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Lecture 10. Analytical Chemistry What Is Analytical Chemistry ?

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Lecture 10. Analytical Chemistry What Is Analytical Chemistry ? 5/5/2019 What is Analytical Chemistry ? It deals with: Lecture 10. • separation Analytical Chemistry • identification • determination of components in a sample. Basic concepts It includes coverage of chemical equilibrium and statistical treatment of data. It encompasses any type of tests that provide information relating to the chemical composition of a sample. 1 2 • Analytical chemistry is divided into two areas of analysis: • The substance to be analyzed within a sample • Qualitative – recognizes the particles which are present in a sample. is known as an analyte, whereas the substances which may cause incorrect or • Quantitative – identifies how much of inaccurate results are known as chemical particles is present in a sample. interferents. 3 4 1 5/5/2019 Qualitative analysis is used to separate an analyte from interferents existing in a sample and detect the previous one. It gives negative, positive, or yes/no types of data. Qualitative analysis It informs whether or not the analyte is present in a sample. 5 6 Examples of qualitative analysis 7 8 2 5/5/2019 Analysis of an inorganic sample The classical procedure for systematic analysis of an inorganic sample consists of several parts: preliminary tests (heating, solubility in water, appearance of moisture) more complicated tests e.g. introducing the sample into a flame and noting the colour produced; determination of anionic or cationic constituents of 9 solute dissolved in water 10 Flame test Sodium Bright yellow (intense, persistent) Potassium Pale violet (slight, fleeting) Solutions of ions, when mixed with concentrated Calcium Brick red (medium, fleeting) HCl and heated on a nickel/chromium wire in a flame, cause the flame to change to a colour Strontium Crimson (medium) characteristic of the element. Visible colours occur Barium Light green (slight) with the following ions: Lead Pale bluish (slight, fleeting) Copper Green or blue (medium, persistent) 11 12 3 5/5/2019 Flame test as qualitative analysis of cations A B C 13 14 Physical appearance of inorganic salts Salt Colour MnO, MnO2, FeO, CuO, Co3O4, + + 2+ 1 Ni2O3; sulphides of Ag , Cu , Cu , Black Fe2+, Co2+, Pb2+, Hg2+ 2 Hydrated Cu2+ salts Blue 3 HgO, HgI2, Pb3O4 Red 4 Cr3+, Ni2+, hydrated Fe2+ salts green 5 Hydrated Mn2+ salts Light Pink 6 K2O, K2Cr2O7, Sb2S3, ferricyanides Orange 7 Hydrated Co2+ salts Reddish Pink Chromates, AgBr, As S , AgI, PbI , 8 2 3 2 Yellow CdS 9 CdO, Fe O , PbO , CuCrO Dark brown 15 2 3 2 4 16 4 5/5/2019 Determination of cation or anion The procedure is based on treating the solution with a succession of reagents which are specified to a certain group of constituents. The groups are then treated successively with reagents that divide a large group into subgroups or separate the constituents singly. Portions of the material are dissolved separately, and different procedures are used for each to detect the cationic and anionic constituents. 17 18 Analysis of organic compounds The organic nature of a compound is generally indicated by its behaviour on being heated in the air. Solids usually melt, then burn with either a smoky or non- smoky flame, in some instances leaving a black residue of carbon. The following elements are usually present in these compounds: carbon, hydrogen, oxygen, nitrogen, sulfur, occasionally, phosphorus, halogens, and some metals. Specific tests are available for each of the individual Quantitative analysis elements. 19 20 5 5/5/2019 • It determines number of moles or mass of particular substance in a sample. Examples of quantitative analysis 21 22 • Quantitative data are inherently normally expressed in a numerical format: the sign (negative or positive) the magnitude. Both give the meaningful information. 23 24 6 5/5/2019 Methods used in quantitative analysis involve: . classical methods gravimetric, volumetric, Scale of operations for analytical methods 25 26 . Instrumental methods Electroanalytical (potentiometry, conductometry) Spectroscopic (UV-VIS, IR, AAS, FES) Mass spectrometry Methods involving radioactivity measurement Classical methods of quantitative analysis Methods which involve both separation and quantitative analysis (chromatography, electrophoresis) Other 27 28 7 5/5/2019 Procedure of gravimetric analysis: Weigh the sample to be analyzed Dissolve the sample in a suitable solvent, e g, water Add an excess of the precipitating reagent to precipitate the Gravimetric analysis (gravimetry) is the quantitative analyte Filter the mixture to separate the precipitate from the solution isolation of a substance by precipitation and weighing of the Wash the precipitate to remove any impurities Dry the precipitate by heating to remove water precipitate. Cool the precipitate in a desiccator to prevent the precipitate absorbing moisture from the air Weigh the cooled precipitate Repeat the drying and weighing process until a constant mass for the precipitate is achieved 29 30 Examples of gravimetric calculations Gravimetric analysis yields more accurate data about the Calculate the mass of analyte in the sample. composition of a sample than volumetric analysis does. General calculation of the percent by mass of analyte in a sample: However, the first one takes more time to perform in the . Write the balanced chemical equation for the precipitation laboratory. Volumetric analysis in the other side doesn't reaction. E.g. take that much time and the results that we obtain are in aA + bB → cC the most cases satisfactory. 