solution (or measuring solution from method 1) + 200 µL EDTA solution If necessary.9 g KCl + 25 mL NaOH + 14. The voltammogram is recorded with the following parameters: Working electrode Stirrer/RDE Drop size Measurement mode Purge time Pulse amplitude Deposition potential Deposition time Equilibration time Start potential End potential Voltage step Voltage step time Sweep rate Peak potential (Tl) HMDE 2000 rpm 4 DP 300 s 0.1 mol/L: Dissolve 0. puriss.06 V/s .5 mg/L Diluted solutions are prepared using c(HNO3) = 0.6 ± 0. Cd. adjust the pH of the solution should to 4..1 s 0.8 V .

000 ml -------------------------------------------------------------------------------Method : AB231_2_Det of Tl.28%) Mass : 3.00n 4.764 Calibr.mean -----0.0010) ==================== Determ.530 Std.mth Title : Determination of Thallium acc.050 2.461 2.00n -2.461 0. % -----------------0.281 Mean deviat.192 ng Add.5mol/l NaAc) Remark2 : + 200µl EDTA-Na2 (0.812 -0.461 2.reg/offset -----------5. : 06051653_tap water_Tl.dth Date : 2001-06-05 Time: 16:53:19 Modified : 2001-06-05 17:01:16 User: Cell volume: 11. Tl.063 -0.60 -0.073 1.455 3. to DIN38406/16 Remark1 : 10 ml sample + 1 ml acetate buffer (1. 3 Determination of Tl according to method 2 with the 757 VA Computrace .815e-003 Comments ------------------ Nonlin.Application Bulletin No.114 0.00n 2.674 Y.511 -0.add.00n 2.50 -0. to DIN38406/16 tap water_Tl Tl c = +/- 0.788 0.549 -0. ---------- +/.dev.30 0 500n E (V) 1. : 32.036 µg/l (11. i.207e-010 Final results --------------------------------Tl = 0. Co Page 9 Figures Determination of Thallium acc. Ni.70 -0.755e-011 Comments ------------------ Fig.------0.00u 1. i.00n 3.Res.mass : 10.9e-007 0 -0.------0.00n 1.597 ng/l -----------------MC.28%) Tl 6.050 1.319 µg/l 0.319 µg/l Slope ---------1.584 3.1 mol/l) -------------------------------------------------------------------------------Substance : Tl Comments Mass conc. 231/2 e Voltammetric determination of Zn. Cd.467 0.461 3. Pb.00u c / (g/l) ==================== METROHM 757 VA COMPUTRACE (5.757.delta ------.5mol/ol KCl + 0.444 ng/l ( 11.Dev.40 -500n -0.00n i (A) i (A) 5.100 ml -------------------------------------------------------------------------------Ident Sample volume tap water_Tl 10.036 11.00n 3.000 ng VR ---1-1 1-2 2-1 2-2 3-1 3-2 Substance --------Tl V nA ----. dev. -----------4.50u 2.: 287.165 -0. -------std.

