phagilagasll acetal Spende wide mouth bottle lead dish dy triangle medicine dropper 4 Funnel vack Beneen burner Preumasic trough e——_————- | combustion spoon CPPCC Eo CES CEE C EP Ceo C ESC CEC EEC EEC CCC CCC CC CCC CSS VSS SSS SSS SSS SSS SSF T SFT T EF TESS SSF TFET TFET TFS T TSS FLL LLL LLL LLL LLL ILE LILLIES ES HE ttt ttt tttLA NANVNANVN AVANT ENED TENANT AN ANETTA YN ‘ Fovceps Flovence Flask Glass Plate G— test tube clamp ————> Stirring vod. | Graduased eplinder SLED wire geuze | Buvet clamp | Ks Glass Funne) PO*EEIAIn evaporating chish | tese tube brush Frongulay File De SP CoP ESP CoP EPP EEC EE PC CECE PC EEC EP CLEC EC CCC CEE QS SSS SSS SEES SEF S EFSF FEF TFT TTT TFET STE SSS SESS VIL LPL L LLL LL ISI LLL LILLE EIS SELES ee tt tetNANNVVVNVNAVEN ENTE VEN AN TT AN TT TT ENV YN 4 4 E = thistle tbe } Ring Sand anc : ivon vings condense | ATT Different Filtration OR v. RISA AA RAR AAR RRR QPS SSS SSS SSS SSS SESS SSS FITTS FSF F FFF F FFF TSS SF SHSS PEEP LL ELLIS LLL EEL LL ELL LE LLL SELL SS EttSNNVNNVVNVVUNVV VEU V EVE DOVE V EVV EVN ; Simple istiMlation exuienent | aa Finang Filterpaper inte Funnel al? 7 Sublimavion equipment _Beehner funel and suction Flask, Balances ‘ LLLLLL LLL LLL ILL L ILLES ELLIE ESE LEIS ttt QS SSS SSE SSS SEES EES FSET FETT FEE TESTS TET TFET FTES TS SS CPSP PSPC ESSE SECC ELEC CPPS E EEE SELLE EPL ELE EEE LES 2 ||CPPP SES eee CEE Peo CCC EEE EPC o CELE EEC EEE E PCC EES NANA ANAN ANNAN TATA EAA LAAT LAAN AA WN Separation and Purification of Organic compounds A.Solid Compounds: 1 Filtration Y.Extraction ¥ Crystallization £.Sublimation B.Liquid Compounds: ) Simple Distillation Y.Fractional Distillation A.Solid compounds Experiment No. 1(Filtration) separation and purification of compoundsmay differ in their properties at to permit an immediate and quantitative separation through difference in: ) Solubility \ Density Y Temperature 4.Kind of solvent and other properties. in this process advantage is of for thatcomponent of mixture of substances, may be readily soluble in given solvent where as the other component may be relatively insoluble. EB ae VEEL LLL SELL LES ELLE ELLE PLL ESL LL ES EES QS SSS SSS SS SESS TFT FEF ETT STF FEES SETS FFF ESSE S SEESDEPP S Sooo PE EE Sooo ECC E EEE EE CEE EES PE EE SEEPS CELLS SNNVANVNENAN AVENE ENO EN DVT ENED EDV YN The mixture is taken with solvent and filtered, the soluble component may be recovered from filtrate by evaporation of solvent; while the less-soluble component will remain on filter-paper oa! fe Flask Simple filtration iy ppl ba Ugule ached i) al pall Sale US Gl sill AWS lhl g 95 cull E93 Sylyall days Chyhall gb ght ype NN al yall Lal ABD Chall ag Ay gall yal Abit Organic compound soluble in non-polar solvent ( acetone , ether, ccl, alcohol) and insoluble in polar solvent like H20 Inorganic compounds insoluble in non polar solvent and soluble in polar- solvent. PELPLL LLL LLL LLL SELLE LLL LE LL EES ES Stet QS SSS SESS SEES T TF FFE T TTT FSFE FSET ETFS SST TF OSANANVNANVVANVT TARTAN EVEN ATV N EN EEN TN AA AAA AA A ee ed Filtration : there are (2) general method offiltration A.Solid substance has crystallized