1. Dnyanasadhana College, Thane
Department of Chemistry
S.Y.B.Sc.
Welcome
Dr.G.R.Bhagure

2. SYBSC ANALYTICAL CHEMISTRY Sem.III
INTRODUCTION TO
ANALYTICAL CHEMISTRY By
Dr.Bhagure G.R.

3. Defination 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
Area of Analytical Chemistry
Qualitative Analysis
Quantitative Analysis

5. Analytical Methods
Chemical methods
Physical Methods

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

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

8. Optical methods Emission spectroscopy. Absorption spectroscopy.
Atomic absorption Spectroscopy.
Infrared Absorption Spectroscopy
vFluorophotometry
vi) Turbidimetry and Nephelometry
Raman Spectroscopy

9. Electroanalytical Methods of Analysis
Potentiometry
Amperometry
Conductometry
Polorography

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

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

12. Separation Method
Classical methods
Modern Methods

13. CLASSICALMETHODS Classical methods Precipitation Filtration
Centrifugation
Distillation
Crystalisation

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

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

16. Steps Involved in the Analysis Of Sample
1. Aim/Purpose of analysis
2. Sampling
3. Selection of Analytical method
4. Dissolution of the sample/ processing a sample
5. Separation of interfering substances
6. Actual Measurement /analysis
7..Interpretation of the measurements

17. Aim/Purpose of analysis:
The purpose for which analysis is required must be mention specifically.
Ex.i) In forensic science Laboratory analysis of blood sample and food sample is carried out which may be used as evidence in the court of law.
To maintain the quality control of the product.

18. 2) Sampling:
The various steps/ techniques used to get sample is called as sampling.
Sample: A part of bulk material which represents all essential characteristic to that of bulk is called as sample.
Sampling techniques are not same for solids, liquids or gases.
Each type of material has its own sampling techniques/method to obtain sample.

19. Selection of Analytical method:
The success or failure of an analysis is often critically dependent upon the proper selection of method.
While selecting an analytical method following factors have to be considered.
Concentration of the component.
The complexity of the materials/presence of interfering material
The probable concentration of the species of interest
Degree of Accuracy

20. Sensitivity and detection limit
Selectivity
Duration of an analysis
Speed ,time and Cost of analysis
Availability of equipments
Skill person for handling the instrument.
All the above factors should be taken into account combinedly, to select the proper method.

21. Dissolution of the sample/ processing a sample :
Sample obtained cannot taken directly for the analysis because sample may not be in proper physical form and no suitable sample size.
Most analyses are performed on solutions of the sample.
Inorganic sample are dissolve by (1) treatment with hydrochloric acid, nitric acid, mixture of hydrochloric and nitric acids, sulphuric acid or perchloric acid, and
(2) fusion with an acidic or basic flux followed by treatment with water or an acid.

22. (2) fusion with an acidic or basic flux followed by treatment with water or an acid.
Organic solvents are preferentially used to dissolve the samples of organic nature.
After dissolution sample solution is diluted to known volume.

23. v) Separation of Interfering Substances
The interfering substances are the compounds or elements that prevent the direct measurement of the species being determined.
There are two ways to achieve separation (i) by isolating the desired Constituent in a measurable form by precipitation, filteration or by Masking of substance.
Ex.Cycnide ion can be used to mask Cd, Zn when determination of lead is carried out.
(ii) By removing the interfering substances from the desired constituent by filtration/distillation

24. Actual Measurement /analysis:
Instrument or Volumetric glass ware should be standardized or calibrated before measurement.
Replicate measurement with different aliquot of same sample is carried out to avoid error.
Ex. In volumetric determination at least three B. R. are taken to avoid error.

25. Processing data:
Replicate measurements/ readings are subjected for statistical treatment.
Mean, mode, median, range, standard deviation is calculated to know the central tendency and dispersion of the measurement.

26. Interpretation of the Measurement:
The result obtain after analysis and processing is express in common terms such as Normality, Molarity, PPM, percentage etc. Obtain value/result is then correlated with other factors to understand and to achieve proper conclusion.

