BAS ee ees 2 Se DS 2. D2 DD: DY See + 2 NAME =} M. Nishanth. ROLL NO = of BRANCH : Ece Lan weriny pha mee GE 6163 CHEMISTRY LAB - Icoooaoe COOKUe COCGOOER CORE abe GOGU0eNo. | CONTENTS {Expt.[ BATE | NAME OF THE EXPERTMENT | PAGE | NO. 2a e5 | Determination of Chloride content in water by Argentometric Method (nhohr's Method) 3 f 27 jaqol% | 1 r Determination of Dissolved Oxygen inwater (Winkler's Method) | e | Be 1B ~] Determination of Molecular Weight of Polyvinyl Alcohol using Ostwald Viseometer, ~ 3.091% } [pH metry - Determination of — Strength of HC] by NaOH 3-418. | s 3.413, | of acids (HEI Vs CHscOCH) | Conductometric titration Acid with strofg Base Conductometrie titrati pote ol hort procedures nihumathulla. ka Viva = voce questions and answers Chemistry Lab - 1 Page iStep I: Standardisation of Silver Nitrate TITRATION -T Standard NaCl Vs AgNOs ‘ Indicator: Potassium chromate. | Volume of Naci | Buret¥e Reading (ml) | Wy [eesscageciee lies jf? Tritiel [inl Calculation of the Strength of Silver Nitrate: . Volume of Sodium chloride,” WV; = 20 ml Strength of Sodium chloride Ny = 0.01N Volume of Silver Nitrate Vee Ody -B Strength of Silver Nitrate Net O £0506 According to the law of volumetric analysis, : ViNs = VoNe HN: Ne V7 20 ¥.0.01 Strength of Silver Nitrate Nz sesame emanate nihumathulla. ka Chemistry Lab ~"T Page 2 » YOODETERMINATION OF CHLORIDE CONTENT IN WATER BY ARGENTOMETRIC METHOD (MOHR'S METHOD) Experiment Number: Date: 29, /2-'5 AIM: To estimate the amount of chloride present in the given water sample, being supplied with standard solution of sodium chloride of strength O.0IN and ch Seisanaraly N/20 solution of silver nitrate, | pi PL Generally water contains chloride ions (CI') in the form of NaCl, KCI, Cacle and MgClz, The concentration of chloride ions is more than 250 ppm is not desirable for dtinking purpose. The total chloride ions can be determined by Argentometric method (Mohr's method) In this method Cl lon solution is directly titrated against AgNO: using potassium chromate (K2CrO,) as the indicator, AGNOs + Ch -——-——» Ag; + NOY (in water) _- (white precipitate) At the end point, when all the Ci’ ions aré removed, the yellow colour of chromate changes into reddish brown due to the following reaction. BAGNOs + KeCrOg —-———-» AgarOx] + KNOg (yellow) (reddish brown precipitate) ee terres nihumathulla, ka Chemistry Lab - I Page 3‘Step IL: Estimation of chloride ion TETRATION - Ir Water sample Vs Standard AgNOs “si | Volume of | Burette Reading (mi) 13 | Concerdant | No | water sample |} pn Value _ (nl) | (nl) | Pape Pa ee to ee on | 3 20 o. | of the Strenath Volume of Silver Nitrate | Strength of Silver Nitrate Nie 0.0080 Volume of Water sample Ve = 20 ml Strength of Water sample (Chiorite jon) = N2EO-OOKAS According to the law of volumetric anclysis, VIN = VeNe Strength of Water sample (Chloride ion) Nz = .O.QOQUHS:.....N Oe re Te tn Ne iihumathulla, k.o Chemistry Lob =I Page 4d <>}PROCEDURE: Step I: : RA =1 Standardisation of AQNO;, The burette is washed with distilled water and rinsed with small amount of AgNOs solution, Then the burette is filled with the some solution upto the zero mark without air bubbles. | The pipette is washed with distilled water and ringed with the small amount of standard NaCl solution, 20 ml of this solution is pipette out into a clean conical flask, Im! of 2% KaCrO, indicator solution Is added and titrated against AgNO; solution taken in the burefte, The end point is the change of colour from yellow to reddish brown, The titration is répeated to get concordant value. Step It TITRATION - IT Estimation of chloride ion 20 ml of the given water sample is pipette aut into a clean conical flask and I ml of 2% KeCrOs indicator solution: is added. It is then titrated against standardized AgNO: solution taken in’ the burette, The end point is the change of colour from yellow te reddish brown. CE nihumathulla. ka Chemistry Lab - I Page 5Calculation of amount of chloride ion: The amount of chloride ion present in 1 litre (1000 ml) of the given water sample = Strength of chloride ian X Equivalent weight of chloride ion = C0083. x 3545 =. LEED D oe rn ren nihumathulla. ko. Chemistry Lab ~ I Page 6d RESULT: The amount of chloride ion present in the whole of ae » the given water sane 7 nihumathulla. ka Chemistry Lab «I Page TStep I: Standardisation of Sodium thiosulphate: TETRATION -1 Ki€rOr Vs NazS203 Indicator: Starch [SL [Volume of KeCreOy | Burette Reading | Volume of NazSzOa | Concordant | (nl) { (nl) f (ml) | Value, (nl) Calculation of the Strengt! ium. thio: Volume of Potassium dichromate. Vi = 20 ml Strength of Potassium dichromate Ny = 0.02N Volume of Sodium thiosulphate Vez 20-8 mf Strength of Sodium thiosulphate © Nes 6. 