from a solution and it is necessary to separate the crystals from cold liquid by filtration Simple filtration B.Hot solution has to be filtered to remove trances of insoluble impurities and kept hot mean while to prevent crystallization of the main solute pueall A qeye LS lal ola G5 aatuuall lye er Filter paper Buchner _ funnel HF Buchner flask (the apparatus used in this type of filtration ,the Buchner flask, Buchner funnel ) VIL LLLL LLL ELLE LE LLL LLL LLL LL ELE LLL LEE QS SSS SS SESS SSE STSF EES S TSF FFE FETT T SF FE SOTTO SSSNANNVVVVVVVVVVNTDEV EVV EVVVVVHEEE HD CoCo CLEP ESE Eo ECE CECE EE EPEC ECE E SE PEPE CC CC oP CESS Hel pd Qnty he pled (9S Lente (gli Alec) gy pull ell diy pall ode gadis coed gb Lal gh Quad he Abin y ASIAN je Gail pl AN GY dann Gans 1A ob Sas cy Apparatus used : (Watch glass ,beakers , conical flask ,glass funnel , stand , filter paper stirrer , cylinder) Procedure : ) Weight (0.5 )gm of salt. Y Weight (0.2 )gm of benzoic acid. Mix the salt with benzoic acid in small beaker. £.To mixture add ( 30 )ml of distill water. © Shake vigorously and filter , wash the residue. ‘Place the filter paper in oven (90 ]C° to evaporate the water . cet le fb Jad B42 Jb at fy G58: A V.Evaporate the filtrate on heat till dryness . A Weight filter paper and beaker. hill Ghee wy ‘Calculate the percentage of salt and benzoic acid. 10. Repeat the experiment by using (30 )ml of alcohol as solvent,why? )) Record the results. Results and calculation : F, = weight of filter paper F, = weight of filter paper after dryness FeFcF VE LLPS LL SLL LLL ELL LL ELL LEE S EEL ES PS Et tt QS SSS SSS SSS SST FTF FIST TSF SEES FST TTS SESE SETS SSSSMNVVVANUVVVVVVVV VDT EVOVVVVV UDEV VN YD DPPC E LESSEE SEE EEE ELSE CLS S EPC C CCCP S CPPCC PCL LS (benzoic acid) etl Lee es AIM SALI) 55 W, = weight of beaker W2 = weight of beaker after evaporation W=W2_ Wi Gipsy gp I ee any AI BALI Oy wnew Mrz. X 100 Percentage of salt = Frew MIX Percentage of benzoic acid = X100 Percentage of salt cr Percentage of benzoic acid = es x 100 Discussion and conclusion : PLE LL LLL LIL ELLE E LL ELE LE LEE SSIS St ett S SSS SSF FSS FSS FSS FSF FSGS FSF FFSESF SSF SESFESHEF TSH TOSSSNNVVVVVVVVEVEVEVEVEVVVEVVV VED HHI Name : Date: Experiment NO : NAME OF EXPERIME Aim of Experiment : Theory : Apparatuses : Material used : Procedure : Results and calculation : Discussion and conclusion : CPP o ooo ooo eee eee eee Peo e eee CCPC eee CCC CPPCC CC Ce eS VSS SSS SSS SSS SSS FFF FFF FFF FFF FFF TFS SFO FTF TET TSS PELE LLL ELLIE LLL LLL LLL LLL LLL LEED DL SL ttLS NANANVVVNVV EVEN EVEN EEN ETAT ANTE NY Experiment No. 2 (Extraction) extraction: Is a method of separation of solvent distribute between mixture of two solvent immiscible in each other , it is influenced by factors such as : ) Type of sample Type of solvent ¥ Solubility {.PH-value °.Number of extraction Ale Liial oh yall yee Ay gata CLS yall Jad Litto Adnan Le git 2S) Lay bl gf USGA! eat Apel 4 ptanll OLS yall chet sf goes Be ha dplae ee gpaee AS Leal lee iy sal oa Jani as 4 cee cial gia g Sian Y og patee Cydey (gill! Jp lal pg A hall BLN phy Casha igs Jit Ge Ga Ge BAS iy