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Microscale Experiments in Chemistry - the Need of the New Millenium 4 SERIES I ARTICLE Microscale Experiments in Chemistry - The Need of the New Millenium 4. Physical Chemistry Experiments on Microscale Shriniwas L Kelkar, Dilip D Dhavale and Jeevan G Chandwadkar It is evident from the earlier articles in this series that consider­ Shriniwas L Kelkar is a Reader in Organic able time and money can be saved if the academic laboratories Chemistry at University are to adopt microscale techniques. In this context, however, the of Pune. After an active . research career and point regarding consumption of large quantities of chemicals publishing work on appears irrelevant from the physical chemistry point of view. heterocyclic chemistry, he is now devoting his Most of the experiments are already being performed with entire time and attention instruments and require per se small amounts of chemicals. to propagate the small­ scale experiments. On However, we felt that many of the traditional procedures should demand, he is available to be reviewed and rewritten to bring about not only further conduct workshops for training teachers on reduction in chemicals, time and energy but also bring theory microscale techniques. closer to the laboratories. Dilip D Dhavale is a In the physical chemistry domain, the undergraduate syllabus Reader in Organic Chemistry at University includes experiments to demonstrate basic principles such as of Pune. He is pursuing adsorption, partition coefficient, measurement of viscosity, sta­ his research career in carbohydrate chemistry. bility constants of complexes, etc. It also includes experiments He had been associated to illustrate the most important principle of 'chemical equilib­ with popularizing microscale chemistry rium'. The students are introduced to several instrumental from its inception in methods such as spectrophotometers, potentiometers, pH meters India. and conductometers for quantitative estimations, rather than by Jeevan G Chandwadkar is the conventional pipette-burette titration. a Reader in Physical Chemistry at Department One of the common experiments carried out in all the under­ of Chemistry, University of Pune. His research graduate laboratories is the determination of the stability con­ interests are molecular stant of triiodide ion. The standard procedure prescribed re­ structure and zeolites. quires that the distribution coefficient of iodine is first deter­ mined between carbon tetrachloride and water. This is used in the next step to estimate the concentration of iodine in aqueous layer containing KI. For this, about 50 ml of carbon tetrachlo­ ) ride (CCI4 saturated with iodine (I) is to be equilibrated with ------~~-------­ RESONANCE I April 2001 15 SERIES I ARTICLE Part 1. Newer Ways of Teach­ 200 ml of aqueous solution of KI. Iodine is then partitioned into ing Laboratory Courses with the aqueous layer as KI3 and as 12 in carbon tetrachloride. After New Apparatus, Resonance, Vo1.5, No.10, p. 24, 2000. separation of the layers, iodine in each layer is estimated by Part 2. Experiments Which Bring titration. Taking into consideration the high cost of iodine, Theory Closer to Laboratories, potassium iodide and CCI4, we thought of looking at this experi­ Resonance, Vo1.5, No.12, p.6, ment specifically to reduce the required quantities to less than 2000. Part 3. Microscale Inorganic just a tenth of the prescribed volumes. The convention is to Qualitative Analysis and New shake 250 ml of immiscible liquids in a separating funnel for Methods of Titrations for Intro­ about 20 minutes in order to attain equilibrium of the solute in duction at All Levels in Chemis­ the two phases. Simultaneously, the thermal equilibrium is to try Laboratories, Resonance, Vo1.6, No.2, p.14, 2001. be maintained. With reduction in quantities, 'shaking' is re­ placed by 'agitation' by the Pasteur pipette. This can be easily done while keeping the container in the thermostat during this process. For effective agitation, the lower layer is taken into the Pasteur pipette. The pipette is withdrawn just about a centime­ ter above the upper layer and the liquid is injected through the upper layer by force using a rubber bulb. This is repeated a number of times to ensure thorough mixing of the two layers. We took aliquots at intervals of two minutes to find the parti­ tioning and found that the time taken for equilibration of iodine in the two layers is reduced to just about 3 to 4 minutes. The separation of the two layers was done by Pasteur pipette. In the previous article, we described the use of Beral pipettes for carrying out the titrations on microscale. However, one of the limitations in the use of Beral pipettes became apparent when we tried to apply the same technique here. The number of drops for the same volume of water and any other volatile liquid are not the same. This is obvious since the drop size is determined by the surface tension of the liquid. To