POLARIMETRY a.

the concentration of the substance

used and,
 is used in chemistry in a
b. the length of the tube placed in the
variety of ways.
polarimetry machine.
 primary use is to
This can be seen in the following equation
determine the angle of rotation of an

optically active substance using

polarized light the polarized light will

either shift clockwise or

1) The polarimeter machine will be turned
counterclockwise and the amount it
on by your TA prior to the beginning of
shifts will determine the angle of
the lab.
rotation.
2) Prepare your solution with your
 Polarimetry is important in
unknown substance and note its
chemistry because it allows one to
concentration.
determine the difference between
a. To prepare the solution
enantiomers using optical activity as a
using your unknown substance, weigh out
measuring point.
the desired mass of substance and using
o Enantiomers are two
a funnel transfer it to a volumetric
stereoisomers that are mirror images of
flask.
one another but are non-superimposable.
b. Rinse the weighing tray and funnel
Techniques in chemistry
using deionized water.
used for the identification of
c. Using deionized water, fill the
substances such as melting point however volumetric flask to its midpoint, fill the
this test would prove non conclusive for volumetric flask to the line with a glass
pipette
the identification of enantiomers in d. stopper the flask
e. dissolve the solid by shaking the
that they will provide identical melting
volumetric flask up and down.
point.
3) Next ensure that the polarimeter
The specific rotation value is
sample holder is clean.
dependent on a variety of factors mainly:
Note: There are three sections
to the polarimeter sample holder
 the silver cap
 the black washer and
 a clear lens (Be careful not to break the
lens)
SAMPLE HOLDER PREPARATION PROCEDURE
a. Rinse the sample holder with deionized
water and then empty into a waste beaker.
b. Next use deionized water to calibrate
the machine. To do this, fill the sample
holder to the top with deionized water
and ensure no bubbles are present. If
there are bubbles present tilt the
sample holder to ensure the bubbles are
in the curved part of the holder and not
in the top or bottom of the sample
holder.
4) Next open the hatch of the
polarimeter and place the sample holder
into the tube opening and then close the
hatch again.
5) to calibrate the machine
ensure that there is a uniformly colored
circle visible through the eyepiece.
Note: that the inner and outer zeros on their
vernier scale are aligned which shows
that the machine has been calibrated
6) Next discard the deionized water in the
waste beaker
and fill the sample holder with your
prepared solution.
7) Ensure minimal bubbles
are present or if they are present, they
are present in the curved portion of the
sample holder as shown previously.
8) Place the sample holder back in the
machine and begin to take the reading.
You should observe a half dark circle on
the left and a half dark circle on the
right when you rotate the dial in
opposite directions.
9) Adjust the dial so
that one full circle is seen. Now you can
read the observed degree of rotation
using the numbers on the outer dials.
OBSERVED ROTATION VALUE
 The outer scale is the whole number for
the observed rotation reading
 The inner scale is the decimal point for
the observed rotation reading.
 To make the reading, note where the
zero on the inner scale meets up with
the numbers on the outer scale.
 In this example the whole number is 1.
Note the decimal C where a line in the
inner scale matches up with the line on
the outer scale
 in this example the decimal number is 1
therefore, for this sample the reading is
1.1
 If you take your reading on the left side
of the machine and the zero on the
inner scale is above the zero on the
 outer scale, this means you have a chiral molecules with optical activity such as
sugar that has a negative degree enantiomers.

of rotation  It can also be used for the

 If you take your reading on
the right side of the machine and the
zero on the inner scale is below the
zero on the other scale, this also means
determination of an antiemetic excess
of a mixture of enantiomers.
 At the end of your experiment ensure
that all utensils are properly sterilized
and return to their designated location.
12) Discrepancies in your findings with

that you have a sugar that has a literature value may be a result of

negative degree of rotation experimental error such as sample

 To complete this reading, take the preparation or incorrect reading from

number you obtain and subtract it the scale. Ensure that all results as
from 180 degrees
well as potential sources of error are
10) When you find your observed optical
copied down in your lab notebook
rotation value, you are able to solve for

the specific rotation using equation 1.

Divide this observed optical rotation

value by the concentration of your

solution and the length of the tube.

This final optical rotation reading can

be used and compared to known literature

values to determine what the compound at

hand is.

11) As you can see from this

tutorial,

 Polarimetry is a useful and

efficient tool used in the field of

chemistry for the determination of

PAPER CHROMATOGRAPHY
OBJECTIVES:
I. Perform paper chromatography and
learn its techniques.
II. Determine Rf values for six amino acids.
III. Identify an unknown amino acid using
its Rf value.
Today's lab, you will be determining the
identity of unknown amino acids using
paper chromatography.
 Chromatography is a method to
separate mixtures based on the
differences in affinity for the mobile
phase and stationary phase.
o Mobile phase is solvent that
will move up the stationary
phase which is the paper.
o The distance that the amino
acids on your paper will travel
depends on their SIZE,
STRUCTURE, CHARGE and
POLARITY since every amino
acid has its unique structure,
the distance traveled by each
sample will also be different
 You will be calculating what is called an
RF value which is the distance travelled
by the spot on your chromatography
paper relative to the distance traveled
by the mobile phase
 let's get started
PROCEDURE
1. Get a piece of chromatography paper
draw a light pencil line 1.5 centimeters
from the bottom.
a. Mark 9 points on the line about two
centimeters apart and two
centimeters apart from each edge.
b. Number each spot one through nine
be sure to use a pencil and not a pen.
Be sure to not touch the paper more
than is necessary gloves are
recommended.
c. While your partner prepares the
paper go ahead and prep your mobile
phase in your amino acid samples,
get a 1000 milliliter beaker and pour
in 50 milliliters of the solvent
d. Cover the beaker with an aluminum
foil
e. About three drops of each amino
acid as well as your unknown into a
separate well on the stock plate
create a key by using table 12.1 so
you don't except your amino acids.
f. using a toothpick apply a tiny spot of
the amino acid on your
chromatography paper.
g. The spots do dry up quickly so go
ahead and re-spot until you have
done this a total of four times do the
same for the rest. Be sure to use a
different toothpick for each amino
acid.
h. Growth chromatography paper with
the spots on the inside. Staple the
edges near the top and the bottom.
i. Stand the paper with the pencil lying
down inside the chamber cover and
wait for about 30 minutes.
j. After 30 minutes, take the piece of
paper out of the chamber and Mark
the solvent front with the pencil. It is
the farthest distance that the solvent
has traveled.
k. Remove the staples and lay it flat on
a paper towel to dry. To speed up the
drying process you can blow lab air
onto the paper. Again, be sure that
you have marked the solvent front
before you dry the paper.
l. Once the paper is dry spray the paper
with ninhydrin solution. Ninhydrin
reacts with the free amine group in
the amino acid present, giving it a
purple color.
m. Dry the paper in the oven for about 5
minutes. Dry spots will now be visible
circle each spot because the
ninhydrin spots will fade over time
now you are ready to calculate your
RF values.
THIN LAYER CHROMATOGRAPHY

 Thin layer chromatography is one form

of solid liquid chromatography.
 It's used to -- for the rapid separation
of very small amounts of organic
materials.
 It can only be used to separate organic
materials that have boiling points above
about 150 degrees.
 So, these are relatively nonvolatile  When a non-polar mobile phase is
materials. present, the non-polar mobile phase
And in our case today we'll be separating passes over the plate, and it leaves the
colored pigments coming out of a plant leaf. polar compounds attracted to the polar
support. So, the molecules will in the
 The technique of chromatography is case of the TLC --the non-polar
based on the principle that compounds will move up the plate a
components in a mixture will distribute little faster in this case than the polar
unequally between two immiscible compounds.
phases. And this is the basis for liquid-
liquid solvent extraction which is Another figure which illustrates the separation
another separation technique that we of a component mixture by normal phase
will do on a small scale for the first time chromatography. In this little figure, you're
in this experiment today. seeing three pigments that have been
 The liquid phase is called the mobile separated.
phase.
 And then we have a solid support which
is called the stationary phase.

In our case today the solid support is silica gel

which is a polar material. At this point you
should be looking at a figure that illustrates
what happens in what we call normal phase
chromatography. And that's where there's a
stationary phase where the stationary phase is a
polar solid like silica gel like we're using today.
 What this shows is -- how we intend to
 When a solution containing polar and a do this experiment we'll spot our leaf
non-polar compound come in contact pigment on the bottom of a TLC plate,
with the TLC plate, the polar molecules put it into what's called a developing
are attracted to the polar support, while chamber which is a sophisticated name
the non-polar molecules remain in for a glass jar with a lid. And we'll put a
solution. little bit of solvent, the mobile phase in
the bottom of the jar, put the plate in
the jar, screw the lid on.
  And in about 20 minutes or so the liquid
will move up the surface of the TLC
plate by the force of capillary action.
 And as it does it carries the pigments
along with it. And depending on the
polarity of the mobile phase it will
determine whether the polar materials
move faster or the non-polar materials.
PROCEDURE:
 goggles on.
 We use hibiscus leaf since they're
readily available to us.
 Take one of these leaves and you're
going to rip it into small pieces and put
it into mortar.
 put in some solvent. Grind these leaves
essentially to a pulp in the presence of
some solvent.
 Mix of petroleum ether and ethanol
will be use as a solvent and the
petroleum ether is very volatile and it's
going to evaporate.
 And the colored pigments happen to
be soluble in pet ether. And so, these
are just alkanes. So, we've got a mix of
polar and non-polar.
 remove the liquid and leave the pulp
behind. But we'll use a Pasteur pipette.
The more liquid you remove the harder it is to
get the last bit. But I do want to try to get a lot
of liquid. Because in our next step we're going
to suffer some losses.
 What we're going to do now is a liquid-
liquid extraction.
 So I'm going to extract this ethanol
petroleum ether mixture with water.
 I'm going to add an approximately equal
volume of water to the tube. We've
formed two layers.
 The reason is petroleum ether is a
hydrocarbon. It's non-polar and water
is polar so they don't mix. So, it's
essentially oil and water like that.
But if we shake it up, we're going to end up
with an emulsion, and we'll never be able to
separate these. So, the recommendation is that
we swirl the term gently.
Now, one of the things that this solvent
extraction accomplishes is it will remove the
ethanol.
The ethanol will be miscible with water so the
ethanol will go into the water.
And what will be left behind when we're done
will be our organic pigments in the hydrocarbon
phase.
 So, we've accomplished this, the first
extraction, by swirling that for a
minute.
 Remove the aqueous layer. The
aqueous layer is the bottom layer. We
don't want the aqueous layer.

