1. Dnyanasadhana College,Thane Thane. Department of Chemistry M. Sc
Dnyanasadhana College,Thane Thane. Department of Chemistry M.Sc. Analytical Chemistry Sem-I Introduction to Analytical Chemistry: Dr.G.R.Bhgaure

2. SYLLABUS
Unit –I
1.1 Introduction to Analytical Chemistry: Classification of analytical methods, an overview
of analytical methods, types of instrumental methods, instruments for analysis, data domains, electrical and non electrical domains, detectors, transducers and sensors, selection of an analytical method, accuracy, precision, selectivity, sensitivity, detection limit and dynamic range, classification of techniques: calibration curve, standard addition and internal standard methods. [7L]
1.2 Quality in analytical chemistry: quality systems in chemical laboratories, cost and benefits of a quality system, types of quality standards for laboratories, total quality management, quality audits and quality reviews, responsibility of laboratory staff for quality. [8L]

3. Definition of
Analytical Chemistry
Analytical Chemistry is branch of chemistry which deals with the study of theory and practice of methods used to determine composition of matter.

4. Quantitative Analysis
Areas of
Analytical Chemistry
Qualitative Analysis
What?
Quantitative Analysis
How much?

5. The Language of Analytical Chemistry1
Analysis: A process that provides chemical or physical information about the constituents in the sample or the sample itself. 2
Analyte's: The constituents of interest in a sample. 3
Matrix: All other constituents in a sample except for the analyte's. 4
Determination: An analysis of a sample to find the identity, concentration, or properties of the analyte. 5
Measurement: An experimental determination of an analyte’s chemical or physical properties.

6. The Language of Analytical Chemistry6
Technique: A chemical or physical principle that can be used to analyze a sample. 7
Method: A method is the application of a technique for the determination of a specific analyte in a specific matrix. 8
Procedure: Written directions outlining how to analyze a sample. 9
Protocol: a protocol is a set of stringent written guidelines detailing the procedure that must be followed if the agency specifying the protocol is to accept the results of the analysis.
Protocols are commonly encountered when analytical chemistry is used to support or define public policy.

7. Areas of Analytical Chemistry
Qualitative Analysis
Quantitative Analysis

8. Analytical Methods
Chemical methods
Physical Methods

9. Chemical Methods of Analysis
Classification of
Chemical Methods of Analysis
Gravimetry or
Gravimetric analysis
Volumetry
Volumetric analysis

10. Classification of Instrumental methods
Optical methods
Electroanlytical methods
Separation methods
Miscellaneous methods

11. Optical methods Absorption spectroscopy Emission spectroscopy.
Atomic absorption Spectroscopy.
Infrared Absorption Spectroscopy
Fluorophotometry
Turbidimetry and Nephelometry
Raman Spectroscopy

12. Optical methods

13. 2. Instrument: Single Beam Colorimeter
Monochromatic light
Photocell /PMT detector
Read Out
Device
U.V.Light & visible light
Filter or
Monochromator
Absorption spectroscopy

14. Atomic Absorption Spectrophotometer
Rotating Chopper
Hollow
Cathode
Lamp
P.M.T.Detector
Flame
Amplifier
Read Out
Grating
Power
Supply
Sample Solution
Absorption spectroscopy

15. Emission Spectroscopy Atomic Emission Spectroscopy
Flame Emission Spectroscopy

16. Emission Spectroscopy.
Flame Photometer
Slit
Collimating
Mirror
P.M.T.Detector
Amplifier
Read Out
Fuel
Oxidant
Prism Monochromator
Sample Solution

17. 2. Instrument: Single Beam Fuorimeter
Monochromatic light
U.V.Light & visible light
Primary filter
Secondary filter
Photocell /PMT detector
Read Out Device

18. Turbidimeter visible light Filter Photocell Detector Read Out Device
Sample Cell
visible light
Filter
Technique is used when concentration of suspended particles are high
In this intensity of transmitted light is measured

19. Nephelometer visible light Light Trap Photocell Detector Sample Cell
Graduated Disc
Collimating Lens
Light Trap
visible light
Photocell Detector
Technique is used when concentration of suspended particles are less
In this intensity of scattered light is measured
Sample Cell
Read Out Device

20. Electro analytical Methods of Analysis
Potentiometry
Amperometry
Conductometry
Polorography

21. Radioanalytical Methods:
Isotopic Dilution Methods:
Neutron Activation Analysis:

22. Thermogravimetric Analysis Differential Thermal Analysis
Thermal Methods
TGA
Thermogravimetric Analysis
DTA
Differential Thermal Analysis

