Instrumental methods 63 SSS ee Module III Instrumental Methods Thermal analysis Introduction These methods are based on the measurement of dynamic relation ship between temperature and any one ofthe property such as mass change or heat change et. “Technique Instrument Parameter | Plot ‘employed / principle measured Thermo balance Mass Mass vsT = Pe ee DTA appara (Compuzon offen ofthe | at AT Ws. Temy ‘Thermo gravim Principle ‘Thermogravimetric Analysis is a technique in which the mass of a substance is monitored as function of temperature, as the sample is heated from room temperature to temperature as high as 1200°C in a controlled atmosphere, monitoring the weight normally carried out in ai the weight is recorded.as a funct as thermogram(g) w! gen, Helium or Argon, and temperature. The graph obtained is knowa,Instrumental methods 65 of inorganic compounds, Meno Teme t0 Instrumentation ‘The main components of TGA apparatus are the following Sample holder Furnace with temperature programming facility ‘Theme balance ‘Temperature sensor en iagram of TGA apparatusApplications of Thermogravimetry and quantitative information about a decomposition + Gives both quai action, reactive gases, Allows analysis of reactions with at, oxygen, oF other reactive Bas * Can determine the purity ofa mineral, inorganic compound, or organic materi, Distinguishes different mineral compositions from broad mineral types, such, ay borax, borie acid and silica gels 10} A sro scm ‘i on, = ‘TGA of polymers ‘Mass, mg —> © “400 200 300 400 500 600 700 Temperature *C > TGA will not give any information regarding, phate change such as trans into another and melting of a solid into liquid. These transitions do nol irinvoivs heat change, Instrumental methods 67 Differential Thermal Analysis (OTA) aC,0,H,0) ina current of airEngineering Chemisty LE _—— SS Tastrumental methods 69 |_| comeeter 7 J t ‘Chromatographic Methods er Introduction Te ‘Chromatography is on ofthe accurate techniques analytical separations. This ' a method was invented by a Russian botanist Miiag ‘The term chromatography is coined from two geek. fmm ‘sraphein tcans ‘to wite™.No other separation method ng being | [eee] Hse Principle Fumece f Seurea ot power phase. Eg: a column of adsorbent, pape, a thin ted on inert solid, a thin layer of adsorbent coated over glass xothermic The components ofthe mixture ‘hey are cared by the mobile phase throu the relative affinity of the components tow Classification Decomposition Endothermic — st — ‘Temperature Fig3.6 DTA of polymer Application of DTA 1) ma, information sichas melting pit tanstintemperatrceicofarystlige | 2, whereas TG, (give these data abt does not involve change 2) » 4) 5) tudy of decompositon temperatur of inorganic solids.2) Based om the mobile phase, it can be classified 35 sent meets 1 8) Liquid Chromatography: The mobile phase oy ceca mn ee aay ‘solid (GSC ) of liquid supported on inert so! (GLC). Column Chromatography: ‘Column chromatography is one ofthe most useful methods forthe sep ‘ofboth solids andi sold -liguid technique in which the Wid. The principle of column chromatogra a cena ne ‘The usual adsorbents employed in column chrom ¥ ¥ « calcium carbonat Fie. 3.7(@)TLC ( Revalue () Column Chromatography ‘Thin layer Chromatography ‘components at di hhas reached near the top of the plate, the plate is removed from the developing chamber, 2. nsepaation of compounds ater omni synthesis obtain des .To separate or puri i dlololin homie 3.To separ ‘purify natural ‘Sompound mixtures like alkaloids, glycosi :ire we volved. Usually Instrumental methods _73 fon techniques are usey contains Gas chromatography (GC) Principle tied and the separated components of 1 compounds are not coloured, 0 the followin Chemical analysis of mixtures of volatile organics compounds is generally done using GC ‘The principle of GC is the differential distibution of the components between two pases ic). Themobile phase ayed onto the plate gp ‘$0, spray, Ninbydri the techniqu mpounds appear ag emecsi TLC) The most common support used in GLC is diatomaceous recto srhase sa old (GSC) the principle of separation is from 0 fi, 3.7 (4) is parition (ratio of distance