All right, so we have the organic layer, add an
equal volume of water, we do the same thing
again. You notice that this time that the
aqueous layer is colorless pretty much.
Now, we don't have all of the pet ether layer
left. Part of that was because part of that
organic mix was ethanol and it went into the
water. Now I'm just going to pipette this stuff
into our smallest Erlenmeyer flask
Here we go into the Erlenmeyer.
 Dry this organic material with
anhydrous sodium sulfate crystals.
 Add powder, then swirl
 Sodium sulfate will take the water out.
 And then once this solution is dry we'll
be able to spot it onto our
chromatography plate and begin the
experiment.
PREPARING THE TLC PLATE
And it's a piece of plastic that is coated on one
side.
So you'll notice that one side is very smooth,
and the other side is rough. But you have to be
very careful with the rough side. That's the
working side.
What we're going to do is take a ruler and a
pencil. Now, make sure you use a pencil and not
an ink pen. Because the ink has organic colored
pigment, and it will chromatograph.
 draw a line, a pencil line one centimeter
from the bottom of the plate.
To do the spotting we use an open end or both
ends open capillary tube. I put the capillary into
the solution, and you notice that the solution,
can you see it wicks up, it wicks up into the --
that is capillary action.
And that same phenomena will be what moves
the liquid up the plate.
 Make a small pot. A very quick spot.
 The reason is the darker spot, the more
-- the easier and the more pigments I'm
going to see. The easier it will be to see
the pigments.
Developing chamber
It's three parts pet ether and one part acetone.
So the pet ether is very non-polar.
The acetone is very polar.
  Put the TLC plate into the developing
chamber without splashing. I don't
want the liquid level above the level of
the line.
 It dissolves the pigment right off of the
plate and into the solution and the
experiment is over.

 So the only way this is going to work put

in a small layer less than a centimeter in
depth. Now we put the lid on. Just let Mark the solvent front. And very quickly I want
the jar sit stationary. We don't want to mark the spots. The colors are still fresh.
agitation because it will create waves,
and then that will destroy what's called
the chromatographic front.
 Wicking process is very rapid at first.
And unfortunately it kind of slows
down.
 But please keep your attention on this
or don't be too inattentive because you
have to stop it, you have to stop the
experiment before the liquid reaches
the top of the plate. We got five pigments in this short experiment. I
 And at that point we'll remove the plate think perhaps if we'd let the solvent front go up
and draw a pencil line where the top of some of these dots might have separated into
that solvent front is. even more spots.
And we need that distance, the distance from Presumably one of those green ones is
the target line that I drew with pencil to the line chlorophyl. But this is the technique that
that we're going to draw with pencil where organic chemists use to separate very small
marking the solvent front, we'll need that amounts of higher boiling organic compounds.
distance in order to calculate what's called the
RF values.
SIMPLE DISTILLATION  Also, connect the water lines in order to
let water flow in opposite direction to
Steam distillation - Lemon essential oil 🍋
vapor, as shown below
 To extract lemon oil, we will need to
grate the peel.
 Put it into a flat- bottomed flask using a
funnel.
 Add water to wash all the remaining.
As the water will be distilled later, you
can use tap water
 Add more until it reaches half flask

 Complete the circuit by eliminating

bubbles
 Add a stir bar in the flask
 Place a receiving flask
 Connect the heat and the stirring. Good
stir is important to prevent overheating.


 Now it is time to assemble the

distillation apparatus.
 Remember to connect the refrigerator
in order to let bubbles escape when
they reach the highest part of the
refrigerator.

 After a few minutes, it began to boil

 Notice how the vapors climb up through 
the system.

 The extraction comes now, perform a

 The vapors contain the compounds the liquid-liquid extraction using hexane as
lemon has. The oil is co-distilled with a solvent.
the help of water and then, as it is  Place a separatory funnel in the stand
immiscible with it, it forms two phases. and make sure the stopcock is closed.
That’s why it appears as a cloudy liquid  Pour the extraction liquid in it carefully.
here, in the condenser.
 Distillate
 Steam distillation allows to separate
compounds that are immiscible with
the distillation liquid (usually water). It
is used commonly to separate essential
oils from plants or other sources.
 Lemon has a pleasant odor and it is
used in perfumery and cosmetics
industry.  Wash with water few times.
 The main component of lemon  10 ml of hexane are added into the
o Limonene- a terpene. It is funnel and the stopper is placed.
immiscible with water and also
less dense (0.84 g/ml) so it
forms a phase above the water.
 The oily drops in the distillate are being
extracted properly.
 Turn off the stirring and the heat and
removed the heater. This helps to stop
the distillation.

 Shake it releasing the pressure that may

form in the funnel constantly. After
that, let it stand for a few seconds.
 Open the stopcock and drain the
aqueous phase into an Erlenmeyer
flask.
  use during that course the first of

these is routs law which predicts that

the vapor pressure exerted by a liquid

in a mixture is equal to the vapor

pressure of that liquid when it is pure

times its mole fraction within the

mixture

the second is dalton's law which

 Close the stopcock when an organic
phase reaches it and, predicts that the total pressure in any
 Recover it in a separated container.
system is equal to the sum of the vapor
 Repeat the process using 5ml of hexane
 Boil the hexane to separate the oil. pressures of each component regardless
o It begins to boil at about 62.6-
degree Celsius of the identity of that component and
 When about 10ml was left, pour the finally we need to think about ideal gas
liquid into the final container. Wash
the beaker with 2 ml of hexane. law for a moment PV equals NRT is the
 Continue the evaporation process of most commonly shown arrangement of this
hexane. Use only low heat.
 Place the thermometer in the solution particular equation but we need to
to monitor if it is hexane left or not.
rearrange this to PV over NT equals R
 At some point, it reaches more than 80
deg. C, so I stop the evaporation. giving us an equation which has a
 The product was 1.89g of oil.
constant result for all gases at all
 The yield was 2.42%. It is expected to
yield for about 2.5% to 4% in lemon times because of this we could say the
peel extractions.
pressure of compound a and the number of
welcome to a brief discussion of the
moles of compound a can be related to
fundamental concepts behind simple
the pressure in the system overall and
distillation in order to properly
the total amount within there notice
understand how it is that simple
that in this case when we arrange the
distillation can allow us to purify one
equations this way for two different
liquid from a mixture we need to go back
sets of gases if they're contained
to general chemistry and think about
within the same space volumes will
several of the important laws that we
cancel and of course if they're within
the same space they must be at the same well the partial pressure exerted by

temperature meaning the temperatures benzene would be 1200 Torr if we apply

will also cancel from this equation rounds law to this system what we find

leaving us with a more simple equality is that the partial pressure exerted by

we can rearrange this equality to arrive the toluene is actually 150 tor because

at an expression where the number of it's mole fraction is 0.5 and similarly

moles of a over the total number of benzene is expected to exert a vapor

moles is equal to the partial pressure pressure equal to half that of pure

of a over the total pressure in other benzene at this temperature or 600 Torr

words the mole fraction of any compound relying on ideal gas law to convert

is simply equal to is partial pressure these partial pressures to a mole

in the system divided by the total fraction we arrive at the conclusion

pressure within the system now let's that the vapor above this liquid is in

take a look at how we can use these fact not 50 mole percent benzene but

three observations to predict how a rather 80 mole percent benzene so by

distillation will behave boiling the mixture we have created a

shown here is a beaker filled with a vapor which is more concentrated in

liquid it's a binary mixture of two benzene than the original liquid now we

different compounds in this case we're need to come up with an apparatus which

going to say that the blue spheres will allow us to take advantage of the

represent molecules of toluene and that fact that this vapor is of a different

the red spheres represent molecules of composition depicted in this image is a

benzene so the depiction here would be simple distillation apparatus or a

of a mixture which is about 50 mole simple still the components of the

percent benzene and toluene simple steel are as follows a boiling

we go to the data tables we find that at flask which is placed on a heat source

the boiling point of this mixture the next is a three-way condenser or it's

partial pressure of toluene or pure at still head whose purpose is to divert

this temperature it was 300 Torr vapor from the headspace of the boiling
flask into a cooler environment where it now diverted into the West condenser

can be recondense and collected the where it can later be collected and

cooling is provided by a device known as you'll notice if you watch carefully

a West condenser which is a long narrow that only about one in five molecules

tube with a water jacket around the which escapes this boiling liquid is

outside water is plumbed in the bottom actually toluene or as one in two

and out the top of the West condenser in molecules in the embroiling liquid is

order to provide cold surface area on toluene so to take a look at an overall

which simple still as it operates we'll look

vapor can rican dense next we had a at the entire system now again we built

vacuum adapter at the end of the West our simple still by attaching a boiling

condenser the vacuum adapter serves two flask to a steelhead which diverts the

purposes first diverting the flow of our flow of gas into a West condenser and

condensed liquid into our receiving that liquid then drains through the

flask and second having a hose barb open vacuum adapter ultimately landing in the

to the atmosphere which means that we're receiving flask where it is collected if

not heating a closed system finally the we begin with the mixture of 50 mole

material flows through the vacuum percent benzene our calculations based

adapter into a receiving flask which is upon route

placed over an ice bath or kept cool in Dalton's and ideal gas laws leads us to

some other fashion so that the condensed the prediction that what will accumulate

