Inorganic Synthesis

1
Inorganic Synthesis
HOMO of CO

• 3 weeks
• 2 syntheses
• 1 magnetic susceptibility analysis

2
Which are like yours how do they differ?
Cobalt Syntheses
44 sodium tricarbonatocobaltate(III) 3-hydrate
46 bis-tetraethylammonium tetrachlorocobaltate(II)
Copper Syntheses
8 bisethylenediaminecopper(II) nitrate
10 tetraamminecopper (II) sulfate monohydrate
11 bisethylenediaminecopper(II) diiodocuprate(I)
12 bisacetylacetonatocopper(II)
41 cis-bis glycinato copper (II) monohydrate
Nickel Syntheses
23 hexaamminenickel(II) fluoroborate
24 dinitrotetramminenickel(II)
42 hexamminenickel (II) chloride
43 bis(dimethylglyoximato)nickel(II)
Iron Syntheses
47 tris(acetylacetonate)iron(III)
Variations in a) transition metals - different
of d-electrons b) ligands -
number/geometry/strength(splitting/color)
3
Procedures vary, but for all the following
applies

• DO NOT USE BUNSEN BURNERS!!!!!
• Most solvents (acids, bases, organics) are on
  trays
• Cart by the side bench
• ethylene diamine acac
  (2,4-pentadione, acetyl acetone)
• 30 hydrogen peroxide pH paper
• parafilm P2O5 dessicators
• product vials

4
The balances must never be moved and must be kept
clean!!!
Make sure the bubble is centered in the circle!
Use the analytical balance to weigh the starting
material containing the compound with the metal
(the limiting reactant). Other materials can be
weighed on the top-loading balances.
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Notes on Yield
You will be graded on your yield, so work
precisely. yield is based on the mass of
starting material containing the metal. Ligands
are added in excess. If you have slightly
less/more, it is ok. M XL ?
MLX Carefully follow instructions for filtering
and recrystallization given in your manual to
avoid excess loss of material.
6
Check out items from the stockroom
Request equipment by synthesis number. Return
everything clean at end of day for the next days
section. Check out tubes for paramagnetic
synthesis required for week 2 or week 3 when you
are ready to prep your sample.

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Funnels, funnels, everywhere funnels! Which one
do you use and why?
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Recrystallization
Used to purify product Dissolve product in
minimum amount of hot solvent and then cool
slowly. - too much solvent results in loss of
product Product should crystallize out because
solubility lower at lower temperatures.
Products usually collected by vacuum filtration
w/ Buchner funnel ( filter paper) - choose
appropriate size filter paper - wet filter paper
first with solvent
Recrystallized products usually washed with small
amount of cold solvent to remove layer of
impurities adhering to crystals. - stop suction
and add cold solvent - stir gently and then
reapply suction

• Drying of crystals done either in air, oven, or
  dessicator as described in procedure.
• How do you know it is dry?

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• PLEASE READ LABELS
• 100 ethanol is not 95 ethanol.
• Ammonia (NH3) bottles are labeled as ammonium
  hydroxide, NH4OH. Why?
• Dilute ammonia is 6M and concentrated is 15M.
• Concentrated acetic acid is the same as glacial
  acetic acid.

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Lastly

• Remember to record observations (after each step
  where you observe a change) in your notebook to
  help determine reactions.
• Return WASHED vials for starting materials after
  thoroughly cleaning them (toss the baggies).
• Week 2 - reconvene in class first to discuss
  paramagnetic susceptibility.
• Week 3 - attendance is required, finish
  experiment, begin report.
• Have fun!
• DO NOT USE BUNSEN BURNERS!!!!!

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Week 2 3

• Remember reports are due 2 days after the third
  week of the experiment start working on it this
  week!
• Attendance is required during week 3
• Today start the second synthesis
• Finish the first synthesis
• Paramagnetic susceptibility measurement
• Please work on the wet bench, next to the sink,
  not near the balances.

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Week 2- Paramagnetic Susceptibility
Two MSB-1 balances are located in the instrument
room. Empty tubes from the stockroom to fill
with your sample Instrument room has standard
sample to use for determining constant. Record
the info that is provided and taped onto the
counter.
When you are done, clean mortars pestles and
your borrowed tube before returning to the
stockroom. The vacuum line has a special tubing
to dry your glass tube. The equations,
background information, description of how the
balance works are in your manual, as you know
since youve read it already. The instructor or
lab assistant will help the first students, then
each student must help another, etc.
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Your products

• Turn in products to your days basket
• Label vials with
• Name
• Date
• Compound name/formula
• Mass
• Section

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Cleaning Up

• Unplug all hotplates
• Wash starting materials vials
• Brush out spills inside the balance
• Clean up counter, especially around the balances