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The document describes the procedure for vacuum filtration. Key steps include: 1) Clamping a filter flask and connecting vacuum tubing to apply suction. 2) Placing a Buchner funnel on top and wetting a filter paper inside to adhere. 3) Pouring the solution through and allowing suction to separate the solid. The document also describes the procedure for determining melting points using a DigiMet apparatus. Key steps include: 1) Setting the starting and stopping temperatures and ramp rate. 2) Loading sample capillaries and packing them. 3) Inserting capillaries into the heating block and beginning the temperature ramp. 4) Observing samples and

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23 views

Flow Chart Exp 2

The document describes the procedure for vacuum filtration. Key steps include: 1) Clamping a filter flask and connecting vacuum tubing to apply suction. 2) Placing a Buchner funnel on top and wetting a filter paper inside to adhere. 3) Pouring the solution through and allowing suction to separate the solid. The document also describes the procedure for determining melting points using a DigiMet apparatus. Key steps include: 1) Setting the starting and stopping temperatures and ramp rate. 2) Loading sample capillaries and packing them. 3) Inserting capillaries into the heating block and beginning the temperature ramp. 4) Observing samples and

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sf444wgt8r
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© © All Rights Reserved
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Set up vacuum filtration

1) Clamp filter flask using the three-prong clamp


2) Connect the vacuum tubing (thick-walled) between the vacuum fixture inside the
fume hood and the side-arm of the flask. Place a rubber adapter in the neck of
the flask to provide a seal for the Buchner funnel.
3) Place the Buchner funnel on top of the vacuum flask. Be careful not to knock
down the assembly as the Buchner funnel is not held tightly until the vacuum is
turned on.
4) Add a filter paper inside the Buchner funnel and wet it with solvent making up the
bulk of the solution filtered. A dry filter paper will not adhere to the Buchner
funnel and solid could escape to the vacuum flask.
5) Turn on the vacuum by turning the yellow dial counter-clockwise until you feel
resistance.
6) Slowly pour the solution through the Buchner funnel. You can swirl the solution
gently to suspend all the solution prior to pouring. Small volumes of solvent can
be used to complete the transfer of the solid, or you can use a spatula to scoop it
out.
7) Once the separation of the liquid from the solid is completed and the solid is
mostly dried, turn off the vacuum by turning the yellow dial clockwise. Remove
the vacuum hose from the filter flask.
8) Transfer your solid to a tared weighing paper or watch glass, scraping gently to
release the solid from the filter paper without ripping the latter.
9) The filter paper is then disposed in the solid waste.

DigiMet

1. Push the START TEMP button and the ↑/2 and ↓/3 buttons to set the starting
temperature for the melting point determination. (It is advised to set this 10 °C
below the initial temperature reported by the literature MP range.)
2. Push the RAMP RATE button and the ↑/2 and ↓/3 buttons to set the temperature
ramp rate (°C/min). It is advised to use a ramp rate of 10 °C/min.
3. Push the STOP TEMP button and the ↑/2 and ↓/3 buttons to set the starting
temperature for the melting point determination. (It is advised to set this 10 °C
above the final temperature reported by the literature MP range.)
4. Push the STOP TEMP button again and the display will show the apparatus’
current heating block temperature. The device is ready to go.
5. After loading the glass capillary (capillaries) with sample(s), insert the capillary
into one of the three “tube tapper” holes located to the front of the TUBE
TAPPER button. Push the TUBE TAPPER button to pack the compound to the
bottom of the capillary. It may take several pressings of the TUBE TAPPER
button in order to pack compound down the tube.
6. Push the START/STOP button to preheat the heating block to the starting
temperature. The PREHEAT LED will be lit.
7. Once the READY LED is lit, the heating block is holding the desired starting
temperature. The glass capillary tube containing the sample (up to three samples
can be run at the same time) are inserted into the heating block found directly
behind the eyepiece monocle.
8. Push the START/STOP button to begin heating the block at the specified ramp
rate. The MELT LED will be lit.
9. During the heating ramp, observe the sample inserted in the heating block using
the eyepiece monocle.
10. During the heating ramp, push any of the 1, ↑/2 or ↓/3 buttons to record and save
the temperature at any point in time during the melting point determination (i.e.
the initial and final temperatures of the MP range). You may record up to 4
temperatures for each of the 3 sample holders.
11. When the COOLING LED is lit, the experiment is finished. To end the experiment
immediately (before the specified stopping temperature); push the START/STOP
button.
12. If data is recorded during the experiment, once it is finished the DATA LED will
be lit. To read back the data collected, simply press the 1, ↑/2 or ↓/3 buttons to
toggle through the recorded temperatures.

Recrystallization
(summarize procedure needed with specific reagents and their respective quantities, as well as
equipment and glassware to use)

Equipments
- Buchner funnel
- Hot plate
- Erlenmeyer flask
- Filter paper
- Vacuum
- Clamp
- Digimet

Method

1. Dissolving the impure solid in the solvent.


■ Heat the recrystallization solvent to boiling (always use an Erlenmeyer
flask). A good rule of thumb for the amount of solvent to use in
recrystallization is around 10 mL per gram of crude product. Use this
estimate as a starting point.
■ Very carefully, using a disposable pipette, transfer some of the boiling
solvent to the Erlenmeyer flask containing the solid to be purified. (It should
be enough solvent to make a slurry with the solid that is being
recrystallized).
■ Heat the solute and solvent solution. Continue to add solvent portion-wise
until all of the solute is dissolved in solution. Be careful not to add too much
solvent.
2. Cooling and crystallizing the pure product.
■ With minimal disturbance, gently remove the hot solution from the hot plate.
■ Once the solution is at room temperature, transfer the flask to an ice bath.
■ If crystals do not begin to form after several minutes, gently scratch the
bottom of the Erlenmeyer flask with a glass rod or scoopula. This is called
“inducing nucleation.”
■ Continue to cool the solution to promote crystallization of the target product.
3. Isolating the pure product.
■ The pure product can be isolated by suction filtration.
■ If required, the pure product can be placed under vacuum to remove all
traces of solvent.

Liquid-Liquid Extraction
(summarize procedure needed with specific reagents and their respective quantities, as well as
equipment and glassware to use)

1. Ensure the stopcock is closed.


2. Place the separatory funnel in a secured ring clamp.
3. Add your mixture to the separatory funnel, then add an equal volume of the
immiscible liquid specified in the experimental procedure. Components will move
to the layer in which they are more soluble in once mixed.
4. Shake vigorously to mix the layers and vent regularly, aiming up and toward the
back of the fume hood. Venting is very important as it releases pressure buildup
and prevents the separatory funnel from exploding.
5. Place the separatory funnel back in the ring clamp and remove the cap in case
pressure buildup is still occurring.
6. The layers are now separated, with the bottom layer being the denser liquid.
Open the stopcock to drain the bottom layer into a flask.
7. Drain the top layer into a separate flask.

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