Experime 4 nt 1: Determinati acid solution ination of the strength of NaOH by using standard oxalic Prineiple: An a. = An acid-t fi Renae ‘base titration is a neutralization reaction that is performed in the lab in “ermine an unknown concentration of aci or ase, The moles of ae wil equal ar bas atthe equivalence point The neutralization method comprises volumetric ‘ased on reactions of acids with alkalis, i.e, neutralization of acids and bases: the moles determinat H* (aq) + OH (aq) —> H,0(1) The neutral i A utralization method is used for determining the amount of acid (alkalimetry) or alkali imetry) in a given solution. At the equivalence point, neutralization is complete. Moles of H’ = Moles of OH NaOH is a secondary standard substance, Thus oxalic acid can be used to prepare a standard solution. Standard oxalic acid solution reacts with NaOH solution and produce sodium ‘oxalate and water. COOH COONa econ) all ire) coon COONa “Apparatus: Conical flask, pipette, burette, dropper, pipette pump. Reagents: Standard oxalic acid, Sodium hydroxide, Phenolphthalein indicator. Procedure: (i) Take 10.0 mL of supplied oxalic acid (0.05M)solution by a pipette into a conical flask (ii) Add approximately 25 mL distilled water and add 1-2 drops of Phenolphthalein indicator in it. (iiiyThen titrate the acid solution with NaOH solution from a burette until the color of the solution turn to pink. (iv)Repeat the titration for at least three times and the agreement between the titrations ‘should be within 0.1 mL. record your titrations data in tabular form as followsLaboratory Rules: a intained in the Laboratory. of students on 4 certain day will be eriment allotted to them. An ances. Students, of their own, Strict discipline has to be mail The experiments to be performed by groups announced beforehand. Students will perform the expt experiment may be changed under unavoidable circumst shall not be permitted to change the experiment schedule. the required apparatus are Before you start the experiment check against the list that ‘ ad present in the working place. Any discrepancy must be immediately reported. Additional apparatus may have to be issued by the students when required. ner must sign for them, and upon return, the receipt must be singed by laboratory assistant. Your experiment schedule makes it necessary to keep the working place clean and in order. If you have to use any instrument for your experiment, make sure that you learn how to handle it by discussing with your teacher. Do not throw anything in the sinks or in walking spaces. This must be strictly followed. Leave them in the proper places. Do not talk unnecessary in the lab. Do not borrow any instrument or glassware from your fellow classmates unless authorized by a teacher. If you do not know how to do an experiment do not hesitate to talk to your teacher. They are in the class to help you.‘Table: Determination of the strength of NaOH with standard oxalic acid motion using phenolphthalein as an indicator Nook] Watume of See ne | i ret observation | oxalie a0 id ee er rere ete | oie burette burette (mL) | | reading | reading | (mb) | (mb) 7 | + a L 2 (y) Calculate the strength of the alkali solution. Calculation: a=No of moles of acid b.VaM, = a.VeMy b =No of moles base Va= Volume of acid Ve = Volume of base M, = Molarrity of acid Mp= Molarity of base NB. « NaOH readily absorbs COs and water vapor from the air and hence there is a change of weight therefore, it is a secondary standard substance. © Oxalic acid is a crystalline substance, stable at atmospheric conditions and corresponds exactly to its formula, which can be obtained chemically pure. « Phenolphthalei ‘ator’s color change pH range is 8.3 to 10.0 and produces red color at basic solution whereas colorless at acidic or neutral solution.Experiment 2; 5; + Standardization of dichromate solution ant ition. of Sodium thiosulphate solution with standard ind determi ot siauderd thiemiGhiesiic, of copper from a given solution by the Principle: Sodi = Sodium thiosulphate thiosulphate can be peony la eae Potassium iodate or iodine, Pi iodide and iodine ary standard substance. Sodium h a standard solution of potassium dichromate or ‘otassium dichromate is reduced by an acid solution of potassium, berated as shown below: Cr,0;+ 6 By + 14H = 2ce* * 3h + 7H a ie dlue to the atmospheric oxygen can be prevented by the addition of solid SAHCOs resets with acid, forming