31 32 8 5/5/2019 Calculation – working example When an sample of impure potassium chloride (0.4500g) was dissolved in water and treated with an excess of silver nitrate. 0.8402 g of dry silver chloride precipitate was obtained. Calculate the percentage KCl in the original sample. 33 34 KCl (aq)+ AgNO3(aq)→AgCl(S) + KNO3(aq) Molecular mass of AgCl =142.5 g/mol So the same number of moles of KCl reacted = -3 Molecular mass of KCl = 74.5 g/mol 5.9 x 10 moles Mass of KCl = 74.5 g/mol x 5.9 x 10-3 moles = 0.4396 g 0.8402 푔 -3 Number of moles of AgCl = 푔 = 5.9 x 10 moles 142.5 0.4396 푔 푚표푙 % of KCl = ∙ 100% = 97.7% 0.4500 푔 Ratio between KCl and AgCl from balanced reaction is 1:1 35 36 9 5/5/2019 Quiz Sources of Error: If 20.0 mL of 0.600 M BaCl2 reacts with 25.0 mL of 0.500 Reason of error result comparing with M H2SO4, the expected mass of BaSO4 produced is ... real status Incomplete precipitation too low percentage of analyte Incomplete drying of too high percentage of sample analyte Contamination of too high percentage of precipitate with other analyte ions 37 38 Quiz There are two main areas of application for gravimetric In a particular gravimetric analysis, the precipitate of methods: barium sulfate was balanced before it was completely dried. The likely impact of this error on the calculated 1. Analysis of standards to be used for the testing and result is ... calibration of instrumental techniques. 1. a higher result than the correct value. 2. Analysis requiring high accuracy, although the time 2. minimal, because the calculation assumes a hydrated sample is produced. consuming nature of gravimetry limits this application to small numbers of determinations. 3. minimal, because the mass of water is likely to be very low. 4. a lower result than the correct value. 39 40 10 5/5/2019 Volumetric analysis (volumetry) can be simply a titration based on: a neutralization reactions between acid and base a precipitation reaction in which insoluble precipitate is formed (argentometry) complexation – reaction between metal ions and standard solution in which complex compounds are formed (titrant Volumetry e.g.EDTA- ethylene diamine tetra acetic acid). redox- reaction between oxidizing agent and reducing agent. Volumetric analysis is linked with instrumental determination of equivalent point. 41 42 Rules of thumbs for successful volumetric analysis Application of volumetric analysis .The titrant should either be a standard or be standardized. Volumetry analyses: .The reaction should proceed to a stable and well defined equivalence point. 1. wastewater e.g. measure ammonia levels in .The equivalence point must be able to be detected. combination with other reactants to quantify other .The titrant’s and sample’s volume or mass must be accurately known. chemicals present. .The reaction must proceed by a definite chemistry. 2. food products - help determine their nutritional .The reaction should be nearly complete at the equivalence point. implications.e.g. acidity of the orange juice In other words, chemical equilibrium favours products. 3. improve wine production by measuring its acidity .The reaction rate should be fast enough to be practical. 4. pharmaceutical industry to ensure quality control or to make the process more efficient. 43 44 11 5/5/2019 Quiz . It’s true or false. • A volume of 20 cm3 of sodium hydroxide is Standards is the reagent solution of known neutralized exactly by 40 cm3 of 2 M conc. which is used to completely react with hydrochloric acid. What is the molarity of the target analyte sodium hydroxide? In volumetric analysis the volume of a reagent of known conc. needed to completely react with the target analyte is measured. 45 46 • Instrumental Methods involve analytical Instrumental analysis measurements of some sample properties (conductivity, electrode potential, light absorption or emission, mass-to-charge ratio, fluorescence etc.). These measurements are made using instrumentation (equipment). 47 48 12 5/5/2019 Applications of Instrumental Methods 1. Bioanalytical: biological molecules and/or biological matrices (e.g., proteins, amino acids, blood, urine) 2. Environmental: pesticides, pollution, air, water, soil 3. Material science: polymers, characterization of new materials 4. Forensic science (application of science to the law): body fluids, DNA, gun shot residue, hair, fibers, elemental analysis, drugs, alcohols, Block diagram of an instrumental measurement poisoning, fingerprints, etc.
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