23. Separation Method
Classical methods
Modern Methods

24. 1 2 4 3 5 CLASSICALMETHODS Classical methods Precipitation Filtration
Centrifugation
Distillation
Crystallization 4 1 2 3 5

25. MODERN METHODS Chromatography
Adsorption
Partition

26. Adsorption Chromatography Column Chromatography
S+L OR S/G
Thin Layer
S+L
Column Chromatography
Ion Exchange
Gas Solid Chromatography
S+G
Gel Chromatography
Chromatography
MODERN METHODS

27. Spreading the slurry by Hooper
Materials used in TLC
Glass Plate
Spreading the slurry by Hooper
Mobile phase
Developing chamber

28. OH OH
Silica Gel OH
Silica Gel OH OH OH
Mobile
phase OH

29. Sample to be applied on this area
Thin
Chromatography
S+L
Less Polar
More Polar
Adsorbs weakly and separate very fast
Adsorbs stronger and separate very slowly
Sample to be applied on this area

30. Partition Chromatography
MODERN METHODS
Partition Chromatography
L+L OR L+G
Paper Chromatography
L+L
HPLC
Gas Liquid
L+G

31. Solvent Front S O L V Solute front E N t F W Solute front
Paper Chromatography
L+L
Original Line

32. Selection of Analytical method:1
Concentration of the component. 2
The complexity of the materials/presence of interfering material 3
The probable concentration of the species of interest 4
Degree of Accuracy 5
Sensitivity and detection limit 6
Duration of an analysis 7
Speed ,time and Cost of analysis 8
Availability of equipments 9
Skill person for handling the instrument
All the above factors should be taken into account combinedly, to select the proper method.

33. Performance characteristics of analytical Method :1
Precision: It is the agreement between Individual observations of same set. 2
Accuracy: It is defined as closeness of the observed value with the true value. 3
Limit of detection(LOD): Minimum amount of concentration of a component that can be detected with a given degree of confidence. 4
Limit of Quantification (LOQ): Minimum amount of concentration of a component that can be estimated with a given degree of confidence is termed as LOQ.

34. Performance characteristics of analytical Method :5
Limit of Linearity (LOL) : It is defined as maximum concentration range up to which instrument is produces linear response. 6
Sensitivity: It is a measure of ability of method to discriminate between two small concentration differences in the analyte. 7
Measurement of Sensitivity:
It is is measured in terms of slope of the calibration curve. If the slope is greater sensitivity of the method is high and vise-versa.

35. Performance characteristics of analytical Method :8
Selectivity: It is defined as degree to which the method is free from interferences from other components present in the matrix. 9
Dynamic range:
It is the concentration range from limit of Quantification (LOQ) to Limit of Linearity (LOL).

37. Quantitative Analysis1.
Calibration Curve method: 2.
Method of Standard Addition 3.
Internal Standard Method:

38. Quantitative Analysis:
Calibration Curve method:
A calibration curve is used to determine the unknown concentration of an element in a solution. The instrument is calibrated using several solutions of known concentrations. The property to be measured of each known solution is measured and then a calibration curve of property measured v/s concentration is plotted.
The property of a sample solution is measured .The unknown concentration of the element is then calculated from the calibration curve

39. Calibration Curve method
Sr. No.
Concentration of
KMnO4
O.D. 1 5
0.02 2 10
0.04 3 15
0.06 4 20
0.08 25
0.1 6
Unknown
0.05

40. Calibration Curve method:
Measurable Property is directly proportional to concentration
Measurable Property

41. Method of Standard Addition:
When Standard Addition Method is useful
Sample composition is unknown
Sample composition affect on analysis
To nullify the effect of Matrix

42. Method of Standard Addition:
In this method the property of unknown (X) is first find out against blank. Then a series of standards having definite amount of unknown (X) plus varying amount of standard are prepared and diluted to same volume in each case .Their property is then measured. A graph of measured property against concentrations of standard (S) gives a linear curve. The concentration of the unknown can be determined by extrapolation of line which cuts to X axis.

43. Method of Standard Addition
Sr. No.
Volume Of Sample Solution
Concentration of
KMnO4
O.D. 1 5
0.02 2
0.06 3 10
0.08 4 15
0.1 20
0.12 6 25
0.14

44. . . . . . Standard addition method Property Absorbance---
Absorbance---
X X+S X+2S X+3S X+4S
Concentration-----
Concentration of Unknown.

