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Unit 1 MPAT Notes

modern analytical analysis technique

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34K views70 pages

Unit 1 MPAT Notes

modern analytical analysis technique

Uploaded by

pikurao1305
Copyright
© All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
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' FF a L First Sessional Exam 2093 _ _ Modern Pharmaceutical Analytical Techostagy Techniques (nik I Q. Explain LY-Visible Spectrascopy . _—Ans- OY= Visible Spectrascopy o || Introduction &— I'spectroscepy | the branch oF Science that deals With the Study OF foteractron of matter wit light oR LIE is the branch of science hat deals wih Ihe Study of /oleacton _ | log electromagnehc radiation With matte. 9 Electromagnetic. Radiatfon -|_f consist oF d'screfe packages OF energy wibich are Caled as photons. “A Photons consists of an_ascillating electric freld Ce) fan osc magnetic Field cr) wwhien are perpendicular 10 e9¢h ofper | q Frequency () ££ Ih Is defined as the ne. oF Himes electrical Field radiation asesllaky un one second ~The unit for Frequency vis Herts Cx) yt tax = 1 cyde per second ~b aretength a): e eases! okfhe ware Il Sime phase te distance between two nearest_crest or throughs The unit for wavelength .is nano mefer (nm) SS Scanned with CamScanner EAS i @ | Ul~Visible Spectroscopy Visible spectrum Ss ir Is ise rir or spa igh 2, E}ectror i‘ Is Visible - The visible a is the portion of- fhe electromagnetic Violek lndign___ Blue_ Green (400 ~ 4go- __tHo~__40~ \# | Theon) Yellow) Orange S7Or.. SBS- aoe Uitrq violet shit spesos rie Bom train of ©! higher electri. within-q_molecwe oran fon From_q lower bo 4 energy _leve) and the Ultraviolet emission Spectra asisos | From the reverse type of. transiHon _ | Types of Electronic Transition. RX of CAnti-bondit). i — oy ac# (Anti=bondin). _¢-cnon-bondins Dare n>¢* Jeo Was Scanned with CamScanner fr) enetgy value order for Hansi tion d>s* > n>st It > noe set 3a bt -|6 electron From orbital is excited fo corresponding. antibonding orbitol o* ~The energy required js large for Mhic_tansitien, Example methane, ce4g) has CH bond only and can undergo s->s* transition and Shows absorbance moxing at 125 1m b) | n> 6* | - saturated compounds containing coms with lone pair of electmas | ilko N,0,S and halogens ae capable of N—> s+ transitfon, ¢) || + Ie* “lI electron in a bonding orbjfal Js excited fy tworrecponding anti~ | [boning orbifos yr. | {compounds eontaining multiple bonds Like alkenes , alkynen, Carbony! _nittilea, aromatic Compounds, ehe undergo IT—> IC transition. Example + Ajkenes. dy nse -lAn eleotron From non- bending orbita) Js promoted tv anti-bonding 3t* orbital. Compounds containing double. bond involving hetery afm, (Cc=0 ,C=N 5 N=0) undergo such tfansition | ©) | 6-74 franciHen £ IC-* 54 Hansitfon - there ejectronic_transiten are_forbidden Hransrtien gare only s—Lheoretfca) possible Scanned with CamScanner _ias =, Term inolog 4) || Chromophore. -| The. Poltof a mojecule responsible for imparting called as_chromophore- Ae “|The functional group containing taultiple bonds capable op labsorbing_fadiations above 200m due te n->yct and Tee Liransition ‘ “£9. NOpy N=0 C=0,.C=N CEN, CC) CS. b)_|_ Auxachrome. ophore which modify. Sa ality ot Ehuophore es csofi alight salieri are: Is OF} Thefunctfona) grup _wJiMp nan sandleg electrons that doe | nog absorb radiation jn pear UY 1 region _but when attached — ______|fo a_ chromophore alters te wavelength