Mortum MM). Si LAB MANUAL Anatyticat Tecunigues (T) LABORATORY EXERCISES COURSE NO: AC 509 ~ 3'4 YEAR 5T4 SEMESTER AVAILABLE AT APPLIED CHEMISTRY PHOTOSTATE SHOP UNIVERSITY OF KARACHIwee EXPERIMENT 1 OBJECT: POTENTIOMETRIC LOCATION OF END POI Chemical: 1M NaOH, unknown acidic solutions A and B. Theory: Potentiometric titration is a volumetric method in which the potential between two ele measured (referent and indicator electrode) as a function of the added reagent volume. The most common potentiometric measurement is that of pH. pH was defined originally as ~ logy 4 0 log(I/C +1) , where C, . is the concentration of hydrogen ion. Today instead of C, , one would write a. 1, the activity of hydrogen ion. ‘The measurement of the pH of a solution is simple in principle, of it is based on the measurement ’ of the potential of hydrogen electrode immersed in the solution. The left-hand, i.e. the reference: electrode of the cell is typically a saturated calomel electrode (SCE) with potential E(cal). The — PH of the cell is therefore E+E(cal) ie : (-4) mao Procedure: Calibrate the pH meter with the help of standard bufter solutions of pH 7 & 4 Booker Take 20 ml sample in 50 ml beaker, Dip the electrode & note the pH of sample. Now add 1 ml base from burette and note the pH on each one m! addition of basic solution till the value is fairly constant i.e. pH 14 Repeat same step for sample B eS .. L f. 1C- ran-ple 1fto > See, | Calculation: Ny Draw graphs b/w pH & vol. of base utilize & find out the concentration of unknown acidic solutions. 2. Find the end point by First & Second derivative method and calculate the strength of acids.EXPERIMENT 2 OBJECT: DETERMINATION OF PHOSPHATE/NITRATE ION IN GIVEN FERTILIZER BY A ELECTRO ANALYTICAL METHOD Chemical Fertilizer, 1 — 2M HCl, 0.1M NaOH. ‘Theory: Ion exchangeis an exchange of ions between tw0 electrolytes or between an electrolyte solution and acomplex. In most cases the term is used! to denote: the piosssses of purification, separation, and decontamination of aqueous: and other ion-containing solutions with solid polymeric or mineral ‘ion exchangers! Jon exchange resins are highly ionic, covalent as beads. There are two general types of ion exchange r called cation exchange resins, and those that exchange negative fons, resins. The "reactivation" process is called regener cation (as a source of hydronium ions) and liqui hydroxyl ions for the anion, Resin is regenerated on site using hydrochloric or sulfuric acid and sodium hydroxide (caustic) to regenerate the cation and anion resin respectively When solution of fertilizer is passed through the column the cation ions present in it form acid. ‘and washed out through the column which is then neutralize with base. ly cross-linked, insoluble polyelectrolytes supplied cesins: those that exchange positive ions, called anion exchange ration and is carried out using a strong acid for the d caustic (sodium hydroxide) as a source of Procedui Prepare a column of cation exchange resin. The resin bed should be about 20 em long and lem wide and it should be free from air bubbles. Wash the column with 50 ml water then regenerate it with 20 ml 1M HCI. Again wash it with 50 ml water to remove the excess HC! from column. Weigh accurately 0.8 — 1 gm of given fertilizer and dissolve in 10ml distilled water. Introduce concentrated hydrochloric acid 0.1 ~ 0.5m (it converts all the phosphate to phosphoric acid! nitrate to nitric acid), The pH of this solution should be less than 2. Pass the sample solution, through resin column and collect the sample in another 250 ml beaker. Wash the column with 250 ml water. Now collect all the washing in separate beaker. After 150 ml of water has passed out, freshly collect 20 ml solution in small beaker and note the pH. If pH of the effluent is more than 4 it means washing of the column is complete. Measure the total volume of aftluent and titrate 20 ml of it with 0.01 MNaOH by using potentiometer. ja6 “between pH & volume of NaOH utilize. First inflection point is at 4.5 pH at cond is at 8.5. " Take volume between the two inflection points and calculate the amount of phosphate/ ion in given fertilizer.1, 0.1 N Iodine solution. 