travelled by the sample SPO! Re oie reat Fable 8.1 Comparison between GSC at Gistance travelled by the solvent font ‘Table 8.1 Comparison between GSC and GLE ‘The Ayvalue can be used o Wenify compounds duc to the uniqueness of ca Point of diferences ese cue. en comparing to dif mee ‘Stationary phase Liquid Gas L Packing ofthe eoluma Both packed and ae ‘capillary column car ] beused Length ofthe column 072m 310 300m. ‘Thermal stability of Good stability Less stable above stationary phase 300°C Reactions inthe column | Packing may catalyse Packing does not some heres coy | cotstvse Applicability soil forthe % To check the purity ofa sample eparation of voat % To determine the appropriate so oe ** sppropriate solvent for a column-chtomatographic separation Trin cie, _bstances monitor a columnehromatogrphic se Pemonitr a colanmehromatographic sepsation : | *T tation aL reaction, by bserving the appearance of a cdsppexance ats wet74 Engineering Chemistry ei i rr i) Canier Gas ‘Sample injection system The columa iv) Stationary phase Y)_ One or More Detectors with appropriate read oUt . ff ad eer fred hI ort | | Lom J = Fig. 3. 8 schematic diagram of a gas chromatograph 1D Carrier gas ii) Columns {In the column, the different components in the vapourised samples are separated from je pases deptnlee in aes each other sacking. Two hyped ferent components a1jffrenttime. The time | ny. which between the sample injection port and the detect arison of the GC retention tng © 9 anbe determined with high accuracy, *4by taking GC of blood or urine sample, Instrumental methods 77 SSS ee High Performance Liquid Chromatography (HPLC) ‘compounds which are noncanbe soils ube of egth abou 3g jwith OCH, group instead of pediocin in Guard Cotumas < . A shor guard column is Lept before the analytical co jamn. This helps to remove partic ‘tier present in the solvent and thereby increases the ife of analytical column opens such as UV-absorbance, Solute detectors respond 10 ee Er ‘ot possessed by mobile phase Aluorescence propenies ofthe solute molecules Procedure solvent is vanced in Sesctime The: f ‘tc. The tomponents that emerge out ofthe column are detected and recorded Singers ereraly wed nomal phase Instrumental methods 79 Conductivity Electrical energy is taken through matter inthe form of electric current. la order to have clectic curent, charge caries and driving force are essential. The charge carriers can be cither electrons or ions. A battery or suitable source of electric energy ean be used provide the diving force. ‘The substances which allows the passage of electric current through themare called conductors while those which do not allow flow of electric current are called insulators. Conductors are of to types Is and semiconductors. tons, acids, molten salts low when compared with metals. This is ‘sistance of a conductor of unit lenth and unit area of ef0ss 1 is ohm em ‘ease with which the current flows through a conducto ation, so of resistance is called conductance. The unit of conductance is ohm’ or mo80 Engineering Chemis Instrumental methods 81 ) re ed speiic conductance 1s defined ag gy Specific conductance of KCI Feld btweqa two electrodes of lent i be lution = conductance x celleonstant conductance of 0.1 M KC! solution in the given cell as desribed below, the an be determined fed with finely divided re welled withthe ends of plating are strongly fixed such that di consists of two elestrode pl polarisation effects). The Wires that are sealed through two glass tubes. The between electrodes remains unaltered. | conductivity. cell containing the test solution A kx resistance box. An [oe | a as ‘fms resistance of conductivity cll an be determined 1 nee of conduct Conductance of solution (C)= Fig3.11 Conductivity measurement Catt constane |, the distance between two electrodes (I) and the area | Ina condveti | cell constant K fixed. This cons kal Unit of cell constant is em! or ra! Determination of cell constant sp.conduetance of standard ‘Conductance of standard KClin 0.01288 ell" 1200x10 cellconstant = 0.1 MK i conductance) of 0.1M KCl soliton is 0.01288 ohm ‘onductivy of given NaCl solution = conductance $6010" x10-73 10? oberon!