COs, which sweeps ar out ofthe flak and solution the solubility of iodine in water is low, a considerable excess of KI must be used in ‘odometric determination of oxidizing agents. The iodine liberated by the reaction then dissolves by forming the unstable complex salt Kh] with K Kl +h == Kil oh + bh == The liberated iodine (12 or 13’) reacts with thiosulphate solution rapidly and stoichiometrically, if the pH of the solution is less than 5: 28,0; + —& S,Oe + 2 or 28,0, iy SO ena ‘A very sensitive indicator for iodine is starch solution. When an excess amount of potassium iodide is added to an acidic solution (pH ~ 3.5, adjusted by the addition of CHsCOOH) of Cu, two reactions occur simultaneously. First, the Cu’* oxidizes is itself reduced to Cu’. Second, the Cu” immediately react with of white Cugl2. ide to form a precipitate 2cu* + ar == Cul,(s) + Ip r+ hh By titrating the tri-iodide with a standard sodium thiosulphate solution in presence of starch indicator, copper can be accurately determined. Keep in mind that Cu (If) is not normally a strong enough oxidant to oxidize I but the oxidation occurs because of the insolubility of the product, Cugl. Apparatus: Conical flask, burete, pipette, measuring cylinder, watch glass. Reagents: Potassium dichromate solution, NazS:0s solution, NaHCOs/ NazCOs, Procedure: Standardization of Na;S203 solution (i) Place $0 mL cold recently boiled distilled water in a 250 mL. conical flask and adds 5 mL 10% KI solution (lodate free).Determination of the amount of copper: (i) di (iv) ilst gently rotating the flask in order to ii mL of concentrated HCI slowly whi : (ii) Add 3 mL of concentrate S167 M KaCt30r Solution the liquid. Run in 10 mL of standard 0. le boiled out water 7 k with a (iii)Mix the solution well and wash the sides of the flask wit aaa ate from the wash bottle. Cover the flask with watch glass an dark for 5 minutes in order to complete the reaction. 50 mL of cold boiled Giv)Rinse the stopper or watch glass and dil.ute the solution with 1 out water. (9) Titrate the liberated iodine with the NazS:0; solution containes constantly rotating the liquid so as to thoroughly mix the solutions. (vi) When most of the iodine has reacted as indicated by the solution acq| yellowish-green color, add 2 mL of stare! flask; the color should change to blue. (vii) Continue the addition of the thiosulphate solution drop wise and liquid constantly, until | drop changes the color from greenish-blue to light green. ‘The end-point is sharp and readil.y observed in a good light against a white background, (viii) Tabulate the date in a suitable table. ‘Table 1: Standardization of Na:S;0; solution No of Volume of | Burette reading ‘Average observation | Potassium (Na:S;0;) burette dichromate Final Difference | reading Solution burette burette (mL) (mL) reading (mL) | 2 3 (ix)Calculate the strength of sodium thiosulphate solution. pH control: Pipette out 10.0 mL of supplied solution into a 250 mL conical flask. Add drop by drop dil.ute NaOH solution until a faint permanent remains and this is removed by means of a drop or two drop of acetic acid. Add 5 mL ofa 10% KI solution. After the addition of the KI solution, run in standard 0.1 M Na2Sz0; solution until the brown color of the iodine fades. ‘Add 2 mL of starch solution and continue the addition of the Na,S:0s solution until the blue color commences to fade, instantly become Add about 10 mL of 10% NHiSCN solution. The blue color more intense,wi ‘Tabulate the data in a Suitable table. ‘Table 2: Estimation of Copper content Nal of Burette reading Average ‘opper (NaS:03) burette sulphate Final Difference reading solution burette burette (mL) (mL) reading (ml) (mL) ! (vii) Calculate the concentration of copper in the supplied solution. NB. Sodium thiosulphate (Na;S;0;.5H20) is available in a state of high purity but because of its efflorescence nature the amount of water of crystallization in it has some degree of uncertainty. Thiosulphate is also decomposed by atmospheric oxygen (2 NazS;03 + O2 = 2NazSO, + 2S) as well by the action of microorganisms (thiobacteria). ide ion is oxidized to iodine by the oxygen of the air Or+4H* + 41 =2lp +2H30 and the Cr (II1) forms accelerates further the air oxidation of I, The starch solution must be added at the very end of the titration, when very little iodine remains and the solution being titrated have a faint (straw yellow) color. If the starch is added