and intensity of aksorpHan =| example! Benzene Amax =255 nm, pheno! Amax =270.9m,— Aniline Amox = 280 nm, * i Absorption 4 latensity shifts 8 | K stuperc ic ShiFe . étypsochromic shift Bathochnmic shift —— | Absorbance COlue shift) CRed shit). | ay - i ! — > Aimy. Scanned with CamScanner (| ia 22 | Bathochmmic Shift Cred shift) : when an absorption maximum of 4 compound shifts fo longer ath, it is known as bathochromic shift of red Shift - shifts fo shocler_ oo -lshen_an absorption maximum of 4 Compoun ik ts Knows i Yupsochromic shift Cblue shift) “ f shit co niensity of qg compound tnereased, Jt is 03]| Huperehromic shift when absorpHon I enon as _hyperchromic shite. mic Shift * od tahen absorption intensity of a compound decreased , .if is Known as _hypechromic_Shi Fe p+ Jaws Involved in UV Visible Cpectroscopy a)! Beer's Jaw when the beam of monochromatic tight Js passed through thing medium, the ° °. intensity of jatfon_with increase i fn Cc) 0 Absorbing Species ws directly proportfona) fo phe etnfensity CL) Of the jneident Light AB D A \ D AB>CD A SS { ¢ cna Fig - Absorp ton shifts eaitn change in polarihy of the solvent | ~ the Increase in polarity of-the solvent generally shifts N—* € nro | bands fochorler_wavelengtn and 7 n* bands to Jonger wavelength, \ Chojce of-solvent \ A suiable Solvent for_ultravioler §pectmpscopy Should meet folfostng | Sit | tt showld pot sitself_absorb radiatians un the region under ceguirement | 02 (nvesHgation | dtshould be Jess polar so that it has minimum _Jnteractfony with the cdute molecules. \ | ‘||Solvent2_ which are fransparent ahove 2Jonm are Drhexane, cyclohexane, | | methanol , water and ether . Benzene 5 Chlorofenn and carbon fetrg— | Chloride can_not_be used becayse they absorbs wi) the Tange of about | 240-280NM. Scanned with CamScanner fet | Hist of common cojvents Which are generally used For fending OV spectra Stnoi| solvent wavelength L ol. || water x 20s nm (1.910 4°) 02. | methano) ‘ 2jonm (2030 4°) 03 | Ethano 2)o nm C2040 A°) o4.| Ether 20 Nm (a|sv AP) a chloroform 24S 0m C2370 4°) | Principles of QV-Yisjble Spectroscopy The OV fdiation region extends from lo nm to 400m € the — | Visible _radio#on region extends From 400 nm {0 £00 An _ UV. region! 200: nm‘ fo 400 nm fer UY region: B@ Below 200 0m | Far suv Spectroscopy vis Studied under Vaccum condition : T |The common solvent Used for Preparing Sample }0 be analyzed Js either ethyl alcohol of bexane. |The principle af ov Visible Spectroscopy ds based 0 beers Jambert's Jaw» A= ect where =. Absorbance __€= Mojeawar extinction coefRident c = Cone. oF-sarple += path length. Scanned with CamScanner SF _lnshumentation qssoviated with (V=Visible spectroscopy - ol “The essential component? Of specsirophofomeler aye A-soufce of. electromagnesi« fadjatjon . 02 A menechromator Cfo jsvlae q_partiavar wavelength or range of _ wiarelengtn) . 08 | A-sample compartment. 8 et ol! A-deleator and associated electronics Cfo meqswe fhe intensity of Cleetromagnetic radiation). os.