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    DocScanner 7 Oct 2022 5-43 PM

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    DocScanner 7 Oct 2022 5-43 PM

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    Nsbsbshshsh

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    23 views7 pages

    DocScanner 7 Oct 2022 5-43 PM

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    CHAPTER 5 os Chromatography a Q % *, EXPERIMENT 5.1 & To separate the coloured components present in the mixture of red and blue inks by ascendi paper chromatography and find their R,values. APPARATUS, Gas jar, glass rod, filter paper strip (Whatman No. 1 filter paper), jar cover and a fine capillary tube. REQUIREMENT A mixture of red and blue inks, aleohol and distilled water, PROCEDURE 1. Take a Whatman No.1 filter paper strip (20 x 2.em) and draw a line with pencil above 4 em from one¢ Draw another line lengthwise from the centre of the paper as shown in Fig. 6.1. ‘Chromatographic Solvent Glass rod to paper front ‘hang paper ceed 3 coming a : ogo Original line about different = p 4.cm above the edge constituents @ ‘Jar cane ‘of the Pure Point to put the mature, i ca ee . : 025 or Tlowet 2, With the help of fine capillary tube, put a drop of the mixture of red and blue inks at the point P. wail in air. Put another drop on the same spot and dry again. Repeat 2-3 times, so that the spot is rich in mixture. 3. Suspend the filter paper vertically in a gas jar containing the solvent (eluent) with the help of aia in such a way that the pencil line (and the spot) remains about 2 em above the solvent level (aleohel distilled water in 1 : 1 ratio) (Fig. 5.2). 22 CHROMATOGRAPHY ES 4, Cover the jar and keep it undisturbed. Notice the rising solvent along with the mixture of red and blue inks. After the solvent has risen about 15 em you will notice two different spots of blue and red colours on the filter paper. 5, Take the filter paper out of the jar and mark the distance that the solvent has risen on the paper with a pencil. This is called the solvent front, 6. Dry the paper. Put pencil marks in the centre of the blue and red spots, 7. Measure the distance of the two spots from the original line and the distance of the solvent from the original line. 8, Calculate the R,values of the blue and red inks by using the formula R, = Distance travelled by the blue or red ink from the point of application iu Distance travelled by the solvent from the original line Chromatographic paper Solvent front : >> Spots of diferent constituents, A |__ Original spot of the mixture fee, Aen ay er Fig. 5.3. Calculation of R values. OBSERVATIONS AND CALCULATIONS, fh nao Substance Distance travelled | Distance travelled |B Valuc byaliferent components | byantoont Red ink + Blue ink Acm (Red ink) Xem AK Bem (Blue ink) Xam BK PRECAUTIONS 1. Use good quality pencil for drawing the reference line so that the mark does not dissolve in the solvent in which the chromatography is carried out, Always make use of a fine capillary tube. Keep the jar undisturbed and covered during the experiment, A spot should be small and rich in mixture. Allow the spot to dry before putting the strip in the jar, . Keep the strip erect. Do not let it to he curled. Do not allow the spot to dip in the solvent. nonnep To sepa tograph: Proceed as in Experiment 5.1. rate the coloured contponen iy and determine their R, values. : ats present in the given grassiflor COMPREHENSIVE CHEMISTRY ACTIVES yy wer by ascending paper chy OBSERVATIONS AND CALCULATIONS Distance travelled | Distance travelled by Colour ofthe spot | bythe spot from the | the solvent from the original line original line Green ‘Aon Xem AK (Chlorophyll) Yellow Bem Xen BX (Kanthophyll) Red Cem Xem ox (Carotene) ‘a mortar and extract the juice with acetone. Use this solu ‘Note. In the above experiment, crush fresh flowers or grass in for making the spot. pia EXPERIMENT 5.3 raphy and determine their R,values. APPARATUS Gas jar, glass rod, filter paper strip (Whatman