2. Starch indicator. 3. Vitamin C tablet. ‘Theory: Redox titrations are based on an oxidation-redi These most commonly use a potentiometer or & are two types of redox titrations 1. Todometric titrations 2. Todimetric titrations yteand titan, NGAP EME uction reaction between the anal’ redox indicator to determine the ‘ia } a When an analyte that is a reducing agent is titrated directly with a standard iodine solution, the 4 method is called "iodimetry". ‘When an analyte that is an oxidizing agent is added to excess iodide to produce iodine, and the ae iodine produced is determined by titration with sodium thiosulfate, the method is called "iodometry". f Starch is the indicator of choice based on redox titrations involving iodine, sintee star forms an : intense blue colored complex with iodine. 3 Procedurt Dissolve the given tablet in 250 ml water. Take 25 ml of solution and titrate it with 0. solution by using starch indicator. First appearance of the deep blue color shows the which exists for at least | minute. f tion: Calculate the number of mg of Vitamin C per tablet by usi i: a 34 ml of 0.1 N of Iodine solutions react with 300 mg al a reEXPERIMENT 4 OBJECT: DETERMINATION OF ACETIC ACID IN VINEGAR Chemicals: ae m NaOH, 2. Phenolphthalein Indicator 3. Natural and synthetic vinegar Procedure: E i Dilute 10 ml vinegar in 250 ml water in volumetric flask. Pipette out 20/25 ml solution and titrate it with 0.1 M NaOH by using phenolphthalein indicator. Repeat the same. procedure for i both natural and synthetic vinegar. Caleulation: Calculate the % acetic acid in viniger sample by using given relation. 1 ml 1 M NaOH required to neutralize 0.06005 gm of CH;COOH(o2 NAe ee SM zoo, : (om) -46-4) (BO “Vine (0 2)CS em EXPERIMENT 5 \ OBJECT; PREPERATION OF BUFFER SOLUTIONS, im Instrument pH meter Magnetic stirrer ‘Theory: A butler solution is one in which the pH of the solution is “resistant” to small additions of either a strong acid or strong base. They are of two types 1. An acidic buffer solution is simply one which has a pH less than 7. Acidic buffer solutions are commonly made from a weak acid and one of its salts - often a sodium salt, 2. Analkaline buffer solution has a pH greater than 7. Alkaline buffer solutions are commonly made from a seg base and one ofits salts. eS (1) WALPOLE ACETATE BUFFER (pH 3.6-5.6) *) wt Stock Solutions: : Mr -136-0B+ (@ _0.2M Acetic acid &, Gi) - 0.2 Msodium acetate“) 3 CH sNa 02 Sa ¥ ‘Mix the stock solutions in the proportions given below and note the pH. Acetic Acid Sodium Acetate | pH Vol. I 2 remiss x: Le 2. [4 |i ica ca Lo 3. 2 (16 14 co. ee 4. paar (8 Tame CTE 7 Et « [10 Orme C208 o 6 ery 2 Gre 7 7. e [16 4 Wise 7% Rs « [14 6 Cats p y 4 a 8 4 BD ve Unknown A a Bo, iF iS YS Unknown B. 10: Zz Rp. 4 BO, Soll Draw graph between volume of acetic acid and volume of NaOH against 0-1 K:25 0-912 -o@e # —— loo0- MICHAELIS BORATE BUFFERS (pH 7.6-12.3): 0.L M NaOH 0.L MHCI Borax: 3 gm boric acid + 25 ml 1M NaOH / 250 ml water. Mix the stock solutions in the following proportions and note the pH. 0.1MNaOH | Borax HH Vol ik De WA 18 Etna Di ARETE! 16 $+ 36 3. Nav 16 14 a 4. eM 12 a.4 “5 2 ey 10 Mw 10 10- S| a 6. 