ual Aapalls cual Aiba ela) i Aglare ig aly ype Ghyll gs SEY Apne WLS ye cduF UI eLall gS Yili lglh Ugiliny bigs Sy janelle dy panel CLS pall Uf Aystaall Chyhall dig 3 acd * Organic compounds soluble in non-polar solvent like (CCL,, CHCL, diethyl, ether , Benzene , acetone ) * Inorganic compounds soluble in polar solvent like H,O and insoluble in non-polar solvents. CPPS Sooo eee eee eee CEE EEE Pee CCE Eee oP CCC CSCC CC CES SSS SESS SSS SSS SESS SSS ESSE SESS SSF SSS 555555559495 VPP LL ELLE ELL LE LLL LLL ELLIS ES Eh Pht tteSNNNVVVVEVEVOVEVEVVVEVEVOVEVEVEVEVEDV EN #This method is depend on solubility of solute in one of two layers *#Thecommonest solvent s used for general extraction method are Ether and Chloroform Solution of liquid in liquid are : ).Completely miscible Y.Completely immiscible Y Partially immiscible Limmiscible Solution : they are mixture of liquids , which are insoluble in each other ( oil and water )( CCL, + H,0 ) Such solvents form two layers ,the light layer on top and heavier layer on the bottom. 2.Miscible Solution : they are mixture of liquid ,which are solution soluble in each other ( alcohol + water ) ( acetone + water ) 3.Semimiscible solution :they are mixture of liquid , which slightly soluble in each other ( ether + water ) CPSP CSP E PoC CEP CeCe ECC CCC CEP CeCe eC Cee CCC CSC SSS QS SSS SESS SESE ESSE FEES FESS EES SES EEF SESS SSS SESS VELL E LLL LL ILL LLL EL EL EL ELLE LESS LetteSRVNVNVVVVVVNVVEDVVAV VE VAV EVAN TES YEN CPP P PELE SSPE EEE ECC CEE EEE SECC CC SoC CCC oo SCLC S SL eishl e— Lighter layer aqueous Layer) H20 Benzore ——Sp-t#—— heavier Layer i Corganic Layer) Ft chiovole t Hel: ot hloyorerm ccly ove 3 | Zyp\\ Epil ach (immiscible Chloroform solution ) + HO Benzoic acid + Salt Organiclayer + aqueous layer CCL, or CH Benzoic Cl; + water (H,0) + salt LLL LLLL LISLE LSS ILL ELL ILI LESS SS SL Sted VSS SSS ESS FEES SESS ESSE SESE S SESE SESS SESS SSS SESS SSa SS ual) gad placa Juaill Ais * A mixture of benzoic acid and salt can be separated by extraction using chloroform (CHCLs ) and water ( HO ) as solvents The chloroform (CHCLs;) layer ( organic layer ) is lower layer and contain benzoic acid , while water ( aqueous layer ) is upper layer and contain salt . The two layers are evaporate to dryness to get residue (benzoic acid and salt ) in two beakers, weighting the residue ,then calculate the percentage of each. CPPCC LES E PCL C EEE E ECC CELE Seo PCC Ee SPCC CCS CPPCC eS VPS SSS SSS SS SESS SES EEF FFF TTS FSFE SSF TST S SSF SSS VELL L LLL LLL LIFE ILLS SLI LE SI LS DES ttt tttCPPCC EPCS PCE LEPC CECE CCCP CCPC CSC CPP CP CLC CSCC SSS SVVVVNVUVVVVVVVEVVVOVUEEVVV EVV VET E EN YEN Procedure : ) Weight benzoic acid (0.2 )gm and (0.5 )gm of salt then mix them \.Add ( 30 ml ) of distill water ( D.W. ) Y Heat the solution. *.Pour the solution in separatory funnel. °.Add (5 ml) of chloroform. \ Stopper the separatory funnel and shake vigorously. 7.Allow the two liquids to separate into clear layers and separate the aqueous layer from organic layer. ‘Pour the organic layer in small beaker( ). 9,Add (5 ml) of chloroform to aqueous layer and stopper the separatory funnel and shake. 