0/92 Nl According to the law of volumetric analysis, - ViNi = VeNe NtDETERMINATION OF DISSOLVED OXYGEN IN WATER WINKLER'S METHOD: Experiment Number: 4 ate: 2q-la- Zorg, ed Al = To determine the amount of dissolved oxygen in the given water sample by Winkler’s method, a standard solution of KeCr2O, of strength 0.02N is given. PRINCIPLE: Oxygen dissolves in water to the extent of 7-9 ings/lit at « temperature range of 25° ~ 35°C. The estimation of dissolved oxygen in water is useful in studying corrosion effects of boiler feed water and in studying water pollution. The amount of dissolved oxygen in water is estimated using Winkler's reagent (Potassium bromide + Potassium bromate). Water sample. is collected carefully avoiding aeration/deaeration in ground stoppered flask, Enitially Manganeous sulphate and alkali iodide reagents ore added and the reactions oceur as follows, i Mr? + 20H? ne MnfOH)el (white) Nn(OH)z + 402..—-———+ MnO(OH)2| (yellow brown) The precipitate dissolves in Concentrated HeSO, liberating iodine and the liberated iodine is titrated against NazS203. MnO(OH)2 + 2H2504 Min(SOq)2 + 3H20 Mn(SOa)z + 2KI + MnSO, + K2SO.+ Iz 2Na2S203 + Ip. NazS205 + 2NaT rrr renter nihumathulla, ko Chemistry Lab -I _ Page 9Step II: Estimation of Dissalved Oxygen: JRA 4 NazS2Q; Vs Water sample Indicator: Starch ‘Si, | Volume of water | Burette Reading | Volume af NazS203 | Concordant No | sample 4 (mi) | Value (ml) (mi) jalculation of the Strength of water sample: : Volume of Sodium thiosulphate Vis alpen, tl 94.0198..M Strength of Sodium thiosulphate —* N Volume of Water Sample (dissolved oxygen) V2 = 100 ml Strength of Water Sample (dissolved oxygen) Np za° auextal Nl - According to the law of volumetric analysis, MiNa= VaNe Strength of Water Sample Chemistry Lab ~ I Poge 10 ) PER: a CAD 9 O00 Go +9PROCEDURE: TITRATION - 1 Standardization of Sodium thiosulphate ‘The burette is washed and rinsed with sodium thicsulphate solution. Then the burette is filled with the given sodium thigsulphate solution 20 mi of 0.02N potassium dichromate solution is pipette out into a clean conical flask. To this, 5 ral of sulphuric acid and 15 ml of 5% potassium iodide are odded. This is titrated against sodium thiosulphate solution’ When the solution becomes straw yellow colour, starch indicator is added and then titration is continued. The end point is the disappearance of blue colour and appearance of light green colour, The titration is repeated to get concordant value: TITRATION - II Estimation of dissolved oxygen 100 - 150ml of the water sample ts taken in the iodine flask 2 ml of ‘Manganese sulphate and 2 mi of alkali iodide are added. The stopper is replaced and the flask is inverted and sheked several times for the rough mixing of reagents, The flask is left aside for some time, When half of the precipitate settles down, the stopper is removed and 2 ml of concentrated sulphuric acid is added, ‘The stopper is replaced and the flask is inverted several times for complete dissolution of the precipitate, 100 ml of this solution is pipette out and titrated against standardized sodium thiosulphate solution, When the solution becomes light yellow, starch indicater is added. The titration ig continued until the blue colour disappears, From the titre value the strength of dissolved oxygen is calculated and hence the amount of dissolved oxygen in'the water sample is calculated, nihumathulla, ke Chemistry Lab ~ I Poge 11Calculation of amount of Dissolved oxygen: _ The amount of dissolved oxygen present in I litre (1000 ml) of the tap water es = Strength of dissolved oxygen X Equivalent weight of oxygen I | ° nihumnethulla. ke Chemistry Lab - I Poge 12 -~ / a 4 ; a RESULT: a The amount of dissolved oxygen present in 1 litre e909 mt of the top weter ‘. . 