COLOUR PLATINUM COBALT (VISUAL COMPARISON) - 15: 3025 (PART=4) PRINCIPLES i Tac sample colour is measured by visual comparison with the known solution of Standard chisroplatinate, The Platunate produce the colour inthe form of chloroplatinate ion. (1 colour unit = I ma platinum per litre, APPARATUS: Nester eylinders SO'ml~ 6 Nos ii, Fitter assembly with fiter paper 0.45pm iv Centrifuge Note: ii & ii will be use f the turbidity present in the sample. Because the true colour cannot measured. so the removing of turbidity CHEMICALS: Patan cheopatnate,Cobtions chloride, i) Ca PREPARATION: we 1 Standard Chloroplaunave solution: Take 0.1264 jum chlorplatinate & 0.10 g cobalt 100 ml beaker containing 10m! Con. HCL dissolvs¥ properly and make up to 100 ml with distilled water ix Stondand Mas solution is 500 colour units This pnovURe: i 1 Take the 6 nessler evlinder in nessler stand as described below Standard chloroplatinate solution 50 ml sample 50 ml cis) Weter ee oe UN Known Ones 1 Units 2 Units Units 10 Umass Make up 50 ml 0 esek eylinder with dist, Water 2. Compare the Sample (Unknown) with Standard calution (Kuewn) ander a whate surface 3. Which s ample zndard solaou s anatebed with sample, its eolour ants is the enloue of. 4. {le sample wills not mach any standard, stl be ‘0 colour units RESULT: x canon - oar aris Celelaben = At @limetié tele of Somughae 4 opou MEPHOD: é 18; 3025 PART-5) APPARATUS: ‘Who month glass stoppered bottles | Iter, astivated carbon colour CHEMICALS: Hydrochlorie aeid, Activated Cor / The Wide mouth glass stopper bottles (lite) is rinse with hydrochloric acid (10ml) and make completely by rerestod washing with edour fee diated water which i prepared hy pass the dsiled water throwgh the ost (rreanarion OF APPARATUS: PROCEDURE: {As soon as possible after collection of sample, fill a Wide mouth glass stoppered bottles ({ fiter) half (S0Omi) o sample, insert the stopper and shake vigorously for 2 to 3 seconds and then quickly observed the odour. The sams taken for observation of edaur shall be at room temperature RESULT: pour; ages Disinea War | ACKIVATED, CARBON Burette coLouM Activated, Carhon Odour Free Distilled Water a Lae eeTASTE METHOD: V5: 3025 (PART ~8) APPARATUS: 100 Mi Beskers CHEMICALS: Sodium Chloride, REAGENTS: 1 Sodium Chloride: Take | g of Sodium Chloride salt dissolved in odour & Taste free distilled water and make up to 500ml. tins solution is used to rinse the mouth, PROCEDURI After collection of sample maintain the temperature at 15°C to 27°C. Then transfer the sample in 19 mal beakers (3 Nos) ‘Then select any 9 lactory Persons (At least 5 Persons) and give the samples to selected person -{ and ask to hotd for several seconds and discharge \t without swallowing (cating). Same manner remaining two beakers allow give to the same person | minutes twne intervals. Not the 3" heaker rating from the rating scale for sample record result on the data form which is given below. Runse the ‘mouth with taste snd odour fee distilled water and rest for one minute before repeating for next sample ‘The same manner give sample other 4 persons and note the result on the data form. Then note the Moan value from Rating, Seale DATA FORM PERSONS NAME Beaker-1 Beaker? [Beaker-3__| Rating Scale Persons -1 © ® ae Persons I b 5 1B = i Persons -{Il a _ ae 4 [Persons -IV A i Persons -V ¢ ae = al Twould be very happy to aocept this water as my evervelay drmking water by) T would be happy to accept this water as my everyday inking water ©} Tam sure that | could aecopt this water as my everyday drinking water 4d) Teould accept this water as my evervday drinking water, RESULT: TASTE Agroeable (Rating Seale A)TURBIDITY METHOD: NEPHELOMETRIC - Ts: 3025 (PART — 10) APPARATUS: ‘Turbidity Meter, Filter assembly CHEMICALS: Hexamethylene