overcome this difficulty, a fixed volume (O.5ml) of CCl4 is taken from the reaction flask using a measuring cylinder in a test tube and potassium iodide is added to it to extract the dissolved iodine. This is titrated against the standard thiosulphate solution by the new method. The experimental results are within the limits of errors as those obtained in the normal scale experiment. The cost effectiveness of this method would be evident if we compare the prices vis-a­ vis the consumption of carbon tetrachloride, iodine and potas- ------~~-------- 16 RESONANCE I April 2001 SERIES I ARTICLE sium iodide and also elimination of apparatus such as separating The recent trend in funnels, burettes and pipettes. chemistry is to understand and The recent trend in chemistry is to understand and explain the explain the chemical and physical interactions on a molecular basis. In this chemical and direction, our attention is focused towards the reduction of size physical of the voltametric cells required in potentiometry. A typical interactions on a concentration cell used in the estimation of Ag+ ions can be used molecular basis. in several experiments like determination of stability constants of silver complexes, solubility products of silver salts, and halide estimations by argentometric titrations, etc. The main difficulty normally faced in assembling a cell, is the connectivity of the two half-cells. We used a 'U' shaped glass tube with 8 mm id (inner diameter) and 7 to 9 cm height and filled half of this with a warm solution of agar-agar gel containing requisite concentra­ tion of potassium nitrate to build a salt bridge. The glass tube may be replaced with polymer tubing. A small wooden plank with two holes is adequate to hold it vertically. The sleek assembly is very easy to construct, reduces the cost and also forms an unbreakable assembly. The upper unfilled part of the 'U' tube can be used as half-cells now. Building cells this way have many advantages as listed below: 1. The continuity of the bridge is never broken. Besides being a ~-- PoIytbcoe tubing Test !IObJItion:=:::t!~--t-. 14---- Agar Apr gel + KN03/ICCI Figure 1. Cell assembly. ------~~-------- RESONANCE I April 2001 17 SERIES I ARTICLE The volume of the good conductor, the set agar-agar gel is quite stable, does not electrolyte spill off and the assembly thus remains always clean. solutions required 2. The liquid at the top of each of the arms protects the bridge to construct the from drying. A small cotton plug on each end of the agar gel cells is just around would guard it from any pricking by the electrode. 1 to 2 ml. This reduces the 3. In each of the cell compartments, the solutions can be added consumption of or removed very easily with the Beral pipettes. Even cleaning the cell can be done very easily. AgN03 substantially. 4. The volume of the electrolyte solutions required to construct the cells is just around I to 2 m!. This reduces the consumption of AgN03 substantially. 5. Expensive metals in thin wire form are soldered to copper wire that is supported through an empty ballpoint pen refill. These are used as electrodes. 6. The same bridge could be used repeatedly with reproducible results. If needed, it could be refilled easily. 7. The e.m.f. generated in the cells is easily measurable on digital multimeters (which are accessible and available in the market). The following experiments could be performed using this appa­ ratus. a. Halide estimation by potentiometric titration A concentration cell is set up in this experiment. A silver electrode in about 0.5 ml ofO.IN or O.OIN silver nitrate solution serves as a reference, while the other half-cell contains silver electrode in the test halide solution measured by standardised Beral pipette. It is titrated against standard silver nitrate solu­ tion added through another standardised Beral pipette. Thus a microscale titration is performed with results of the same stan­ dard and accuracy as obtained by normal titrations. b. Estimation of solubility product The e.m.f. value upon addition of the first drop of silver nitrate -8------------------------------~------------------------------- 1 RESONANCE \ April 2001 SERIES I ARTICLE in the above titration could be used to estimate the solubility product of the particular silver halide formed. c. Verification of Nemst's equation )// Over a KN03 salt bridge, a concentration cell Ag/Ag+(c 1 KNO//Ag+(c2)!Ag is formed. Keeping c1 constant, c2 is varied systematically by adding required quantity of distilled water. The linear variation of e.m.f. with log c2 can be shown graphi­ cally and c1 can be determined from the intercept. The slope will be close to the anticipated value of 0.059. Five different solutions of this complex are prepared with vary­ ing thiosulphate concentrations. A concentration cell is set up (vide supra) and the smallest concentration of c2 of Ag+ in the complex is estimated in an identical way.
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