A.

SCHEMATIC DIAGRAM OF PROCEDURE

1. Preparation of the metal complexes
a. K3[Al(C2O4)3]・3H2O

0.5 g KOH (in 50 mL beaker)

dissolve 3.5 mL H2O

0.09 g of 1x1 cm pieces of Al foil

cover

decant

residue supernatant

cover with a paper and label place into a new beaker

3.25 g oxalic acid dihydrate

heat mixture to boiling w/

occasional stirring

0. 5 g oxalic acid dihydrate

*if necessary until a clear

colorless solution is obtained

allow solution to cool

3.5 mL ethanol

filter white product

residue filtrate

wash w/ 1:1 (v/v) etOH-H2O sol’n dispose in alcohol

waste bottle
wash w/ ethanol
air-dry

K3[Al(C2O4)3]・3H2O (white crystals)

1.5423 g
b. K3[Cr(C2O4)3]・3H2O

0.75 g oxalic acid dihydrate + 1.70 mL warm water (in 50 mL beaker)

0.25 g K2Cr2O7 in portions

heat solution to boiling when reaction has subsided

0.33 g K2C2O4
H2O
cool to room temperature when the oxalate
has dissolved

0.70 mL ethanol (dropwise)

cool

filter

filtrate residue: blue-green crystals

dispose in waste wash w/ 1:1 (v/v) etOH-

bottles for alcohol H2O sol’n

wash w/ ethanol

air dry

K3[Cr(C2O4)3]・3H2O
0.4142 g
c. K3[Fe(C2O4)3]・3H2O

2 g K2C2O4 in 2.5 mL hot water (in 50 mL beaker)

0.80 mL of 0.6 g/mL FeCl3 aqueous sol’n

(in ice for 30 minutes)

induce crystallization by scratching the walls of the

beaker if no crystal appears
decant mother liquor

supernatant residue: green crystals

dispose in waste bottles redissolve in 3.5 mL warm

for halogenated wastes water

cool in ice
filter

residue: green crystals filtrate

dispose in waste bottles for
wash w/ 1:1 (v/v) etOH-H2O sol’n halogenated wastes

wash w/ ethanol

air dry

K3[Fe(C2O4)3]・3H2O
1.4537 g
d. K3[Co(C2O4)3]・3.5H2O
1.03 g H2C2O4 2H2O + 3.07 g K2C2O4 H2O in 20 mL
boiling water (in 250 mL beaker)

1.0 g CoCO3 (in small portions)

allow to cool to about 35oC (place in cold

water bath if necessary)
6.0 g PbO2

2 mL 1:1 sol’n of glacial acetic

acid-water (dropwise over
about 10 minutes)

filter

filtrate residue: unreacted PbO2

20 mL ethanol (dropwise, using buret) dispose by wrapping

in a paper and label
filter

filtrate residue: green crystals

dispose in waste
dissolve in 20 mL water while slowly
bottle for alcohol
adding 23.2 mL ethanol w/ stirring

air dry

K3[Co(C2O4)3]・3.5H2O
4.2318 g
2. Study of some properties of the tris(oxalate)metallates
A. Magnetochemical studies

Procedure for the operation of the magnetic susceptibility balance:

a. Calibration
a.1. Turn the range knob to the 1x scale and allow 10 minutes for the apparatus to warm up.
a.2. Determine the mass of the empty sample tube on the analytical balance.
a.3. Adjust the zero knob until the display reads 000.
a.4. Place the empty sample tube into the tube guide and take the reading R.
a.5. Pack the sample tube with the calibrant. Solid samples are first ground to a very fine
powder and then packed up into the tube by repeated tapping on a wooden surface (fill in
1 cm portions).
a.6. Determine the sample mass (in grams) using the analytical balance and measure the
length of the sample in tube in centimeters.
a.7. Measure the temperature (oC) of the air near the balance.
a.8. Place the packed sample tube into the tube guide and take the reading R. If the display
goes off scale, turn the range knob to 10x scale, re-zero, and multiply the reading by 10.
a.9. Tip out the powder from the tube, repack, reweigh, measure the length, and remeasure
R to eliminate packing errors.

b. Measurement of Xg for compound:

Use the same procedure that was done for the calibrant.

B. Infrared spectroscopy

Prepare mulls of the compounds with Nujol mineral oil and obtain the IR spectra.