Tetramine, Hydrazine Sulphate REAGENTS: 1 Mexametiyloe Tesamie Staion ANT | Take 10 g of Flexamethylene Tetramine salt dissolved in 100m! of distiled water > Livdrazine Sulphate Solution va Take 1 g of Hvdrazine Sulphate salt dissolvec sh £0 ml of distilled water Turbidity Standard Suspension I (400 NTU Solution) Take 5 ml of Hexamethylene Tetramine Solution and 5 ml of Hydrazine Sulphate Solution ia 100m! standard Fiask Mixed well and store in dark room for 24 hours a room temperature. Then makeup the solution up to 100m! with Distilled water Propare freshly every month 4 Turbidity Standard Suspension Il (40 NTU Solution}: Take [Oml of Turbidity Standard Suspension I (100 NTU Solution) and make up to 100 ml vrith distilled water Prepare fresh every sveekly = Repeat the steps which are given in above unt! the meicr shows concoréan: ResuLt TURBIDITY 2nru 4 RK Coletcten ts - uate: E\ Flrsth Rendle » g/t = a Me Mais Oo ovllygecien oF Vee Veclaseree ora al oy the Stomple baleenpH VALUE METHOD: ELECTROMETRIC - 1S: 3025 (PART~ 11) APPARATUS: pH Meter, Magnet Stirer, Thenmomter 05 Least Count) CHEMICALS: pH Buffor Tablets 4.00, 7.00 & 9.20, REAGENTS: 1 pH Buffer Solution 4 00 Take 4,00 pt Bulfer tablet and dissolved in 1 tlm! of distilled water 2 pli Buiter Sohution 7:00 “Take 700 pH Buffer tablet and dissolved in 110ml of distilled water PROCEDURE: ‘+ Set the temp knob in actual solution temperature which is finding by thermometer ‘= Take 7 00 butfer solution and immerse the electrode then adjust the reading to 7 00 using CA}. (7.90) knob + Take 4.00 buffer solution and immerse the electrode then adjust the reading t 4,00 using SLOP (4.00) knob. = Repeat the steps which are given in above until the meter shows concordant values. ‘Take sample water in beaker and immerse the electrode and stir gently note the reading after 20 seconds. RESULT: pl VALUE BSTORS‘TOTAL DISSOLVED SOLIDS METHOD: GRAVIMETIC = 1823025 PART- 16) APPARATUS: Drying Oven, Desiveators, Analytieal Balance, Evaporating Dish (100m!) PROCEDURE: + Take 100ml evaporating dish, wash with distilled water and kept m oven for ene hour at {113 Then coo! mn desiecators for 15 minutes, take the empty weight of the dish (W>) ‘© Kepr the same evaporating dish on a water bath with 100 ml sample and de continne evaporation unl; she sample cevaporaté : + Afier complete evaporation of water cesidue wrll form, transfer the dish to an oven and kept for one hour at 103° ‘Then cool in desiceators For 15 minstes, take Ui finel weight ofthe dish (W2) CALCULATION: : - Total Dissolved Solids, Me 1900x1900 «awe. ‘Vehumie of the Semple aken (100m!) [060 x Wart mlyenenn Hf Wa ethewstte reed fi ‘TDS METER METHOD vreble Resehic , msl = PROCEDURE: ‘Set the temp knob in actual solution temperature which is finding by thermometer Function knob in CHECK position adjusts the reading to 1.000 using BACK SIDE knob Function knob in CELLCONSTANT position. adjusts the reading 1.000) using CELL.CONS? ANT knob Function knob in TDS position immerses the electrode in sample water which is taken in beaker and sti geatly nove the reading after 30 seconds. = Range knob is selected depending the sample TDS. For Product water 20ppm & 200ppm, for Raw Water 200ppm. 2000ppm and above, tps So0me¢ ALKALINITY METHOD: POTENTIONMETRIC (TITRATION) : 1S; 3025 (PART —23) APPARATUS: : pH Meter. Magnetic Stirrer & Burette CHEMICALS: Sulphuric acid, Phenolphthalein, Methyl Red, Bromocresol ireen Indicators, Sodium Carbonate, REAGENTS: 1. Sulphunc Acie (0.2) Take 2.8 ml of Sulphuric Acid inake up to $00 ml with distilled water {akg lof Sulphss eid (2N) ke upto 500 m-th dled wate. 3) Dissolved 0.5 g of Phenolphein mn 100 mal of (1:1) algobo ~ water mixture. — PRocepurr: {if phenolphthalein alkalinity absent add 2 10 3 drops of mixed indicator