w(HCl) = 30% • Dimethylglyoxim disodium salt octahydrate.step 0. CAS 75006-64-3 • Ni stock solution. c(NH3) = 2 mol/L 112.start U. Pb.5: c(NH4Cl) = 1 mol/L.name Tl_Std Auxiliary parameters ------------------------V.ampl 50 mV t.5 mL NH3 + 53 mL HCl.name buffer Soln.020 mL Method: AB231_2 SEGMENT Tl_Seg -------------------------------------------------------------------------------- 1 2 3 Instructions t/s ------------.3 Main parameters ------------------------Rot.end U.a.0 10.total L V.name EDTA_sol Rot.speed 2000 /min Rot. • Ammonia solution. Only ultrapure water should be used.cell t. β(Ni ) = 1 g/L (commercially available) 2+ • Co stock solution.304 g Dimethylglyoxim disodium salt in 10 mL ultrapure water.Application Bulletin No.0 0PURGE (REP SEGMENT REP)1 PURGE ADD>M ADD)2 END Main parameters ------------------------V. • Standard solutions: β(Ni ) = 1 mg/L 2+ β(Co ) = 0. filled up to 500 mL with high purity water.0 10. suprapur.0 ms 40. Tl.meas -800 mV Auxiliary parameters ------------------------- U. Ni.014 mol/L.speed 2000 /min Segm.meas t. • DMG solution: c(Na2DMG) = 0.----STIR 5.1 mol/L Dissolve 0. to DIN 38406/16 -------------------------------------------------------------------------------- 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 Instructions t/s ------------. 231/2 e Voltammetric determination of Zn. Cd. 4 Parameters for the determination of Tl according to method 2 with the 746 VA Trace Analyzer Method 3 Determination of Ni and Co Reagents All of the used reagents must be of purest quality possible (analytical grade or suprapur).mth OPERATION SEQUENCE Title : Det.p.pulse normal 20. 2+ .add 1.standby U. β(Co ) = 1 g/L (commercially available) 2+ Ready-to-use solutions: • NH4Cl buffer pH 9.10 s U.000 mL V.name Tl_Seg Soln.fraction mL Soln.0 HMDE DPMODE 4 5 6 MEAS 0STIR SWEEP 7 8 0MEAS END 180.add 0. puriss. of Tl acc. w(NH3) = 25% • Hydrochloric acid.step Sweep rate -800 mV -200 mV mV Meas.0101) ================== Method: AB231_2 . Co Page 10 ================== METROHM 746 VA TRACE ANALYZER (5. suprapur.0 (ADD PURGE STIR 10.1 mg/L Diluted solutions are prepared using c(HNO3) = 0.0 ms 6 mV 60 mV/s Fig.speed 2000 /min Drop size 4 U.----SMPL>M DOS>M DOS>M PURGE STIR 300..746.add 0.200 mL V.

0.013 V/s .8 V .5 ± 0. Ni.13 V The concentration is determined by standard addition. Co Page 11 Analysis Measuring solution: 10 mL (diluted) sample + 0.004 V 0.2. .97 V .1. The voltammogram is recorded with the following parameters: Working electrode Drop size Stirrer/RDE Measurement mode Purge time Pulse amplitude Deposition potential Deposition time Equilibration time Start potential End potential Voltage step Voltage step time Sweep rate Peak potential (Ni) Peak potential (Co) HMDE 4 2000 rpm DP 300 s 0. Pb.05 V .5 mL NH4Cl buffer + 0.29 g DMG in ethanol and fill up to 25 mL. or DMG in triethanolamine: c(DMG) = saturated Dissolve 500 mg dimethylglyoxime in 100 mL TEA:H2O (1:1). Remarks • If the disodium salt of the dimethylglyoxime should not be used. Cd. DMG in ethanol: c(DMG) = 0. adjust the pH of the solution should to 9. • Na2-Iminodiacetate 0.3 s 0.0. This solution is used when a big excess of Zn disturbs the Co determination. DMG can be dissolved in ethanol or triethanolamine.1 mL DMG solution If necessary.1 mol/L Dissolve 0. Tl.Application Bulletin No. 231/2 e Voltammetric determination of Zn. Our tests have shown that the determination of Ni besides Co is then not possible any more because Ni is also complexed.0.7 V 90 s 10 s .2 mol/L: This solution is used in the DIN norm to mask Zn by the Co determination.1.25 V 0.

