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(Elemental) Analysis Modern Methods in Heterogeneous Catalysis Research 29.10.2004 Chemical (Elemental) Analysis Raimund Horn Dep. of Inorganic Chemistry, Group Functional Characterization, Fritz-Haber-Institute of the Max-Planck-Society Outline 1. Introduction 1.1 Concentration Ranges 1.2 Accuracy and Precision 1.3 Decision Limit, Detection Limit, Determination Limit 2. Methods for Quantitative Elemental Analysis 2.1 Chemical Methods 2.1.1 Volumetric Methods 2.1.2 Gravimetric Methods 2.2 Electroanalytical Methods 2.2.1 Potentiometry 2.2.2 Polarography Outline 2.6 Spectroscopic Methods 2.6.1 Atomic Emission Spectroscopy 2.6.2 Atomic Absorption Spectroscopy 2.6.3 Inductively Coupled Plasma Mass Spectrometry 2.6.4 X-Ray Fluorescence Spectroscopy 2.6.5 Electron Probe X-Ray Microanalysis 3 Specification of an Analytical Result 4 Summary 5 Literature Backup Slide The Analytical Process strategy problem solution characterization representative sampling chemical sample object of investigation information preparation measurement evaluation data diminution analysis smaller sample for measurement analytical sample measurement data result Backup Slide The Analytical Process strategy problem interpretation characterization representative sampling chemical sample object of investigation information preparation measurement evaluation data diminution analysis smaller sample for measurement analytical sample measurement data result Backup Slide Analytical Problems in Science, Industry, Law… Science Industry Law example: Determination by X- example: manufacturer of iron - example: Is the accused guilty ray Absorption Spectroscopy of Shall I by this iron ore or not ? or not guilty ? the Fe-Fe Separation in the Oxidized Form of the Hydroxylase of Methane Monooxygenase Alone and in the Presence of MMOD Rudd D. J., Sazinsky M. H., Merkx M., et al. Inorg. Chem. 2004, 43 (15), 4579-4589, 2004 Motivation Motivation fundamental interest Motivation human fate money future developments murder conviction precision (e.g.) genetic fingerprint fits – lifelong 53 ± 5wt% vs. 53 ± 1wt% prison genetic fingerprint does not fit - accuracy (e.g.) acquittal 53 ± 1wt% vs. 51 ± 1wt% 1. Introduction 1.1 Concentration Ranges concentration ranges in elemental analysis trace components side main components components 1 ppt 1 ppb 1 ppm 1 ‰ 1 % 100 % ppt (w/w) ppp (w/w) ppm (w/w) ‰ (w/w) % (w/w) 10-12 g/g 10-9 g/g 10-6 g/g 10-3 g/g 10-2 g/g pg/g ng/g µg/g mg/g 0.01 g/g ng/kg µg/kg mg/kg g/kg 10 mg/kg 1. Introduction 1.1 Concentration Ranges mass ratio 10-2 10-3 10-6 10-9 10-12 1 % 1 ‰ 1 ppb 1 ppt 0.27 L 2.7 L 2 700 000 L 2 700 L 1 ppm 2 700 000 000 L concentration ranges in trace analysis 2.7 g 1. Introduction 1.2 Accuracy and Precision accuracy: precision (uncertainty): Ø can be defined as the Ø describes in a positive (negative) consistency between the mean manner the influence of random of an analytic result and the errors on an analytic result value held as the true value Ø describing quantities: Ø has to be verified before each analysis by means of standards 2 å (xi - x) Ø describing quantities: s = i Gaussian n - 1 distributed errorx = ± x - xˆ' errors! 2 ± x - xˆ' wrong å (xi - x) 2 i relative errorx = ×100 v = s = xˆ' results n -1 main and trace and side ultra trace component analysis analysis 1. Introduction 1.3 Decision Limit, Detection Limit, Determination Limit Ø the lower the concentration of an analyte, the more difficult becomes its qualitative detection and its quantification Ø stochastic errors become more and more pronounced Ø the decision limit and the detection limit are lower limits characterizing the performance of a method to discriminate a true value from a blank value Ø the determination limit guaranties the quality of a quantitative result (user specific) t × s t × s y = y + f ,a B Þ y = y + bx Þ x = f ,a B k B n k B NG NG b× n for a = b x = 2× x EG NG DIN 32645 2. Methods for Quantitative Elemental Analysis 2.2 Electroanalytical 2.1 Chemical Methods Methods 2.3 Spectroscopic Methods Ø atomic emission Ø atomic absorption Ø volumetric methods Ø potentiometry Ø inductively coupled plasma mass Ø gravimetric methods Ø polarography spectrometry Ø X-ray fluorescence Ø electron probe X-ray microanalysis 2.1 Chemical Methods 2.1.1 Volumetric Methods - Principle principle of volumetric methods evaluation of the result 100 p = VB × k × N × in % me p = percentage of the analyte in the sample VB = volume in ml dropped in from the burette k = stoichiometric factor (mg analyte/ml) A + B ® C + D N = correction factor for the theoretical value k e = weighted sample (in mg) 2 2 æ s ö æ s ö 2 s P me VB æ s N ö = ç ÷ + ç ÷ + ç ÷ Ø fast, complete and stoichiometric well p è me ø è VB ø è N ø defined reaction inserting typical values Ø the extend of the reaction can be monitored (e.g. pH, electric potential) s 0.1% < P < 1% Ø the point of equivalence can be p detected precisely (e.g. sudden color change, steep pH or potential change) advantage: high precision!!! 