45. Internal Standard Method:
When Internal Standard Method is useful
It is useful for analysis when quantity of sample analyzed or the instruments responses varies slightly from run to run.
Such response are difficult to control
When sample loss occur during sample preparation

46. Internal Standard Method:
A series of standard solution containing the same elements as that present in sample solution is prepared. A fixed quantity of suitable internal standard is then added to each of standard solutions, blank and sample solutions alike. The measurable property of each of above standard solutions and sample solutions are measured. The measurable property for each of above standard solution (Is) & (Ii) and sample solution (Ix&Ii) are measured at different wavelength one corresponds to element and other corresponds to the internal standard. These measurements are made against blank .The ratio of measured property of the standard solutions to that of internal standard (Is/Ii) are plotted against the concentration of standard solutions. This gives a straight line from this curve concentration of sample solution can be read by finding where the ratio (Ix/Ii) falls on concentration scale.

47. Internal Standard Method:
Sr. No.
Volume Of Sample Solution
Concentration Internal Standard (ppm)
O.D. 1
Blank 5
0.02 2
sample
0.06 3
0.08 4 10
0.1 15
0.12 6 20
0.14

48. Property of Internal standard
Internal Standard Method
Property of Sample
Property of Internal standard
Concentration of Unknown.
Concentration-----

49. Property to be measured
Types of Instruments

50. Signal/Characteristic property
Instrumental Methods
Emission of radiation
Emission spectroscopy (X-ray, UV, visible,
electron, Auger); fluorescence,
phosphorescence, and luminescence
(X-ray, UV, and visible)
Absorption of radiation
Spectrophotometry and photometry (X-ray, UV, visible, IR); photoacoustic spectroscopy; nuclear magnetic resonance and electron spin resonance spectroscopy
Scattering of radiation
Turbidimetry; nephelometry; Raman spectroscopy
Refraction of radiation
Refractometry; interferometry
Diffraction of radiation
X-Ray and electron diffraction methods

51. Polarimetry; optical rotary dispersion; circular dichroism
Rotation of radiation
Polarimetry; optical rotary dispersion; circular dichroism
Electrical potential
Potentiometry; chronopotentiometry
Electrical charge
Coulometry
Electrical current
Polarography; amperometry
Electrical resistance
Conductometry
Mass-to-charge ratio
Mass spectrometry
Rate of reaction
Kinetic methods
Thermal properties
Thermal conductivity and enthalpy
Radioactivity
Neutron Activation and
isotope dilution methods

52. DATA DOMAINS Electrical and Non Electrical Domains,
Detectors, Transducers and Sensors,
Sensors

53. Data domains
Information contained in Chemical and physical Characteristics of property of interest is called as data domain.

54. Non-Electrical domain
Current, voltage, frequency, charge, pulse width, are called as electrical domain
Physical and chemical property , scale, position and number are called as non electrical domain

55. Instruments converts
Information for human
Interpretation in terms of property interest and manipulation
Nonelectrical domain
Information contained in Chemical and physical Characteristics of property of interest
Nonelectrical domain
Transduction processing
Electric Domain

59. CLASSIFICATION OF TRANSDUCERS
The input transducer
The output transducer
The input transducer is called the sensor, because it senses the desired physical quantity and converts it into another energy form.
It converts information in electrical domain to information in non-electrical domain (Voltmeters, computer screens, ADC)

60. Types OF
TRANSDUCERS
PHOTO TRANSDUCERS
THERMAL TTRANSDUCERS
BIOSENSOR

61. PHOTO TRANSDUCER
Photo transducer is device that converts light energy into electrical energy are called Photo- transducer

62. PHOTOCELL DETECTOR
(--) D D G C E- G B A +

63. PHOTO TUBE DETECTOR
Photo Cathode
Collector Anode -
AMPLIFIER RECORDER

65. A SENSOR
A sensor some time also called as detector that measures a physical quantity and converts it into signal which can read by an observer

66. Thermal Transducer
Thermocouple
Thermocouple sensor used for high temperature measurement.
Thermocouple converts temperature to an out put voltage which can read by a voltammeter. Hg
Mercury in glass thermometer converts measured temperature.
Uses :
Cars, Aero plane, Chemical plant ,Elevators, Doors , Manufacturing machine ,robotics.

67. Biological Sensors:
A biosensor is an analytical device used for detection of analyte that combines a biological component with a physiochemical detector.

68. Thermal Transducers Infrared radiation generally does not have sufficient energy
to produce a measurable current when using a photon transducer. A thermal transducer, therefore, is used for infrared spectroscopy. The absorption of infrared photons by a thermal transducer increases its temperature, changing one or more of its characteristic properties. The pneumatic transducer, for example, consists of a small tube filled with xenon gas equipped with an IR-transparent

69. SIGNAL PROCESSOR :
A device, such as a meter or computer, that displays the signal from the transducer in a form that is easily interpreted by the analyst.

70. Amplifier:
An Electronic device that increases the power of signal

71. Amplifier
Weak Signal
Strong Signal

72. Thank you