18...ppm, a Oe penne a nihumathulla, ka Chemistry Lab’ I Page 13nihumathulla. ka ostwald's Viscometer Upper mark Lower mark | | jee de tig cans ae Lic ignte” | est | Mpc - 1 = Ned o-lph |p aa _| Cheinistry Lab = T Je ow de LedDETERMINATION OF MOLECULAR WEIGHT OF POLYVINYL ALCOHOL USING OSTWALD VISCOMETER Experiment Number: 5. : Date: 1 BZ AIM: To determine the molecular weight of polyvinyl alcohol using Ostwald Viscometer, a 1% polyvinyl alcohol solution is provided. PRINCIPLE: Molecular weight of a polymer is nothing but the averege molecular weight This can be determined by measuring the intrinsic viscositp(n) of a dilute polymer Solution, The intrinsic viscosity is related to the melecular weight by the following relationship, n= KM where, Intrinsic viscosity, K da = Constants for a given polymer - solvent combination “at agiven temperature, M= Average molecular weight, MATERIALS REQUIRED: Polyvinyl alcohol, Solvent, Viscometer, 50 ml Std,flask, 20 ml graduated pipette and Stop watch, Chemistry Lab = T Page 1sGRAPH Concentration Calculation: Molecular weight of the polymer Mark - Hownik equation is given by m= KM fog n= log K + alog M log M= ger teak | | AV Anti log of p22 —Heak a M= molecular weight of the polymer. For polyvinyl alcchol K = 45,3 X 10-5 gm/dl a= 0.64 nihumathulle, ko istry Lab = I Poge 16Important Viscosity definitions: 1, Relative viscosity (nt) 2. Specific Viscosity (Ney) 3, Reduced Viscosity (Med) Hea 2 Nep/C 4, Intrinsic Viscosity (nq) Soe limny/e oO Where, n= absolute viscosity of a_polymer solution, no absolute viscosity of a pure solvent, += flow time for the polymer solution, flow time for the solvent. PROCEDURE: : r solutio if ferent concentrations: Polymer solutions of different concentrations say 0.15%, 0.30%, 0.4 0.60% and 0.75% are prepared from the given polymer stock solution. Step IT: Flow time of solvent: 20 mil of the solvent is taken into the viscometer and is sucked through the capillary tube upto the upper mark, without any cir bubbles. Now note the flow time of the solvent to flow from the upper mark to lower mark, Step ETT: Flow time of polymer solutions: Now fill the viscometer with 20 ml of one of the polymer solution into the viscometer and determine the flow time as before, Similarly the flow time of the other polymer solutions are determined Note: For each polymer solution, wash and rinse the viscometer with the solvent, From the flow times, reduced viscosity (nay/c) can be calculated, Graph is plotted between nep/¢ Vs Concentration. Straight line is obtained with an intercept called intrinsic viscosity (ni). nihumathulla. ka - Chemistry Lab = T Page 17Calculation: 163 on © log nj = logke | 4a nh) >@- Be Ke (aga) Tm fat aso. by =3 e.3o- (09 (45:3 Ke J Meg pqs 209 Ved n= Ah OTB m: antileg of Ciognj- log) q Antlog = 4 ho78 hikumathulla, ka ‘Chemistry Lab - I Page 18RESULT: ‘The molecular weight of the given. polymer =. 215% a x nihumathulla, ka Chemistry Lab - I Page 19pH ———+ Volume. of NaOH (ml) —» Volume of NaOH (ml) ———+ Ss etter tn ae ES alhumathulla. ka mistry Lab ~ I Page 20pH METRY - DETERMINATION OF STRENGTH OF Hcl By NaOH Experiment Number: fy - Date: 3.4: ets AIM: To determine the strength of given HCl by pH metry, a standard solution of NaOH of O.1N is provided, PRINCIPLE: Since the pH of the solution is related to the H’ ion concentration by the following formula pH= = log [H'] measurement of pH of the solution gives the éoncentration of H’ ions in the solution, When NaOH is added slowly from the burette to the solution of HCI, the fast moving Hons are progressively replaced by slow moving Na fns, As a result pH of the solution increases. . HE| + NaOH ——-—» NaCi + H20 The increase in pH takes place until all the H’ ions are completely neutralized (upto the end point), After: the end point, further addition of NaOH increases pH sharply as there is an excess of fast moving OH’ ions, MATERIALS REQUIRED: 1, pH meter. 2. Glass electrode. 