liquid remains in the liquid phase if we in the receiving flask is in fact 80

place our liquid mixture back into the mole percent benzene

boiling flask and we heat this mixture and over time we will collect a usable

will notice that the vapor will still amount of our enriched benzene sample

begin to form at a ratio of 80% benzene the liquid vapor composition plot is

to 20% toluene however in this case typically used to try to predict how

because we have the steelhead attached efficient a simple distillation will be

instead of simply escaping the vapor is when separating two compounds from one
another in order to construct a liquid select the composition with which we

vapor composition plot a plot is know we'll be starting and then

generated on which temperature is determine the composition of the

plotted as a function of mole percent of distillate when a simple distillation is

one constituent of the binary mixture in performed in our next installment we'll

our case we'll use benzene we can start discuss what to do when we want to have

by tracing a line at the temperature at that 100 percent pure sample rather than

which we know our mixture was boiling at something that is in our example eighty

this particular temperature a mixture of percent pure

50 mole percent benzene and toluene is hello welcome to this organic chemistry

expected to boil recall from our lab video today we're going to talk

calculations we determined that that 50 about simple and fractional distillation

mole percent benzene mixture will let's begin by talking about some

actually be 80 mole percent when it theoretical aspects first let's just

reaches the vapor phase so we're going imagine that you have a pot on top of

to plot these two points along our your stove and you fill it let's say

temperature line first the 50 percent about halfway with with water like

liquid composition and then the 80 you're going to make pasta or something

percent vapor composition if we were to like that

perform similar calculations for a range if you supply heat to the pot from

of temperatures in a range of underneath here eventually the

compositions what we would find is that temperature of that water is going to

there is a curve associated with the increase an increase in increase until

behavior of these systems and we can it reaches about a hundred degrees C

then connect the dots to produce what is which is the boiling point of water at

known as a liquid vapor composition plot that point particles are going to start

now that we have this information we can going from the condensed liquid phase

instead of using the routs law into the vapor phase they're going to

calculation simply go to the plot and start coming up if you have a lid here
you're going to see droplets form and for probably the the most important or

eventually it's going to become a the most common use of a simple

rolling boil where the big bubbles here distillation is to purify a liquid from

droplets are coming up here some material that's going to remain

they're condensing at this point and solid so if you have some material that

then the drops are coming down as well is dissolved in that liquid and it's

so we have this upward vaporization and solid at the end you will get the liquid

then a downward condensation and over here and the solid particles will

whenever we're at boiling that's going remain but you can also use this method

to be an equilibrium between condensed or the fractional distillation method to

phase separate two different liquids and

and vapor-phase so for distillation that's going to be what we do in this

we're going to be collecting the lab so we begin with a liquid here in

distillate so the distillate is the our lab we're going to have a 50/50

vapor phase as it's being formed we're mixture of two different organic liquids

going to collect that and so and as we start supplying heat to the

distillation is a very important system we're going to have particles

technique for purifying compounds so you going up in a distillation and then

can we have these little hickman stills particles also excuse me in a vapor

that can purify less than a milliliters phase and in particles also condensing

a milliliter of material and also you so you're going to start seeing little

can imagine those giant distillation drops forming here at first and with

towers that you may have seen pictures continued heat those particles are going

of in petroleum refineries so you get to reach their way up here and there in

tons and tons and tons of material can the vapor phase eventually they're going

be distilled so down here is an to hit the thermometer once they hit

illustration of a simple distillation that thermometer those particles are in

apparatus we have our initial liquid the vapor phase so they are at the

right here and distillation is valuable boiling point we're going to see that
thermometer video has all these little points going

temperatures start shooting up from room inward and all that does it increases

temperature to whatever the boiling the surface area and the more surface

point of the liquid that's coming off is area you have from this point right here

and then gravity is going to cause some up until this point right here the more

of those particles to come down here and vaporization condensation vaporization

right here we have a cold water condensation events can occur and the

condenser so this is cold we're going to more of those events that can occur the

have that right about the temperature of better the separation between the two of

water and ice about 4 degrees Celsius the two liquids will be so the V grow

and that vapor phase is going to column right here

condense in here so this is called a that v-groove column is going to

condenser because it condenses the vapor increase the amount of condensation

phase back into the condensed liquid vaporization condensation vaporization

phase then we're going to have liquid equilibrium events that occur as the

particles that just pour down here and liquid travels up and gets condensed in

drop and start filling up this side and the condenser so it's going to increase

our and our set up we're going to have a the ability of the distillation to

graduated cylinder here not a round separate those two liquids so in this

bottom flask but the same idea holds type of a graph right here we're looking

true for the fractional distillation at the temperature of the distillate now

right at this point instead of that will be the temperature that's

connecting the round bottom flask being recorded right here that's the

directly to this three-way adapter we're temperature that's being recorded right

going to have something called a V grow here as the distillate comes up

column and I'll try to draw that here interacts with the thermometer and then

these are our little ground glass joints comes over to be condensed comparing

that connect everything the V grow that temperature as a function of the

column and you're gonna see it in the total volume of distillate we're looking
at a 50/50 mixture while in terms of time so we see no more

of acetone and cyclohexane in your drops coming off and then eventually we

mixture you're not going to know what start supplying more heat more heat more

your mixture is you're gonna have to heat and then we end up reaching the

determine that but in this mixture this boiling point of cyclohexane the

is what we're doing in the video and cyclohexane comes off and then that just

it's a 30 milliliters total so 15 carries on all the way until we get all

milliliters of acetone 15 milliliters of the material off well it turns out that

cyclohexane so let's imagine what would when we do this with a simple

a perfect distillation look like imagine distillation we usually don't get a

that you're able to separate out the perfect separation unless the boiling

acetone which has a boiling point of 56 points are very very different so in a

degrees Celsius and separate that from simple distillation we expect to see

cyclohexane which has the boiling point mixtures of material distilling and the

of 81 Celsius what would this look like way that that's often going to look is

what's really important to note here is something like like this it might be

that this x-axis is not time it was a somewhat linear or it might be kind of a

volume of the distillate it's based on shape that has a little bit of an S

the on the volume if it's a perfect curve to it something like that so that

distillation we would see no temperature will be our simple distillation usually

change we wouldn't see anything that's what we see but you might get a

happening and then eventually once we pretty it might look more like the Green

start getting that material into the Line it depends on the cess on the

into the vapor phase and interacting system but it would look more like that

with the thermometer and condensing we what about the fractional distillation

just see all of this 15 milliliters when we do the fractional distillation

being collected it all gets collected remember we have that V grow column that

all the way up to the boiling point of allows for a much better separation

acetone and then it just hangs out for a because of all that surface area it
allows for a lot more of these graduated cylinder 10 milliliter

vaporization condensation vaporization graduated cylinder that's the glassware

condensation events to occur so in a we will also need a small clamp a larger

fractional distillation that's going to clamp some boiling chips and then

look more like the perfect distillation finally our heat source which is going

we have in green here at least that's to be this thermo well right here and

our expectation it's not going to be there is an attached to very AK right

perfect but ideally it would look more there which will control the power to

like that green that green line so the determine how much heat is given is

fractional versus simple distillation provided to the system now we are ready

should have plots that look like this to set up our experiment what we're

and the more s-shaped this is the more going to do today is separate a mixture

it represents that green line the better of two organic liquids right here we

your separation will end up being have 15 milliliters of one compound 15

there's a French term that chefs will be milliliters of another compound when you

well aware of called Meisel plus were going to run this experiment it

everything in its place would be unknowns you'd have to figure

before you begin cooking a meal you out what they are but I'll let you know

should have all of your cookware ready what this is this is 15 milliliters of

to go all of your ingredients ready to acetone and 15 milliliters of

go out and easily accessible before you cyclohexane we're going to separate

begin we should do the same thing these by both simple and fractional

whenever we set up an experiment here is distillation and compare how well the

all of the material that we're going to two distillation techniques work let's

need for today's experiment we have a 50 begin now by setting up our apparatus I

milliliter round bottom flask a have the clamps already in place and

three-way adapter a thermometer adapter ready to go I have a lab jack here

of thermometer a condenser a vacuum that's going to allow us to adjust the

adapter and then a 50 milliliter height of the thermo well and right here
is the very act that will be what problem so this is connected right here

controls the amount of current that and I'm gonna take this power to show

enters the thermo well which is directly you it's extremely important that it's

related to how much heat will be connected with a small three fingered

provided into the sample very important clamp where this finger of the clamp is

do not plug that in yet directly under the lip of the flask you

if you plug that as soon as you plug don't want to have this connected any

that it starts heating up also very other way or it won't be stable this

important make sure you have the very right here is the stable way to connect

act if you directly connect the thermo that flask to a clamp alright at this

well to the outlet it's going to get point we should put in our sample I'm

extremely hot extremely quickly so we're going to go grab a phone

not going to plug that in yet we're there's a funnel here is our mixture

going to begin something I see students pour all of that in alright now we're

do all the time they set up all the ready to set up our apparatus the first

glassware but they forgot to put in the thing the three-way adapter it was right

boiling stones I have a few right there here

we want to put those in before we begin by the way this is the simple

and they forgot they forget to put their distillation not the not the fractional

sample so let's start by with our small yet and then we're going to put in the

clamp connecting our flask that we will thermometer adapter so the thermometer

be using for our distillation to a adapter is this cylindrical piece has

vertical post it's very important that this ground joint these glassware pieces

we use a vertical post if there's any all sort of fit together like Lego

sort of adjustments here if it gets because of their they have these ground

moved it's just going to go to the right glass junctions 14:20 junctions we're

or to the left if we use a horizontal going to slide the thermometer inside

post it can go up and down causing our here be careful not to really jam it in

mixture to spill out that would be a big you could break so just ease it in to
about there now the height of that use one of the Keck clamps that Keck

