PRELAB FOR EXPERIMENT # 1: DETERMINATION OF MELTING POINTS

Your name TAs name

Your Partners name Lab Section
PURPOSE:
In this lab we will learn to 1) find the purity of solids by measuring their melting points
!) identify an un"nown by performing a mi#ture melting point
MATERIALS USED:
Compound M.W.
$g%mol)
M.P.
$
o
&)
Den!"# $g%ml) $%&%'d
'rea ())** 1+* 1++* irritant
Trans,cinnamic acid 1-.1(1 1++ 1!-. irritant
P%()!n* "+e o,!d !n % me,"!n* po!n" (%p!,,%'# "u-e
1 Ta"e a small amount of urea and trans,cinnamic acid in two separately labeled
watch glasses /a"e sure that the samples are finely powdered $with the use of a
metal spatula)
! 0ently tap in some of the solid into the open end of a thin,walled capillary tube
$(,1 mm of solid should do it)
+ In2ert the capillary tube $open end facing up) and drop the tube down a long glass
tube 3epeat procedure se2eral times till solid is pac"ed tightly at the closed end
of the thin,walled capillary tube
%. Me%u'!n* "+e me,"!n* po!n" o. pu'e u'e% %nd pu'e "'%n/(!nn%m!( %(!d
1 Turn on the melting point apparatus /a"e sure that the apparatus has cooled to 4
11*
o
& before placing the capillary tubes in the melting point apparatus
! 3aise the temperature of the melting point apparatus so that the rate of
heating is slow during the melting of the solid $1,! degrees%min)
+ 3eport the melting range $ie the temperature at which the solid 5ust
begins to melt and the temperature at which all the solid has melted) for both pure
urea and pure trans,cinnamic acid
-. Me%u'!n* "+e me,"!n* '%n*e o. u'e% %nd "'%n/(!nn%m!( %(!d
1 6eigh e7ual amounts of pure urea and trans,cinnamic acid $4 () mg of each
substances should do it)
! /i# the two compounds together and ma"e sure that the mi#ture is finely
powdered $with the use of a metal spatula)
+ Pac" some of the mi#ture in a thin,walled capillary tube
- 3eport the melting range of the mi#ture $*)8*)) of urea and trans,cinnamic acid
/a"e sure that the melting point apparatus has cooled down to 41))
o
& before
placing the capillary tubes in the melting point apparatus
(. Me%u'!n* "+e me,"!n* po!n" o. un)no0n
1 3epeat same protocol gi2en in part $a)
! 3eport the melting range $ie the temperature at which the solid 5ust begins to
melt and the temperature at which all the solid has melted) for the un"nown
d. De"e'm!n!n* "+e me,"!n* '%n*e o. % m!1"u'e o. #ou' un)no0n %nd u'e% %nd
o. % m!1"u'e o. #ou' un)no0n %nd "'%n/(!nn%m!( %(!d.
1 6eigh e7ual amounts of pure urea and trans,cinnamic acid $4 () mg of each
substances should do it)
! Li"ewise weigh e7ual amounts of your un"nown into two separate watch glasses
+ Add the pre,weighed urea to one watch glass containing your un"nown Then
add the trans,cinnamic acid to the other watch glass
- /i# each of the components and obtain their melting points