1g 2 ty eis fe 16 MOA [4 [z=4o = 14m 6 D4! i oem WOOF "12 8 [os : B [0.1 MHCI Borax, pH Vol ia 2 18 iG 2. 4 16 4 Ey 6 14 4. [8 12 Et 10 10 6. 18 D 7. 16 4 a 8. 14 6 9. 12 8 ‘alculations: @ between volume of Borax and volume of NaOH against inst pH ‘0.04M Phosphoric Acid 0.04M Boric Acid * 0.2 MNaOH Take 10 ml of each aed and prepare 30 ml stock solution and note its pH value. Now a in given proportion and note the pH. Sodium Hydroxide (ml) fi 10 i 20 255 30 35 40 45 else] apo) | S| Calculations: Draw graph between volume of NaOH against pHy EXPERIMENT 6 OBJECT: PREPERATION OF BAUME. SOLUTIONS. Procedure: h the help of Baume meter note the Ba Transfer the given solution in 100 ml cylinder and wit! 1 B t with the help of given relation. concentration. If Be of solution is less than 33 then increase i . 106 gm salt when dissolve in 100 ml water then solution is 0 49.358.) Es - ‘Now transfer the solution again in beaker add 10 ml water in it, mix and transfer in 100 ml : measuring cylinder and again not the Baume concentration. Repeat the same procedure 10 times — and calculate the normality Or Molarity of the solutions. OR From the prepared solution of 33°Be make 31°Be, 29°Be, 27°Bi a i Q ¢ ti a > ‘e, 25°Be and 23°Be solution by using above given relation. Calculate the normality or molarity of prepared solutions. "ie Ve. Roume fo 23 Baume Ka rors bh , 26< - 4 553 ieee, 2.33 4Wn 2EXPERIMENT 7 OBJECT: conpucro iC LOCATI Ee Chemicals: 0.1M NaOH, unknown acidic solutions A and B Theory: Conductometric titration is a type of titration in which the electrolytic conductivity of the reaction mixture is continuously monitored as one reactant is added. The equivalence point is the point at which the conductivity undergoes a sudden change. In this experiment we shall be concemed with electrical conduction through aqueous solutions. Although water is itself a very poor conductor of electricity, the presence of ionic species in solution increases the conductance considerably. The conductance of such electrolytic solutions depends on the concentration of the ions and also on the nature of the ions present (through their charges and mobilities), Conductance behavior as a function of concentration is different for strong and weak electrolytes. The conductivity of a solution depends on the concentrations and mobilities of the ions present. It is convenient to define a quantity, the molar conductance A, _ 1000K« a c Where ¢ is the molar concentratior pressed in mol.dm™, 1000 is the factor arising from the fact that 1 dm* =1000 cm’. Thus, the molar conductance is expressed in S-cm? -mol". The molar conductance is sometimes described as the actual conductance of that volume of solution which contains one mole of solute when placed between parallel electrodes 1 em apart with a uniform electric field between them Procedure: Set the measuring cell constant on the unit 1.00 cm ' with control knob K = emt" First of all wash the electrodes thoroughly with distilled water; note the conductance of distilled water at room temp. Pipette out 20 ml sample in 50 ml beaker, adjust the electrode and note the conductance of the sample. Now add 0.5 ml base from burette and note the conductance on each 0.5 ml addition of basic solution (continuously stir the solution with the help of glass rode). 4 The observed conductance may cither in increasing or decreasing order.1. Sample A with 0.1 M strong base 2. Sample B with 0.1 M strong base 3. Displacement titration ammonium chloride with 0.1 M strong base 4. Displacement titration sodium acetate with | M HCI. Draw the graph b/w conductance and volume of base / acid consumed. Find out the end Poa from the graph and calculate the strength of unknown solutions.