thermometer is extremely important we clamp is going to hold this in place now

want the thermometer the bottom tip of you may be tempted to put a kick clamp

it to be right at the same line as the right here do not do that if you put a

bottom of this part of the 3-way oops I clamp here you won't screw up the the

went a little too high at this part of way that this clamp is connected to the

the three-way adapter that's really glass it will actually weaken the

important because we want to read the connection it will make it more likely

temperature as our distillate is coming to come apart so no cap clamp here just

up and going over to the condenser all just the exterior clamp but there is a

right now we will use condenser this is kit clamp here and then we're gonna put

going to be the the piece of glassware our vacuum adapter now for some

that has a it provides cooling to the distillation you would want to use

system and it takes that distillate in vacuum if you have a high boiling point

the vapor phase and condenses it back to we don't need to use vacuum today but

a condensed liquid phase if you haven't we're gonna still use this adapter

seen a condenser before it's really let's ignore that beeping so then we're

important to kind of consider how this going to use that adapter right here and

looks there's an interior tube and that now this is where that larger plant

connects if we look this way it goes comes in this larger clamp is just

right through here right through the providing some support for this part of

tube then there's an exterior jacket the system to prevent any glassware from

that exterior jacket separating

is where the water will flow we're gonna so this Junction right here could

flow water through one of these inlets separate because of the weight of this

and an out the other Inlet we're going part of the system pushing down but if

to talk about which one goes which way we keep a clamp here that's pretty

the water comes in in just a second so loosely connected we don't want to have

first we connected now we're going to this really tight if we haven't really
tight you could pause things to separate well we're going to want the cold water

just loosely just kind of taking care of to enter from here and exit here the

the gravity holding things up you want reason is as we come up from the bottom

this whole setup to be high enough that gravity it will cause all the liquid to

your 50 milliliter graduated cylinder stay and fully filled the jacket before

can fit underneath now you're you're it leaves if we had the cold water enter

going to begin taking measurements with from the top we would just have a river

a 10 mil of your graduated cylinder now at the bottom here flowing out so let's

you are living dangerously if you just connect that water source the way we

set it down there so you can take a have this setup is that the red-tape

beaker put it upside down and then thing behaves the exit where the water

connect the set up the graduates is going to leave so I'm going to set

cylinder in this way so that our drips that right here connect it to that point

come down just to make it completely and then the cold water coming away from

clear what we're doing here as we start the pump has a blue tape that's going to

boiling this sample vapor is going to be connected right here

come up here it's going to come over now you want to get that on there nice

condense and then it's going to drip and tight if you feel a lot of

down into our graduated cylinder and resistance don't force it you don't want

we're going to be taking notes at each anything to break especially anything

two milliliter increment what is the that's glass in your hands you don't

temperature reading right here now we want that to break so if you connect

still have one thing left to do we have that and we're ready to begin now

to connect this condenser to the water something you want to be really cautious

source so I have a question for you of these are plastic tubes when you lift

should we have the cold water flow in this bare yak we're not there yet

from here and exit here or should we thermo well you want to make sure that

have the cold water flowing from here that tube isn't touching this can get

and exit here what do you think really hot that's its job to get hot so
you want to bend the condenser Inlet going to set up our fractional

away distillation it's going to be a very

because if you melt that tube during the similar set up except we're going to use

during the distillation you're going to this V grow column so this V grow column

have a big flood all the water's going is going to go right above the flask

to go everywhere it's going to damage that is undergoing the distillation so

the two so we're just about ready to it's going to go here between here and

begin what I'm gonna do now is lift this then up here will be our free way

thermo well I'm gonna move the camera so adapters so the B grow column is a long

we can see this a little bit better cylinder that has these little points

we're gonna lift the thermo well and we that go inward into the cylinder these

don't want this to be really forced up nooks and cranny's if you will all this

against the glass but you want the does is it increases the surface area

bottom to be just barely just there it that the distillate must move through

just started to touch just barely before it goes up here and eventually

touching I'm actually gonna go down just over into the convention that increased

about a mil of the millimeter we don't surface area increases the number of

want to be forcing those together to vaporization condensation vaporization

create any stress in the glass okay now and condensation events that the distal

we are ready to begin I have our thermo is that the distillate must undergo as

well I'm gonna set it to our very act it passes through so this will allow for

I'm gonna set it to about half strength better separation hopefully at least

we'll see what that is that's what we're expecting to see so

you sure to put the graduated cylinder I'm going to set up that distillation

here I'm gonna start the heat so not apparatus right now

gonna start to heat right now I'm gonna we're using the same mixture of liquids

turn on the water flow and then start to that we used over there in the simple

heat so here we go distillation

now on this side of the fume hood I'm in this step we're going to use two
extra pet plants that we didn't use in each component is in each of those franc

the simple distillation right here and in the fractions but this is being

right here that's just going to make the recorded during the covert crisis the

whole setup a little bit more stable GCS are not up and running right now so

okay now we have our fractional we will skip that as part of this video

distillation setup you want to be this concludes our video I look forward

cautious with the fractional to seeing you next time in an organic

distillation because it's a little bit chemistry lab

it's a bigger setup it's a little bit you

wonky but if you put this clamp over Distillation plot

here everything should be nice and hey everybody its professor Davis here

static and ready to go now we're ready from chem survival comm and the YouTube

to start our experiment channel chem survival I'm going to talk

well that wraps up this video on how to to you today about something called a

set up your simple in your fractional distillation plot which you'll probably

distillation x' in your experiment be creating in your organic chemistry

you're going to be really careful to lab soon now a distillation plot is

measure the temperature of the really just a way of documenting how

distillate at each two milliliter effective a distillation run was and so

increment of distillate as it comes out I'm only going to explain that to you

into the graduated cylinder but for this today

video I just wanted to show you the if you're not familiar with the process

setup and things to look for once this and theory behind simple and fractional

is all cooled down I can clean all the distillation you should probably check

glassware just by rinsing with some out my micro lectures on the topics

acetone into the organic waste also in available at these links now for those

your experiment you would check the of you who are already familiar with

effectiveness of the separation using distillation let's take a look at a

gas chromatography to see how much of boiling flask I've represented it here
as a simple still but it could just as component but there's only so much red

easily be a fractional still so what I'm component in the mixture so as i allow

going to do as i run my still is use the all that red component to begin

thermometer that i placed here next to vaporizing andrey condensing elsewhere i

the sidearm to measure the temperature find that there's less and less of it to

of the vapor passing through the steel be had and eventually my distillate has

head and i'm going to plot that as a a lot of blue in it so if i've plotted

function of the volume of the distillate the temperature as a function of volume

that i've collected so why on earth what collected I expect that temperature to

i want to do such a thing increase over time now we already know

well the reason is that presumably the from our distillation discussions on

vapor which is moving through the still routes and Dalton's laws

head is at the same temperature as the that mixture can never boil at a

boiling point of the distillate that temperature outside of the extremes

i'll be collecting so by measuring the defined by the pure liquids boiling

temperature within the still head i'm in points but as the still gets better and

effect measuring the boiling point of better at separating the two the

the distillate that i've collected and i distillation plot is going to have a

can use that information to glean some different slope and different limits

knowledge about how pure my distillate specifically the slope will increase and

really is so i'm going to start off by the limits will get further and further

just marking the boiling points of my apart as my still gets better and better

pure components the red would be the at separating these compounds so for

more volatile and in this case let's example if I had run a simple still and

make the blue component the less obtained the yellow distillation plot I

volatile and then i'm going to apply might switch to fractional and see

some heat and as my mixture begins to something like I see now so the

boil as we might expect we'll see a take-home lesson here is that wider

vapor which is enriched in the red temperature ranges and steeper

transitions in a distillation plot are want to be sure that thermo l is the

indicative of a more effective appropriate size for the round bottom

separation that's all for now folks I'll flask attendees be sure it's just

see you next time the holidays are just snuggly now we're ready to go

around the corner don't forget to buy let's get those electronics connected

something for that special nerd in your we're going to plug our stir plate into

life at the Chemistry gift shop at Cafe the non variable power outlet because

Press we're going to use the dial on the serve

Procedures for simple distillation plate to designate how fast that serves

[Music] but our thermo L on the other hand we've

hey guys we're going to build a simple got an external control for that so

still now so for that we're going to let's plug that into the variable power

need a round bottom flask of appropriate outlet the one that's got the variable

size a three way connector to the art power of marking right next to it

steel head we're also gonna need a great now we want to get that round

thermometer adapter and thermometer bottom in place so let's put a clamp on

ticker that we're going to connect a our rail usually one of the knuckles

West condenser a vacuum adapter that's that's available in your main lab drawer

going to direct flow down into a 10 mil once that's in place we're going to

graduated cylinder and of course we're place again your appropriately sized

going to have some connectors and this round bottom flask in there I recommend

pin bar and some others clamps and you sort of squeeze down on that to

things in place so let's get started in finger clamp and then spin the wingnut

order to build our apparatus we'll need it's a lot easier to do this way instead

a lab jack we're also going to have a of fighting against all that tension if

stir plate now that's also a hot plate you don't squeeze down the clamp

but we're only going to use it for initially and the next thing you want to

stirring this time and we're going to do is get that plate and from well

use a thermal well as our heat source we position directly beneath the round
bottom flask so that it will keep it place that and give it a little twist

very nicely each time I add a new piece of glassware

once I crank the lab jack up you can see to be sure that I get a good gas tight

if it's very snugly and nicely next seal

we're going to catch our three we adapt there we go now I've clamped everything

for this we need a gas tight seal so I in place and that part of my build is

want to apply just a pea sized dollop of complete

vacuum grease you're going any more than the next thing I want to do is place my

that that's all it takes the apply thermometer so I can monitor the

that's the mail into the ground glass temperature in the field a to do that I

joint and then insert it into the female will use my thermometer adapter again

end giving it a twist to be sure that we with a dollop of vacuum grease and then

get a nice clear ring all the way around I'll place my thermometer through the

once we have a clear ring around that rubber adapter on top which is gas tight

joint know that we have a gas tight seat already so there's no need for grease

next I'm going to place a two finger here I'll push that down until the bulb

clamp on the adjacent rail this is going of the thermometer ever so slightly

to hold our flow director which I'm below the sidearm where that vapor is

going to place here and try to when moving the condenser this is going

approximate roughly where it would be if to help me measure the boiling point of

I were to put my condenser in between my the distillate I collect next I'm going

still head and that newly placed flow to place a ket clip which has a large

director here I'm a bit high so I'm side and a small side just like the

going to bring it down that's better glass joint does right over that

now that it's there I'll put a bit more condenser notice that when I put the

grease on the male joint of the downward large side over the female and smalls it