|| A cecorder of dicplay. te Slit Rotating Disc \ fh. “fo Sy Caitor ea > = io Sample cel) ¢ \ | | Ught __ Diffraction | | groting, BS) , Deter | min. peiman OT TT Rorating r | disc i A | | fete | yt Refercene | Defeator eal | fo |] Out pF] / Sample | beleetor fig’ Schematic representation of ()y-visible Speotroscopy. Scanned with CamScanner Hl a EI = = ol. & source of-electromagnette fadiatHon. sowce of tight ——- The_best_ source op rtight J fhe one hich us More more intense 2 which gives fange of spect frorn !8o-360n, 4) _Hudmagen discharge Jamp «In bis lamps, hydrogen gas js Stored under relatively High preswe, | [Link] electric discharge vis passed through the. lamp, excited | ——-tydrgen_ialecues wll be_praducer_waneh_ cri dt tan causes ho emit a continous ae b) > dtydmgen Jamps eover the range 2500- [200A° | These are stable, robust ¢ widely used, _ Ocucterjum amp : lite is simjlar to hymen discharge Jamp» but Filled «| dewontal Lin_the place oF hydrogen. lp opfers Ss Hmeo more fotenctty than ofher fypes. This i i iti te balan $$ oO) Xenon discharge _ tn this lamp , Xenon of Jo-30 atmospheyic pressure Js file! — jo_ond_has two hungsten electrode -The Intensity ds greater — | than “hina gent dicchargeidlamp — wiinon is on NR Mercury ase Thi: contains mercury Vapour and _opres bends whidare |Shorp The Specinurn Js Oot continuous. Honce it i not widely — sed Scanned with CamScanner [oom] Lew [T 77] o2. 1A monochromajor 3 A wavelength selector that yseo diffraction grating or) Prism y and that allows continuous Variation oF-nominal wavelength . ) | Filters ‘ | =! Gross_Fi jecen of coloured glass which transmit limi | Wavelength) ranges OF the spectrum. | UV. __Dirference Is atsorbed wnbude fo Fig. Single beam Speetrophofemeter.. 1) Double Geam uy- spectrophotomely iy 1 JER the one Which two beams y —__Shaped_mjtror_called as beam Sp! —_ pper s.a. device consisting oF “a ciruslar_dikc. One third oF the disc ds Opaque _and ane third is transparent , remaining one third &_¢/rrored, —. dE Splits the: monochromayfc. beam of Light into twobeams of epua) Intensities. _ —Abvontages ow —— 3 Frain rapid. scaming oe wide J. region pee —Rluefuadions duote radiatfon: sowce are minimized, _fFdoesn't require adjustment of the transmiffance at OU. and /00% af each wavelength: =| Shigiveo rato of intensitioa oF sample of reference beams Simulereced, Scanned with CamScanner _Disadvantagoa ~ | Construction ic complicated + | (nstrument is expensive: “Application for UY Visible Spectroseopy ol | Quaitative £ Quantitative Analysies —____—- en [Ih is used for charaderiaing armmatic compounds Conjugated | Olefins. JK ean be used ho find owt molar Conc. oF He sojuse unger _study-_ 02! Detection of Impurities + Iki one of-the important method fo defect Impurities in orpang _Additiona) peaks can be observed due fo impurities inthe sample and it (an be compared with that oF Slandad Itaw)-mobest al . cal stauetute elucidation of omganic Compounds: | The presence or absence of _unsaturatjon, the presence of-heter Latoms Jike S)N»0 or halegens can be determined o4!| structural analys® Of-omganic compounds + fea coal theAmax p_fonger A “coated Isift). and reduotion ofthe compound or wsaiwratfen of-double.— bonds Jeads fo the opposite opfect je. hypsochromic shift b)||_ Effect of-geomelricdsomerism t t | Trans dsomer absorbs at longer wavelength Hhan_cis=[sorners- llofs fo trans conversion ts bathochromic shit ¢ hyper- Chromic eF Fook | Alkyl substtfudlon Lg shih. the Amar fo longer wavelength Chathochrom/c shift) Scanned with CamScanner —_——_} ~d) Nur “The addition oF rings Causes ——“4 ol. | Methods Na) caleedl o% SimwjJaneous multi component methad + a — e29dY) — Ce= Ge19%2, * “Absorbance ratio method derivative Spectrophotomelric method Acayi—Aray2 or Y= Aide) ~Azave2 = ARAN = Qe Ae Scanned with CamScanner ae 4 woodward Fieser rule q | Homoannulor diene? This q cydic diene having conjugated double bond in the’ Sint a 6) djeleroannuiar diene * This @ cyclic diene an Which double bonds in Conjugation ae pment win_dieterent