3, Beaker, 4 Standard N/10 NaOH rrr nihumathulla. ka Chemistry Lab - I Page 21 | |Ge eao Oe oO e Chemistry Lab - T nihumathulla. k.a5. Approximately N/10 HCl. 6. Burette, Pipette, Glass red etc., PROCEDURE: The burette ig filled with standard NaOH solution. Exactly 20 ml of the given HCI solution is pipette out into a clean beaker. Tt is then diluted to 20 ml by adding distilled water. The glass electrode is dipped in it and connected with a pH meter. TITRATION - I First a preliminary titration is carried out by adding standard NaOH solution in portions of 1 mi from the burette to the H¢l solution taken in the beaker and pH of the solution is noted for each addition, This-process is continued until atleast five readings are taken after the eid point and the range at which the end point lies Is found out by plotting velume of NaOH added against pH TITRATION - IT Another titration is carried out by adding standard NaOH solution in portions.of 0.1 ml tear the énd.palht and pH of the solution is noted after each addition. The addition of NaQH is continued even ‘after the end point for further 1 ml, The accurate end pointiis féund out by- plotting ApH/AV against Volume of NaGH added. From the end point, the strength of HC! solution and hence the amount of HCl can be calculated + | nihumathulla, ka Chemistry Lab = I Poge 23 awJQ | Diop ft 14, 4 & 1___ 18 é Lh a ba 16. | is tag pap eed call [ae | | | ee Ke Lye eer 112, Chemistry Lab - I Page 24 nikumathulla, ke 370 OOoO8,CeK93S354h0yD B) SLNo | Volume of | NaOH (ml)! AY (imi) nihumathullo. ko Chemistry Lab ~ Page 25Calculation of Strength of HCl a Volume of Sodium Hydroxide Vi ld... ml Cfrem graph) e + Strength of Sodium Hydroxide Ni = QIN S Volume of Hydrachloric acid Ve= 20 ml 7 Strength of Hydrachloric acid Ne= ’ - According to the law of volumetric analysis, . VIN = VeNe 2 Nez Ye Strength of Hydrochloric acid ~ Calculation of Amount of. Hal: | ~ The amount of HCl present in. litte of 1 Ie given salution 5 a = Strength of HCl X Equivalent weight of HCl > sy 365 : x g a: acrglom : : 2 er ree neem nihumathutla. k.a Chemistry'Leb «I Page 26 aRESULT: 1, Strength of the given HC! solution 2, Amount of HCl present in { litre of the solution = nihumathulla. ka Chemistry Lob - 1. Page 27 vyGraph: Conductance. Vs Volume of NaGH I sg 8 S HS i 3 AT casi pote 5 8 1 a Volume ef NaOH (ml) —————+ ia err eet crete enn saa nihumathulla, ka Cheinistry Lab = I Page 28CONDUCTOMETRIC TITRATION OF STRONG ACID WITH STRONG BASE Experiment Number: Date: 3-4.20r8 AIM: To determine the amourit of hydrochloric acid present in 1 litre of the given solution by conductometric titration using standard sodium hydroxide of 0.5N. PRINGIPLE: Solution.of electrolytes conducts electricity due to the presence of ions. The specific conductance of a solution is proportional to the concentration of ions in it, The reaction between HCl and NaOH may be represented as Hel + NaOH ———» Natl + HO When the ‘Solution of hydrochlori¢ acid is titrated with NaOH, the fost moving hydragen ions are progressively replaced by slow moving sodium ions, AS a result conductance of the solution decreases. This decrease in conductance will take place until the end point is reached. Further addition of alkali raises the conductance sharply as there is an excess of hydroxide ions, A graph is drawn between volume of NoOF added and the conductance of solution. The exact end point is intersection of the two curves. MATERTALS REQUIRED 1, Conductivity bridge. 2. Conductivity cell, 3, Beaker, 4. Standard 0.5N NaQH nihumathulta, Chemistry Lal Page 29TABLE TITRATION OF STANDARD NaOH Vs HCl Conductance (mho) | SI, No Volume of NaOH added (mi) | 1 0 a hho ee ee gg ~ FBS, 4 et A io =<] ‘eae nT | a a0 nihumathulle, ka ‘Chemistry Lab- I” Page. 305. Given HCl solution. 6, Burette, Pipette, Glass rod ete, Pre Rl The burette is filled with sodium hydroxide solution upto the zero level. 