Preparation of an Iron Complex Introduction In this experiment you will prepare a complex compound of iron; potassium trioxalatoferrate(III), K3Fe(C2O

)3! In this compound each oxalate li"and has two #onds to the iron(III) ion, and hence this compound is an example of a chelate! $ou will aim at o#tainin" the maximum yield of product of the hi"hest purity permitted #y this method! $our final product should #e in the form of #ri"ht "reen crystals, free from dust spec%s, filter paper fi#res, etc! &ac%"round It is of interest to compare the properties of chelated iron(III) ion with that of the normal iron(III) ion! 'he compound will #e prepared #y first preparin" iron(II) oxalate, FeC2O !2(2O, and then oxidi)in" this with hydro"en peroxide, in the presence of potassium oxalate, to con*ert it to the ferric+oxalate ion Fe(C2O )33+

'hus all the iron in the iron(II) ammonium sulphate is con*erted to ferrioxalate, one third of the ferrioxalate #ein" formed from the iron(III) hydroxide! &oth (2O2 and Fe(O()3 are unsta#le to heat! ,otassium trioxalato ferrate(III) is photosensiti*e, i!e! it decomposes when exposed to li"ht, reformin" iron(II) oxalate! Chemicals- 2 . sodium hydroxide, ethanol, ethanedioate (oxalic) acid, /!0 . hydro"en peroxide, iron(II) ammonium sulphate, potassium ethanedioate (oxalate) 'echnician1s note /! sodium ethanedioate (oxalate) cannot #e employed in this experiment! 2! Iron(II) ammonium sulphate should #e fresh and "reen in appearance! 3! .olarity of hydro"en peroxide should #e rou"hly determined #y titration! ,rocedure /! 2issol*e 3!4 " of iron(II) ammonium sulphate, Fe5O !(6( )25O !7(2O in 24 cm3 of warm water! 8dd to this warm solution, with stirrin", 32!4 cm3 of an oxalic acid solution made #y dissol*in" /9 " of the acid in /99 cm3 of water! 2! Cautiously heat the mixture to #oilin", and then allow the yellow "ranular precipitate to settle! 3! 2ecant the supernatant li:uid and wash the precipitate #y stirrin" it with 49 cm3 of hot water! 8llow the precipitate to settle and a"ain decant the clear li:uid! ;epeat with a further 49 cm3 of hot water!

! 5uspend the washed precipitate in a warm solution of 4 " of potassium oxalate in /4 cm3 of water! 8dd slowly from a #urette /2!4 cm3 of /!0 . (2O2, stirrin" continuously and %eepin" the temperature at a#out 9 oC! 6!&! If hydro"en peroxide is added too :uic%ly, the heat li#erated would decompose the peroxide and the iron(II) ion will not #e completely oxidi)ed to iron(III) compound! $our yield of product in the last step reflects how "ood your performance in this experiment! 4! (eat the mixture to #oilin"! 7! 8dd the #oilin" mixture, in one portion, /9 cm3 of a solution of oxalic acid containin" /9 " of the acid in /99 cm3 of water! If the mixture has not turned to a clear "reen, add oxalic acid solution, drop #y drop, until it #ecomes clear (up to 2!4 cm3 may #e re:uired!) 3! 'he solution should now #e "reen due to the presence of the ferrioxalate ion! Filter the hot solution if necessary and add /4 cm3 of ethanol! 0! If any crystal appears, redissol*e them #y warmin" the solution! 5et aside in the dar% to crystalli)e! 8fter crystalli)ation, decant off the supernatant li:uid, wash #y decantation with a little water, and finally with ethanol! <! 5pread the crystals on a fresh filter paper and allow them to dry in the air! =ei"h the dry crystal and record the result! >uestions for discussion /! Iron(II) ammonium sulphate is used as the startin" material rather than the use of iron(II) sulphate! ?xplain! 2! =hat is the name of the product in step (/) + (2)@ 3! ?xplain the use of hot water rather than cold water in step 3! =hat is the purpose of carryin" out step 3@ ! (a) =hy is potassium oxalate solution used rather than water in step @ (#) =hy should the temperature of the mixture #e %ept at a#out 9 oC@ 4! (a) In step 4, what do you o#ser*e@ (#) =rite an e:uation for the reaction in step 4! 7! =rite an e:uation for the reaction in step 7! =hy should excess oxalic acid #e a*oided in step 7@ 3! =hat is the function of the use of ethanol in step 3@ =hy is it effecti*e@ 0! =hy is it necessary to exclude li"ht in step 0@ <! =hy are the crystals finally washed with ethanol@ End