earlier, when there is still much iodine in solution, the large amount of i compound formed reacts slowly with the thiosulphate, so that it thiosulphate. ine-starch easy to add too much ‘An error in the titration may arise from adsorption of triiodide ion by the Cul precipitate. Triiodide ion is held so tenaciously on the surface of the preci between thiosulphate and triio leis incomplete. The problem may be overcome by adding small excess of potassium thiocyanate to the mixture, which metalesizes Cul to Cu(SCN): Cul (s) + SCN’ === Cu (SCN) (s) + 1 Since solid Cu(SCN) has almost no tendency to absorb iodide ns, the previously adsorbed tri-iodide is released so that the thiosulphate titration can be finished. However, thiocyanate should not be added at the begi thiocyanate,acid against a strong alkali. R stance in which a solution of a strong s acid, HCL ; Prineipale: A strong acid, hydrochloric ai a vsetion occurs. For each amount of Moe base, sodium hydroxide NaOH, is added. The the faster moving ole, amount of hydrogen ions is ra eee erica cisatedscl tion cation is replaced by the slower moving Na’ ion, and the events : wtinues ul as well as the measured conductance of the cell fall. This cont TS eae a point is reached, at which we have a solution of sodium chloride, i nd the increase in conductivity or conductance is observed, since more ions are bens Ce ‘a the titration of a strong acid with a strong base, the conductance has @ m! ae equivalence point, This minimum equivalence point can be used instead of an to determine the endpoint of the titration. The conductance of a dil. acetic acid solution is due to the smi F, from the dissociation of the weak acid. When a small amount of alkali is added and the H ions are neutralized an equal amount of H” ions are not generated by further dissociation of the weak acid because the CH;COO’ ions suppress the dissociation due to common ion effect. Therefore the conductance decreases. amounts of H’ ions resulting Upon the further addition of alkali, the conductance increases because of the increases of Na’ tons and of CHsCOO” ions. After the end point, the conductance increases at a sharper rate due to increases of the last moving OH ions, in addition to the Na’ ions, Apparatus Conductivity meter, Beaker (250mL), Burette, Pipette. Procedure i) Wash the conductance cell with hot distilled water. ii) Take 10mL of the supplied acid solution in a beaker, Place conductance cell in it and add sufficient water to keep the electrodes of the cell immersed, i) Get a graph paper ready for plotting conductance data, iv) Measure the conductance before the addition of NaOH. v) Charge the burette with the supplied 0.2M NaOH solution. Add 1 mL. liquot portions of the alkali solution from the burette, stir the solution, and measure the conductance after each addition, vi) Record all the data in a tabular from. Table -1 Table for the recording of conductance against volume of NaOH vs HCI Volume of NaOH (mL) Conductance (us)ie = Table -2 Table for the 2 Fecording of i if CHsCOOH 18 of conductance against volume of NaOH ys Volume of ji added. measure the first few (2-3) points by adding te the decreases in conductance. The selector the next point. he end point gives a steeper straight line nt and volumes of NaOH at the end point from the graph. Calculate the concentration of strong acid and weak acid, (Volume-corrected) consist of intersect is that at which the ‘conductivity undergoes a sudden change. Marked increases or decrease in conductance are associated e changing concentrations of the two most highly conducting ions- the hydrogen and hydroxy! 1g colored solutions or homogeneous suspension (¢.g.: wood pulp suspension, wi ion, redox: Known to us where are known to us where indicators are used to locate the end point e-g. methyl ‘orange, phenolphthatein for acid base ti for iodemetry type redox process. ical conductance measurement can be used as a tool to locate the end point. ion of a strong acid, hydrochloric acid, HCI for instance in which a solution of a strong base, sodium hydroxide NaOH, is added. The reaction occurs. For each amount of NaOH added equival ff hydrogen ions is removed the faster moving H” cation is replaced by the slower moving Na’ ion, and the cond ions. T Jing added and the neutralization reaction no longer removes an appreciable number any of them. Consequent ion of a strong acid with a strong base, the conductance