20 ml of the HCl is pipette out into a clean 100 ml beaker. The conductivity cell is placed in it and then diluted to 50 mil by adding conductivity water, so that the electrodes are well immersed in the solution, The: two terminals of the cell are connected with a conduetivity bridge. New 0.5 ml of NaOH from the burette is added to the solution, taken in the beaker, stirred for some time. and then conductivity i¢ measured. The conductivity is going on decreasing upta the end point. This process is repeated until at least five readings are taken after the end point has been reached, Now the graph ig platted by taking volume of NaOH in the X - axis and conductance In the ¥ - axis, The end point is noted from the graph and the amount of HCl present in 1 litre of the solution is.calculated, Chemistry Lab - I Page #1Calculation of Strength of HCl: Volume of Sodium Hydroxide Vy -3:f... ml (From graph) Strength of Sodium Hydroxide Nis O5N Volume of Hydrochloric acid V2 = 20 ml Strength of Hydrechloric acid Nez > According to the law of volumetric analysis, VIN = VoNe % > LAM, ON a Net Strength of Hydrochlori¢ acid Calculation of Amount of HCl: The amount of HCl present in i litre of the given solution = Strength of HCl X Equivalent weight of HCl Chemistry Leb =I Page 32RESULT: The amount of HCl present in 1 litrg c Gn e a ¥ ihunathulla. ka Chemistry of the given solution ils gins Lab +E Page 33GRAPH: CONDUCTANCE Vs VOLUME OF NaQH | A x r elk ye B [rowed A et ° 3 egg e 8 i Volume of NaOH ———» . A nen reentrant rt = nihumethulla, koa Chemistry Lab ~I Page 34CONDUCTS: RIC TITRATION XTURE OF ACIDS (HCl.Ws CH;COOK To determine the amount of a strong acid and weak acid (HCI and CHsCOOH) present in one litre of the given mixture of acid solution by conductometric titration using standard NaOH of-0.5N. PRINCIPLE: ° Solution of electrolytes conducts electricity due to the presence of ions. Since the specific conductance of a solution is proportional to the concentration of lons in it, conductance. of the solution is measured during titration. When the sodium hydroxide is added slowly from the burette to the solution, HCl (strong acid) get neutralized first. Since the fast moving H’ ions are replaced by slow maving Na’ ions, decrease it conductance take place until the end point is reached, Hel+ NaOH ———~-» NaCl + HzO (first neutralization) After the complete neutralization of all HCl, the neutralization of CHsCOOH starts. CHiCOOH + NaOH =————®. CH3COONa + H20 (second neutralization) Since CH;COONa is stronger electrolyte than CHsCOOH, conductivity slowly increases until all CHsCOOH is completely neutralized. When the end point is reached, addition of NaOH will cause sudden increase in the conductance, This is due to the presence of fast maving OH" ions rrr rihumathulla. ka Ghemistry Lab = T Poge 35TABLE TITRATION OF MIXTURE OF ACIDS (HCI Vs CHsCOOH) Vs NaOH 8 | | a | oct wee ] 05 | - woh ee BED 10 | is |. 15 4 os | te Ase | 2.0 | LO... 28795 jo Pe nihumathulla. k.a 19 20 or ‘Chemistry Lob =I qo qs ineMATERIALS REQUIRED: (i) Conductivity bridge. (ii) Conductivity cell, (ili) Beaker. (iv)Standard 0,5N NaGH. (v) Approximately N/10 HCl Vs SEucQOH saan (vi)Burette, pipette, glass rod ete,, | PROCEDUR' The burette is washed well with water and rinsed with the given standard NaOH solution. Lt is filled with NaOH solution up to the zero level. 20 ml of the given.mixture of dcids (HCl and CHsCOOH) is pipette aut intoa clean 100 ml beaker, The conductivity cell is placed in it and then diluted to 50 ml by adding conductivity water, so that the electrodes are well immersed in the solution. The two terminals of the cell are connected with a conductivity bridge, Now 0.5 ml of NaOH from the burette is added to the solution, taken in the beaker, stirred for some time-and then conductivity is measured. The conductivity is going on decreasing upto the end point, This process is repeated until atleast five readings are taken after the end-point (A) has been reached, After the end point, again NaOH is graduelly added, which causes increase in conductance. This increase in conductance is observed until the end point (B) is reached. After the second end point, sudden increase in conductance is observed on further addition of NaQH. The reading (conductivity) is continuously measured for each addition of NaOH and are tabulated. Now the graph is plotted between the | volume of NaOH Vs Conductance, hihumathulla. Ka Chemistry Lat Page 37 SHel: Volume of Sodium Hydroxide Va = 0B. ml (1 re vay Strength of Sodium Hydroxide Niz 0.5N | Volume of (mixture) Hydrochloric acid Vz. = 20 ml Strength of (mixture) Hydrochloric acid = Ne = According to the law of volumetric analysis, VINi = VaNe Strength of Hydrochloric acid Calculation of Amount of Hi ‘The amount of Hel present in litre of the given salution = Strength of HC] X Equivalent weight of HCl = .QMABLS.... X 36.5 = BARD...gms RE TEE nihumathulla, ko Chemistry Lab.