facing adapter from my three-way over the male I get a good snug

connector and on the downward facing connection I'll do the same thing at the

portion of my condenser as well and I'll other end to be sure that that condenser
stays in place because it's not clamped heat source and I'm going to add my

itself finally I'm going to need a 50/50 mixture of ethanol and water to

receiver and for this I'm going to use a the boil and flask I'm also going to add

beaker to get some elevation and I'm a spin bar so that I can agitate the

going to use a graduated cylinder to mixture and be sure that I get even

collect my distillate because it's so heating and avoid bumping in my still

very important that I know exactly what once that's reattached I'm going to

the volume of distillate is as I've raise my eat source and my stir plate

collected now I'm ready to apply my and now it's time to run my fill I'll

cooling water to my condenser so I'll begin by activating the power to my fume

take a nice flexible water hose and hood after which I will turn on my stir

attach that to the lower hose barb on my plate to a setting of about two to three

condenser this is where the water will hundred this setting will give a nice

go in so I'll place the other end of steady stir and avoid bumping so here is

that hose over one of the water spigot an example of one that is stirring at

in my fume hood about 220 I'm not to do it

of course that water will need somewhere next I'm going to turn on my thermal

to go so I'm going to place another hose well by activating the Vera stat and

on the upper hose bar and that will run turning in to about 70 to 75 this should

to the well sink in the back of the clip give me a nice even heating it will

next I'm going to turn on the water allow my skill to run nicely before too

being sure that I'm very careful about long a nice even boil should be observed

which one of the green knobs I'm turning if my stirring rate and my heating rate

so I know which which water spigot I'm are appropriate next I'll start to see a

activating and it will fill the tube in little bit of vapor condensing if you

the bottom to the top now the jacket of look closely in the vertical part of the

my West condenser is completely filled steel head you'll see that vapor

with cold flowing water now it's time to condensing and rolling back into the

load my samples so I'm going to lower my boiling flask where it came from
but before too long you'll start to welcome to a brief introduction to the

notice that vapor also condensing in the principles behind fractional

sidearm and this is where it will distillation we're going to begin our

condense reach the cold area of my still discussion with a question based upon

and then roll downward into the one of our earlier discussions which you

collection flask if you watch carefully may want to view if you haven't yet and

as this procedure continues plotting the that would be the simple distillation

temperature in the still head as a lecture the question we'll be asking in

function of the amount of distillate this particular presentation is can

collected then we notice it over time it distillation be used to obtain liquids

slowly increases this is because the of greater purity than those predicted

temperature within the still head is by routs Dalton's and ideal gas laws in

essentially the bulletin point of the other words can we somehow instead of

distillate and since I'm running a achieving our atmo percent benzene

simple still which is not capable of purification as we did in our previous

achieving a great separation the example achieve a higher purity of

composition of that distillate is slowly benzene and a distillate

changing after a significant period of now you'll recall from our previous

time you may actually notice that it discussion that if we have a 50/50

eventually levels off this is because mixture by mole of toluene and benzene

all the ethanol has been removed or just and we boil that mixture on a hot plate

still in water at this point so once we we expect the vapor above that boiling

get to about half of the total volume mixture to have a composition of 80 mole

that was added to the flask we can get a percent this is based upon our

few data points that show us that we calculations using routes Daltons and

have arrived at that point and then ideal gas laws but of course the

we're ready to stop question always comes up is it possible

you to get a distillate that's 99% benzene

Fractional Distillation or 100% benzene and the answer to this

question is yes but we have to think also a boiling flask for a second round

carefully about how we build our of distillation and let's start this up

distillation apparatus in order to and see what happens

achieve this shown here is a schematic as I boil my 50 mole percent benzene

of a simple distillation apparatus like solution in the first boiling flask then

the one that we discussed in our recondense the vapor in another region

previous lecture call what each part is of the glass where the accumulating

and the purpose for it in this apparatus distillate is expected to be 80 mole

now if we build a simple still charging percent benzene by our calculations if

the boiling flask with 50 mole percent however I heated this second flask

benzene and toluene thereby vaporizing

we then channel the vapor into another this 80 mole percent benzene I would

region of the glass we're condensing it have to apply a new set of calculations

with a jacket of cold water we expect using a new set of mole fractions and

the accumulating distillate to be of a vapor pressures the consequence of this

composition that is predicted by routes is that I would have an even higher

of Dalton's and ideal gas laws to be 80 purity distillate collecting in my

mole percent benzene at this point I second flask in the case of benzene and

often challenge my students is it toluene this is a highly pure distillate

possible to create a distillate of of about 99 to 100 mole percent benzene

higher purity from such a sample the it will be very very pure the reason for

most common answer that I get to this this can be seen in the liquid vapor

question is yes if you redistill the composition plot to the left if I begin

distillate and that is in fact true what with a 50 mole percent liquid I expect

I've got here is a schematic of a simple to collect an 80 mole percent vapor now

distillation apparatus if that vapor is then condensed and re

in which I have attached the collection distilled I'm starting from the liquid

flask from apparatus one to yet another portion of that 80 percent line meaning

still had in condenser thereby making it I get another step along the liquid
vapor composition plot reaching a recall again that we're beginning with a

position on the phase diagram where it's boiling of 50 mole percent liquid our

approximately 90 with 7 mole percent liquid vapor composition plot predicts

benzene so I have successfully in this that the vapor which will be ascending

case achieved a higher purity distillate the column should be of an 80 mole

from my 50 mole percent started material percent composition however as it

however this is a very large apparatus ascends the column the column

and would require a great deal of time temperature drops and our small aliquot

to build and a great deal of energy to of mixture here is expected to condense

run and there's actually a much easier along the walls of that fractionating

way to accomplish the same effect the column and in doing so it becomes a

tool which we use to achieve the same liquid this 80 mole percent benzene

effect as in the previous example is a liquid will then potentially reeve aper

fractional still which differs from a eyes and in doing so become even more

simple still only by the addition of enriched just as though we had run a

something called a fractionating column second distillation on it so some of the

the fractionating column is inserted toluene will reflux back into the

between the boiling liquid and be still boiling flask whereas more the benzene

had sometimes it's packed with solid achieves a second round of vaporization

materials to provide additional surface if we allow this vapor to condense we

area and we'll discuss why that's 7 Moll see that we now have a 97 mole percent

but for now let's just take a look at mixture if our drop that were to

our fractional still in which we have vaporize once more we would expect to

charged the boiling flask with 50 mole have a highly pure sample about a

percent benzene in toluene what will go hundred percent pure benzene and toluene

on inside of that fractionating column this is the principle on which a

as the vapor begins to ascend well let's fractional distillation apparatus

watch a small aliquot of vapor move up functions now that we've considered the

the column and we'll see what happens behavior of just a small aliquot like a
single drop of mixture within a would have a distillate of about 97 mole

fractionating column let's try to get a percent benzene looking at the top of

better visualization of what it really our hypothetical column we have a

looks like what's really going on inside situation where only benzene is reaching

of that fractionating column so here that position and therefore if we were

again I built a fractional still and I to divert vapour from the top of a

charged the boiling flask with 50 mole column to a condenser we should collect

percent benzene and toluene let's zoom a sample which is essentially 100 mole

in on that fractionating column again percent benzene or absolutely pure

and see what's going on inside benzene so what we're really achieving

what you notice is going on here is that here is the same effect as multiple

the toluene molecules due to their lower distillation x' but we're only running a