27. Performance characteristics of analytical Method
Precision:
It is the agreement between Indiudual observations of same set.
Accuracy:
It is defined as closeness of the observed value with the true value.
Limit of detection(LOD):
Minimum amount of concentration of a component that can be detected with a given degree of confidence.
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.

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

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

30. Quantitive 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

31. Calibration Curve method:
Property is directly proportional to concentration
Property

32. 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.

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

34. 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.

35. Internal Standard addition methodAx
----- At
Concentration-----

36. Application of Analytical Methods:
Analytical chemistry is applicable to each and every branch/field. If one tries to prepare the list of application the list will be unending. All industries irrespective of what they produce, all of these depend upon the applications of analytical methods. The application of analytical chemistry is as follows;

37. Research and Development :
In every industry research is carried out to develop new product which are having application. In this area the analytical characterization and its quantification is carried out by various analytical methods. Ex.IR spectroscopy, UV spectroscopy, Mass spectroscopy .Gas chromatography etc.
Quality control unit :
In every industry there is Quality control unit where the quality of raw material as well as finished product is monitored/ checked by analytical methods.
Ex. Gas chromatography, HPLC, Flame emission spectroscopy, AS can be used in
Qualitative and quantitative analysis.

38. UV Spectrometer

39. Mass Spectrometer

40. HPLC Instruments

41. Organic Industry :
The industry which manufacture the organic bulk chemicals can be called as Organic Industry. To determine the composition, purity and quality of both raw material as well as finished product. Analytical methods are also required to improve the process used, percentage yield and waste products are used.
Quantitative information on the purity level and impurity level are obtained by advanced instruments like Gas chromatography, HPLC, Flame emission spectroscopy, Atomic Absorption Spectroscopy.

44. Pharmaceutical industry:
In research and development wing of the company analytical chemistry plays very versatile role. As per patent law no pharmaceutical company can duplicate the product of another company. So every company has to continue the R.D. to develop new product. Analytical techniques like Gas chromatography, HPLC,Mass spectroscopy, GCMS, thin layer chromatography is useful to find out progress of the reaction and quantification of the product .Thermal methods are used to find out thermal stability of the product.
All the mentioned techniques are also used to maintain the quality and quantity of various ingredients present in medicines.

50. Metallurgical Industry :
The property of any alloy depends upon the adequate proportion of element present in it.
Ex.In steel alloy properties of steel depends on carbon content and proportion of other element such as Cr,Mn,Ni etc.
Analytical methods such as Atomic absorption spectroscopy, vacuum emission spectroscopy are used to find out the various elements present in steel alloy, brass alloy, bronze etc.

55. Electronic Industry

56. Electronic Industry:
The analytical methods like Neutron Activation Analysis are used to find out purity of and trace of impurity(10-12 gm) in semiconductor material like Silicon, Germanium.
The purity of these semiconducting material is very important for the durability any electronic gadgets like
Transistors,
Television,
Mobile phones,
Lap top etc.

57. Environmental pollution:
Testing the Purity of Water :
Analytical methods like pH metry,
Conductometry,
Potentiometry,
UV Spectrophotometry ,
Atomic Absorption Spectroscopy
Are used to check the quality and monitoring the quality of potable water, The water required for construction industry, industrial operation, medicinal preparation, is checked by all the above technique.

58. Industrial Effluent Analysis
The analysis of Industrial effluents is also carried out by all the above technique, if any parameter such as COD, BOD, Heavy metals are beyond the permissible limit, as prescribed by State Pollution Control Board , Central Pollution Control Board, legal action can be taken against company .

59. Waste from Industry and domestic waste polluting the natural water resources

60. Air Pollution Monitoring

63. Air Pollution Monitoring
Analytical techniques like Gas chromatography, Elemental analyzer HPLC are used to check
the composition of air ,
Gases from industry,
process plants,
Hotels,
Vehicles.
If the gases from any industry is beyond the permissible limit as prescribed by State Pollution Control Board , Central Pollution Control Board, legal action can be taken against company

64. Life begins with chemistry and ends with chemistry
GOOD LUCK
Life begins with chemistry
and ends with chemistry