EXPERIMENT#4 Conductimetric Titration and Gravimetric Determination of a precipitate 1 Neutralization and Conductivity • The conductivity of a neutralized acid-base mixture is dependent on the salt produced! • If the salt produced is a soluble salt, then the neutralized acid-base mixture will be a good conductor of electricity. Soluble salts produce lots of free moving ions in water! • If the salt produced is an insoluble salt, then the neutralized acid-base mixture will be a poor conductor of electricity. Insoluble salts produce very few free moving ions in water! 2 Neutralization and Conductivity Acid + Base → Water + Salt Lots of free moving ions in the water! H1+ Cl1H1+ Cl1- H1+ H1+ Cl1- Cl1- Cl1- OH1H1+ HOH HOH 1+ H1+ OH1- Na Na1+ Cl1- 1+ Cl1H HOH1OH1OH Na1+ HOH H1+ Na1+ Cl1- OH1Na1+ OH1Na1+ OH1- OH1Na1+ Na1+ 3 Neutralization and Conductivity Acid + Base → Water + Salt Very few free moving ions in the water! 1- SO42- 1+ H H1+ 21+ SO4 H H1+ H1+ H1+ SO4 2- SO42- OH H1+ HOH HOH 2+ H1+ 1- Ba OH H1+ SO42HOH 1OH HOH H1+ OH1OH1- Ba2+ 1- HOH HOH OH H1+ 2+ 1+ H Ba SO4 42BaSO4 BaSO OH1Ba2+ OH1- Ba2+ OH1- OH1- OH1- OH1Ba2+ 4 Neutralization and Conductivity 4) In general, potassium hydroxide is a ______________ conductor of electricity. good Write the equation for the neutralization of potassium hydroxide with hydrochloric acid. 1 KOH(aq) + 1 HCl(aq) → __________________________ 1 K Cl(aq) + 1 HOH(l) ______________________ Compared with potassium hydroxide, how well does the resulting mixture of the neutralization of potassium hydroxide with Hydrochloric acid conduct electricity and why? The resulting mixture conducts as well ___________________________________ because KCl is soluble in water. ___________________________________ 5 Neutralization and Conductivity good 1) In general, sulfuric acid is a ____________ conductor of electricity. Write the equation for the neutralization of sulfuric acid with barium hydroxide. 1 H2SO4(aq) + 1 Ba(OH)2(aq) → __________________________ 1 Ba SO4(s) + 2 HOH(l) ______________________ Compared with sulfuric acid, how well does the resulting mixture of the neutralization of sulfuric acid with barium hydroxide conduct electricity and why? The resulting mixture conducts less well ___________________________________ ___________________________________ because BaSO4 is insoluble in water. 6 Gravimetric Analysis • Gravimetric Analysis – one of the most accurate and precise methods of macro-quantitative analysis. • Analyte selectively converted to an insoluble form. • Measurement of mass of material • Correlate with chemical composition • Why? • Simple • Often required for high precision 7 Gravimetric Analysis • Precipitation Techniques – Add precipitating reagent to sample solution – Reacts with analyte to form insoluble material – Precipitate has known composition or can be converted to known composition • Precipitate handling involves – Quantitative collection (no losses) – Isolation of pure product • Measure mass of precipitate • Calculation of original analyte content (concentration) 8 Gravimetric Analysis • Desirable properties of analytical precipitates: – – – – Readily filtered and purified Low solubility, preventing losses during filtration and washing Stable final form (unreactive) Known composition after drying or ignition • What steps are needed? 1. Preparation of the solution 2. Precipitation 3. Digestion 4. Filtration 5. Washing 6. Drying or igniting 7. Samples dried, triplicate portions weighed 8. Weighing 9. Calculation 9 EXPERIMENT#9 Conductimetric Titration and Gravimetric analysis for Ba(OH)2 • The chemical reaction: Ba(OH)2(aq) + H2SO4(aq) BaSO4(s)+ H2O(l) • Equipment: H2SO4 • • • • • • • • • • Conductivity probe Drop counter Drop counter 250 mL Beaker 50 mL Graduated Cylinder 10 mL pipet Magnetic stirrer and stirring bar Ba(OH)2 Filter paper Filter Funnel Micro-balance Drying Oven Magnetic stirrer Conductivity probe Stirring bar • Chemicals • 0.1 M sulfuric acid, H2SO4, solution • Barium Hydroxide, Ba(OH)2, solution Ba(OH)2 • Distilled Water 10 Conductimetric Titration of Ba(OH)2 by H2SO4 • The chemical reaction: Ba(OH)2(aq) + H2SO4(aq) BaSO4(s)+ H2O(l) • At the equivalence: 𝐞𝐪𝐮𝐢𝐯𝐚𝐥𝐞𝐧𝐜𝐞 𝐧𝐁𝐚(𝐎𝐇)𝟐 = 𝐧𝐇𝟐 𝐒𝐎𝟒 equivalence MBa(OH)2 × VBa(OH)2 = MH2SO4 × VH2SO4 𝐞𝐪𝐮𝐢𝐯𝐚𝐥𝐞𝐧𝐜𝐞 𝐌𝐁𝐚(𝐎𝐇)𝟐 = 𝐌𝐇𝟐 𝐒𝐎𝟒 × 𝐕𝐇𝟐 𝐒𝐎𝟒 𝐕𝐁𝐚(𝐎𝐇)𝟐 • Use the conductimetric curve to 𝐞𝐪𝐮𝐢𝐯𝐚𝐥𝐞𝐧𝐜𝐞 determine 𝐕𝐇𝟐 𝐒𝐎𝟒 : Intersection between the two slopes • Calculate 𝐌𝐁𝐚(𝐎𝐇)𝟐 Volume H2SO4 (mL) 11 Gravimetric Analysis of Ba(OH)2 Ba(OH)2(aq) + H2SO4(aq) BaSO4(s)+ 2 H2O(l) • • • • • Heat the mixture Filtration of white the precipitate Dry the precipitate Weigh precipitate Calculate 𝐌𝐁𝐚(𝐎𝐇)𝟐 • 𝐧𝐁𝐚𝐒𝐎𝟒 = 𝐦𝐁𝐚𝐒𝐎𝟒 𝐌𝐌𝐁𝐚𝐒𝐎𝟒 • Based on the stoichiometry of the reaction: 𝐧𝐁𝐚𝐒𝐎𝟒 = 𝐧𝐁𝐚(𝐎𝐇)𝟐 = 𝐌𝐁𝐚(𝐎𝐇)𝟐 × 𝐕𝐁𝐚(𝐎𝐇)𝟐 𝐌𝐁𝐚(𝐎𝐇)𝟐 𝐦𝐁𝐚𝐒𝐎𝟒 = 𝐌𝐌𝐁𝐚𝐒𝐎𝟒 × 𝐕𝐁𝐚(𝐎𝐇)𝟐 12