Separation by STEAM DISTILLATIONS

							 Separation by
    STEAM
DISTILLATIONS
Set up is similar to
Simple Distillations.
The b.p. is the temp at which the vapor pressure
       equals the atmospheric pressure.
The b.p. (green) would be very high . . .
If insobl, their v.p.’s are added together . . .
Therefore, no need for a thermometer!
Set up by a water
     outlet . . .
 Start setting up
 with a suitable
    ring stand.
  TIGHTEN THE
       ROD
 so your set-up
      doesn’t
    WOBBLE!!
 Place the
 burner on
  the ring
stand next.
  Then, add
the iron ring,
 leaving 2-3
  inches for
  the flame.
  The wire
gauze goes
on top of the
 iron ring.
   Your
 LARGEST
  flask is
   clamped
directly on top
  of the wire
gauze. Leave
NO air space!
  Put your
 mixture into
   the pot
BEFORE you
assemble the
 apparatus.
 The 3-way
   adapter
 (still head)
  is added
atop the RB
    flask.
Use the glass
    stopper
instead of the
 thermometer
   assembly
      The
condenser is
CLAMPED to
    another
  ringstand!
Water enters
 the LOWER
     end.
 An Erlenmeyer
 flask in an Ice
water slurry is the
    receiver.
• DON’T TRY TO
  HOLD IT WITH
  YOUR FINGERS!
• IT WILL BE
  VERY, VERY
  HOT!!
• Try clamping it.
With a good hot
flame, distill the
benzoic acid-pdb
    mixture as
directed in your
   lab manual.
     Conduct the
 “clogged condenser
drill” soon after solid
 begins to collect in
     the receiver.
  Once
 again,
 using a
hot plate
  is an
 option.
At this point you
should have the
     Volatile
 component in
the Erlenmeyer
 flask, and the
   non-volatile
 component on
  the RB flask.
CLAMP the filter flask, and, using
 the thick-walled vacuum tubing,
 collect the volatile component on
        Buchner w/ suction.
• Transfer the non-volatile component
  into a beaker. Cool the contents in an
  ice slurry. Acidify to pH~3 w/ conc.
  HCl, and collect the product on
  Buchner with suction.
 Leave the benzoic acid out to
  dry, but close off the pdb.
 Retain these products for the
next experiment: Extractions.
1)How can you tell when distillation is
    complete? (Zubrick, p. 188 f.)
2) Collect the purified components
     SEPARATELY on Buchner w/ suction.
3) Do NOT leave the volatile component
   open to air-dry.
4) Prepare your Reports and your products
    to turn in at your NEXT LAB.