000 ng VR V nA ---1-1 1-2 2-1 2-2 3-1 3-2 Substance : Co i.------.39%) 2.3 -0.0n -50.80 -0.4 -0.: 557.00 -1.927 -29.927 -31.90 -1.0n -100n -15.6e-009 -5.6e-007 0 0 -500n 0 500n 1.00n -25.6 3. : 41. : 09151108_MeerwasserNiCo.529 ng/l (18.927 -82.mass : 10.258 -47.276 -0. i.10 -1.9 ------------------ Comments .delta Comments ----.757.927 -78.656 ng/l -----------------MC. Co Page 12 Figures Ni + Co in Meerwasser Meerwasser -150n Ni -125n i (A) -100n -75.0n -5. Pb.Application Bulletin No.Dev.0n Co -25.dev.0n 0 -0.9 -0.220 ng/l ( 7.8 -0.0010) ==================== Determ.0n -10.mth Title : Ni + Co in Meerwasser Remark1 : -------------------------------------------------------------------------------Substance : Ni Comments Mass conc.3 -128.00u 0 50.967 -50. Cd. 231/2 e Voltammetric determination of Zn.5 -30.mean Std.39%) Mass : 6.-------0.77%) -25.050 ml -------------------------------------------------------------------------------Ident Sample volume Meerwasser 10.162 ng Add.-----.-----.820 ng/l 0.8 2.0n -50.616 ug/l 0. Ni.0n c / (g/l) 100n 150n c / (g/l) ==================== METROHM 757 VA COMPUTRACE (5.dth Date : 1999-09-15 Time: 11:08:54 Modified : --User: Cell volume: 11.20 E (V) Ni c = +/- Co c = +/- 0.046 ug/l (7.923 -130.000 ml -------------------------------------------------------------------------------Method : Ni-Co Meerwasser.927 -126.50u 2.7 -80.00u 1.0n -125n -20.0n i (A) i (A) -75.4 1. Tl.0n -2.

290 -12.----.93 Substance --------Ni Co Calibr. Y.552 ng/l MC. Co acc.34 0.meas -700 mV Auxiliary parameters ------------------------- U. : 0.91 2-2 -1.reg/offset ------------3.start U.delta Comments ---.086 -0.999e-011 Comments ------------------ Fig.fraction mL Soln.820 ng/l Slope ----------5. Cd.02 1. Co Page 13 Mass conc.616 ug/l Co = 2.082 -24. -------std. Pb.-----.add.050 1-2 -1.name buffer Soln. std. Tl.046 7.: 2.name DMG_sol Rot.Application Bulletin No.step Sweep rate -700 mV -1300 mV mV Meas.479 ng/l ( 18.mass : 1.-----.392 0. dev. Ni.429e-010 Final results --------------------------------Ni = 0.500 mL V.0 0PURGE (REP SEGMENT REP)1 PURGE ADD>M ADD)2 END Main parameters ------------------------V. -----------1. of Ni.add 0.482e-002 -1.201 pg Add.0 45.086 -11.354e-001 ------------------ ------------------ Nonlin.end U.100 mL V. 6 Parameters for the determination of Ni and Co according to method 3 with the 746 VA Trace Analyzer .77%) Mass : 28.pulse normal 20.254e-009 4.----SMPL>M DOS>M DOS>M PURGE STIR 300.746.add.step 0.name NiCo_Std Auxiliary parameters ------------------------V.mean Std.Res.0 HMDE DPMODE 4 5 6 MEAS 0STIR FSWEEP 7 8 0MEAS END 90. to DIN 38406/16 -------------------------------------------------------------------------------- 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 Instructions t/s ------------.----STIR 5.62 -12.standby U.529 18.mth OPERATION SEQUENCE Title : Det.32 -0.086 -12.0 (ADD PURGE STIR 10.30 s U.cell t.082 -25.10 -25.meas t.76 3-2 -1.010 mL Method: AB231_3 SEGMENT NiCo_Seg -------------------------------------------------------------------------------- 1 2 3 Instructions t/s ------------.049e-008 -3.000 ng VR V nA i.900 -11.add 0. ---------- +/.0 ms 4 mV 13.0 10.0 ms 40.------.Dev.33 mV/s Fig.770 Mean deviat.89 3-1 -1.------1-1 -1.name NiCo_Seg Soln.add 0.0101) ================== Method: AB231_3 .speed 2000 /min Rot.speed 2000 /min Segm. 5 Determination of Ni and Co according to method 3 with the 757 VA Computrace ================== METROHM 746 VA TRACE ANALYZER (5.speed 2000 /min Drop size 4 U.total L V.dev.089 -0. i. % -----------------0.ampl -50 mV t. 231/2 e Voltammetric determination of Zn.26 0.9 Main parameters ------------------------Rot.37 2-1 -1.