Analytical Chemistry Introduction and Quality Systems | Dnyanasadhana College

1. Dnyanasadhana College,ThaneThane.Department of ChemistryM.Sc. Analytical Chemistry Sem-IIntroduction 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]

12. Optical methods

13. Monochromatic light Photocell /PMT detector 2. Instrument: Single Beam Colorimeter 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

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

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

18. Turbidimeter 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 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

24. CLASSICALMETHODS 4 1 2 3 5

26. Chromatography MODERN METHODS

27. 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. 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. MODERN METHODS

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

32. Selection of Analytical method: • All the above factors should be taken into account combinedly, to select the proper method.

33. Performance characteristics of analytical Method:

34. Performance characteristics of analytical Method:

35. Performance characteristics of analytical 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

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

44. Standard addition method Property .. .. . 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:

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