volatility are more likely to condense single distillation using a

and fall back into the boiling flask fractionating column if we look back at

whereas the more volatile benzene our liquid vapor composition plot

molecules have a much greater tendency starting from a 50 mole percent mixture

to traverse the entire length of the of the two we expect that a single

fractionating column reaching the top distillation should yield an 80% pure

this is accomplished based on multiple distillate

rounds of vaporization and condensation if we were to run a second distillation

as the mixture moves through the column we would expect that we would have a 97

so we expect that near the boiling flask percent pure distillate and if we were

will find a region in which the to again collect that and redistill it

composition of the material is about 80 once more we expect to have a situation

mole percent benzene moving higher up where we have essentially 100% pure

along the column we find region where we benzene if we were to set up a

have about 97 mole percent benzene so if fractional still and then empirically

we were to divert the vapor at this determined that the collected distillate

point into a condenser and collect it we is 97 mole percent benzene we would

report that our still is operating at
two theoretical plates meaning that it
is producing a distillate of similar
purity to that which would be expected
in two rounds of serial distillation and
similarly if we have about a hundred
percent pure sample of benzene in
toluene we would then report
our still is operating at about three
theoretical plates this gives us a way
to report on the efficiency and the
effectiveness of a fractional still
Fractional distillation is used for the
separation of two or more liquids whose boiling
point
differ by less than 75 degrees.
To do a fractional distillation, you
start with the same piece of equipment
that you do for a simple distillation,
in that you have the distilling flask.
And it should be raised off the bench top,
sitting on a wooden block or an iron ring,
and clamped securely to a ring stand.
What you then want to do is add a piece of
equipment
called a fractionating column on top of the
distilling flask.
The purpose of the fractionating column is
to add surface area and thus, multiple
vaporization
condensation to occur between the point that
the
liquid is distilling and that it is collected
at the end.
So this is an example of a fractionating column
that
we're going to use in the 2311 class.
Notice that we're not going to add water to cool
this
condenser, because we want it to get warm as
the vapors
ascend up the column.
Another example of a fractionating column
looks like this.
This is called a Vigreux column,
with lots of cool indentations of the glassware.
Again, this adds surface area so that we
increase
the number of vaporizations and condensations,
which are called the theoretical plates.
The number of theoretical plates,
for example, with a simple distillation,
is only two or three.
These two fractionating columns would add
approximately 6 to 10 additional theoretical
plates and aid in the separation of the 2 liquids.
All right, once we have the fractionating column
there,
then we can just add the remainder of what
looks like
our simple distillation piece of equipment on
top.
And as long as this clamp is nice and secure,
it should rest easily on top of our distilling flask.
So many of the principles that we have for
simple
distillation apply here.
One, you want to make sure that you have a stir
bar or
boiling stone in the distilling flask.
Then you have your thermometer and
thermometer
adapter, and the ball should be below the side
arm so you
can accurately record boiling points.
We have our cooled condenser,
with the water coming in at the bottom,
exiting out the top, and anchored with a plastic
funnel in the sink, and then a teared receiving
flask for collecting the liquid that has distilled.
Again, you'd record the boiling point at the start
of when you see drops enter the receiving flask
till the end.
You could also collect multiple fractions,
so you might want to have a second or third
teared
receiving flask if you are in actuality separating
a
mixture of liquids.
When you're ready to start the distillation,
be sure that you plug your heating mantle into
the variac control, and not directly into the
outlet.
Now you're ready to begin your fractional
distillation.
Welcome O Chem students. In this video we're
going to do a fractional distillation.
Now we've done a simple distillation and that's
where, that's the type of distillation where we
separate
a volatile compound from a non-volatile
compound. In a fractional distillation we have
two volatile compounds
whose boiling points are relatively close
together. And that means within 40 or 50
degrees of each other.
You probably want to use a...
or 40 or 50 degrees or less you wanna use a
fractional distillation over a simple distillation.
In our laboratory, in our experiment we're going
to separate Toluene which has a boiling point of
111
degrees from Cyclohexane which has a boiling
point of 81 degrees so the difference in
temperature
between those two boiling points is around 30
degrees. So we need to do a fractional
distillation.
Now before I do the setup, I want to talk a little
bit about the theory of the fractional distillation
and for that I'm gonna use this phase diagram
which shows if you look on the x axis of the
phase diagram
it's showing 100 percent cyclohexane on the left
hand side and 0 percent toluene
at the origin of the plot. And over on the far
right you'll see it's 100 percent toluene, 0
percent cyclohexane.
And the temperature scale is on the y axis and
so if you read on the far left you'd see the
boiling point of
cyclohexane is in the low 80's and the boiling
point of pure toluene is around 111.
So what's all that stuff in the middle? Well that's
the mixture. That's the percent mixture of those
two
solutions. We're going to separate 20mL of
Toluene and 10mL of Cyclohexane so it's kind of
a two to one
mixture. For the purpose of the explanation,
let's pretend that the mixture is actually 3 to 1.
Lets pretend it's 75 percent Toluene and 25
percent Cyclohexane and if we do that then we
can kind of
start our discussion by looking at point A on
that diagram.
If you look, point A that corresponds to the mix,
75 percent cyclohexane 25 percent toluene.
Well that mixture has boiling point of 100
degrees, that particular mixture.
Now if you notice the line up above, that's the
composition of the vapor. The vapor at 100
degrees
has a composition that's 58 percent
cyclohexane and 42 percent toluene.
So the liquid was 75, 25. And the vapor is 42,
58. The vapor is much more concentrated
in the higher
volatile compound or the lower boiling, more
volatile compound, cyclohexane.
So let's say that we condensed that vapor.
That 58 percent, 42 precent. If we condense the
vapor we get a liquid that has compostion equal
to point C
on the diagram. The liquid at point C would boil
at 90 degrees. At 90 degrees you can see the
vapor
would have a composition that's now 83
percent cyclohexane. So wait a minute, we
started with a
solution that was 25 percent cyclohexane in our
example.
At 100 degrees the vapor was 58 percent. We
condense that vapor and then we boil that
vapor off.
We boil that solution and that solution
produces a vapor that's 83 percent in
Cyclohexane and if we condense
that, that'll give us the solution of composition
D.
So what I want you to understand from this
diagram is that the, at any particular
temperature
the vapor composition is always higher in
concentration in the more volatile component.
And this is kind of the basis of the fractional
distillation. We're going to heat the pot. The pot
will produce vapors.
The vapors will rise up a vertical column. A
column that we didn't have in the simple
distillation.
In fact, let's take a look at a diagram of what the
fractional distillation is gonna look like.
We'll go to this diagram of a fractional
distillation setup and you see it's different from
the simple distillation and
now that there's a vertical column there and it
shows that the vertical column is packed with
something.
And we'll discuss what that's about in a minute.
But the vapor now has to climb up the vertical
column
before it can condense in the horizontal
column.
What happens in a fractional distillation is the
temperature in that vertical column is highest
down by
the steel pot. Down by the flask there that
contains the liquid that we're distilling.
As the vapor goes up the column the
temperature in the column decreases. So the
temperature at the top,
that's called the head temperature. The
temperature at the top of the column is lower
than the temperature
down at the pot. And this is because the vapor
that climbs the column condenses, redistills,
condenses,
redistills, and every time it condenses and
redistills the vapor gets more concentrated in
the more volatile
lower boiling component. So as we do the
separation of toluene and cyclohexane what'll
happen is
the cyclohexane vapor will concentrate at the
top of the column and the toluene will
continuously be returned to
the still pot. So what we'll see is the
temperature at the head of the column will get
the 81 degrees
as the cyclohexane starts to boil. As the
cyclohexane is condensed off now the
composition in the still pot
is shifting to higher and higher levels of toluene
and so the temperature is going to rise.
The head temperature is going to rise gradually
and this allows us to take off several fractions
thus the term fractional distillation. We're
gonna do three fractions. You should be looking
at
another slide that will show you the three
fractions. The first fraction we'll collect we're
gonna call it "pure"
and I'm putting pure in quotes. It's not gonna
really be pure but it'll be mostly cyclohexane.
And we'll collect that fraction between the
boiling points of about 81 and 84 degrees.
So when the head temperature on the
thermometer is around 81 to 84 that'll be the
cyclohexane fraction.
When the temperature exceeds 84 we'll switch
flasks and collect a middle fraction which is a
cyclohexane
toluene mix. And we'll continue to collect that
fraction between 84 and 100 degrees.
And when the temperature at the top of the
column finally reaches 100 degrees we switch to
collect
the third fraction which I'm calling and again
"pure" toluene, pure in quotes. And anything
over 100 degrees
is going to be mostly toluene. So we'll have a
lower boiling fraction that'll be heavily
concentrated in
cyclohexane and a higher boiling fraction that's
heavily concentrated in toluene and a mid
fraction that's
a combination. So, it won't have been a
complete separation. It will be a partial
separation but
this is the way that gasoline and other things like that that they put in here to provide
petroleum products are separated by fractional this surface area for the vapor and condensate
distillation. to mix.

So it's common, very common industrial But we're gonna go with steel wool. That's what
technique and it's a technique that we'll have to we have and it's cheap and easy and so we have
use sometimes a

when we have to separate materials that are jar of steel wool so we're gonna take a little
closely boiling. steel wool out of the jar and we're gonna pack
our
So, I think at this point I'm ready to show you
how we're gonna setup the apparatus. short fat condenser with some steel wool. Now
the most common mistake when you get to this
(Music)
point
We're ready to setup our apparatus now and it's
is using way too much steel wool. So, cause it
all the apparatus that we had before for a
doesn't look like much in your hand but when it
simple distillation
gets in that
except this time we're going to use two
little tube, you'll be surprised how much it is. If
condensers instead of one. And we're gonna
we have too much wool in the column the
use this
column will tend to
I call it the short fat condenser. That'll be the
flood. The condensate will not be able to get
vertical condenser and the long skinny
back into the steel pot and will form a liquid
condenser will be the
plug here
horizontal condenser this time.
and that's not good. So, we want some steel
But before we use this condenser it needs to wool but not too much steel wool.
have some packing in there and the purpose of
So what I do, we'll see how this is. I'm gonna
the packing
start like this and I'm gonna physically kind of
is we want to provide a lot of surface area in pull this apart.
this column for the condensed vapor to
Make it finer.
mix with the rising vapor. And it's a lot of
Maybe get rid of a little of it here. It doesn't
surface area provides a place for the
look like much now but when it gets in the tube
condensate to re evaporate.
you might be surprised at how much it is.
And so chemical engineers call this having a lot
of theoretical plates in a distillation column. Alright, I'm going to insert this in the tube. I
need a spatula.
The more theoretical plates the more efficient
the fractional distillation. So there's all kinds of So with the end of the spatula I'm going to push
designs for this down into the tube.

