Chem 31.

1 EXPERIMENT 2 Recrystallization and Melting Point Determination

I.

Objectives 1. To clarify the meaning of p rity in the chemical sense 2. To apply the method of recrystallization in the p rification of a solid sample !. To recognize melting point as a physical property that can ser"e as an inde# of p rity $. To determine the melting point of a s %stance sing a simple apparat s &. To compare the melting point of a p re "s. imp re sample of a s %stance Procedure A. Selection of a Solvent for Recrystallization 1. 'sing the tip of a spat la( place a small amo nt of the cr de sample into a test t %e. )dd a%o t & m* of +ater. 2. If the sample is not completely sol %le( gently heat the test t %e in a +ater %ath. !. If a sol tion is o%tained in hot +ater( allo+ the sol tion to cool slo+ly at room temperat re. $. ,ompare the size( color and crystal form of the res lting crystals +ith the original solid material. &. Repeat steps 1 - & sing. a/ 0&1 ethanol2 and %/ ,,l $ . Recrystallyzation !ote" 3et aside a small portion of the cr de sample and determine its melting point 4proced re ,/. 1. 2. !. $. Prepare a hot filtration set - p. 5eigh 6.& g of sample and place in a test t %e. )dd 7.& m* sol"ent into the test t %e 41& m*8gram of cr de sample/ 9eat the t %e in a hot +ater %ath +ith stirring ntil all the solid dissol"es. &. If the sol tion is colored( s+irl +ith a small pinch of acti"ated car%on after the sol tion has cooled do+n to at least & 6, %elo+ its %oiling point. :. ;ilter the hot mi#t re rapidly 7. )llo+ the filtrate to cool to room temperat re slo+ly. #O !O$ A%I$A$& $'& (I)$*R&.

II.

Chem 31.1 <. )fter the mi#t re has cooled to room temperat re( place the test t %e in an ice - +ater %ath( along +ith the test t %e of p re sol"ent. 0. If crystals do not form( scratch the inside of the test t %e +ith a stirring rod. 16. ;ilter the crystals %y s ction 11. 5ash the crystals +ith the cold sol"ent 12. ,ontin e the s ction ntil no more sol"ent passes thro gh the filter 1!. Determine the melting point of the recrystallized sample. ,ompare the melting point range o%tained +ith that of the cr de sample. 1$. P t the rest of the sample in a "ial and la%el it properly. 3 %mit to yo r instr ctor. 3. (eltin+ Point #etermination 1. P l"erize a small amo nt of the sample +ith the aid of a clean +atchglass and stirring rod 2. Ma=e a heap of the po+der. >ently thr st the open end of a melting point t %e 4a glass capillary closed at one end/ into this heap. Tap the capillary t %e gently to ca se the sample to collect at the %ottom of the capillary t %e. Repeat this step ntil a sample 1 - 2 mm high has collected in the %ottom of the t %e. !. )ssem%le the melting point determination set - p as sho+n in the fig re. $. 9eat the oil +ith a moderate ? nsen flame. )llo+ the temperat re to rise fairly rapidly to +ithin 1& to 26 degrees %elo+ the e#pected melting point of the sample. Then ad@ st the flame size so that the temperat re rises no more than 2A! degrees per min te @ st %efore( d ring and @ st after the period in +hich the compo nd melts. &. Record the range of temperat re from the first "isi%le e"idence of liB id 4the sample appears moist( or a tiny drop of liB id is o%ser"ed/ to the complete liB efaction of the sample. III. ,uestions 1. 5hat is a crystal and +hat is meant %y recrystallizationC 2. 9o+ does recrystallization free a s %stance from imp ritiesC E#plain ho+ each step in recrystallization contri% tes to the remo"al of the imp tities !. 5hat m st %e considered in choosing a sol"ent for recrystallizationC $. 5hat is melting pointC 5hy can it %e sed as an inde# of p rityC

Chem 31.1