Chapter 2 Experimental techniques in chemistry Filtration:Definition:The separation of a liquid from a solid by a porous medium (filter paper or filter mat)

is called filtration. Explanation:It is a separating technique having large number of applications in the field of chemistry. For this purpose porous media is required having small pores. The separation is obtained by passing the mixture through a porous medium. The liquid in the mixture passes through the medium and the solid particles are retained on the surface of the medium, because solid particles can not pass through the medium. Reason:The reason in this phenomenon is that the liquid particles have no definite shape and can change their shape to pass through the pores but solids having the definite shape can not change their shape and therefore can not pass through the medium which result in their retaining on the surface of the medium. Applications:It has so many applications in the laboratory some of which are as under:1. The filtration is a basic process in the formation of crystals of substances. 2. It helps in purifications of water. This porous media can be of two types:1. Filter paper and Filter mat. 2. Sintered glass crucible and Gooch crucible. Filter paper:It is made up of cellulose also containing little ash in case qualitative filter paper and the space of the cellulose fibers form the matrix of pores. Filter mat:It is made of pure asbestos having pores in it. Sintered glass crucible:It is made of fibers of glass and amorphous (i.e. randomly organized on the microscopic level) disk of solid glass that are arrange randomly having pores between them. Gooch crucible:They are made usually from porcelain clay, but platinum and silica made crucibles are also available and are in the use of the chemist. Qualitative and quantitative purpose:Qualitative purpose means separation of solid or precipitate from the soluble ones only. Where quantitative purpose means separation of solid or precipitate from the soluble ones with mass measurement also; Whenever the quantitative analysis is to be performed on the solid that is separated from the liquid through liquid, then the filtration is performed with the sintered glass crucible. Requirements for quantitative analysis:There are two important requirements for the quantitative analysis which are as follows; 1. The filtration of the mixture should be quantitative and it should be performed by the sintered glass crucible so that all the solid particles in the mixture must be trapped by the medium. 2. Then the solid particles should be given temperature either by oven or any other source so that the liquid traces present should evaporate leaving the pure liquid crystals. After drying the solid particles are ready to weight. Choice of the medium:The medium is chosen for the filtration after seeing nature of solids particles and some of the other factors. Filter paper:Made of:It is cellulose made material and contains little ash when the filter paper is qualitative. The ash should not exceed 0.0001g. It is available in different sizes. Use:It is used in separation of mixture especially suitable medium for separation of gelatinous precipitates. Applying of filter paper:It is applied in the glass or Teflon funnel. Applying method:1. The filter paper is folded properly and after moisting it is fitted in the glass funnel. Created by Asad Ali Awan

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Then the funnel is placed above the clean beaker with the help of stand such that the few cm of the stem of the funnel is in the beaker. 3. The mixture is putted on the filter paper by passing it by the glass rod to the sides of the filter paper in order to avoid the splashing; solid particles are retained by the filter paper because of their definite shape and the solution is filtered in the beaker below the funnel. Precautions:1. The funnel should be relative in size the filter paper. 2. Filter paper should be 1-2 cm below the brim of the funnel. 3. Apex of funnel (15cm) should be along wall of the beaker with an angle of 60 in order to avoid splitting. 4. Filter paper should be fitted carefully and accurately in the funnel that the mixture does not pass through the gap between the filter paper and the wall. 5. If any precipitate, becomes attached or adhere firmly to the side of the beaker, must be removed carefully with the help of tipped rod called police man. Folding of filter paper:1. The filter paper is first folded in the half, then in the quarters. 2. Then the filter paper is opened at the angle of 60 such that three sides are on one side of the other side on the other side. 3. After this step the filter paper is moisten and is used in the filter paper. Relating terms:Mixture:The solution to be filter is called mixture. Retained:The solid particles remaining in the filter paper are called retained Filtrate:The filtered solution is called filtrate. Filter mat:Made of:It is made of pure asbestos having pores in it. Applying:The filter mat is applied in the filter crucibles. Method of filtering:The solution to be purred is put in the filter crucible with the filter mat. The filter mat is in the form of solid. The solid particles retained in the crucible on the mat and the filtrate expelled out. It is then heated in order to evaporate liquid traces present in the filtrate. Crucibles:Large metal Crucibles are simply used to melt the metals and the smaller ones made of glass etc are used for the filtration. Construction:The filter crucible is made of platinum metal powdered and sand (silica) and asbestos and glass wool i.e. powdered glass. Types:Filter crucibles can be of two types:1. Gooch crucible 2. Sintered glass crucible. Gooch crucible:These types of crucibles have small holes at their bottom. Construction:They are made from the porcelain clay. However they are also made form platinum and silica (sand). For better and effective filtration filter mat or filter paper is also used at the bottom of the crucible. Applying method:For the rapid filtration, gooch crucible is provided with the suction pump used to produce the vacuum. The crucible is holded in the gooch funnel. This gooch funnel is passed through the rubber holder in to the receiver called the filtration flask which usually has capacity of 750 ml liquid. The mixture is putted in the gooch crucible and after filtration the solid particles are retained at the filter mat or filter paper and the filtrate reaches in to the filtration flask. The filter crucible can be heated to evaporate the traces of liquid from the solid particles. It is best medium for the rapid filtration. Sintered glass crucible:The type of the crucible having sintered glass bottom without the need of the filter mat or filter paper is called sintered glass crucible. Construction:Created by Asad Ali Awan

It is made of fibers of glass and amorphous (i.e. randomly organized on the microscopic level) disk of solid glass that are arrange randomly having pores between them. The sintered crucible is used to heat the ppt. to the high temp (400 C). For this purpose the crucible is made of Pyrex glass which is very resistance to the heat. (Silicates, B2O3 + Al2O3) Size and shape:The sintered glass crucible is present different shapes and sizes which can be tall and wide. Advantages:1. They are made from the Pyrex glass which is very resistant to the heat. 2. Through the sintered glass crucible, the quantitative analysis can be done. 3. They are readily cleaned. 4. They have ability to be heated up to 400C. 2. Crystallization:Definition:The process in which crystals are formed from a saturated solution by cooling and evaporation is called crystallization. Technique type:It is a purifying technique. Explanation:Crystallization is an important industrial technique used to get a pure product. When this process is carried, the crystals having definite composition becomes separated the solution of different and varying composition. The impurities are present in the mother liquor and they cannot not enter in to the crystals, even if enter, they only adhere to the surface. So through this method a substance can be purified accurately. The crystallization is usually carried out from the saturated solution or from the molten state of the substance, but it can be carried out from the vapour phase directly but it is an occasional way for the crystallization. Principle:In order to get the crystals, the solute is dissolved in the suitable solvent in order to get the saturated solution at the high temperature. When the saturated solution is formed, it is filtered to remove the impurities and then it is cooled, the extra solvent is change in to the crystals. Crystals are separated from the mother liquor through the filtration. Then they are washed by the cold solvent and dried in folds of filter paper in sunlight or in oven. Suitable solvents:The solvent used in the crystallization are usually water, ethanol, and propanone. The impure solvent or the solute is usually dissolved in minimum quantity of solvent. Example:Purification of naphthalene:C10H8 (solid) is dissolved in C6H6 at high temperature. As Filtration is a separating technique, so the solution is the filtered. As the impurities are insoluble are removed by the filtration of C10H8 solution. On slow cooling solution gives pure crystals of C10H8. Term relating:Mother liquor:The solution containing the crystals is called mother liquor.

Created by Asad Ali Awan

Created by Asad Ali Awan