10.Allow the two liquids to separate clear layer. 11.Pour the organic layer in first beaker which contain the organic layer then pour the aqueous layer in another small beaker ( )of known weight and evaporate till dryness. ‘Y.Weight the two beakers . \Y.Calculate the weight of benzoic acid and salt. ) £ Calculate the percentage of each. The properties of solvents: ’ It must be volatile ( has low boiling point ). ’.Immiscible with water. ¥ Solubility of solute in the solvent must be high. PELL LLL LLL LLL LES L LLL LLL LI LLL LIES LS ISS S PSS FSES FSF FFF SSF SF FSF F FFF FFF FF FFF F559 99559959994NNNANVNVVVVVNVVU VEN V TTT TENT ETE ONS ‘ AB pee eA Sy Slant al 5S GS ol Ging Hall ol 9 ALi Aplatly Repeat the same experiment by using another solvents like ether or ccl,? Why ? explain that ? Bcd peal cya) Ata yA ait Ail) Aa igs Gf: Abad Oe gi AS HY Lead astitly (gil all Jp tall Llis (te sain J alll Aah A badly cll Gee Ci eb lat og gall Qual (Gy all Ce PLGA Sub paliinwall gh ppitall gto Go igh yeas irae Yo Ei » Qosll SAAR A ARR RRR RRA AAR SSS SSS SSS SSS SSS SSE SFT FFF FSFE FFF FSS SSFP SESE S FT TES PLL L LLL LLL LLL LLL LLL LL ESS SLL LL LES tt ttNANVNAVAN AN EN ANETTA ETAT VN TATE YY A CPPCC LEE L EE ESE ELEC ECE C ECE CCCP ECC CCC CCC CC CECE SS (Crystallization)Experiment No. 3 “This method involves the process of preparing a saturation solution by dissolving substances (solute ) in desirable solvent at an elevated temperature and filtering while hot. The substances should separate in crystalline form upon cooling. Bashy Alas By sh Sale| Ashen iis (Sash c AS ye Sal Ay pz Salall Cuts 15} gid Ullal (Siang Maal! Xp geconll ol gall 25 5 48g pas 5 al pal iy Ll ob ies lop AU,t8 cole Bobalydy of gh Aue gh pay Ay pels Guha Iba te gs y Gulia Gushe GLI! gle aia Cue. Wg cl ill 1S 15 ly Ua Sutlly Alall gles sep ddigall Solel lgetd Mp 0 35.555 yo US gy Col ya Bae B ysl! Sale| Ashe gpa 2 je Bae AGEN) dee I SS any La lgnell Ap. js Cab 1S) Las Salall GW Sy a 4 5 Savin (gill Gusdall ual Sh yg Ris gle Ain Ga i AIL Mays le kl ye Lgl pall Saba git Gf Gans. ehegl Gud) LB AGE gue Sal 48 Ga gh5 coll Cuda) Ulex 5 yay Yul SY ally oul cet Ug yall ol yal ge Jelits Y gill ud Jet Gos. DEE IE ety Gall asd) OS of Laas gpl ale plate JSS CNS, Maal oly gly galas gill Cub Slavia acais € cots lS y la AE Gail ph gf ASLAN ol gall Gla 93 AE 44d Gy 9S gl Cuda lara Can. gee SaLall asad Ll gies LLL LLL SLL LLL LLL LES ELS LESS SLE LES ES SSS S 999999944995 4559995 994594599599 F955 4559995999 5999%SNNNVVVNVNVVVVN VLU VAN TATA V ATTN TNE ENS RIAA AAA lt consists in first finding a solvent which will dissolve the crude material ( ) Readily when hot but to a small extent when cold. The crude substance is then dissolved in a minimum of the boiling solvent , the solution filtered to remove an insoluble impurities and then cooled, when the solute will crystallize out, leaving at room temp. ,the crystals are then filtered off. * solvent for crystallization has following properties: 1. Dissolves the solute readily at an elevated temperature. Y Dissolve the solute only sparingly at lower temperature. ¥.Give no