No. 1 filter paper), jar cover and a fine capillary tube. CHEMICALS REQUIRED To separate Co" and Ni** ions present in the given mixture by using ascending paper chrom Sample solution containing cobalt (II) and nickel (II) ions, acetone, concentrated aqueous ammonia, Rubeari spray reagent. PROCEDURE Ss i iment tun jame as in Experiment 5.1. Use a mixture of acetone (90%), concentrated hydrochloric acid (5%) and water eluent. After elutic ring i *r elution and drying, place the paper in a large, dry, covered beaker containing a smaller bed! concentrated aqueous ammonia. After about two mii " . ‘nutes, remove the pay if ides wit sei eagent Alon it dry. Nickel boames Vb a ae pase ent at eae orange band. Evaluate R, values of the two ions, OBSERVATIONS AND CALCULATIONS, Colour of the spot Blue purple (Ni*) ‘Yellow orange (Co™) aitirnt components | Détgneetranlied [Valve Acm = Bem os a Xem Bx ‘CHROMATOGRAPHY RESULT R,value of Ni = Mor > R,value of Co = ‘The above experiment can be carried by using a mixture of @ Iron (ID) and cobalt (1) i) Iron (11) and nickel (11) (iii) Copper (ID) and iron (11) w! y EXPERIMENT 6.1 salt), [FeSO,.(NH )},S0,-6H & To prepare a pure sample of ferrous ammonium sulphate (Mohr’s THEORY sulphate and ammonium sulphate .quimolar mixture of hydrated ferrous xrystallization when Mohr’s salt is prepared by dissolving an e« water containing a little of sulphuric acid, and then subjecting the resulting solution to «1 green crystals of ferrous ammonium sulphate. FeSO,. (NH,),S0,,6H,0 separate out. FeSO,7H,0 + (NH),S0, —> FeSO,(NH,,S0,6H,0 + H,0 Ferrous sulphate Ammonium sulphate ‘Mohr's salt 392 ‘Molecular masses : 278 132 REQUIREMENTS ‘Two beakers (250 ml), china dish, funnel, funnel stand, glass rod, wash-bottle, Ferrous sulphate crystals, ammonium sulphate crystals, dilute sulphuric acid and ethyl alcohol. tripod stand and wire-gauze. PROCEDURE 1, Take a 250 ml beaker and wash it with water. Transfer 7.0 g ferrous sulphate and 3.5 g ami sulphate crystals to it. Add about 2-3 ml of dilute sulphuric acid to prevent the hydrolysis of fe sulphate, 2, In another beaker boil about 20 ml of water for about 5 minutes to expel dissolved air. glass rod until the salts have completely dissolved. 4, Filter the solution to remove undissolved impurities and transfer the filtrate to a china-dish. 5, Heat the solution in the china-dish for sometime to concentrate it to the crystallisation point. Mohr’s salt separate out. 7, Decant off the mother liquor quickly. Wash the erystals in the china-dish with a small quantity to remove any sulphuric acid sticking to the erystals. 8. Dry the crystals by placing them between filter paper pads. 26 > pREPARATION OF INORGANIC COMPOUNDS Glass rod Glass rod Fillorato Residue ft behind Funnet— Fig. 6.1. Heating of solution, Fig. 6.2. Removing insoluble impurities by filtration, Fig. 6.3. Concentration of solution, OBSERVATIONS Weight of crystals obtained Colour of the crystals Shape of the crystals X_Note. The crystals of Mohr’ salt are monoclinic in shape. PRECAUTIONS 1. Cool the solution slowly to get good erystals. 2. Do not disturb the solution while it is being cooled, 8. Do not heat the solution for a long time as it may oxidize forrous ions to ferric ions, Ex? & To prepare a pure sample of potash alum (Fithari), [K,S0,Al,(SO,),24H,0}. THEORY OH } EXPERIMENT 6.2 Potash alum is prepared by dissolving an equimolar mixture of hydrated aluminium sulphate and potassium sulphate cryouai tam @mount of water containing a little of sulphurie acid and then subjecting the resulting solution to “nstallisation, when octahedral crystals of potash alum separate out. K,80, + Al,(S0,),.18H,0 + 61,0 —> K,S0, Al(SO,), 24H Potassium Aluminium Potash alum sulphate sulphate Molecular masses 114 666 REQUIREMENTS ‘To beakers (250 ml), china dish, funnel, funnel stand, glass rod, wash-bottle, tripod stand and wire-gauze, ‘@ssium sulphate, aluminium sulphate and oh PROCEDURE PRECAUTIONS ~ yi

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