distillation columns. There's all kinds of three Now, maybe if I hold this up against my jacket,
dimensional packings, rings and spheres and my lab coat, maybe you can see through there.
I hope you can see some of my white lab coat
coming through when you look at the steel
wool.
If you can't see daylight through the steel wool
that's way too much.
You need to be able to see daylight through the
steel wool.
For a joke one year, I told the students it needs
to be thin like the bald spot on the back of my
head.
One of the girls goes Dr. Davison you need to
take more wool out then. Hahaha.
So we do need to see some daylight. Now we're
good. Now we're ready to do the setup.
So, I'm coming over here like normal. Let me get
this on the other side here.
I've got the clamps. Alright sand bath, I'm not
actually going to do the distillation today. I'm
just gonna setup
the equipment. So, we'll have the steel pot, the
big flask. Put the stir bar in. We'll put that in the
sand. We're gonna
clamp that.
Alright now listen, my advice on this is get this
down in the sand. The same advice I gave you
on the simple
distillation. We want this down in the sand
otherwise you may be here for the whole three
hours and not get
any distillate over.
That flask needs to be down in the sand.
Alright, now that's clamped. Now we put on the
packed column.
And we hold it in place with a keck clip.
Adapter.
Another keck clip.
Now we'll put the horizontal column on.
Keck clip.
I've just put the horizontal condenser on. I'm
getting ready to put the receiving flask on.
I need a lab jack to raise this up.
So I'll need this thing called the vacuum
adapter. That'll go on with a keck clip. Receiving
flask goes on.
Ok, I don't have quite enough lab jack here so
I'm gonna bring in another lab jack to support
this.
And also, I want to try to clamp this column. I
don't like it to have just a single support.
In fact I'm gonna clamp it a couple of places. I'm
gonna clamp the horizontal column.
And then maybe I can just, maybe I can do that
about right in here.
I don't want this to tip over
when the big earthquake comes.
And this will be the fun one. I don't know if I can
see. I have to try to get this one on.
I'd like to get the horizontal one clamped so it
won't fall over.
It looks like I got this one right at the same spot.
Well, I'm having a hard time getting this third
clamp on here so I think what I'm gonna do is
just make sure I've
got the receiving flask well supported by the lab
jacks. This thing with two clamps on the vertical
column
it should stay upright, shouldn't tip over. We
should be good.
But nevertheless make sure this receiving flask
is supported. That looks to be a lot easier than
trying to wrestle that third clamp on there.
Now we need to connect the cooling water. So,
remember it goes in the bottom connection.
In the bottom.
Out the top.
Or maybe you put the hoses on before you set
the condenser up.
Anyway there we go. In the bottom, out the
top. Make sure the hose doesn't touch the back
of the hot plate so
you don't burn through the hose.
Now we need the thermometer adapter and
the thermometer.
Alright so I want to make sure that the O ring on
the thermometer adapter, that's up here,
makes a tight
seal. So push that down so there's a good seal.
Rubber O ring to the glass.
Now, I'm gonna position the thermometer bulb
so that the top of the blue bulb is right about
the middle
of this horizontal takeoff.
And at that point then I screw down the yellow
cap
and the O ring inside locks the thermometer in
position. So, now the thermometer's
not gonna drop, come loose and I made sure
I've got a good seal.
Before you start running the distillation double
check all of these joints and make sure they're
snug.
Even though there's a keck clip on there, the
keck clip keeps it from coming apart but it
doesn't necessarily
guarantee snugness. So make sure the system,
all the joints are snug otherwise vapor will
escape.
It's gonna take the easiest way out and the
easiest way is not when it gets here. It's gonna
be some other
short cut along the way.
So, we're just about ready to go. Now there's
one other thing that you're gonna have to do
many of you are gonna have to do. Maybe not
all but the people that are gonna end up setting
their equipment up
over in the hoods. There's a lot of air flow past
your setup in the hood.
And this condenser and the whole setup gets a
lot of air cooling because of that rapid air flow.
So, to help this thing along, it's a good idea to
wrap the flask and the vertical column in some
aluminum foil.
Just get some aluminum foil, wrap a little bit
around the bottom down here around the flask.
And then wrap some,
wrap some around the vertical column.
And yes you can't see in there when you have
the aluminum foil on there so that's kind of a
disadvantage.
I would like to be able to see in there what's
going on,
but sometimes we have to sacrifice that
visibility. So I might get another piece of
aluminum foil and make it
better around here. And I've got daylight here
so I'd probably have another piece of foil but
for the time being I'd like to have that open so I
can see when the liquid starts to boil. When it
starts
to boil it's gonna take a while for those vapors
to get up here. So here's something that the
students don't understand. Is you have boiling
here but the temperature here is sitting at 22
degrees.
The temperature here hasn't moved and Dr.
Davison it's boiling for 15 minutes and the
temperature hasn't
gone anywhere. Crank the heat up, wrap it in
aluminum foil and then try to be patient.
Because eventually the vapors will climb the
column. It is gonna take a fair amount of heat
to drive the vapors up this vertical column. It'll
help if the column's insulated with the
aluminum foil
but it's still gonna take a lot of heat. And it
doesn't happen instantaneously. So you will not
see a temperature change until you see the
vapor touch the bottom of the bulb.
And so you may have this wrapped up but again
I kind of like to be able to have a look in there,
see what's going on. See when the vapor's
coming up. Once you see the vapors at this
height
all of a sudden the temperature will shoot up.
So, for a long time you'll have nothing.
Boiling but nothing and then all of a sudden the
temperature will shoot up.
So, don't turn your back on it. Don't walk away
on it. Take some looks inside every once in a
while.
What you'll see is if you can look in at the steel
wool you'll see the steel wool getting wet.
The wool is wet and now you know well the
vapors are at least that high and there's a lot of
condensate
and you'll be ale to see dripping back into the
flask.
Eventually when the vapors get here, you'll see
drops coming off the tip of the thermometer
bulb
as well. At that point, then the vapor will enter
the condenser. You got the water going in this
condenser
so the vapors will condense here, and collect
over in the flask. Now for this separation,
we're gonna need several flasks. So, the first
flask that's for fraction 1, the so-called pure
cyclohexane fraction.
Second fraction is the mixed fraction and the
third fraction, toluene fraction, will need a third
receiver.
So this is how you setup the fractional
distillation. You pack it with the steel wool,
don't pack it too tightly. If you do, the column is
gonna flood and you'll never get the vapor up
here.
So, flooding is no good. Make sure you can see
daylight when you look through the condenser
and you
look through the steel wool.
Wrap the column with aluminum foil and then
be patient. The vapors will eventually get here.
You're probably gonna have to crank the heat in
order to get this to go.
So I think those are the secrets of the fractional
distillation and I'll be coming around to see how
you do.
(Music)
Steam Distillation components at the extreme end of the

welcome to a brief introduction to the plot in this case we'll make this the

concepts underlying the practice of vapor pressure of component a if I plot

steam distillation like to begin our routs law on my diagram I must start

discussion by asking a question and that necessarily at zero for zero multiplying

is what happens when two liquids of an this is routs law for compound a I can

organic nature are not miscible with one similarly place another compound let's

another in our discussion about call it compound B where it's vapor

traditional distillation we always made pressure is at the other extreme of the

the stipulation that our binary mixture x-axis plotting a line gives us routes

of liquids must be miscible but what law for compound B finally we can apply

happens when they don't actually Dalton's all to the situation where we

dissolve into one another at least not acknowledge that at any particular

not intimately at the molecular level composition if we are to take the

and the answer is routs law no longer summation of all the vapor pressures of

applies to the situation so this all the components in the system in this

drastically changes the behavior of our case just the two we can determine what

system and we're going to take a look at the total pressure should be above that

this in the coming moments and actually boiling mixture simply by adding them

discover that it can be useful that and by doing so we've generated a plot

routs law does not apply to systems like of Dalton's law for the system this

these let's begin by reviewing how it is tells us the total pressure above the

that a binary system of miscible liquids boiling mixture at any given composition

is expected to behave you'll recall from when it is boiling recall again that

our discussions of distillation that if these two principles these two laws

we plot vapor pressure as a function of where our foundation for making an

the mole percentage of two components argument for how we could separate two

which are miscible in one another we can liquids from one another using

plot the vapor pressure of one of those distillation when we're dealing with a
mixture of two immiscible liquids standards this is not a good technique

however the landscape of this diagram for isolating these two liquids and in

changes dramatically and that's because fact it is

routs law requires that they be mixed so we can see clearly that there's a

intimately at the molecular level which drastic difference in the behavior

is no longer the case so if we reproduce between miscible & immiscible liquids

our plot but in this case we make the when we heat them up and boil them so

stipulation that the liquids are let's take a look at this miscible

immiscible with one another they will liquid diagram a bit closer and think

establish their own vapor pressures about exactly what's going on here what

independently of their concentration in it's telling us is that components of

the mixture in other words these plots the miscible mixtures establish their

will no longer be sloping lines which own vapor pressures in the flask

intersect at zero at the extremes but regardless of their concentration in the

rather they will be horizontal lines boiling mixture and therefore routs law

indicating that the vapor pressures do does not apply to such mixtures this

not change as a function of again is not a very good observation if

concentration this is true for both it were our goal to separate these two

compounds a and B assuming the Daltons compounds and so we wouldn't use a

law however holds in this situation what traditional distillation to try to

we see is that when we plot the separate compound a from compound B

summation of the two vapor pressures is however this observation will become a

that we end up with a straight line now useful and valuable observation when we

the potential problem with this is that attempt a steam distillation so let's

if we want to isolate these two consider our goal here where we want to

components notice that the ratio of separate a water immiscible oil of low

components in the mixture above the volatility from a non-volatile

boiling liquid never changes which means contaminant and I will just use a again

that by traditional distillation as normal we'll use a little cartoon

system here to represent these compounds is usually about a hundred degrees from

where we'll have blue spheres as water the still at onward the system is going

red spheres as the immiscible oil and to look exactly like any other simple

brown spheres as the non-volatile still will have a West condenser with

material so again our goal in this the cold water plumbed in through the

experiment is to take a mixture of lower of the two hose Barb's and out

immiscible oils and non-volatile through the higher of the two hose

material and somehow isolate that Barb's will have a vacuum adapter to

immiscible oil notice that water is direct the flow of distally into our

really not relevant to this process at receiving flask now that we've reviewed

the moment all we want to do is be sure how to construct the distillation

that we separate our immiscible oil from apparatus let's take a look at how one

our non-volatile material and in this functions begin the experiment by

case of steam distillation water is just charging boiling flask with your

going to provide a medium for us to materials and a little bit of water and

accomplish that goal shown here is a you'll also add some additional water to

schematic of the steam distillation the separatory funnel with the stopcock

apparatus that you'll most likely use in closed in order to provide a reservoir

a teaching laboratory the apparatus well begin by opening the stopcock very

consists of a separatory funnel which is slightly so that the water from the

used as a reservoir for additional water separatory funnel is dripping into the

when needed a boiling flask in which the boiling flask as we apply heat to the

mixture of oil low volatility material boiling flask the mixture will begin to

non-volatile material and also the water boil and of course as you might expect

will be boiled a thermometer is attached water being the most volatile of the

to the device through a steel head so we compounds within the flask will get a

can monitor the temperature and great deal of water distilling out but

you might not be surprised to hear that again remember that the immiscible oil

the temperature and a steam distillation will establish its own vapor pressure in
the head space above the flask this point we've accomplished our goal

