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College of Science

Department of Chemistry

Course Book

Instrumental Analysis for fourth Stage

M.Sc. in Chemistry

Ph.D. in Chemistry

Academic Year: 2010-2011

Assist. Prof. Dr. Kamal Mustafa Mahmoud

E-mail: dr.kamal@uni-sci.org

or kamal_k58@yahoo.com

Mob: +964 (0) 750 454 6198

(Academic Year 2010-2011)

Grading

Number of Units = 8

Theory:

• Three term exams 20 points

• Quizzes 05 points

• Final exam 50 points

Practical:

• Term exam 10 points

• Oral Presentation & seminars 05 points

• Final exam 10 points

• Total (Theory + Practical) 100 points

Course Program

• 1A: Terms associated with chemical analysis.

• 1B: Classification of instrumental techniques.

• 1C: General considerations in evaluating:

• Precision and Accuracy, Errors in

instrumental analysis, some statistical expressions,

• Sensitivity and Detection limits for

instruments, Signal to noise ratio, etc.

Course Program

Ch. 2: Molecular spectroscopy:

2A: Properties of light, nature of electromagnetic radiation.

2B: Interaction between light and a mater.

2C: UV, Visible and IR spectroscopy; principles, techniques and applications.

2D: Beer's- Lambert law.

2E: Sensitivity enhancement by Beer's law.

2F: Instrumentation:

2F1: Radiation sources.

2F2: Cells and sampling devices.

2F3: Wavelength selectors, Filters and monochromators.

2F4: Detectors.

2F5: Readout modules.

2G: Deviation from Beer's law:

2G1: Instrumental deviations.

2G2: Chemical deviations.

2H: Turbidimetry and Nephelometry.

Course Program

• Ch. 3: Molecular emission spectroscopy:

• 3A: Principles, Energy transition levels when a molecule

gains energy.

• 3B: Requirements for fluorescence:

• 3B1: Structural rigidity.

• 3B2: Temperature and solvent effects.

• 3B3: Effect of pH (Chemical quenching).

• 3B4: Instrumentation: Filter fluorimeter;

Spectrofluorimeter.

• 3C: Phosphorescence and Chemiluminescence's

spectroscopy; Theory, instrumentations and

• Applications.

Course Program

Ch. 4: Atomic spectroscopy:

4A: Principles: Band spectra and line spectra.

4B: Atomic emission.

4C: Radiation sources:

4C1: Flame.

4C2: Electrical Arc and Spark.

4D: Flame photometry:

4D1: Flame, types of fuels and oxidants, flame zones.

4D2: Mixing of fuels and oxidants, total combustion method.

4D3: Instrumentation.

4E: Effect of Temp. in atomic absorption.

4F: Atomic absorption:

4F1: Flame, premixed type.

4F2: Radiation source in atomic absorption (H.C.L.).

4F3: Compares between flame photometry and atomic absorption.

4F4: Applications of flame photometry and atomic absorption:

4F4-1: Direct calibration.

4F4-2: Standard addition techniques.

4G: Interferences of atomic spectroscopy:

4G1: Spectral interferences.

4G2: Ionization.

4G3: Chemical reactions inside the flame.

4G4: Self absorption.

Course Program

• Ch.5: Automatic and continuous methods of analysis:

• 5A: Importance of automatic analysis.

• 5B: Classifications.

• 5C: Continuous methods of analysis:

• 5C1: flow Injection analysis (FIA).

• 5C2: Continuous flow analysis (CFA).

•

• 5D: Flow injection analysis (FLA):

• 5D1: Instrumentation.

• 5D2: Dispersion.

• 5D3: Detectors.

• 5D4: Applications.

Course Program

• Ch.6: Electrochemical methods of analysis:

• 6A: Potentiometric methods:

• 6A1: Oxidation- Reduction processes.

• 6A2: Electrochemical cells.

• 6A3: Reference electrodes.

• 6A4: Indicator electrodes.

• 6B: Voltammetry.

• 6C: Polarography.

• 6D: Conductometry.

• Ch.7: Nuclear and X-ray methods.

• Ch.8: Thermal methods of analysis.

References:

1- Principles of Instrumental Analysis. By: Skoog.

West.

Robinson.

Analytical Chemistry

Deals with methods for Identification of one or more of the

components in a sample of matter and the Determination of the

relative amounts of each.

