Lab report

Chemistry lab

Name:Ismail ghous
Student number:92093524
Name of course: chemistry lab 1

5th
april,2021
 Table of contents
1.Lab. safety rules
2.Lab. equipments
3.Distillation
 Laboratory safety rules :
1. Tell the teacher if any accident happens including spills

2. Tie back long hair before beginning a lab investigation

3. Wear an apores, safety goggles and gloves when working with liquids, heat, flames or chemicals

4. Do not eat or drink anything during a lab investigation

5. Do not touch materials until your teacher has given you directions. Make sure to carefully read
directions before beginning your investigation

6. Use tools only as they are supposed to be used. Treat tools and materials with respect. Make
sure they are clean before and after you use them

7. Label containers before you put something in them. Don’t use a substance from a container that
is not labeled

8. Always clean up your work area after an investigation

 Lab. Equipment:
Distillation:
-round bottom flask
-thermometer adapter
-thermometer ticker
-west condenser
-vacuum adapter
-connectors
-round- bottom flask
-clamps
-lab jack
-beaker
-graduated cylinder
-micro lab
-distillation glassware
-Thermistor
-hot plate
1.Distillation:

Distillation is one of the most useful

methods for the separation and
purification of liquids.  It is perhaps the
oldest separation technique known.  It
is most commonly used to purify a
liquid from either liquid or solid
contaminants by exploiting differences
in their boiling points.  
 

Types of Distillation:
simple distillation.
fractional distillation.
steam distillation.
vacuum distillation.
air-sensitive vacuum distillation.
short path distillation.
zone distillation
 
 PROCEDURE
Fractional Distillation Using Micro lab :

In this experiment you will determine

the composition of a mixture of ethanol
and water. You will separate the
components of the mixture by fractional
distillation. You will use the Micro Lab
data acquisition software to monitor
the progress of the distillation. A
thermistor (an electronic temperature
sensor) will be used to observe the
boiling points of the components of the
mixture, and the volume of each will be
determined by collecting the fractions
in a graduated cylinder.
 
PART 1. Calibration of Thermistor.
    At the beginning of the experiment,
the thermistor must be calibrated to
ensure accurate temperature readings.
You will calibrate the thermistor using
samples of water at well-defined
temperatures.
1. For the calibration, you will need
about 50 mL of boiling water.  Heat this
water in a beaker on a hot plate.
Remember to add a boiling stick!
2. Connect the Micro Lab thermistor to
a port on the Micro Lab interface and
open a new experiment.
3. Click “Add Sensor,” select
“Temperature (thermistor)” from the
pull-down menu, and select the port
where you inserted it.  Click “Next” to
bring you the thermistor calibration
window.
4. Click “Perform New Calibration.”
This will open another window entitled
“Calibrate a Sensor.”  
5. Click “Add Calibration Point.” Insert
the thermistor and a thermocouple into
the beaker of boiling water.  You should
notice the measured value of the
thermistor increasing.  Once the rate of
change of the measured value becomes
constant, read the temperature on the
thermocouple (to the nearest 0.1C)
and type that in as the actual value.
Then click “OK.”  
6. Prepare an ice bath (with crushed ice
and some water) in a recrystallizing
dish. Insert the thermistor and the
thermocouple and calibrate this point
as you did for the boiling water. Do the
same for a sample of lukewarm tap
water.
7. In the “Calibrate a sensor” window,
you should see a graph of the three
calibration points you made.  To obtain
a best-fit curve, select “First Order
(Linear)” from the choices on the left.
Click “Accept and Save this Calibration.”
A small window will open asking for
units; enter “(C).”  Save the calibration
as “Thermistor Calibration.”  (If this file
already exists, replace it.)  Click “Save”
and then click “Finish.”
 
The thermistor is now calibrated to
track the temperature of the vapor
during the distillation.
 
 

PART 2. Distillation Setup.

1. Place about half of your sample
(roughly 10 mL) in a 50 mL round
bottom flask. Since you will be boiling
this solution, add a magnetic stir bar.
2. Set up a distillation apparatus
according to the diagram below. Clamp
the 50 mL round-bottom flask (the pot)
at least a foot above the floor of the
hood and construct a  fractionating
column by packing a condenser with
steel wire or glass wool. You should
lightly grease all joints in your setup
unless they are still greasy from
previous usage.
3. Insert the thermistor into a rubber
thermometer adapter fitted onto a glass
straight tube adapter by placing a drop
of glycerol onto the bulb of the
thermometer and gently pushing the
thermometer through the thermometer
adapter.  To avoid injury make sure that
as you push you gently rotate the bulb
of the thermometer. Proceed slowly.
4. Adjust the thermistor so that the bulb
is completely below the sidearm
(leading to the condenser) in the three-
way adapter. This will result in an
accurate temperature reading because
the thermistor will be totally immersed
in boiled vapor. Seal up the hole using
teflon wrap to prevent vapors from
escaping during the distillation.
5. Seal the condenser to the open joint
of the three-way adapter and clamp it.
Use a blue plastic clip to help hold it in
place.  Attach a  vacuum adapter to the
end of this condenser and clip it as
before.
6. Place a 100 mL graduated cylinder at
the bottom of the vacuum adapter.  This
last flask, the collection flask, should be
surrounded with an ice bath to ensure
that any liquid you collect does not
evaporate out.
7. Place a stirring-hot plate on a jack
under your pot. This plate will be used
only to stir and not to heat.
8. Obtain a heating mantle and plug it
into a variac. Plug the variac into the
wall and switch it on. The variac is a
device that modulates AC current. Wall
current is 120 V; a variac can adjust that
to anywhere between 0 and 120 V.
Plugging the heating mantle into a
variac allows you to control the
temperature by controlling the voltage
supplied to it. Test the mantle and
variac by briefly turning the dial up to
100%. The mantle should get warm
within ten seconds or so. Turn the
variac down to 0 once you have
confirmed that it and the mantle work.
The variac should be left at 0 until you
are ready to heat. Place the heating
mantle on the hot plate under your pot.
9. The hot plate and mantle should be
lifted up on a jack. Raising your heat
source allows you to quickly remove it
in case of violent boiling or fire. If you
need to cool your pot quickly, you can
simply lower the jack. Without the jack,
you would have to slide the hot mantle
or hot plate out or lift the hot pot and
risk a burn.
10. The last step towards completing
the distillation apparatus is running
water through the condenser.  What
would be the best way?
11. Start stirring and turn on the variac.
It should be set low at first, to 20-30%,
to avoid boiling too quickly.  If, after a
few minutes, the solution does not boil,
you may increase the variac to 50% or
so.. If increasing the variac setting
doesn’t work, you may want to insulate
your pot with some cotton wrapped in
aluminum oil. Avoid heating too
quickly--boiling too fast can cause the
vapor to travel past the thermometer
too quickly, resulting in an artificially
low measured boiling point.
Furthermore, too much heat could
cause your compound to decompose.
    

As you distill, you should also see drops

of liquid roll down the inside of your
condenser and fall into your collection
flask. Continue distilling until the pot is
nearly dry (less than 25% of its original
volume). Again, you should never distill
to dryness. Lower the hot plate and
heating mantle and switch off the
variac. Remove your collection flask
(now full of your compound) from the
ice.
The End