-T Page 38 eyeFrom the graph the first end point (A) and the second end point (8) are noted, From the end points amount of HC! and CHaCQOH present in 1 litre of the mixture of solution is calculated, Chemistry Lob - £ Page 39Calculation of 51 h of CH;COOH: 4 Volume of Sodium Hydroxide Vi = eB. ml (B-A) 3 Strength of Sodium Hydroxide - Ni = 0.5N 9 Volume of (mixture) Acetic acid Ve = 20 ml - Strength of (mixture) Acetic acid Ne = ss According to the law of volumetric analysis, nn ViNi = VoNe 2 Strength of Acetic acid “s Calculation of Amount of CH;COOH: ° The amount of CH3COOH present ind litre of the given solution oe = Strength of CHsCOOH X Equivalent weight of CHsGOOH > F oO. X60 3 = MS. Gms. 2 my PogeaaTe (® The amount of HCl present in 4 litre of the given solution = (ii) The amount of CH3COOH present in 1 litre of the'given solution =, nihumathulla, k.o Chemistry Lab = T Page 41 wbPr eer Seon, SHORT PROCEDURES a DETERMINATION OF CHLORIDE CONTENT. IN WATER By ARGENTOMETRIC MET HOD (MOHR'S METHOD: im sl. | CONTENTS | TITRATION-I |] TITRATION - IT | No . * "| (standardization of AgNO) | (standardization of, | ‘chloride) jo “T. |Burette Solution | Silver Nitrate ¢ol aire td Silver Nitrate | = ff tagttoy * solistidn tdgNto | 2, | Pipette Solution | Std. Sodium Wat A imi of 2 um bmi ° chromate (kgCrO4) | iromate (KeCrOe) ° solution Sy [solution | sa [Lab temperature | Lab temperature | ow 5. jE pt pont [Yellow tar reddish brown | Yellow to je reddish | « —L pemen) as he 2 6 | | Formula . Nes 3 VaNe Le was 5 i 5 NNN |) nihumathulla. ka Chemistry trate -I « Page 42 ryTITRATION (standardization of sedium | (Estimation of dissolved ‘thiosulphare) oxygen) T Secon thiosulphate td, Sod, solution (Nass Aa (Neos 203) | thiosul phate solution ~ It | 2, [Pipette Solution Std rota mate Water-somple + Jey i | (Ke6r20s) solution” | 3. | Solution to be added | 5 ml of HeSQa+ 151ml 5% | 2 mi Manganese co KE i sulphate + 2 ml alkali - m iodide +,2, ml Conc. ' H2504 = ndieater ~~ ~«| Storch | Starch. re | | | | | | r 4, | Indicator L 4. | Temperature oe _ [eae temperature ie | Lab temperature \ S| 5, | End point Blue te light green. Blue to colou 6 [Formula [Vath Vane Amount = Nx [equivalent wt of Ozx | | 1000 mgs Equivalent weight oF Oxygen = a Fa Obert G60} ssn eS Fi ba Bi a lds eal wenathulla, ka Chemistry Lab - I Page 43 * 20DETERMINATION OF MOLECULAR WEIGHT OF POLYVINYL ALCOHOL. Sere VISCOMETER The intrinsic viscosity is related|to the molecular weight by the following relationship, ‘ n= KM? where, n= Intrinsic viscosity, K & a= Constants for a given polymer - solvent combination at a given temperature, M= Average molecular weight Polymer solutions of different concentrations say 0.15%, 0.30%, 0.45%, 0.60% and 0.75% are prepared. i 20 ml of the solvent is taken.into the viscameter and is sucked through the capillary tube up to the upper mark, without any ain bubbles and the flow time of the solvent is noted, Various concentrations of polymer solutions (0,15%, 0,30%, 0.45%, 0,60% and 0.75%) is taken in the viscometer and their flow time is also measured. . From the flow times, reduced viscosity (My,/C) can be calculated. Graph is plotted between Nsp/C Vs concentration straight line is obtained with an intercept called intrinsic viscosity (ni). * GRAPH of ——+ Lan 1 Condentration ——e aren emanate name earnest ean tenement nihumathulla. ka Chemistry Lab~I Page 44SILNO | CONTENTS [TS TBurette solution t = 2 \ aL | Pipette solution 1 alia 3. Additional solution lL \ | 4 End point 5. Formula MiNi = WaNe Amount + N x Equivalent weight of HQ” fe ey "Equivalent weight of Hydrochloric acid = Graph - I Volume of NaQH (ml) —» ‘Wolinie of NaQH (jl) ———» y ere ore ere rihumathulla. ka Chemistry Lab - £ Page 45,CONDUCTOMETRIC TITRATION OF. STRONG ACID WITH STRONG BASE sINo [CONTENTS TITRATION 1.) | Burette solution | Standard Sodium Hydroxide solu | “Pipette solttion | ydrochlorie sci ‘solution | i rs [Additional solution | 20 il of conduetivity water | 4 “(ead pent | Conductance decreases upta the én point. | | After “that conductance increases | erliempeoeneresi al so | Formula Vd ; VaNez { | Amount = Nx Equivalent weight of HCl pit guivaient weight of Plydrachlarle