Chapter 7 Gravimetric Analysis 7-1 Examples of Gravimetric Analysis • Gravimetric Analysis – Mass of product used to calculate quantity of original analyte. • Has been largely replaced by instrumental methods 7-1 Examples of Gravimetric Analysis • T.W. Richards – Early 1900s, measured atomic mass of Ag, Cl, and N to six-figure accuracy. – Formed the basis for accurate atomic mass determination. 7-1 Examples of Gravimetric Analysis • Solubility Rules – Set of rules that determine whether species are soluble in water. – Precipitation allows separation for analysis • Species form insoluble compounds • Dried and weighed 7-1 Examples of Gravimetric Analysis • Combustion Analysis – Samples burned in excess oxygen. Products measured. – Used most often to measure C, H, N, S and halogens. 7-1 Examples of Gravimetric Analysis • Precipitant – Agents that cause precipitation • Precipitation – In chemical reactions, the forming of solids as a result of a chemical reaction. 7-2 Precipitation • Gravimetric Analysis – Particles should be large enough to be collected by filtration. – Colloids (scattered light, eg: milk) • Particles that are ~1 – 500 nm • Small enough to pass through filters Examples of Gravimetric Analysis • Reactions – Precipitation reactions Example: Determination of Cl by precipitation with Ag Ag+ + C1- AgCl Measuring the mass of solid offers moles of AgCl. Conversions and Stoichiometry -> final value. 7-1 Examples of Gravimetric Analysis • A 10.00 mL solution containing Cl- was treated with excess AgNO3 to precipitate 0.4368 g of AgCl (FM 143.321). What was the molarity of Cl- in the unknown? 7-2 Precipitation • Crystal Growth – Two Phases Nucleation Particle Growth • Homogeneous Precipitation – Precipitant generated slowly by a chemical reaction. • Slow precipitation => More particle growth over nucleation • Similar to cooling rates (nucleation and grains) • Easy to filter 7-2 Precipitation • Homogeneous Precipitation – Precipitant generated slowly by a chemical reaction. Example: Formation of Fe(III) by decomposing urea in boiling water to make OH 7-2 Precipitation • Homogeneous Precipitation 2OH reacts with formic acid to produce formate, used to precipitate Fe(III). Box 7-1 Shorthand for Organic Structures • Simple lines and symbols can be used to shorthand complex structures to save time and space on paper. Box 7-1 Shorthand for Organic Structures • Simple lines and symbols can be used to shorthand complex structures to save time and space on paper. Box 7-1 Shorthand for Organic Structures Exercise: Write the chemical formula (such as C4H8O) for each structure below. 7-3 Examples of Gravimetric Calculations • Relating mass of product to mass of reactant. – The piperazine content of an impure commercial material can be determined by precipitating and weighing piperazine diacetate: Common organic precipitating agents
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