CHEM 297 INTERMEDIATE CHEMISTRY II LABORATORY

WEEKS OF FEBRUARY 21 AND 28

INORGANIC COMPLEX SYNTHESIS AND ANALYSIS
TRIS-(2,-PENTANDIONATO! MANGANESE (III!
M"(C#H7O2!$
SYNTHETIC PROCEDURE
M"C%2 & 2CH$COCH2COCH$ & 2N'CH$CO2 M"(C#H7O2!2 & 2N'C% & 2CH$CO2H
M"(C#H7O2!2 & KM"O & 7CH$COCH2COCH$ & CH$CO2H #M"(C#H7O2!$ & KCH$CO2 & H2(
Dissolve 2.6 g of manganese (II) chloride tetrahydrate and 8.8 g of sodium acetate trihydrate in 100 mL of
water. o this solution add 10.0 g of 2!"#$entanedione (acetylacetone). he add slowly! with stirring! to
the resulting mi%ture! a solution of 0.&2 g of $otassium $ermanganate in 2& mL of water. 'fter stirring for
a few minutes! a solution of 6.8 g of sodium acetate trihydrate in 2& mL of water is added in small amounts!
with stirring. he mi%ture is heated on a hot $late for a(out 10 minutes and cooled to room tem$erature
and the dar) solid is vacuum filtered. he $roduct is washed with water and dried in vacuo over
anhydrous calcium sulfate. he dried com$le% is dissolved in 10 mL of warm (en*ene! the solution
filtered! and the com$le% re$reci$itated (y cooling the solution and adding +, mL of $etroleum ether.
CAUTION) (en*ene is a )nown carcinogen. Do the recrystalli*ation in the hood. -a)e sure you don.t
inhale any (en*ene fumes or s$ill any (en*ene. he recrystalli*ed material is dried at room tem$erature in
vacuo over anhydrous calcium sulfate.
ANALYSIS
1* M'"+'",-, '- .,/0'"+'"'1, (M"O
2-
!
/eigh out a sam$le of the com$ound in the range of 0.+&00 g and $lace it in a tall form (ea)er. Do all the
following in the fume hood. Dissolve the sam$le in several mL of concentrated 0212". 0eat the mi%ture
on a hot $late until the fumes of 12+ are 3ust detected. CAUTION4 0212" is a very strong acid. 12+
fumes should not (e inhaled. Let the mi%ture cool and then add with e%treme caution & mL of concentrated
052+. his ste$ is $otentially dangerous so ta)e ade6uate $recautions against s$attering or s$illing.
7va$orate the mi%ture slowly to dryness and avoid charring the organic material that may remain.
Dissolve the residue in 10 mL of 0.1 - 052+ and dilute to &00 mL total volume (volumetric flas)). Do all
the a(ove in the hood.
8lace two se$arate & mL $ortions of your 3ust $re$ared -n
29
solution in individual "00 mL (ea)ers. 'dd
20 mL of concentrated 052+! 2 -l of concentrated 0212"! & mL of concentrated (8&:) 0+82"! and several
glass (eads to reduce (um$ing. 0eat the solutions until they have almost reached the (oiling $oint and
then add a$$ro%imately 0.& g of $otassium $eriodate and (oil the resultant solution. he characteristic
$in)#$ur$le color of $ermanganate should develo$ within three minutes of the start of (oiling if -n is
$resent; however! continue to heat for an additional & minutes to insure com$lete reaction.
he solutions are allowed to cool to room tem$erature and then 6uantitatively transferred to individual 100#
mL volumetric flas)s. -a)e u$ each sam$le to 100 mL and then determine the a(sor(ance at &2& nm.
Determine the concentration of your two solutions (y using a cali(ration curve (see (elow). a)e the
average concentration.
<ali(ration curve # 2(tain a stoc) solution of =-n2" whose concentration is in the range of 0.020 - and
has (een accurately determined. >se this solution to $re$are the following standard solutions4
1. Dilute 10 mL to 1000 mL. his gives a solution of a$$ro%imately 2 % 10
#"
- in =-n2".
2. Dilute &0 mL of solution 1 to &00 mL. his gives a solution of a$$ro%imately 2 % 10
#&
- in =-n2".
+. Dilute &0 mL of solution 1 to 100 mL (a$$ro%. 1 % 10
#"
-)
". Dilute +0 mL of solution 1 to 100 mL (a$$ro%. & % 10
#&
-)
<alculate the millimoles of -n in your original solution! convert to grams of -n and calculate the : -n in
your sam$le.
2* O/+'"23 %2+'"4
2(tain the I? s$ectra of your com$le%. 'ssign the ma3or a(sor$tions in the s$ectrum to the a$$ro$riate
(ond vi(rations.