rings Poo oo oer |_Endoryclic double Bond: | double bond present ina ting. as- “town In e9 Exocydic double Bond: A double bond in which one of te double bond js a pt ing system _shodn in_ring B 2 ascaglc double at Bord \y = N endoryclic fA double Bond ing. A-ha one endocudic one exacyldc dosti bel 2 Ring @ has only_one_endorycdic double bond ———~ Scanned with CamScanner [sens tiene € polyenes 16) Heteroannularconjugated diene Ton Homoannuar Conjugated diene lb) Awdic conjugated dine a) Acyclic ttiene —yAZ “Increment Q) Each alkyl Substituent or Ring residue | ts nm |b) Exocyclic: double bond = 45m |_©) Double bond | mor Sxugetien 2$3020m: | “Aasechn| “Jue cing residue = a Amax = 253 ¢10+ 10 = 273 1m Parent. “value ALring. are 2 exocyclic double bond = 2x5 = 10 tended conjugation _ 4 exocyclic double bead = 6 Alkyl substifules or ring resid Tetal Amox@ = = 958 P30FS430 = 3/3. 0m Scanned with CamScanner | Ford, -Unsajurated Carbonyl compounds a | _s | ag: An 215 pm. aa R=H 207 nm : X= OH ,OR CAcid or ester) 193 nm 4 = Qlky! Cketone) or sia membrane fing 245 MM Increments || Homoannuar conjugated diene. +35 nm Exowclic double bond tS Om 1 Double bond Oxfending Conjugation +30 nm | Auxoohiome! & 2 ) La/higher = HAlky) group or| tlonm_| t2nm_| +18nm | +120m _| Sm | | ring residue | = |l=cl ftlspm | H2nm | tl2pm | #2 om =| -04 __| 438s nm | +30 nm | 4300m | tsonm =| -sn. - | taspm_| = ~ || Ndo ay (vir _| +95 0m from Zr | =focoms 146 om_| +6 om | +6 nm +6 nm 7ier __{t2s nm {+30 nm +18 om! —+31_nm. = Tow ip3sinm | +30nm | +13 nm “Gal Parent jalue as nm Sr 4 alkyl substituent at «atom = Jo. om o — 4 ting substituent on B Cabon = [2 nm Amax = 2ist lot [2 =237 om | 02. OD Heterannular diene = 24s nm. | a fH fing residue (sxy= 20 nm ‘ Amox_=4IS $20 = 235 om \ J ~~ Scanned with CamScanner ) For acy! benzene ‘derivative =|! | | D& = | I - Parent | X= Alkyl 246 nm. Value | X= et 250 Dm ane R=OH/OR 230 0m | | ortho meta para | =| AdkyL + 80m + 3\nm +10 om. | =| o# fon + 70m | + 7nm__| +250 | =I cl _| Ob om _+ 100m —| Br t2Mm | +2 0m, tisom i = | Nie +13. pm + 18nm 458m 4 =| NHococs +20nmm |. + 20nm +45 nm, | | | Q ‘ te Gg” ‘Parent yolue for acyl | : Ckelone) derivative =2#46 _ nm | | + -Bratom at pasa posHen = 1s nm | Amax.= 246 t/s = 261 am ! _ i 02. Me (oy - Parent Value = 280 9m | ‘Ha = Alkyl Substitution 7 | at ortho posi Hon = +[Link] : Amox =) 230 +3 = 233 0m | | 1 o2 I 0 af | | (0) "Parent Value = 250 099 ; ss | + Ni, (Substitub?) at paras No iHon = SB nm | i _Atngx 52048 = 308 pm Ee Scanned with CamScanner { — ol. tek Base value = 2/7 0m. = _Atkyl_group_axs = _!s_om || Amax_= 232 0m 02) A) Base value =_ 202 pm. To [] Ge membered ring parent enone) _BF + X= Br = 2snm + B- alkyl (ting residue) = 2x12 = 24 nm 7 - Exocydic double bond = 1xS = Som Amox = 202+ a+ 24¢5 = 256 0m Base yalue 214 0m Alkyl groupe = _s xs =_2s 0m Exouclic double bond =8xs= |S nm i _——€ ____ extended conjugatfon = 1X80 = 80 tm ___ t _____| a Amax = 2)4t2st [S$ 80 =284 Nm ou @ase_ value Qs3 nm _ Ht kyl groups or (xs) 200m | __Ung uti = | Exotic double ond 5 nm __kmax_= 253t20¢5= 275m, os. Bose yalue 202:\nm | (s membered ting parent enone) B-GIKUL groups of ring residue = 212 = 240m ~ - ! _Fxoudlic double bond = Ixs = snm | | _ Amex = = 202+ 244+ = 28! nm _ 1 Bs lat = BIS om _ d-substitvents = fo nm i B-substituenh, = 12-nm Exowdic doublebend = 5 nm Max = YSt/OFl2ts = 242m Scanned with CamScanner _ a ol aS Bose" value ya nee | d-clkyl grup xfo__ fo nm B-alkyl group ap[2 2y om Amax = 4S tlofoy = 249 NM | - 28 1 Bae value 