Classical: color, indicators, boiling points, odors. analysis

Instrumental: chromatography, electrophoresis, “Determination”

physical property (spectroscopy, electrode

potential)

1. Gravimetric methods 1.Spectroscopy

2. Volumetric methods 2.Electrochemistry

3.Chromatography

Distinction between Techniques and

Methods

phenomenon that has proved useful for providing

information on the composition of substances.

• Analytical Methods: is a specific application of a

technique to solve an analytical problem.

Types of Instrumental Methods:

• Property • Example Method

• Radiation absorption • Absorption spectroscopy

(photometry,

spectrophotometry, NMR, ESR)

• Radiation emission • Emission spectroscopy

(fluorescence, phosphorescence,

luminescence)

• Radiation scattering • Turbidity, Raman

• Radiation refraction • Refractometry

• Radiation diffraction • X-ray, electron

• Radiation rotation • Polarimetry

Types of Instrumental Methods:

• Electrical potential Potentiometry

• Electrical charge Coulometry

• Electrical current Voltammetry- amperometry,

polarography

• Electrical resistance Conductometry

• Mass Gravimetry

• Mass-to-charge ratio Mass spectrometry

• Rate of reaction Stopped flow, FIA

• Thermal Thermal gravimetry, calorimetry

How to choose an analytical

method?

• Speed

• Convenience

• Availability of equipment

• Number of analyses

• Amount of sample that can be sacrifice

• How reproducible? - Precision

• How close to true value? – Accuracy

• How small a difference can be measured? - Sensitivity

• What range of amounts? – Dynamic Range or linear range

• How much interference? - Selectivity

Precision - Indeterminate or random

errors

This term is used to describe the reproducibility of the results

∑ (Xi - X-)2

Absolute standard deviation: s = √

N-1

Variance: S2

S

X-

Accuracy- Determinate errors

(personal, method, instrumental)

• It is refers to the closeness of a measurements to its

true or accepted values, Xt, and express in terms of

errors.

• Absolute error, E = Xi – Xt (Xi = observed or

experimental value; Xt = accepted or theoretical

value)

• Relative Error = Xi – Xt/ Xt X 100

= Xi / Xt x 100

Sensitivity

• The sensitivity, S, of analytical method or instrument

may be defined as the ratio of the change in the

response, to the change of the quantity (i.e.

concentration);

d Signal

• S= c + Signalblank

dc

• Calibration sensitivity = mC + Signalblank

measurement .

Detection Limit

• Is the lowest concentration level that can be

determined to be statistically different from an

analyte blank.

( s is standard deviation of blank)

level)

• or D.L. = Blank read + 3s

Dynamic Range

At detection limit we can say confidently

analyte is present but cannot perform reliable

quantitation.

Level of quantitation (LOQ): k=10

Limit of linearity (LOL): when signal is no longer

proportional to concentration.

LOL

Dynamic range: 10² to > 10⁶

LOQ

Selectivity

No analytical method is completely free from interference

by concomitants. Best method is more sensitive to

analyte than interfering species (interferent).

Matrix with species A&B: Signal=mAcA + mBcB+ Signalblank

mB

Selectivity coefficient: kB,A=------

mA

k’s vary between 0 (no selectivity) and large number (very

selective).

Calibration methods

Basis of quantitative analysis is magnitude of

measured property is proportional to

concentration of analyte

Signal α[x] or Signal =[x]+ Signalblank

[x]=

m

Calibration curves (working or

analytical curves)

Dynamic Range

Instrument

Response LOQ o

(signal) o

DL LOL

o

o Slope m

o

Signalblank

[X]

Regression equation: y = a + m X

a = intercept = y- - mX-

m = slope = ∑ (Xi – X-)(yi –y-) ⁄ ∑ (Xi – X-)2

Example :

0.9 0.15

2.0 0.24

3.1 0.33

4.1 0.42

(μg ⁄ ml or mg ⁄ l)

Define Variance and Covariance:

Σ (xi - x-)² Σ (x - x -)(y - y-)

Sxx= Sxy = i i

N–1 N–1

x = 2.02 y = 0.238

Sxx = = =2.707

4 4

4

= 0.9562 = 0.23905

4

Define Variance and Covariance:

Sxy

Slope: m = = 0.23905 =0.0883

Sx 2.707

b = y- – mx-

= 0.0596

Calibration expression is

The End of Lecture

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