Iodometric Determination of Copper

(Experiment 11) INTRODUCTION The object of this analysis is to determine the amount of copper in an ore sample (reported as the mass percentage of Cu) by an "iodometric" titration method. Li e most analytical procedures based on redox chemistry! this experiment involves a lot of steps and some complex reactions that must be fully understood ahead of time. The ore sample is first dissol"ed in hot! concentrated #$% & 'hich oxidi(es Cu! yielding Cu)* in solution. +fter some steps to ma e the solution less acidic! an excess of ,- is added. This reduces Cu)* to Cu* in the form of insoluble Cu- and! more importantly! . . produces -& ('hich is just -) * - ) in solution. . . ) Cu)* * / ) Cu-(s) * -& . The liberated -& is then titrated 'ith a standard sodium thiosulfate ($a )0)%&) solution! . reducing it bac to - . 0tarch is used as an indicator because it forms an intense blue color . 'ith -) ( actually! -& ). The end.point is the disappearance of the blue starch.iodine color. . . -& * ) 0)%&). &* 01%2). The amount of Cu in the ore sample is thus determined by the o"erall stoichiometry of these t'o reactions3 moles Cu)* 4 moles 0)%&).. The same titration procedure! 'ith the starch.iodine indicator! is also used to standardi(e the . $a)0)%&. 5rimary standard ,-%& is pre.treated 'ith an excess of ,- 'hich again yields - & in solution for subse6uent titration 'ith thiosulfate. . . . -%& * 7 - * 2 #* & -& * & #)% . . -& * ) 0)%&). &* 01%2). . Thus! the o"erall stoichiometry for the standardi(ation procedure is that one mole of -%& re6uires 2 moles of 0)%&).. UNKNOWN The "copper ore" un no'n 'ill be a po'dery solid containing Cu in "arious ionic forms! mainly Cu%! along 'ith other oxides that do not interfere in this Cu analysis.

REAGENTS and STANDARD SOLUTIONS Preparation of 0.10 M sodium thiosulfate (Na2S2O !. 8oil /99 mL of :- 'ater for 19.1/ minutes. Cool to room temperature and add 1)./ g $a )0)%&./#)% and ; 9.9/ g $a)C%&. 0tir to dissol"e the salts. Transfer to a clean bottle and store in a dar place. (8oiling the 'ater is necessary to destroy micro.organisms 'hich can metaboli(e the thiosulfate ion. + small amount of $a)C%& is added in order to bring the p# to about <.)

Preparation of standard 0.01 M "#O solution. :ry ; 1.) g of pure ,-%& at 119 =C for about one hour. >eigh (to ? 9.1 mg) ; 1.1 g of ,-%& and 6uantitati"ely transfer it to a /99 mL "olumetric flas . :ilute to the mar 'ith :- 'ater. Preparation of starch indicator solution. 0tarch solutions should be freshly prepared and 'ill be pro"ided by the lab T+. :issol"e ; ) g of "soluble starch" per 199 mL of :- 'ater. 8oil the mixture gently! if necessary! to obtain a clear solution. Standardi$ation of 0.1 M sodium thiosulfate (Na 2S2O !. 5ipet four /9.99 mL ali6uots of the standard ,-%& solution into )/9 mL conical flas s. 5roceed 'ith each flas to completion of the titration before starting the next one. (#ere the concern is to a"oid error . due to air oxidation of the - ion.) +dd ; ) g of ,- and stir to dissol"e. +dd ; ) mL of 2 @ #Cl and titrate at once 'ith thiosulfate until the solution becomes pale yello'. Then add ; ) mL of starch indicator and titrate until the blue color disappears. (-f the starch indicator is . added too early! the -& tends to form a inetically stable complex 'ith starch from 'hich the . -& is released too slo'ly! resulting in endpoint detection problems.) Aepeat the titration 'ith each of the other ,-% & samples. :etermine the molarity of $a )0)%& to four significant figures! paying careful attention to the o"erall stoichiometry.

PROCEDURE -- Anal !i! of C" Ore Un#no$n 1. :ry ; &./ g un no'n at 119 =C for one hour. >eigh (to ? 9.1 mg) three 1.g samples and transfer each to a )/9 mL bea er. 5roceed separately 'ith each sample as follo's. ). +dd / mL of concentrated #$%& (%aution3 Handle concentrated acids carefully in the fume hood!) and heat belo' boiling in the hood to dissol"e the un no'n. Cool and add 19 mL of concentrated #)0%1 and heat until yello' 0%& gas is e"ol"ed! then cool. Cautiously add &9 mL of :- 'ater! boil the solution for 1.) minutes! then cool. +dd concentrated ammonia drop'ise until the deep blue color of the Cu($#&)1)* complex ion appears. Then add & @ #)0%1 to ma e the deep blue color just disappear. Binally! add ) mL of 7/C phosphoric acid and cool to room temperature. (This procedure adjusts the p# to a proper range.) &. Each of the Cu)* solutions should be completely analy(ed before the next one. +dd ; 1 g of ,- (to precipitate Cu-) and titrate 'ith standard $a )0)%& until the solution is pale yello'. +dd ; ) mL of starch solution and continue the titration to a faint blue color. +dd ; ) g of ,0C$! stir for about &9 seconds! and then finish the titration to the . disappearance of the blue color. (,0C$ is used because -) and -& tend to adsorb on the surface of solid Cu-! thus becoming less a"ailable for reduction by the thiosulfate. Thus! iodometric titrations in"ol"ing reduced copper tend to yield lo' results unless the . adsorbed iodine is liberated by adding 0C$ 'hich competes 'ith the adsorbed iodine on the surface of Cu- particles.) 1. :etermine the percent Cu for each trial. Aeport the indi"idual results! the mean! and the standard de"iation.