214 0m Ikyl group Bas Js nm | Exoqjclic double bond Ss 0m | Amox = 214 +IstS = 2.34 0m i or ieee 03. a2 Cisoid (8ase value) 253 0m | Alkyl Substituent i s_nm Jatyc7 “cody Ring resid ye: SAS [som Exocyelic double bond som __Amox = 2sats tis +S = 278 9m Scanned with CamScanner __IR-Spechestopy. Anjroduction s— Infrared spectroscopy CLR Spectroscopy) or Vibrational Spectroswopy) involves the Interaction of infrared radiation with mater. J cover Tange. of _fechniques, mostly based on absorption Spectmscopy. —— As.with_all_spectroxopic_tecnnique, Infrared Specirescopy CIR) is 9_Characterizarion fool chemists use fo help determine the molecub, | Structure . ON instrument calied an_ infrared Spectrom eter ———-JR specira_is_ mainly used in_structure_elucidatan be determine the | functional grows. i Is agency already known that: _ Energy of amolecule = Electronic energy + Vibrational engroy + Rotational enegy ee Principle | then the enesgy {the form! oF IR_is applied ond iF the oppiied _ LAB Frequency = Nofuas Frequency of ribratfon, thé absorptron ———_| oF JR taken place_ahd a pear js observed. 1 ~feaules are excited to the higher energy state from fhe round State «hen they absorb .|R radiation . +The _bands_cotrespond_to the characteristic funettono| [Link] ——— The bonds present ind chemico! Ginicture) substance. “Thus an IR ~———|Speattum of a compound is considered as the Fingerprint for | ——_Lults _chemica} _ Identi ication ne 4 ~tdhen_g compound is exposed fo LR fadiation , jk Selectively ——absorhs_the fadiazion resusting [n_yibration oF Me molewlen ~—— 2£ the compound, siving rise fe clesely packed absorption | bands, colled 09 JR absorption spectrum Scanned with CamScanner -— R_ spectroscopy bosed cn_tloake!s lau Suppose {190 ome aed Ma sseo_aye_conneded through spring Chond),, then the ene. tibetin can be reprinted by Fillo, g_ amc “lt 1 ft { } i = reduce masc js _expressed as 1 a y= torre. Cm tm) [here Y= Frequency 4 = reduce mass 2 C= Velocify oFatight: K= force constant _of-bond _ | Pssasil “Theory &#/ Range of JR Spectra. _ T : a A+ Near infrared (overtone region). 08 -um ~ 2-um) B. | Middle infrared} O}. functional region 2. ‘um — 3 um .Cfundamental region). 02. Fingerprint region. gum -|s-um C- Far Inffared) ¢Rototiona) Vibration) [Sum —. [000 -um, | ueisa + _ Gritetia_ fora: compound fp absorb 1g radiation Change. {n_dipoje moment + Caulsesa._changa iD « Gs _eleottic dipole... er re eae Snead olens 1 /6r nok at all. . ues 0 lngg ae cr ects — —-Acpolar_bond {s Usually IR- active. ae abso ct ty Scanned with CamScanner — - coneet wavelength of hater bpodjation \ | A moleule absorbs radiation only ae Beguine ae the —] ‘ncident tadjation_is equivalent_fo the nodural Freguene iaton “of. the part of tte molecules. ae - | APter absorption of the correct ccavelenght oF 1 (odjations, the |. | molecule Vibrates at [ncreased amplitude due fp absorted JR energy . ~ + | tcl has noturay vibrationa) Froquengy of 7x10'%/c i: (ot00 wi) 5 when dC} sample ds exposed fo IR podiatfons, « only the L Cadiations oF Frequency. 8-7 XId ube of bes ase_abst . ore _transmitied:. ates h Molewlar Vibfations » = + A Moleave may not be Jooked upon as a rigid assemblage oF Qhoms- a z : / 3 Ratner it may be regarded as a sort of Aexible system : compnising_OF-balls_OF varying massen representing tne atoms of |. lq molecule and sotings oF Varying. —Strengths representing the Chemie) bonds of gq molecules . Ina molemsle , ajoms are oF Stationary but Bond Alucuate |. Continuously due fo different _Npeo.o of libration ,___-_+ Classification : hs i Mode of Vibration : - | Stretching ee ibn eri peti | “ ft [ [ f a et i a e a 8 | | a! {Ht Scanned with CamScanner — —— ——— 7 Te vit or motecues cme f-pou no hype ____|| stretthing ®ending += $$ = Li A.