Chemistry Labs

Problem 1

A 0.4062 g alloy sample containing tin and lead is dissolved in hot HCl\ce{HCl}/HNOX3\ce{HNO3} (Pb → Pb(II), Sn → Sn(IV)); on cooling a precipitate of tin compounds and a lead compound appears. 25.00 cm325.00\ \mathrm{cm^3} of 0.2000 M NaX2HX2EDTA\ce{Na2H2EDTA} is added (the precipitate dissolves) and the solution is diluted to 250.0 cm3250.0\ \mathrm{cm^3}. A 25.00 cm325.00\ \mathrm{cm^3} aliquot, buffered at pH 6 with hexamine and Xylenol Orange indicator, is titrated with standard 0.009970 M Pb(NOX3)X2\ce{Pb(NO3)2}: the colour changes yellow→red at 24.05 cm324.05\ \mathrm{cm^3}. Then 2.0 g of solid NaF\ce{NaF} is added — the solution returns to yellow — and titration resumes to a second endpoint at 15.00 cm315.00\ \mathrm{cm^3}. (FX−\ce{F^-} binds SnXIV\ce{Sn^{IV}} strongly but not Pb(II) at pH 6.) (1.1) What lead compound precipitates in step 2? (1.3–1.8) Give the roles of hexamine, Xylenol Orange and NaF\ce{NaF}, and the key ionic equations of the two titrations. (1.10) Calculate the weight percentages of Sn and Pb in the alloy.
Step 1 of 4: Precipitate and its dissolution
PbClX2(s);PbClX2(s)+HX2YX2−→PbYX2−+2 HX++2 ClX−\ce{PbCl2(s)};\qquad \ce{PbCl2(s) + H2Y^{2-} -> PbY^{2-} + 2H+ + 2Cl^-}
Analysis

The sparingly soluble lead compound is PbClX2\ce{PbCl2} (or a hydroxo species); excess EDTA dissolves it because PbYX2−\ce{PbY^{2-}} is a very stable complex even at pH 6. Hexamine is the pH buffer, Xylenol Orange the metallochromic indicator (free: yellow; Pb–XO complex: red).