ac Graph: Conductance Vs Volume of NaOH — $———— Equivelent Point Conductance (1/R) ——+ Volume of NaQH (iil). -———> Chemistry Lab - IGONDUCTOMETRIC TITRATION OF MIXTURE OF ACIDS {Hel Vs CH;COQH) [SLNO | CONTENTS | ‘TITRATION { ja os L Burette solution | Standard Sodium Hydroxide soluti: : 1 2, _ | Pipette solution Mixture-of acids (HCh& CHsCOOH) | | E . [3] Additional solution 20 mi of conductivity water -—~ | | = - - ——. = ~ ~ | 4 | End point | nce decreases slowly then increases | | | | sharply, finally conckictance increases | | 1 ‘ \ | | | | | foes athe peer re Formula Vint = Vai, | | | : | Amount 4N x Equivalent weight of HCl | | Attount 3 Nx Equivalent weight of CH:COOH ~~ Equivalent weight of Hydrochloric acid = a Equivalent weight of Acetic aci Volume of NaQH ——-——» nihumathulla, ka Chemistry Lab -T Page47VIVA - VOCE QUESTIONS AND ANSWERS. Determination of chloride content in water by argentometric method (Mohr's method, 1. What is the permeable limit of chloride’ in drinking purpose? — Less than 250 ppmy~ 2, Name the indicator used in this process. » + 2% Ke€rO4 (2g KaCrO, dissolved'in 100 m/H20) Potassium Chromate. » What is the end product of this process? — AgeCrO, (reddish brown precipitate) 4. In which form water contain chloride ions? — Water contain chloride ions in the form af Nacl, KCl, CaClzand MgClz. a What happens when standard AgNO is tittated against water? ~All chiaride ions are removed as Agcl. 6, Why does AgNO; combine first with chloride ions in the water and not with K2CrO4? i —+ Ag’ + Cl —+ AgCl (curdy white precipitate). AgCl solubility is higher than CrO4* ion. 2 Ag’ + CrO,” ——» AgzCrO4 (reddish brown precipitate), N What is the use of Argentometric method? — It is used to determine the total chloride ions present in water, What is the end point of the titration? — yellow to reddish brown (due to the formation of AgeCrO) = 2 What is the equivalent weight of chloride ion? — 35.45, eens eR nihumathulla, ke Chemistry Lab - I Page 48n w s N |. What are iodometric titrations? | DETERMINATION OF DISSOLVED OXYGEN IN WATER WINKLER'S METHOD) —» Iodometric titrations are those in which iodine is generated by the reaction of an iodine with and oxidizing agent like KMnOz, KoCr207 etc.., Give the ionic equation showing the reducing property of sodium thiosulphate? ay 25203 ————+ S4Q,"" + 2e° thio sulphate ion _ tetathionate ion How dissolved oxygen from water can be removed? — By mechanical deaeration: By spraying water in a perforated plate fitted tower which is heated from sides and is connected to vacuum pump'te reduce pressure inside, At high temperature. and low pressure solubility of oxygen in water decreases. By chemical method: : 2NazSO3 + Oz * ZNazSO4 Sodium sulphite sodium sulphate NasS +202 ———* NarS0s Sodium sulphide NoHy + 7 ———** Np + 2H;0 Hydrazine What is the amount of oxygen dissolved in water? 7-9 mgs/lit at a temperature af 25°C - 35°C, What is the purpose of estimating dissolved oxygen in water? — The estimation of dissolved oxygen in water is useful in studying corrosion effects of boiler feed water and in studying water pollution What is Winkler’s reagent? Potassium bromide + Potassium bromate. . How is iodine liberated when KI and HeSOx are mixed with KsCr2Or? ~+ KeCr2Or + TH2SO04+ OKI » KeSOq + Cre(SOx)s + TH20 + 312 ett nihumathulla. ka Chemistry Lab ~ Page 49The liberated iodine is titrated against: NazS203 2NazS203 + I » NagS20, + 2NaT 8. What is the reaction takes place when mangancus sulphate mixed with alkali - iodide? = Mn®* + 20H ——-—» Min(OH}et MnlOH}e + 402 “- MnOQ(OH)e) (yellow brown) What happens when Con.H2S04 liberating iodine and the liberated iodine is titrated against NazS20;? —+ The precipitate dissolves in Conc. Hz$0, liberating iodine and the liberated iodine is titrated against NasSzO3 MnO(OH)2 + 2H2S04, ———» Mn(SOx)2 + 3H20 Mn(SOu)2 + 2K ——--——+ MnSO4 + KeSO, #2 2NagS203 + Iz ——---—-—-» Naz$20¢ + 2NaI 10. What is the equivalent weight of oxygen? — Equivalent weight of oxygen is 8, 11. What is the indicator used? + Starch, (CsHioOs)s, @ polysaccharide. 0 nihymathulla, ko “Chemistry Lab +I Page 50a) DETERMINATION OF MOLECULAR WEIGHT OF POLYVINYL ALCOHOL USING OSTWALD VISCOMETER 1. What is a polymer? i + Polymeris a macromolecule formed by the combination af smaller molecules called monomers. 