| Stretching ( Gond_length_al! peregyns adr awh gE “Theso_vibration_involve_a_contrhuees change in the tolercefomic | distance along the axis of @ bond between fusoafone. c-4 ar Stretching [types ‘= \ a)| Asymmetrical! Tivo bends dnerease or decrease intength Asymmetial, b) symmetries 3 Two bende [ncrease or decrease Jn length sgmmestice) B.|| Bending here is continuous change sin the angle between two bends én | Bending Vibrations . || (ae | me “Typeo a.) Ta-plane ibratnt | ob. Rocking : Bond angle maintained but“ both bonds mare within Ihe plane. : 02. Stissoring : Bond angle cleerease b.| ut -plane Vibration : Ol. wagging : Both atoms tnove to one side op plane 02. Twisting: one ato Us above fhe Pane ¢ the_other fs boleu) the: plane ER SIE Ss tle a St Recking wagging isting Scanned with comScorner Wes. ~~). Coupled _bibr s wena Ot ath “OCCWR at diFferent_| frequencies o€-highec awe Lqumber are called coupled _ Libration «| Fermi resonance: (—__$_—_———$——= — = oe Factors affecting. (roleular baton: | Symmetrical — lower [Link] vision he | _ Asymmettical ~ higher wave tuber sokvasndl Sapae) | ah IR_Spectrum “absorption be bands are ieee eoTeA Frequendion.. Then the eneray of 5 eae fo coincide with the fundamental mode. of ditterent ibration “This_fype of resonance js called fermi Peronauce 4 o3 Electronic ef feoh! st Changes .th_the absorption Frequencies for a particular group faker place_wlhen the Supstifvents next fo that of partiasler gry + Lore changed . The frequency. shift includes : «Inductive offect +i effect decreasing wave humber 5 ‘Inductive. effect —j\ effect increasing Wave numbe, k - Me someric_ofteot Jengthing of bond «ili be weak, decrease lp force constant » decreased value number 2A. ttydragen Bonding a i ae an TPE ——L “d-Bonding gives rise fe downward Frequency shifts. | ~~ stronger is d- Bonding_, greater js fhe absorpifon shift foubyd ~——| dower wave number | "| L Scanned with CamScanner “Instrumenfatfo _ (the main parts of IR spectromeler ae are_as_ Pollo ol. Radiation cource re oo. athena of. a Saacattc ¢ Sampling anata _ : f fester - 7 N\ v Lp z ‘SOUE I lest nine ete” Optra! a Arete fie Won ~Aropiiir Delecty. BREE 0 608 spactréphaidinetee = RadiaHon Sousce IR instruments res reqult@-q eource of adiant eneray «ahi emit IR _——__ltadiation tahich_ must be steady, Linkense onough for detection 6) Incandestent: rire ¢) | Glober Source | f-extend over He desired earelength « Variou $ Sources or-IR | fodiations are as follows! Nerst glower eta yb A 840 ovio pei Hl Ee 4) Nernst Gloser sl (Sq cylindrical ¢[-2 am_diamoter °ry_approx 20mm/ong) of rare earth { oxides. . JL = Scanned with CamScanner ay od. O38. ™ " Platinum wires are Sealed foe ene anilalen ren ont passed though [he cylinder sntsiia po k Tho Nera can redgh femps of 2200 f mat | Advantages: _RadiaHon intensity is. approx. thrice thato £ nicome4 (ola pSuican mcr pv the: near’ infrared fegions ots fadiations over q wide range oF wovelengin, ent oF fadiaton remains Steady cand constant.