2.1 Chemical Methods 2.1.1 Volumetric Methods – Acid Base Titration n- + acid – base reaction: HnA + nBOH V A + nB + nH2O (zA=n, zB=1) zB ×CB ×VB Ka VS +V æ K w - pH ö + - titration curve: t = = - pH + ×ç - pH - 10 ÷ K w = [H ][OH ] zA ×C A ×VA 10 + Ka C S ×VS è 10 ø strong acid – strong base weak acid – strong base different Ka – strong base - H+ + H+ pH = pK a,Ind ± 1 Ø choice of the indicator depends on Ka Ø very weak acids (bases) can be titrated in non-aqueous solvents as liquid ammonia or 100% acetic acid 2.3 Chemical Methods 2.1.1 Volumetric Methods - Complexometry m+ m+ complex formation: nL + M V MLn most used ligand - EDTA n- m+ (m-4) + H4-nY + M V [MY] + (4-n)H (zA=1, zB=1) [MY (m-4) ] [M m+ ] = K f ×[EDTA]total ×aY 4- complex formation only with Y4- Þ buffer required indication: HI2- + Mm+ V MI(m-3) + H+ e.g. Eriochromschwarz T applicable for the determination of: Mg2+, Ca2+, Sr2+, Ba2+ at pH 8-11 Mn2+, Fe2+, Co2+, Ni2+, Cu2+, Zn2+, Cd2+, Al3+, Pb2+, VO2+ at pH 4-7 Bi3+, Co3+, Cr3+, Fe3+, Ga3+, In3+, Sc3+, Ti3+, V3+, Th4+ at pH 1-4 2.1 Chemical Methods 2.1.1 Volumetric Methods – Redox Titration redox reaction: nBOxB + nARedA V nBRedB + nAOxA (zA=nB, zB=nA) - 2+ + 2+ 3+ examples: MnO4 + 5Fe + 8H V Mn + 5Fe + 4H2O Ce4+ + Fe2+ V Ce3+ + Fe3+ titration curve z ×C ×V t = A A A zB ×CB ×VB Q RT t 0 < t < 1 U = U A = U A + × ln nB F 1-t Q Q nAU B + nBU A t = 1 Ueq = nA + nB Q RT t > 1 U = U B = U B + × ln(t - 1) nAF - 2+ indication: self indication (violet MnO4 ® colorless Mn ) - redox indicator (InRed F InOx + ne ) potentiometric endpoint detection 2.1 Chemical Methods 2.1.2 Gravimetric Methods precipitation reaction: n M z+ (aq) +n Az- (aq) « M A (s) + - n + n - Ø precipitation of the ion to be determined by a suitable precipitating agent Ø filtering and washing of the precipitate Ø transformation into a compound of well defined stoichiometry (drying/calcination) ® weighing examples 2+ 2- 2+ 2- -10 2 2 Ba + SO4 F BaSO4 (KL=[Ba ]×[SO4 ]=1×10 mol /l ) as BaSO4 3+ - 3+ - 3 -38 4 4 Fe + 3OH F Fe(OH)3 (KL=[Fe ]×[OH ] =1×10 mol /l ) as Fe2O3 n - n + z+ æn + ö z- æn - ö n + +n - ç ÷ n + +n - ç ÷ [M ] = K L ç ÷ [A ] = K L ç ÷ èn - ø èn + ø [M z+ ]×V Ø for analytical purposes: a p = 1- z+ ³ 0.997 [M ]o ×V0 2 2 Ø advantage æ s ö æ s ö s m me ma s m = ç ÷ + ç ÷ 0.01% < < 0.1% Þ one of the most precise analytical methods m è me ø è ma ø m 2.2 Electroanalytical Methods electrode reaction, IFaraday=0 (potentiometry) Ø ion-selective electrodes Ø potentiometric titration electrode reaction, DC, no electrode I ¹0 (voltametry) Faraday electroanalytical reaction, AC, high Ø polarography methods frequency Ø coulometry Ø conductometry electrode reaction, AC, IFaraday¹0 Ø AC polarography 2.2 Electroanalytical Methods 2.2.1 potentiometry, potentiometric titration Ø principle Þ measurement of the cell potential (potential between two electrodes at zero current) Ø relation of the cell potential and the analyte concentration typical reference electrode calomel electrode - - Hg2Cl2(s) + 2e V 2Hg(l) + 2Cl 0.05916V E = E 0' - log[Cl - ]2 2 Ø electrolyte = saturated KCl solution (3.8mol/l at 25°C) Þ [Cl-] = constant Þ ref. pot. E = const. 2.2 Electroanalytical Methods 2.2.1 Potentiometry, Potentiometric Titration pH measurement with the glass electrode Cl- determination with a silver electrode + - Ag + Cl V AgCl(s) -10 2 2 KL=1.8×10 mol /l 0 2.303RT 1 E Ag = E Ag / Ag+ - log 1× F a Ag + 0 - E Ag = E Ag / Ag+ + 0.059log K L - 0.059log[Cl ] + + Ag/AgCl/KClsat/H in/H out/KClsat/AgCl/Ag RT E = Dj + Dj + ln10×( pH - pH ) As Diff F in out 2.2 Electroanalytical Methods 2.2.2 Polarography Ø measurement of current – voltage curves (voltametry) gives information of the chemical composition and the concentration of the analytes in the sample -6 -3 (working range 1×10 < cA < 1×10 mol/l) Ø polarography was invented in 1922 by Jaroslav Heyrovsky (Nobelprice 1959) electrode arrangement for polarographic measurements Ø a polarographic cell contains: a polarizable working electrode (dropping mercury electrode) a non-polarizable counter electrode (e.g.
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