has a minimum at the equivalence point. This minimum equivalence point can be used instead of an indicator bye to determine the endpoint ofthe tit conductance is observed,i on} : Experiment 4: Determination of the neutralization curve of a strong acid, w cid by a strong alkali by Pesasune solution of the acid whose strength is to be ‘ A plass lectrode is imirtive to hydrogen ion activity, and has a potential eocanes hie < ‘a standard calomel electrode (watcl eeppenional too 1d to the potentiometer or electronic red bet acumen changes accordingly. The e.m.f. voltammeter. With the addition of alk: of the cell also changes with pH of the soluti E=E° + 0.0591 pH We actually will get value of ly from the scale, because the instrument SO ane to convert emf. value directly into pH value and show it on the scale. The standard alkali solution is added from the burette in small volumes. Upon each addition, the pH is recorded. The pH is then plotted against the volume of alkali added. The steepest portion of the curve indicates the equivalence poi When the solution is very dil.ute or weak acid or bases are involved, the steepness of the ‘curve is less marked and ficult to judge the end point. In such case plot of the curve AE/AY volume of is used. The maximum of the curve indicates the end p Apparatus pH meter. Burette, pipette, beaker (250 mL). Procedure Wash the pH clectrode with sufficient i (ii) Calibrate the pH meter using buffer solution of pH = 0.36 (iii)Again clean the electrode with sufficient water. (iv)Take 100 mL of su 0.01M HCI in a beaker and immerse the electrode of pH meter carefully in the beaker so that it does not touch the bottom of the beaker. (¥) Add 0.5 mL 0.05 M NaOH each time from burette in to the beaker and measure the pH of the solution as the function of volume of NaOH until steady pH is found followed by sharp increase in pH. Record the data in a table as follows. Table-1 Table for the recording of pH against volume of NaOH ys. HCI Volume of NaOH (mL) pH ‘- —Table-2 Table for the recording of pH Against volume of N, 'aOH vs. CH\COOH, Volume of NaOH (mL) pH (Vi)Repeat the whole Process for 0.01 M acetic acid, Record the data in a similar table like Table-1 ) Plot PH vs volume of NaOH for i) HCI and ii) acetic acid indicating point of equivalence in separate graph paper, Glass electrode (p"') ‘The glass electrode for measuring p! consists of a glass indicator electrode and a reference saturated calomel electrode immerse ion of PY. The P™ indi t a thin P" sensitive thin glass membrane sealed onto end of a heavy-walled the tube. This electrode is sensitive to hydrogen ion , and has a potential proportional to P!. The responsiveness of a glass electrode to the hydrogen ion activity is a res Complex process at the interface between the glass membrane and the so P"' of the solution changes accordingly. The emf of the cell also changes with P" of the solution in accordance with the rel E=E?+0.0591 We actually will get of P™ directly from the scale, because the instrument so designed to convert e.m.f. value directly into P! value and show it on the scale, The P* electrode is calibrated against standard buffer solution before the any measurement of unknown P!Table-2 Table for the recording of pH Against volume of N, 'aOH vs. CH\COOH, Volume of NaOH (mL) pH (Vi)Repeat the whole Process for 0.01 M acetic acid, Record the data in a similar table like Table-1 ) Plot PH vs volume of NaOH for i) HCI and ii) acetic acid indicating point of equivalence in separate graph paper, Glass electrode (p"') ‘The glass electrode for measuring p! consists of a glass indicator electrode and a reference saturated calomel electrode immerse ion of PY. The P™ indi t a thin P" sensitive thin glass membrane sealed onto end of a heavy-walled the tube. This electrode is sensitive to hydrogen ion , and has a potential proportional to P!. The responsiveness of a glass electrode to the hydrogen ion activity is a res Complex process at the interface between the glass membrane and the so P"' of the solution changes accordingly. The emf of the cell also changes with P" of the solution in accordance with the rel E=E?+0.0591 We actually will get of P™ directly from the scale, because the instrument so designed to convert e.m.f. value directly into P! value and show it on the scale, The P* electrode is calibrated against standard buffer solution before the any measurement of unknown P!