chemical reaction with solute 4.It is sufficiently volatile so that it may be removed easily from purified crystals. *#Crystallization is effected by the following factors : ) Type of solute Y.Type of solvent used ¥ Time of growth of crystals £ Temperature Ag ay galls Galil Gupdell hits! asl LSB easy BRI Cl gb lg ny Mola BL pe ye SL pS Bald Sls (Ld aay Le ey all cscs | iad SpaS cle Guat Gyms Gude eile AGMA 5) pall ile jo 8 W a9h al NSY Lal clay Y pede by gay Gud 8 Avil auto de chat PILLS F ILLS FILLE ELL LEE ILLES LSE SSS tt tte ee eeNVVVVVVEVEVEVOVEVVVEVEVEVEVEVEVED EDV IN Choice of solvent: Benzene will dissolve hydrocarbon The solvent will dissolve most readily compounds similar in constitutionto. its self, thus alcohol usually dissolve the hydroxyl compounds . The final choice should depend on inflammable of solvent and also on its. Acetanilide , charcoal Apparatus : OPP CCC E LES LE CEL EEE PCC ECE E ELE SPP P CEE ESP CCPC Co oS cost, tog By ghll Alec G3 arias lly AaiLtll Glyde solvent Boiling point solvent Boiling point water 100° Acetic acid 118 C° methanol 64.70 acetone 56.50 Carbon tetra ° chloroform chloral (CCLy) ee CHCL3 og 42%ethanol BO benzene 80C° "i Petroleum ° Dichloromethane 410 ther 35-36 C' Toluene 110° Reagents : Watch glass, beaker, glass rod, Buchner flask, Buchner funnel, filter paper. DELLS L LSI LLL LIL LLL FELL LESS ES SSS et ee tt S 9954459959559 9999999999559 9555 FFF FF 955559594LNANANVVENVNAN EVEN ANTE TA ANN ENYA YY ND CPPS E PEEL PEPE EPC E CELE CEE CEE SCEPC PCCP CCPC CCC CS SS Procedure : 1.Place a sample of impure acetanilide (10 )gm in beaker containing water or weight (1)gm of benzoic acid . Y Heat the contents with stirring. Add about ( 0.5 )gm of charcoal and continue heating with stirring. + Filter the hot saturated solution. © Transfer the filtrated in to (2) separate beaker. 6.Leave beaker (1) in ice bath and water ,and beaker (2) at room temperature . ‘7.Compare the shape of crystals form at low temp. and form at room temp. ‘Filter the solution of beakers (1)and(2). 4.Record the yield. )+.Calculate the percentage of yield . wt of pure substance a ee wt of impure substance Percentage of pure crystals % = PELL LLL LLL ELLE LLL S LLL LLL LL LLL LSS Stet S 9994945494555 5 5995999554955 55599555999 959%SNANVVANAN EVAN VENA VLU EN EN ENT A (és heer Suction | Pasa Sotuveed Soluatien by Quen and 5; Calcul toe Weight A Wy CoP CPPS Eee Pee CEE CCE CCE CCE CC CeCe CC CCC oP CoC CSS VPS SS SSS SSS SSS SE SSS SESS SF FESS SFE FFF FTE FFT SSF SF ST SEGS LILLE LLL LLL LLL LLL LLL LLL LLL LLL ELE SS teNNNAVVVVVVVUNUV UV VU V TVET TTY YY NG RAS AAA duit ge cilia apes elall 8 Uhl all 5 5S (benzoic acid ) chs jill Gaula tale U8 aie, | wp (1) Gaaalall 59 bales de (1+) «ls ol ool eal Gh 4 cod Le AY Ll cLall ye UB Gal y 6 aad 6 il Uylaall GUI Gd yaa 1 wvadall eat phe ASN ALAN 8 at ill ate call pgs ayes si Gad glial! Lally Syl Gust, Gail yl eo ead jh AB yy Soa hal IS y Lk gy mk a ob qual pla putas iS (ple 4 pall ode arin (Buchner funnel) Jains 18 cst jill 4d yy gle glued sf al yall BaLall a Gil pall hot saturation solution (a 35 guts! Jslaall et 8) Se pu ct il el a ABs