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Analytical Chemistry IISomsak Sirichai
Lectures: Tuesday 1.00-3.00 p.m. Friday 8.00-9.00 a.m. C310
303354
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Course Description:Teach fundamental of instrumentation analysis
Spectrochemical analysis
Electrochemical analysis
Chromatographic analysis
Capillary Electrophoresis
UV-VIS, IR, Fluorescence & Phosphorescence,AA, ICP, X-ray, NMR, MS
Potentiometry, Coulometry, Voltammetry
GC, HPLC
CZE
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Gradings
• 2 exams (mid-term, final each worth 40%)• Quizzes (10%)• Paper (10%)
<40% F
Texts:Skoog & Leary, Principles of Instrumental Analysis*Weston & Brown, HPLC and CEKhaledi; High Performance Capillary Electrophoresis
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Introduction
AnalysisQualitative analysis (1)
Quantitative analysis (2)
(1) A type of chemical analysis by which the analyte or analytes in a sample are identified.
(2) A type of chemical analysis by which the amount of each analyte or analytes in a sample is determined.
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analyte(s)
matrix
Matrix-analyte = concomitants
the species to be determinded in the sample
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Classification of Analytical Methods
1. Classical methods
Qualitative – identification by color,indicators, boiling or melting points, odors
Quantitative – mass or volume(e.g. gravimetric, volumetric)
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2. Instrumental methodsQualitative – chromatography, electrophoresis and identification by measuring physical property (e.g. spectroscopy, electrode potential)
Quantitative – measuring property and determining relationship to concentration (e.g. spectrophotometry, mass spectrometry)
Often, same instrumental method used for qualitative and quantitative analysis.
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Types of Instrumental Methods
Signal Example MethodRadiation emission Emission spectroscopy (X-ray, UV, visible), fluorescence, phosphorescence, luminescence
Radiation absorption Absorption spectroscopy spectrophotometry, photometry, NMR electron spin resonance
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Signal Example MethodRadiation Scattering Raman spectroscopy Radiation refraction Refractometry
Radiation diffraction X-ray and Electron diffraction method
Radiation rotation Polarimetry
Electrical potential Potentiometry
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Signal Example MethodElectrical charge Coulometry Electrical current Voltammetry – amperometry polarography
Electrical resistance Conductometry
Mass Gravimetry
Mass-to-charge ratio Mass spectrometry
Rate of reaction Flow injection analysis
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Instruments for Analysis
DataEnergystimulus
Analytes
(in matrix)
Analyticalresponse
Example: SpectrophotometryInstrument: spectrophotometerStimulus: monochromatic light energyAnalytical response: photocellData: electrical currentData processor: current meterReadout: meter scale
Encodedinformation
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Encoded information: detector : device that indicates changes in environment transducer : device that converts non-electrical to electrical data
Non-electrical domians Electrical domains
Physical Current(light intensity, colour) Chemical (pH) Voltage
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Selecting an Analytical MethodDefining the ProblemA definition requires answers to the followingquestions:
1. What accuracy and precision are required?2. How much sample is available?3. What is the concentration range of the analyte?4. What components of the sample will cause interference?5. What are the physical and chemical properties of the sample matrix? 6. How many samples are to be analysed?
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Performance Characteristics ofInstruments; Figures of Merit
Precision: Indeterminate or random errors
• Absolute standard deviation (s)• Relative standard deviation (RSD)• Variance (s2)• Coefficient of variation (a percentage) (CV)• Standard deviation of means (sm)
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1
)(1
2
N
xxs
N
ii
xsRSD
%100xxsCV
Nss m
Absolute standard Deviation (s)
Relative standard deviation (RSD)
Coefficient of Variation (CV)
Standard deviation of means (sm)
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Accuracy: determinate errors (operator, method, instrumental)
% Relative error (%Er)
100% xxxx
Et
tir
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Sensitivity:“the ability to detect (qualitative analysis)or determine (quantitative analysis) small amounts of an analyte in a sample”
CxS x = analytical signal
C = the analyte concentration
Sensitivity : slope of calibration curve
(Larger slope of calibration curve,more sensitive measurement)
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Limit of detection (LOD): “the lowest concentration of analyte in a sample that can be detected”
slopes
C bLOD
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Limit of Quantitation (LOQ)“the minimum injected amount that producesquantative measurements in the target withacceptable precision”
slopes
C bLOQ
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Selectivity:“ability of the method to measure one species of analyte in the presence of other elements or compounds”
Example:
A + Bsample
Signal = mACA + mBCB + SignalblankmA, mB = calibration sensitivity of A, BCA, CB = concentration of A, BSelectivity coefficient: kB,A = mB/mA
k’s vary between 0 (no selectivity) and large number (very selective).
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Calibration methodsBasis of quantitative analysis is magnitude of measured property is proportional to concentration of analyte”
Signal [x] or
Signal = m[x] + signalblank
[x] = (signal-signalblank)/m
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Calibration curve (working or analytical curves)
Instrument response(signal)
Slope mSignalblank
LOD
LOQ
LOL
Dynamic Range
[x]