¢ ove a_long po cae used in air as. kis not oxidised. | petfod_ of Hime. _ oF —r—t~—“—O™———C = eal spor _ FG '3| =p oh ft "| eo 7 Baliaot I a Mognelic (ariadfen a 2 te 4 Ft ets: Nernst Glower- {| ib) Incandescent wife... —__| The incandescent wire Sowre Js “tightly wound calf) co il_ of | nichrome wire, electrically heated fo look. — | FE produces a_fower se ata we Panta | Sources bur-has a donger sDerfking ti fe, — er fhe fi #dvantages : ol. the Nichrone coil | does not require eel 2h ~~ | od Nemnse BT a __ Ft requires tile or no maintenance ¢ gire tong service. ____ ‘This Source Js cimple ¢ rugged This Source lasts longer_in_ thelr Comy arisen fo globar 4 ¢ perch f : fo Hose _ produced. _Dfadvantage. Lt produces ‘IR radian of love int ee by the globar source on by. the Nernst glower. Scanned with CamScanner i | Ze Ge —Nichrome dire | - Ke i | Q- — | Se hondaat oi Sih Gtobar Source Ag | The_Globarcoure js. @_silfen carbic a !SO mm jong) which Is Clectricolly heated ho About [St i Water cosling of Me Clectricol cans! contacts Js Needed eprevent arcing» : The spearo] outpub ./s comparable with the Nernst glosers except | ae nae les than sum) Whereis o output becomes i pa ol The Globay source J's Superior beyond oubout ps . ir on. Jf emits tadiation af S200 ent =| - i: na he el crigarena Nernst glower the globar Js less intense courte btebu) Jo 4. of Sin Carbide rod SS ft smm_diameter , nfong._ - | fig: glebar-coure, 2 05. | MonochnmotoR «fe monochromator jz an OpHcal inshument whic A + Sp ei ich_ Measures fhe Light — Tony ce ta roentgen comits —--— ony e Owpub S/it of ime — ectra_are hen recorded wardensth by wa cuted ae | I Scanned with CamScanner | \ Z 7 = A: [Grating te lipaie ener in gting enciamate rte difac, - grat ng r ides a constant dispersion Rr al wavelengths and a (o.) Lepr jence On temperature = «| towever , they produce reatively Jarge amonft of Scattered Light ‘and require the use of Fillers fo block higher order light. - | due. their Superior dispersion propertien.. distraction gratings auc, beten used tn modern instrument? EF Sendl a prise “The dispersive element in pristn monochromefors Js_4 prism: ‘Vesian tea highlight Utilization eFfiefency and donot profuse i licer ont slg vey tei gn eh _____ | Howerers dispersico_Js dependent on wavelength Chigh foro, See a colic [ 03. _Sample-cell.s L a — - | Infrared spectaseepy routinely is used fo analyze gas Liquid, Land solid samples. ample cells_cire_tmade from_materials, such as Nad) Cer, _ that are_{ransparent fo infrared fodiaHon. —1Gesor_are_onalyeed using «al tha palate of appr _ do cm. | ob sii iro the beam of radiodion Hugh the Sample Several times Scanned with CamScanner FEE = Kado of-dubstances. - IR spectroscopy has been used for the character! erbecttion on oF Saf, — {to quid or gas samples. —_________—- -, Sumpling of solids powauriat ra 0}. || Solid Films + | Solid: Films can be seeending depasifes onto Nad or KBr plate by | allowing aso! fn [Link] solvent fo evaporate crop by dep lon Whe Surfaco .of—the Alof. Some solvents used Gre Chloroform, carbon, felechlonide Ss acoines 2 __| eydlohexane. — 2 A : | 02.| Mull Technique: a ieee [n_this Feahnique Qs small “quantity OF dample is throughly ground ir ind clean mortar until the podder js Very fine. v1 After grinding, tre mulling agent (mineral ¢ oil or Nujol) i | introduced Small quantities just Surtident fo fakeup | the_povdder « |The miglure Js then transferred fo the mull. plates € the plales ase squeezed fegether fy adjust the thickness of—the Sampk | bel between IR transmitting —wirdos- Thés is then mounted i pe be poth of IR beam f the spectrom js ten, | L 3. | press Peller + Feahniques | vi : yl thic_fesnnique jue.q_ smal] ¢ quantities OF. Firaly, gn id solid sample. - is dntimately mixed with About [00 times it Weight-oF » UW Promide, fn