independently of the vapor pressure of and this is how steam distillation works

the water this means that if you look you

carefully you'll notice that every so Extraction and Isolation of Caffeine from tea

often a little bit of immiscible oil caffeine is the most widely consumed

also is carried along into the condenser psychoactive drug and as you likely know

by the moving water vapor this means it's found in many food products in this

that over time we expect to accumulate video we'll be extracting caffeine from

in the receiving flask a mixture of green tea but almost any other type of

water and immiscible oil which is tea could be used for this extraction I

consistent and very constant in used 45 milliliters of dichloromethane

concentration as we do so we slowly water 60 bags and 6 grams of sodium

deplete the immiscible oil in the carbonate 60 bags were added to a beaker

boiling flask until at some point this then 90 milliliters of water was added

process has been carried out to the this was followed by 6 grams of sodium

extent that all of the immiscible oil carbonate once the sodium carbonate is

has been moved into the boiling flask mixed thoroughly the solution is brought

and now there's only water and to a boil by boiling the tea we are

non-volatile material remaining in the separating out the water soluble

original boiling flask at this point we components which is mostly caffeine and

can deactivate our still and take a look tannins the tannins are acidic and react

at what we've accomplished notice what with the sodium carbonate in solution to

we've accomplished is that the red form salts we are going to separate the

immiscible oil material has been caffeine from the water layer using an

moved from the brown non-volatile organic solvent and salting the tannins

material using water as the medium should keep them in the aqueous layer

separation of water from the immiscible boil the solution for about 10 minutes

oil is very simple that can be achieved it is recommended to place something on

usually by liquid liquid extraction at top of the beaker to limit water loss if
the heat is high might bubble a lot and the layers were allowed to settle and

to prevent it from overflowing remove the bottom DCM layer was drained this

the lid and let the bubbles settle after extraction process was carried out a

10 minutes the concentrated tea extract total of three times using 15

was transferred to an Erlenmeyer flask milliliters of DCM each time the organic

the teabags were pressed in order to layer was dried using calcium chloride

release as much water as possible and then filtered into a round bottom

which was then also decanted into the flask the filter is washed with a small

Erlenmeyer flask now 60 milliliters of amount of DCM I set up a distillation to

water was added and the process was remove and recover the dichloromethane

repeated the tea extract was combined at the bottom of the round bottom flask

with the previous tea extract and again we are left with some dry crude caffeine

the teabags are squished to release as this was removed and transferred to a

much water as possible the solution was test tube a small amount of DCM was used

that a lot to stand and cool down to to wash the round bottom flask which was

room temperature this step is optional transferred to the test tube using a hot

and probably not required but I decided plate the small amount of DCM was

to filter the tea extract prior to the evaporated off the crude caffeine was

separation process if you choose not to then recursively is using 95% ethanol

do this you can transfer it directly to the crystals were vacuumed filtered and

a separatory funnel I washed the filter the test tube was washed using ice-cold

with 15 milliliters of DCM but if you 95 percent ethanol the crystals were

didn't filter it you can add the DCM dried under vacuum and we were left with

directly to the separatory funnel so nice white nearly pure caffeine crystals

after adding the DCM you should have two unfortunately yield was quite low and it

layers the separator front was capped was only around 30 milligrams an NMR of

and shaken very gently in order to the product shows that the caffeine is

prevent quite pure

the formation of an emulsion afterwards

In this video caffeine is extracted from tea using
dichloromethane.
The crude extract is purified by recrystallization
with ethanol.
I am going to add about 75 mL of water to a
200-mL beaker.
Then I am going to throw in a few boiling
stones.
I am going to cover the beaker with a watch
glass and turn on the temperature to get it
to boil.
Once it starts to boil, I’ll add two packets of tea.
Okay, after it’s been boiling about 5 minutes
now, I am going to go ahead and take out the
packets, and I will try to get back as much of
liquid as I can by squeezing it between
two watch glasses.
And I’ll grad the other one out.
I am going to remove it from the hotplate and
I’m just going to cool it a little bit
in this ice.
So now I am going to add about 1 gram of
sodium carbonate, which will convert the
tannins
to water-soluble salts.
Okay, and now I will add the solution into a
separatory funnel, and I will leave behind
the boiling chips so they do not get stuck in the
funnel.
For the extraction then I will use about 10 mL of
dichloromethane and I’ll extract it
three times and then combine the extracts.
This is probably the hardest part is to extract
this without forming an emulsion.
So instead of vigorously shaking it, I am just
going to tip it over a few times.
It looks like it worked pretty good.
I have very good separation, a little bit of
bubbles in between, but nothing to bad.
So now I will just drain off the bottom layer.
So I will add another 10 mL or so.
Okay, and again, I am just going to tip it over.
Okay, I got great separation again.
If I needed to, I could potentially put the stir rod
in there to break up some of the
bubbles.
I am going to drain the bottom layer off.
And I’ll extract it one last time.
Okay, you see I have some there, again there is
probably a little bit more, but I’m just
going to set it aside for now.
So, the solution is a little bit cloudy.
There is a little bit of brown spots, so there is
some impurities there, but for the most
part it looks okay.
So now I will add anhydrous sodium sulfate to
dry the solution to remove any water that
may have come over with the dichloromethane,
or come out with the dichloromethane.
Solution is already looking a lot clearer.
Okay, and I'll just let it sit for a few minutes.
Now that it sat for a few minutes in the
anhydrous sodium sulfate, I'm going to transfer
it to
a crystallization dish so it can evaporate the
fastest.
I will just decant it and try not to get any of the to a small test tube.
sodium sulfate to come over.
Okay, you can see I do have some of it left
I'll add this to the hotplate. behind, not all of it made it, but a decent

I'm also going to rinse this one time. amount made it to the test tube.

This is boiling pretty good, but just to help it boil Okay, now I'm just going to add it an ice-water
a little more, I'm just going to put bath to minimize the solubility and hopefully

in that wood stick. purified caffeine will crash out of it.

I'm just going to keep an eye on it just so I don't After it has been sitting in the ice for about 5
evaporate it all and start heating minutes, I'm going to collect it using the

the crude caffeine directly. Buchner funnel.

Well, I can see it starting to solidify a little bit, so I also have some cold ethanol to help with the
I'm going to remove it from rinse.

the heat. Unfortunately, the vacuum is not working right

now in the building, so I got a modified vacuum
Okay, it looks like it is almost all gone there.
here where I'm going to use this syringe and I'm
So with this remaining amount I'll let it
going to pull it up to create a vacuum
evaporate slowly, or at least without any
to suck the solvent through.
heat directly applied to it.
Okay, so I'm first going to take the ice-cold
There is not a lot of it.
ethanol and wet the filter paper.
The color looks really good though, it is not
Works a little bit anyway, works good enough I
yellow or anything, but if it is yellow
guess.
or if it does look a little cruddy, that should be
Okay, I'll try to collect the crystals as best I can.
taken care of when we do recrystallization.
I got quite a bit that never made it out of the
So I'm going to try to scrape some of this up.
flask.
It doesn't seem to working very well.
I guess I'll add some ethanol to it.
Instead of trying to scratch it up, an easier way
Looks like I most of them out of the test tube.
to transfer this would probably be to
Now I'm just going to transfer it to a little vial.
dissolve it in the recrystallization solvent first.
And there we have it.
Okay, so I'm going to add now 100% ethanol to
it to dissolve it and then transfer it Some recrystallized caffeine from ethanol,
formed some really nice needles.
to a test tube.
heyyyyyy dietrich labs sam here so in
Alright, so I have it re-dissolved in hot ethanol
and now I'm going to transfer this this video i figured i would show you a
little science experiment that I did a high-quality the crystals in the other

while ago a while ago I purchased two container I think are a little bit

ounces of pure caffeine from a chemical prettier but these are still cool I'm

supplier and I dissolved it in water and gonna try and film in a way that really

let some of the water evaporate quite a shows them off I don't know if I'll be

lot of the water and then I poured it able to get a really good shot here see

poured the rest out in order to keep the ooh

crystals that formed pretty because that's actually beautiful okay so it's

sometimes they get all crusty when you basically a fishbowl except with

let it evaporate completely but what was gorgeous caffeine crystals growing in it

really interesting is the way or there's I normally keep something over the top

the shape of the caffeine crystals yeah to keep the dust out but that is some

the caffeine crystals were not like big beautiful caffeine almost like spiky

and bulky they were long and spindly and foliage it's really cool okay let's try

somewhat flexible they're they're really filming it from the top

quite thin it's not as pretty from that angle yeah

they're like little spikes and in one of let's film a little more from the side

the containers they form this sort of that's where it really looks cool it

ball like cluster so a ball like cluster shows off the shape nicely so they can

of sort of well pure caffeine spikes get to focus more ideally it's hard to

sticking out it looks really cool so I know where to get it to focus okay so

figured I'd take a moment to show you that's that container now I said that

how they turned out okay so here are the there was one container where the

two containers this one is the the one crystals sort of shot out from like a

I'm focusing on right now these are the cluster well this is that container I

two containers that I have the one I'm don't know if you can see it very well

focusing on right now is by far the but yeah look at that those are

bigger one but I think the crystals are beautiful caffeine crystals and this is

actually a little less nice or less the caffeine that you have in your
coffee and tea in caffeinated beverages

this is exactly that molecule except

this is in pure form and it's been grown

into these big crystals so to think that

stuff that makes you hyper and wakes you

up in the morning and when you drink

coffee and caffeinated tea and soda with

caffeine in it is actually a white solid

that grows fantastic crystals the famous

caffeine forms crystals like that it's

really cool anyway I thought that was

kind of a cool little experiment that

I'd done a while ago and that it was

worth sharing with you so you know it's

not a terribly long video not a terribly

mathematical video but you know it's

it's a neat little experiment Deitrick

out