2. What are the examples of « polymer? © —+ Polyethene, polystyrene, polyvinyl chloride, polyvinyl alcohol(biodegradable polymer) 3, What is a Mark Hownik equation? a n= KM? where, n= Intrinsic viscosity, K & a= Constants for a given polymer - salvent Cambination ata given temperature, M= Average molecular weight. 4. What is meant by degree of polymerization? — Degree of polymerization is'defined as the number of repeating units present in a polymer. 5. What is a viscometer? — Viscometer is an instrument used to.measure the specific viscosity (ns) of liquid, 6. Why do all the monomers do not prodiice polymers? —+ The monomers which contain double bonds and bifunctional group form polymers, 7, What is the ynit of viscosity? — min/sec, nikumathulla, ko Ghemistry Lob - T Page 51 a 4 ey8. What is the unit of relative viscosity? —+ No unit. _ 9. What is viscosity? —+ Viseosity is the resistance of a liquid to flow when a stress is applied is ~ called viscosity. 10, What are the examples for high polymers? ~ + PVE, Teflon, PTFE, Nylon 6,6. - rem nea NE nihumathulla. ka Chemistry Lab = T Poge 2ge pH METRY - DETERMINATION. OF STRENGTH OF H¢l BY NaQH 1. What is pH? = pH = -logio™! What is the! purpose of pH - metry? — Measurement of pH gives the concentration of [H"]. From that, pH can be calculated. |. What happens when NaQH is added to HCl? — pH increases, because the fast moving H" ions are replaced by slow moving Nat ions. > Why the pH is sharply increases after the end point? — Due to the excess of OH’ ions from NaOH, a What is the electrade used in pH ~ metry? — Glass electrode. LY nihumathulla. ka ‘Chemistry Lab = 1 Page 53CONDUCTOMETRIC TITRATION OF STRONG ACID WITH STRONG BASE 1. What is the difference betweeh a solution ahd an electralyte? — Solution contains molecules, Electrolyte contains ions of the molecules which conduct electric current 2. What is meant by a specific conductance? — The reciprocal of specific resistance is called specific conductance 1,1 Ke lip? 5X 3. Why the conductance decreases initially when we add HCl to NaOH? =» The fast moving H” ions are replaced by the slow moving Nia’ ions, thereby concentration of H* ions decreases. 4. What happens at the end point? — The neutralization reaction between HCl Vs NaOH is completed. All the H” ions are completely replaced by No’ ions, 5. Why the conductance increases after the end point? + Due te the presence of excess of hydroxide ions, 6. What is the equivalent weight of hydrochloric acid? 4365 ee RR RRC Page 54 nihumathulla, ka Chemistry Laly =Ia : Be ey CONDUCTOMETRIC TITRATION OF MIXTURE OF ACIDS ‘ (HCI Vs CHsCQOH) ~ 1, Why acetic acid is a weak acid-and HCl is a streng acid? + Acetic acid undergoes partial ignization, Therefore it is a weak acid. “ CH\COOH <=" CHsCOO™+ HY e Hydrochlorie acid undergbes complete ionization, Therefore iris @ ‘ strong acid. ~ Hel=——+ fl «er = 2, Why the conductance is decreases initially? i + Thitially Na’ ions of NaOH replace H' ions of Hé!, So, concentration of H” a ions decreases, Therefore, conductance decreases, 3. What type'of reaction takes place initially? —+ Complete neutralization of H¢l by NaOH. 4, Why is HCl first reacting with NaOH? — Becouse it is a strong acid, undergoes complete ionization, a 5, What is meant by conductance? a — Recip-ocal of resistance is conductance. a all the H’ ions of HCl dre neutralized ond the neutralization of CHsCOOH A starts. é 5 7. Why there is a slow incréase in the conductance after the first end point? ~ — Acetic acid reacts with NaOH gives dodium acetate, which is a strong electrolyte than CH3COGH. Therefore, |conductance is slowly increases: 7a 8, What happens at the second end point? ~ All the acetic acid molecules are neutralized by NaOH, a: nihumethulla, ka ‘Chemistry Lab -T Page 55See nihumathulla. ka (3 \Why there is a sudden increase in the concuctonee after the second end "point? — Due to the excess of hydroxide ions from NaQH. (10, What is the unit of conductance? + mho(ohm’!) 11, What is equivalent weight ef HCl ahd CHsCOQH? s Hel = 36.6 CH;CODH + 60 ay» poate 20M Soohastt, kan salen, kompools es Charnes 8 me oe emcee ma on erm rane ee EN Chemistry Lab Page 56 IO 09 3 “O09 Rey