gle Aa gaz) Salad) ou 38 Of GALad) glaall cat ate Ubal ay 5 Al oboe sith gid oh pall Ay puznall Salad) Ni & ALLAN oda aid ye Galull Sylaall ae 5d UI etl UM AneS pladal'y (16% — V+) cope cual (ye Ball 5 ARS Gilead 9b I ye AS iL ee al AG yy aad Guha Ge Different filtration apparatus LIF LLLL LLL ELLE ELL LLL LLL LLL LEED ttt ttt S 9995999995995 5 5999599999999 9959955959959 99%PNVNVVVVVAVV VN VA RV TN TATA TVA TTT TA ENE YN Figue A32: Arangemest fflker paper, feel, and fa for raviylcaion (vend fe vacua daca ©) Experiment No. 4 (Sublimation) Yr SAAR RRA AAA AAA VPS SSS SSS SSS SSS SSS SESS SSF SFT ES ESSE SES SESS SS SES LLL LLL LL LL LLL LILLIES LLL LLL LLL SES et tttSNVVVVVVVVVVVEVEVEV EHV VENTE HHI A of solid organi beingtransformed directly to vapor state (display the characteristics properly of condensing to solid state)without passing through the intermediate liquid state. Reagents : Benzoic acid + Salt Apparatus used : OF G93 Gee bt GG Seal Qeed Aalto) cy p HAN Cong Agia Balad! COILS Hija Ome FAN Atha Ct pd gh Ge bie ad ie Le La wie geal etl (pasa Alaa) one AyLeall Atta) OPP CLES E PCL E EELS SPCC EEE EEE EEE CCE E EEC CCC CES O oe QPS SSS SSS SSS S ESSE SSS SS SESE FEES ESSE EEE EEE ESS LIP ILL LLL SILL LL LLL L LILLE SEIS EEE StottSNANNNVVVNVVVVEVEVVV UDEV EVV EVV HD ETN CPP Poe PCL o ESE Po CLES EC EEC Ee CECE CCE CC CCE CC CCS S Procedure : 1.Place a (benzoic acid + salt ) mixture in beaker (400)ml , place (200)ml round bottom flask filled with cold water on beaker which contain mixture. Y.The beaker is placed on a sand bath or over low flame. Heating as required from (15)minute to (1)hour , depending on the intensity of heat applied. 3.The material capable of subliming will collect on bottom of cold flask and on the side walls inside the beaker the pure crystalline form. *.Determine the melting point of pure crystals. m. p. of benzoic acid = 121+ 2C° m. p. of salt = 800-850 C° f i Been ) intensity of heat ‘pressure Seah! oul Sublimat e Crgsrals Cold. warer Benzoie acid mixture of CBenzore +5ai) due (Sak) Experiment No. 5 ro LIP LLLILLLLL LIL LLL LL ELL LEE L ELSES LS tt tt S 999 FFF 9994999995999 5 499459599598 F FF FHS 49594ANANVVANEN EVAN AVA VEN RATAN TTA A CPP CESSES CEL CES CSCC CECE ECC EEC EPC EC CEC CEC CCC SSS (Simple andFractional — distillation) The boiling point : may be defined as that temperature at which vapor pressure (the pressure exerted by substances equals the pressure of atmosphere above liquid. The purification of liquid organic compounds by conversion to vapor state with heat and condensation of vapors to the liquid state in known as distillation a definite value at give pressure for every pure organic compound and is known as boiling point. pel) bial) ps bila) lay bids nic og lusty gg) 4 jl yall Mp Mg Lael sila lgiie silat Cy Stacia £1gi] ALid g Lil pual! Lait yb) diy Jb Jariead imple distillation Saseagll hii! If impurities in liquid are non-volatile the liquid may be purified by direct or simple distillation the impurities remaining in the distilling flask. Kins ee Gill 95S oh ial es Gua js nell A pl sha ec nion AB SI ol pall Ls Lge Sanne Gal 2 Lael denny Si