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All equipments like burette, beaker, pipette & volumetric flask should be washed properly with distilled water A burette should be as uniformly cylindrical as possible and the divisions etched shall correspond closely to actual contents The process of filling the pipette should be accurate to avoid excess addition of solutions Do not blow through the pipette to expel the last drop of solution from it
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Index finger should be used for pipetting the solution The flask should be shaking well after adding the indicator and also with addition of each drop of solution from burette
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Towards the end, add the solution drop by drop and swirl to avoid errors
Gravimetric Analysis
Method of quantitative analysis in which any element or compound gets precipitated from its solution by using suitable reagent The precipitate can be collected by filtration, is washed and dried to remove moisture and other impurities and weighed
The mass of the precipitate gives the amount of analyte in the original sample
Electrogravimetry
Thermogravimetry
Principal
Reagent + Analyte
Solid Product
(collect and measure mass)
Desired Properties of Solid Product Should be very insoluble Easily filterable (i.e., large crystals) Very Pure Known and constant composition
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Precipitates should be obtained in a granular or Crystalline form For obtaining a granular precipitate a) The solution must be dilute b) It must contain a little hydrochloric acid c) It must be heated to the boiling point d) The reagent (barium chloride) must be hot and dilute and must be added slowly
Filter paper when folded must be somewhat smaller than the funnel
If possible, liquids should be filtered hot Filter paper can be chemically attacked by some solutions (such as conc. acid or base), and may tear during the filtration of large volumes of solution For precipitates like Al or chromic hydroxides or ZnS filter pump shall be used
Use of Crucibles
They should not undergo any permanent change during the ignition
Platinum crucibles can be employed at high temperatures but possibility of reduction with metals
Silica crucibles are less likely to crack on heating than porcelain crucibles ~ smaller coefficient of expansion Ignition of substances not requiring too high a temperature may be made in porcelain or silica crucibles Fe, Ni or Ag crucibles are used in special cases
Operation of Crucibles
Crucibles after ignition are allowed to cool in a desiccator before weighing Crucibles when hot should be allowed to cool in air until when held near the skin little heat is noticeable
General Precautions
Number of transfers of liquids should be as small as possible to avoid the risk of slight losses
Adjustment of balance
Grinding of sample Calibration of glass measuring device
Grease may be removed by prolonged treatment with chromic acid solution (a mixture of K2Cr2O7 solution and conc. H2SO4) A pipette or burette is clean if there is no formation of drops on the surface of the glass after the liquid is run out
References
Douglas, A.S. and Donald, M.W., 1976. Fundamentals of Analytical Chemistry. USA,804pp Henry, P.T., 2004. An Introductory Course of Quantitative Chemical Analysis with Explanatory. Project Gutenberg, 1213pp Welch, P.S., 2003. Limnological Methods. Narendra Publishing House, New Delhi, 1999pp Greenfield, H., 2003. Food Composition Data, Production Management and Use. FAO
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