Analytical Chemistry

S.Y.B.Sc. Sem-III Presentation

1. 7/21/2019 1 SATISH PRADHAN DNYANASADHANA COLLEGE-THANE- 400604 DEPARTMENT OF CHEMISTRY Introduction to Analytical Chemistry and Statistical Treatment of Analytical Data by Dr.G.R.Bhagure

2. Syllabus Role of Analytical Chemistry (9 L) 1.1.1. Language of analytical chemistry: important terms and their significance in Analytical Chemistry. 1.1.2. Purpose of Chemical Analysis; Analysis Based (i) On the nature of information required: (Proximate, Partial, Trace, Complete Analysis) and (ii) On the size of the sample used (Macro, semi-micro and micro analysis) 1.1.3. Classical and Non-Classical Methods of Analysis; their types and importance. 1.2. Significance of Sampling in Analytical Chemistry 1.2.1. Terms involved in Sampling 1.2.2. Types of Sampling 1.2.3. Sampling techniques 1.3. Results of Analysis. (6L) 1.3.1. Errors in Analysis and their types 1.3.2. Precision and Accuracy in Analysis 1.3.3. Corrections for Determinate Errors (Problems including Numericals expected wherever required)

3. Non Classical Methods

4. 2. Instrument: Single Beam Colorimeter 21 U.V.Light & visible light Photocell /PMT detector Filter or Monochromator Read Out Device Monochromatic light Absorption spectroscopy

5. Grating Read Out Amplifier Sample Solution Power Supply Rotating Chopper Flame Hollow Cathode Lamp P.M.T.Detector Atomic Absorption Spectrophotometer 22 Absorption spectroscopy

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

7. 2. Instrument: Single Beam Fuorimeter U.V.Light & visible light 24 Photocell /PMT detector Primary filter Secondary filter Read Out Device Monochromatic light

8. visible light 25 Read Out Device Turbidimeter Filter Sample Cell Photocell Detector Technique is used when concentration of suspended particles are high In this intensity of transmitted light is measured

9. visible light 26 Light Trap Nephelometer Read Out Device Sample Cell Photocell Detector Collimating Lens Graduated Disc Technique is used when concentration of suspended particles are less In this intensity of scattered light is measured

10. 1.2 SAMPLING Terms involved, importance of sampling, sampling techniques, sampling of gases, ambient and stack sampling, equipments used, sampling of homogenous and heterogeneous liquids, sampling of static and flowing liquids, methods and equipments used, sampling of solids, importance of particle size, and sample size, samples used In order to understand the criteria for evaluating the utility of the analytical techniques, need for the reduction in sample size, methods of reduction in sample size, collection, preservation and dissolution of the sample.

11. Sampling Unit: The minimum size package in the consignment which sample may represent is known as sampling unit. Increment: A stated amount of the material that is withdrawn from the sampling unit is defined as Increment.

12. 1 2 3

13. Cleanliness of apparatus and containers

14. Positive identification of samples

15. Apparatus for sampling of Homogenous Liquids Heterogeneous liquids or immiscible liquids A B Liquid Sample Thief

16. Device for Sampling of static and flowing liquid

17. Heterogeneous liquids or immiscible liquids 1) Two immiscible liquids separating into two layers : Liquid-2 Liquid-1 Height of the layers Height of the layers Sample thief is used to with draw the sample so that gross sample can be prepared .

18. Heterogeneous liquids or immiscible liquids 2) Emulsion or unstable suspension: Two phases are separated by filtration , Solid and liquid are separated The two phases are weighed and then sampled separately. If above is not feasible the entire suspension is stirred vigorously and resulting liquid is sampled . Sample thief is used to with draw the sample so that gross sample can be prepared .

19. Heterogeneous liquids or immiscible liquids 3) sampling of liquids containing partially crystallized solids : Semi solidified liquid or liquid containing crystallized solids are heated, Heating is continued till solid dissolves or melts into liquid. Then sample is withdrawn by sample thief.

20. Ambient sampling Ambient sampling : Sampling of atmospheric gases is called as Ambient sampling

21. Stack sampling: Sampling of gases released from industry is called as stack sampling. PLANT Industry Opening for sampling of gas

22. Sample Thief Assembly For Sampling of gases E Sample Container A s top cock B To Vacuum Pump C stop cock D Sample Probe Hg

23. SAMPLING OF SOLIDS As solid are heterogeneous it is difficult to carry out sampling of solids.Ex.in ores certain lumps are rich in the element of interest and may rich in impurities such as silicates.Lumps of pure solid and lumps of impurities in different sizes may lead to errors in sampling. Such errors can reduced by crushing larger lumps into smaller size or by taking large quantity of the sample. In this context the concept of bulk ratio is important. BULK RATIO= Weight Of The Sample \Total Weight Of Bulk Material SIZE TO WEIGHT RATIO= weight of the largest particle/weight of the sample

24. Heterogeneous material Such errors can reduced by crushing larger lumps into smaller size or by taking large quantity of the sample.

25. Coning and quartering X X V V Cone of the material Material flattened to circle Two opposite parts selected other two are rejected

26. Long pile and alternate shovel method 1 2 3 4 1 and 3 are selected and 2 and 4 are rejected or vise versa

27. Rolling and quartering X X V V Spreading of the material on thin polythene sheet Material flattened to circle Two opposite parts selected other two are rejected Rolling

28. T shape handle Pointed portion to be inserted into soil Auger sampler

29. Split tube thief:

30. Sampling of particulate solids Sampling of particulate solids: dry and free flowing Material called as particulate solids. Concentric tube thief Solid material

31. Concentric tube thief Sharp end Inner Tube Outer Tube Holes

32. Split tube thief Sharp end Slot T-Shape Handle

33. Hand scoop

34. Collection ,preservation and dissolution of sample

35. FLUX Crucible Na 2 CO 3 Pt. Na 2 CO 3 + KN O 3 Na 2 O 2 Pt.

36. All The best