gi (0+) Lille pile ox plated) Baal GL pLbaall Lagre cg ply Sie yes Layla Vda HSLde AL Leas of oye BysLtial Sald) le GES GILG 5 at GLA GS HLA 5 SY) GAY! Sala Bgl) ULE Aa. j2 AB pe gt Lal Lael abil iL Gath Sd AI al galh ot Lay Slapsaall leit 4p pe Aaa 5p dled Say gill ga jall g gi Le Ge (miscible solution) Lajas! jail Ul yy glad [Sy 4p jad i pall $ le n PILL LL LLL LLL LLL LSS ELSES SSS SSL LES ES SES S SPSS FSSS FSS SSS FSS SF FSS SSS FEES FSS FFF FF FSF F999 99%SNNNANAN UNEVEN EVEN AN EVEN ET ENTE VEYA Apparatus used : thermometer distilation flask . cold water receiving flask ‘clamp stand water (© 2006 Merriam-Webster: ne. Simple distillation Pre re : 1.Prepare a distillation set — up using (250 )ml of di thermometer and water, cooled condenser. lling flask fitted with a 2.Add two small pieces of porous plates. 3.Place (100 )ml of ethanol in the flask and start the water (note the water inlet is at lower end of the condenser. 4.Heat the flask with a hot flame until the contents being to boil and adjust the temperature so that distillation precedes at 2 or 3 drops per-second. 5.Discard the first 2 or 3 ml of distillate and distil until 60 ml has been collected. ‘Record the observed boiling range of alcohol . v CLP C ESE S CEE ES EE EEC EE EEE EEC E EEE ECC CLEP PPLE ES VSS SSS SSS SESS SSS ES SESS ESET TEESE ESTEE TTT E HHS EES PEELE L LLL LLL ELLE LLL LLL LLL LL ESE tet tteSNUVVEVEVVEVEVOVEVVVHEVVV UHH VET H THEE ¢ ¢ ¢ + 2.Fractional distillation : seit shit t é If impurities are them-selves volatile liquid then separation of these - mixture from bulk of the required substance is achieved by fractional o distillation. as Lagi eyo cas Gall Sy Css Cyan jae Gulls eal Lindl (gi jell aba) Jawtng a ¥ of 8+) oe oil ~ + + + + + ¢ + - * + + - + + + Fractional distillation ys % + + + + + ¢ + + Sil gual a Solvent Boiling point ‘ 3 Non , eae oe inflammability _| ia ¥ ” ; LILLE LLL ELLE EELS LES ELE EOD EEE Ott ttt tin CPPCC ESE L CEE CECE EP EEC CEC CEC CCC EC CEC CCC CCC CCC SSPNANANVVVNVN TN TN AVANT EN TT ATTA ENE TN methanol 64.70 __Se%Alcohol CCly Bic 76.60 Ether 34.6 C° inflammable Acetone 560 Chloroform 61.20 Benzene 80 Cc Toluene 110 C° Acetic acid 118 C° Petroleum ether 350 Inflammable Theory: CP PPE L CLEP SLEEP ECE EEE CECE ECE CCCP EPEC CC CC EC SS (Melting point)Experiment No. 6 LLLF LLL LLL LLL LLL LLL LL LLL LSS LLL ELS SS SS 8 i a i I i i i i i eeCESS C PPPS ESE LES C CECE ECC EPCS PCL Eo CoP C SC CCC CSC eS SNANANVNVNAN ENTE UN VA VN TN AVANT VAY ND Melting point : for solid is that the temperature which the solid and its liquid in equilibrium ,without changing in the temperature at one atom Pressure . it can be determined by introducing amount of substance into small capillary tube , attaching this to the temperature centered in heat bath (oil bath ), heating the bath slowly and observing the temperature ,at which melting beginning and it complete. Pure substance usually have sharp M.P. for example (145.5 — 146 ) Impure substance of the same compound melts at lower temp. and over a wide range (ex. 140-144) 4The_M.P. used for identification of purity of solid organic compound. Method : ) Place a small quantity of sample on a filter paper . 