q Vibrading bolt milf, ee THe nets ground mixture Js then presed under yey. high a ure_(25090 Ps.) th Cvacunble die_or minipress by form a small | Pallet Cobout |-2 mm thick ftom in diameter) , —— fies is fransparent fo IR padiaten and f is tun as uth. Scanned with CamScanner vi i | nm L [ oe 1 77 _ sampling OF liquids ~ ye quid sam Step Sells can-be-Sendulched sig ud Sam Sample cells op lihalides, Normally Ne, poeta Gi ska oe ae ee ni iactata- _used because they Cannat dissolve alkali halides fe ickness Should be selected so that Me fransm itane leg [between |S-207 solvents elise Chloroform ean be ued. |For mast tiguids, the Sample cell Mhickness Js 0-0 -osmm Some salt FE ‘plates are highly soluble cin water, so the Sample and washing reagent ~ musk be anhydrous: : i+ Jhereare_aifferont types of transmission Solution cells available |___ol- Fixed parh fength sealed cells 02. S@mi-pPermanent Cells are demountable o3. Vafiable path length cells “6 Sampling oF gase- ath The_sample Cel is made up oF-N0) K@[Link] it is Similar to tre” Liquid sample cel! ? Sample cll with o-long path lengin_(S-Iocm ) f= eeded Because the gases shou) rlatively weak absorbance 1 Detector [There are 2 hyper of detectors used in IR Spectraxopy Therma) deteojor ¢ photon defector —~AlThermay_cleators + tohen |R radiations Fall on. detectors , they casa | heating uhh e_ise.2_ poll stsstce-nehs «|| Measured . ‘| Potential difrerence depends © Hhe ame. oF radiation [Thermal elector are_as f//ow)s * Scanned with CamScanner + Golay cell - ; Al Ison the _expansi as as the measusing device. a — athe deter canst of q_small:metal Cylindrical closed ty ¢ square) at one end oe +. ffs spedial_use above so-wn _|-e. [0 the far regions | where tadjation_Js Jess energetic - ‘Disadvantages x aa = 1} In near £ mid JR regio, ths SensitvityJs comparable, __ 4 IR radiation bb, pie IR transparent window | wo [ef oak tt - y 45—¥e gas sariee, a Photohubes >>| |_| : _ r. NN \Tl2 2 ls —Aexible diaphragn tI Fig. A Goky call. 02 | Bolomefer a |Us@_material eohose_tessfance changes ath the change «in the _fempefatuure _dekeolor consist oF responsire lement Of. this thermometer js _ |, Mode up oF Strips of metals Like Platinium or dike) or g | Semi conductor is used. sin the deotor, the device ds called on _thermister. = +The responsive clement made smaller .in size i Blackened, _[é Connected #0) electricy circus} . Scanned with CamScanner Ben i 7 eh ee aol i a a ining A Sli ial ma — detector because: oF simited 01k 7 lokensity OF IR rediatfon 4 | IR fsaliB BNE oni | d =e veel Fst A bobimoter in OB Thesmocoup|e | The Thermocouple detector 8 based upon the act that an electnial, iGurent will Flow when two dissimilar metal wires are Connected fagether at both end and a temp. differential exist between ‘two ends Advantage An efficient thermocouple detect can produce SufFicionty large _ fra temp as Jow as /o-6°k | Severas thermocoupte Can b e connected tn Series tn order ty i —__lenhance the sensitivity of the measurement. The detector th such ry f acase ds referred fo ac a thermopile L| r IR radiation r Defector junction r| Scanned with CamScanner | | | “al thermicter’ * ~ when He Semicanduatoy malerial is used as responsive lemer is & | calied as Hhermisers: 3 This Glows tnuttiple Samples Jo be collected and averaged —__ fegether fesulting:in\an improvement in sensitiviny- Instumentetten Infrared | Hght sure T 7 t pea , i > i ‘ampje inl | so" e} 1. ae fig FTIR Scanned with CamScanner

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