Scribd
Upload
345 views

EXercise 2 (Recrystallization and Melting Point Determination)

1. This document describes an experiment involving the recrystallization and melting point determination of a solid sample to purify it and identify its melting point as a physical property and index of purity. 2. The procedure involves selecting a solvent to dissolve the crude sample, filtering to remove impurities, slowly cooling the filtrate to form purified crystals, and determining the melting point range of both the crude and recrystallized samples for comparison. 3. Questions at the end ask about the definitions of crystals and recrystallization, how recrystallization removes impurities at each step, what must be considered in choosing a solvent, and what a melting point is and why it can serve as a purity index

Uploaded by

Cherryl Surigao
Copyright
© Attribution Non-Commercial (BY-NC)
Available Formats
Download as DOC, PDF, TXT or read online on Scribd
345 views

EXercise 2 (Recrystallization and Melting Point Determination)

1. This document describes an experiment involving the recrystallization and melting point determination of a solid sample to purify it and identify its melting point as a physical property and index of purity. 2. The procedure involves selecting a solvent to dissolve the crude sample, filtering to remove impurities, slowly cooling the filtrate to form purified crystals, and determining the melting point range of both the crude and recrystallized samples for comparison. 3. Questions at the end ask about the definitions of crystals and recrystallization, how recrystallization removes impurities at each step, what must be considered in choosing a solvent, and what a melting point is and why it can serve as a purity index

Uploaded by

Cherryl Surigao
Copyright
© Attribution Non-Commercial (BY-NC)
Available Formats
Download as DOC, PDF, TXT or read online on Scribd
You are on page 1/ 3

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

You might also like