2.Crush the sample to powder with spatula . Y.Place tiny amount of sample in capillary tube. £ Attach the capillary tube thermometer by rubber hand. °.Place the thermometer in oil bath. ‘Heat the bath slowly and note the temp. at which the substance states. Y.Record the melting point . VIL LEL LLP PLL ELLE LESSEE SHES ESE t tt tt te v S F494 9444494944599 59 9999959999999 9%CPP CPPCC EP CCPC EP CP CCE PCCP CCPC CPC EP CCPC CC CC CCC SS LNANVVVNVNEVEN EVE EN TENET TEN EN YY AD Take M.P. of impure mixture of salicylic acid A. Impure mixture of benzoic acid consist of (0.3 gm salicylic acid + 0.9 gm benzoic B. Impure mixture of salicylic acid consist of ( 0.3 gm of benzoic acid + 0.9 gm of salicylic acid) Then take their melting point Experiment No. 7 (boiling point) theory : boiling point : it is that temperature at which the vapor pressure(the pressure exerted by the substance ) equals the pressure of atmosphere above the liquid. ® The apparatus consists of a boil tube which contains liquid for B.P. determination and inverted capillary attached to a thermometer which immersed in liquid bath, heat liquid bath gradually ,when the bubbling becomes rapid, discontinue heating and the temp. is allowed to drop (1-°2) and stream of bubbles which indicate the B.P. of liquid is noted. Method : ) Place ( 2-3 )ml of liquid in the boiler tube by using capillary tube. Y.Immerse the capillary tube in the boiler tube. Y.Attach the boiler tube to the thermometer . *.Immerse the thermometer in liquid bath. ©.Heat the bath slowly. vr PILL LI LLL LILI IL LIS LLL LLL I LL LILLIE LSS StS VSS SSS SSS STS SSS STFS TFS F FSFE EFF SE SF FSFE ESTES SEESPL NANVVVNVNAVVV ETAT ETAT VV TAN YN 6.Note the temp. at which the stream of bubbles begin; then remove the source of heat and the temp. is allowed to drop ( 1-°2) which is mean cool the bath oil take the temperature at which the liquid recodes into inverted tube ( capillary ). Apparatus for determination of boiling point ve CoP PoP P ooo ee Ceo C PCC CoCo CCP e ee Ceo C ECC PCC C PCS S SPSS SSS SSS SS SSS SS SS SSS FSF SESS FSF FFF SST SSS SSS SS PELL LLL LLL ELIE LEIS LLL LLL LLL SLES tte tttePNVVVUVEVOVVVVOVVDVEVHVUV HVE EVEDEDEVON substance Boiling point \ Acetone 560° Y Methanol 650° 7 Ethanol BC t Benzene 810 ° Water 100 c° x Chloroform 62C° thermometer capillary sube boilertube (bath ot) heat Cbener) Apparatus for d Pareb$ine ofl = ———} jetermination of boiling point CPSP ESP EPC E PEPE ESSE PEEP EEE EE EEC CEP CPC CCC CPCS re. LLLP LLL LLL LLL SLL LLL LE LES LS LL ELE SL ttt VSS SSS SS SSS SSS SS STS TSS SSS SFT TTF FSS FTES SESS SS SSLNVNVVVNVVNVVVVUN VEN TUA DTN EE DENTE TEAS substance Boiling point y Acetone 560° Y Methanol 650 i Ethanol 73O £ Benzene sic ° Water 100 C° x Chloroform 620 thermamerer copillary sube > boiler tube ___} PersS$ene ov (both ol) heat cbwnerd Apparatus for determination of boiling point re v v v v v ’ v v v v ¥ v v v ¥ v ¥ v ¥ ¥ v ¥ v v ¥ v v ¥ ¥ v v v v v v v v v J ¥ v v ¥ v v PPPPPLPPE PEEL ELLE LEE ESE SSS Sethe etttitty BECP P CPPCC SEE SEES PPP C CEL CCC Ee See eee SPCC CC SC eE