Chapter 1: Introduction

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Chapter 1: Introduction Chapter 1: Introduction Analytical Chemistry Analytical Chemistry Qualitative analysis Qualitative analysis Quantitative analysis Quantitative analysis Classification of Analytical Classification of Analytical Methods Methods Classical methods (wet chemical Classical methods (wet chemical methods) methods) Instrumental methods Instrumental methods

description

Chapter 1: Introduction. Analytical Chemistry Qualitative analysis Quantitative analysis Classification of Analytical Methods Classical methods (wet chemical methods) Instrumental methods. Comparisons of Wet Chemical and Instrumental Methods. Types of Instrumental Methods - PowerPoint PPT Presentation

Transcript of Chapter 1: Introduction

Page 1: Chapter 1: Introduction

Chapter 1: IntroductionChapter 1: Introduction

Analytical ChemistryAnalytical Chemistry Qualitative analysisQualitative analysis Quantitative analysisQuantitative analysis

Classification of Analytical Classification of Analytical MethodsMethods Classical methods (wet chemical Classical methods (wet chemical

methods)methods) Instrumental methodsInstrumental methods

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Comparisons of Wet Comparisons of Wet Chemical and Instrumental Chemical and Instrumental

MethodsMethodsWet chemical Instrumental

Separation methods

PrecipitationExtractionDistillation

Chromatographiceletrophoretic

Detection methods ColorsBoiling or melting pointsSolubilitiesOdors

ConductivityElectrode potential\light absorption, emissionMass/charge ratio (M/Z)fluorescence

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Types of Instrumental MethodsTypes of Instrumental Methods Separation techniquesSeparation techniques

Chromatographic Chromatographic GasGas LiquidLiquid …………..

ElectrophoresisElectrophoresis Many typesMany types

Detection techniquesDetection techniques Optical spectroscopyOptical spectroscopy

AbsorptionAbsorption EmissionEmission FluorescenceFluorescence

Mass spectroscopyMass spectroscopy AtomicAtomic MolecularMolecular

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Instruments for AnalysisInstruments for Analysis

SignalGenerator

SampleAnalytical

Signal

InputTransducer(Detector)

Signal Processor

OutputTransducer(Readout)

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Instruments for AnalysisInstruments for Analysis

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Selection of An Instrumental Selection of An Instrumental MethodMethod

Defining the problemDefining the problem Performance characteristicsPerformance characteristics

Figure of MeritsFigure of Merits: : Quantitative performance Quantitative performance criteria of instruments that are expressed criteria of instruments that are expressed in numerical termsin numerical terms

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PrecisionPrecisionA measure of the random or indeterminate A measure of the random or indeterminate

errorerror

Relative Standard Deviation

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BiasBiasA measure of the systematic or determinate A measure of the systematic or determinate

errorerror

Bias = µ - XBias = µ - Xtt

µ - the population mean for the µ - the population mean for the concentration of an analyte concentration of an analyte

XXt t – true concentration– true concentration

Standard reference materials (SRM)Standard reference materials (SRM)

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SensitivitySensitivityA measure of the ability of an analytical A measure of the ability of an analytical method to discriminate between small method to discriminate between small differences in analyte concentrationdifferences in analyte concentration Calibration sensitivity (S = Calibration sensitivity (S = mmc + Sc + Sblbl))

SSblbl

Signal

Concentration

xx

x

x

Concentration

SSblbl

Signal

x x

x x

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SensitivitySensitivity Analytical sensitivity (Analytical sensitivity ( = m/s = m/sSS))

m – slope; sm – slope; sSS – standard deviation of the – standard deviation of the measurementmeasurement

Relative insensitive to amplification factors

Signal

Concentration

Increase the gain of the instrument by a Factor of two

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Detection limit (Limit of detection, LOD)Detection limit (Limit of detection, LOD)

The analyte concentration giving a signal equal The analyte concentration giving a signal equal the blank signal, Sthe blank signal, Sblbl, plus three time standards , plus three time standards deviation of the blank, sdeviation of the blank, sblbl

Blank signal

Standard deviation ofthe Blank signal

SSmm = = SSblbl + ks + ksblbl

Analytical Signal

Convert signal response, SSmm,, to analyte concentration

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Dynamic RangeDynamic RangeLowest concentration (LOQ) to the Lowest concentration (LOQ) to the

concentration where the calibration curve concentration where the calibration curve departure from linearity (limit of departure from linearity (limit of linearity, LOL)linearity, LOL)

Blank signal

Standard deviation ofthe Blank signal

SSmm = = SSblbl + ks + ksblbl

Analytical Signal

Convert signal response, SSmm,, to analyte concentration

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Dynamic RangeDynamic Range

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Guideline for Reporting Data Guideline for Reporting Data (Recommended by ACS Committee of (Recommended by ACS Committee of Environmental Improvement)Environmental Improvement)

AnalyteAnalyteConcentrationConcentration Region of reliabilityRegion of reliability< 3< 3σσ Region of Questionable detection Region of Questionable detection

(unacceptable)(unacceptable)

33σσ Detection limitDetection limit

33σσ-10-10σσ Region of less certain Region of less certain quantitationquantitation

1010σσ Limit of quantitationLimit of quantitation

> 10> 10σσ Region of quantitationRegion of quantitation

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99.7%

Question: When the value of 10 sbl

(standard deviation of the blank) is used as LOQ, what is the relative standard deviation of the measurement at this point at the 99.7% confidential level, and why?

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SelectivitySelectivityThe degree to which the method is The degree to which the method is

free from interference by other species free from interference by other species contained in the sample matrixcontained in the sample matrix

S = mS = mAAccAA + m + mBBccBB + m + mCCccC C + S+ Sblbl

The selectivityThe selectivity coefficient for B with respect to coefficient for B with respect to AA

kkB,AB,A = m = mBB/m/mAA

…………………………………………………………………………Note: this is the selectivity of an analytical Note: this is the selectivity of an analytical detectiondetection technique technique

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Calibration MethodsCalibration Methods

Analytical response Analytical response

Comparison with StandardComparison with Standard Direct comparisonDirect comparison

ColorimetricColorimetric

TitrationTitration

Analyte Concentration

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Calibration MethodsCalibration Methods

External External Calibration CurveCalibration Curve

Signal

Concentration

XX

X

X

Normally use the method of least squares

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Calibration MethodsCalibration Methods

External External Calibration CurveCalibration Curve

Two Assumptions:Two Assumptions:

1. Linear relationship1. Linear relationship

2. deviation of the individual point 2. deviation of the individual point from the straight line arises from from the straight line arises from the error in the the error in the measurementmeasurement

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Calibration MethodsCalibration Methods Standard AdditionStandard Addition

Signal

Concentration

Without sample matrix effect

With sample matrix effect (signal suppressed)

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Standard AdditionStandard Addition

Signal

Concentration

C0 C1 C2 C3

xx

xx

Conc. of analyte C0

Sample signalSbl

C1, C2, and C3 are the concentrations of analyte after spiked with stnard, with counting the amount of analyte in the original sample solution.C0 is the concentrations of analyte in sample without spiking

S = mC + Sbl

C0 =Sbl/m

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Internal Standard Internal Standard Add a substance in a constant amount to Add a substance in a constant amount to all samples and, blanks, and calibration all samples and, blanks, and calibration standard in an analysisstandard in an analysis

Concentration

Sanalyte/Sinternal


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