Naomi Bryner Experiment 3: Analysis of a Mixture of Carbonate and Bicarbonate Introduction: This lab is designed to exercise the technique of titration. Standards will be made using serial dilutions. Data collected will determine the amount of carbonate and bicarbonate via indirect and direct titration. Procedure: One liter of 0.1 M HCL and 0.5 L of 0.1 M NaOH were prepared. NaOH solution was standardized using KHP (x 3) and HCL solution was standardized using standardized NaOH solution (x 3). Unknown C (2.2141 g) was diluted with degassed H2O. 25.00 mL unknown solution was titrated using HCl solution, with bromocresol green as indicator (x 3). BaCl2 was precipitated using 25.00 mL unknown solution, 50.00 mL standardized NaOH solution, and 10% BaCl2. This was immediately titrated using standardized HCl solution with phenolphthalein indicator. Reactions: HCO3- + H+ → H2CO3 CO32- + 2 H+ → H2CO3 HCO3- + OH- → CO32- + H2O Ba2+ + CO32- → BaCO3 Ba3+ + 2 OH- → Ba(OH)2 Data: Standardization of NaOH Trial 1 Trial 2 Trial 3 Average KHP (g) 0.5141 0.5127 0.5127 0.5132 Volume (L) 0.02640 0.02680 0.02661 0.07981 Molarity (M) 0.095355 0.093676 0.094345 0.093857 Volume NaOH (L) 0.01058 0.01063 0.01065 0.01062 Volume HCl (L) 0.010 0.010 0.010 0.010 Molarity HCl 0.099301 0.099770 0.999577 0.099676 Standardization of HCl Trial 1 Trial 3 Trial 3 Average Unknown titrated with HCL Trial 1 Trial 2 Trial 3 Volume HCl (L) 0.02845 0.02840 0.02838 Unknown and NaOH titrated with HCl Volume HCl (L) Trial 1 0.02542 Trial 2 0.02570 Trial 3 0.02555 Mass NaOH used: 2.0294 g (500 mL) Mass Unknown C used: 2.2141 g (250 mL) Volume unknown solvent (L) 0.025 0.025 0.025 Volume NaOH (L) 0.050 0.050 0.050 Volume unknown solvent (L) 0.025 0.025 0.025 Calculations: in lab How much KHP for 25 mL 0.1 M NaOH? 0.1 molNaOH 1 LNaOH × 0.025 LNaOH molNaOH 1 mol × 1 mol KHP × NaOH 204.2212 g = 1 molKHP 0.51 g KHP Mass NaOH for dilution 39.995 g [(0.1 MNaOH) (0.5 LNaOH)]× 1 mol NaOH = 1.99975 gNaOH NaOH Dilution of HCl 0.1M×1 L = 16.67 mL 6M post-lab Molarity of NaOH (mass of KHP × 1 mol KHP 1 mol NaOH × ) molar mass KHP 1 mol KHP 1 mol (0.5141KHP g × 204.2212KHP g × KHP 1 molNaOH 1molKHP ÷ Volume NaOH = Molarity NaOH ) ÷ 0.02640 L = 0.095355 M Molarity of HCl MNaOH VNaOH = MHCl VHCl (0.093857 M) (0.01058 L) = (MHCl) (0.010 L) -> MHCl= 0.099301 M Total moles carbonate and bicarbonate MHCl VHCl = moleπ π»2 πΆπ3 +πΆπ3 (0.099676 M) (0.02845 L) = 0.0028308 moleπ π»2 πΆπ3 +πΆπ3 Initial moles NaOH MNaOH VNaOH = molesNaOH (0.093857 M) (0.050 L) = 0.00469285 molesNaOH Excess Moles NaOH 1 πππ MHCl VHCl ( 1 πππππππ» ) = molesNaOH (initial) π»πΆπ 1 πππππππ» ) 1 ππππ»πΆπ (0.099676 M) (0.02542 L ) ( = 0.0025338 molesNaOH (excess) Moles HCO3(Molesinitial NaOH – molesexcess NaOH) × 1 ππππ»πΆπ3− 1 πππππππ» = moles HCO3- (0.00469285 molesNaOH - 0.0025338 molesNaOH (excess)) = 0.0025474 moles HCO3Moles CO3-2 moleπ π»πΆπ3 −+πΆπ3 2− – moles HCO3- = moleπ πΆπ3 2− 0.0028308 moleπ π»2 πΆπ3 +πΆπ3 - 0.0021455 moles HCO3- = 0.0006853 moleπ πΆπ3 2− Relative Percent HCO3- moles HCO3- MolarMassHCO3- (MassUnknown-1) (100%) = Relative Percent π (0.0021455 moles HCO3-)(61.058 πππ)(2.2345 g)-1(100%) = 6.96% Relative Percent CO32moleπ πΆπ3 2− - MolarMasπ πΆπ3 2− - (MassUnknown-1) (100%) = Relative Percent (0.0006846 moleπ πΆπ3 2− )(60.008 Calculated Data Trial 1 2 3 Average Standard deviation π ) πππ Moles HCO30.0025474 0.0021312 0.0025617 0.0024134 0.000221 (2.2345 g)-1 (100%) = 1.84% % HCO36.96 5.82 7.00 6.59 0.670037 Moles CO320.0006853 0.0006996 0.0002671 0.0005507 0.000246 % CO321.84 1.88 0.72 1.48 0.65848 Conclusions: All titrations were performed by one person to minimize error, which worked well as seen by the standard deviation of the moles of HCO3-. Unknown C had an average composition of 6.59% HCO3- and 1.48% CO32-. These compositions are likely false due to a high standard deviation of percent composition. Post-Lab Questions: 1. A primary standard is a very pure and can be used to determine the concentrations of subsequent solutions. 2. A solution that is prepared using a primary standard and is used for a specific analysis. 3. An indirect titration is usually the first titration performed. It is fast and inaccurate, and yields an approximation of the real amount of titrant needed. 4. A titrant is the reagent solution added to the analyte for titration.