solution directly i sample or Tf phenolphthalein alkalinity present add mixed indicator m already titrated solution then Tittate against) 02N Suipburie “cid ‘end point is presence of pink colour (B) CALCULATION: Alkalinity, Mgil = (ASB) _» 0.02 50,000 ‘Volume of the Sampls taken (100m) A ~ Phenolphthalein titration value { / B — Mixed indicator titration value. RESULT: eat Alkalinity 200mg én.cutorior Merion: ARGENTOMERTIC (TITRATION) = t8:3028 (PART-32) APPARATUS. Mognetc Sterer & Bute cheMicats: Potassium Chrome, iver Nite, Sodium Chloride, Nitric Acid Sodan Carbonate REAGENTS mates oF 1. Potassium Chromate Indicator 3D > & Dissolved 5 g of potassium chromate in 100m of distilled water. ot? 2. Silver Nitrate (0.0141) —=— © Take 1 1975 g of silver mtrate dissolved and make up to $00 mi with distilled water PROCEDURE: Take 100 mal of sample add Imi of potassium chromte ttate against Silver Nitrate :0.01-41N) end point presence ot break ted colour Ww CALCULATION Chlonde, Matt Titration value Volume of the RESULT: . Chloride 200meARESIDUAL FREE CHLORI METHOD: 1ODOMETRIC METHOD (TITRATION) - 1813025 PART-26) APPARATUS: plt Meter, Magnetic Stier & Buretts CHEMICALS: ‘Acetic acid Glacial. potassium chloride, Sodium thio sulphate, Potassium dichromate, starch indicator. REAGENTS: F Sodium Thio suifphate (0. IN) Take 12 5g of Sodium Tino sulphate dissolved and mvike up to 300 with dishlled water 2 Sedum Iho sulphate (0.01) Take 50/ml of Sodium Tho sulphate (0.1N) make up o $0C mi with disiled water Starch Indicator: ‘ Dissolved | gof sarch mndicator dissolved in 100 ml of distilled water and boii vigorously for few minutes. PROCEDURE: ‘Take 1000 inl of sample in iodine Aask add Iml of Acetic Acid glacial uid 1 g of Possum iodide and 1 eal of {6 stareh indicator (Freshly Prepared), ee a so Titrate aga the solution with Sodium Thio sulphate (.01N), end point disappearance of blue colour. Note 1 = (After adding of starch indicator if no blue colour developed mean residual free chlorine is BID. ee Ni) Note, 2:- (If raw water taken for esting 100 inl of sample is suicient) CALCULATION: Residual Free Chlorine, Mg == Titration Velus_< 0.01 x _ 33.450 Volume of the Sample taken (10%mi> RESULT: Residual Free Chlorine 0.2 Mgf.y, \ SULPHATE METHOD: TURBIDITY (SPECTROPHOTOMETER ~ 420NM) 3 18: 3025 (PART — 24) APPARATUS: “Magnetic Stirer, Spectrophotometer & Lab glassware CHEMICALS: Banum Calonde, Glycerol, Hydroehlonie Acid, lopropyl Alcohol, Sodium Chloride and Sccvum Sulphate REAGENTS: |. Conditioning Reagent Mix 25m] Glycerol, 1Sml Con, Hydrochloric Acid, $0ml Isopropyl Aleoho! and 150 ml distilled water disw ty 3755 g of sodium chioride. 2. Stock Sulphate Solution: (ml = 0.1 mg of sulphate: Take 0.0735 x of Sodium sulphate dissolved and make up to 500 mal with disited water. 3. Hydrochloric Acid (1:9): 7 ‘Take 10ml of Con. Hydrochloric Acid sand add in to 90m of distilled water and mix well. Cool PROCEDURE: ‘Take 6 No’s of 50m Nessler's Cylinders Nessler’s Cylinder I Take 25ral of sample Nessler s Cylinder tf Toke 2 riot Blank (Distilled Water) Newsler's Cvimder 1 Take | nl Stock Suiphate Solution Im= 4 the of SOs! Nessler’s Culinder 1V Take 2oil Swok Sulphate Solution Nessler’s Cylinder V Take Am! Stock Suiphate Solution Nessier's Cylinder VI Tak “im Stock Sulphate Sofution ‘Add each cylinder Iml of Hydrochloric Acid (1:9) and ml of Conditioning Reagent end 1 g of Beruim Chievide dissolved ‘well and makeup to 50m! with distilled water. Take the OD (or! ABS Values in spectrophotometer ut 420 nm Draw the graph ABS Values Vs Mg of sulphate soluton. Then take the graph values trom graph CALCULATION: A Sulphate. Mg = rah Value 3.1000 Voiume of sample rer (25n49 RESULT: ‘ Swiebate zl at Ln :METHOD: VOLUMETRIC : ANNEX F OF IS: 134287 APPARATUS: Hlot Plate, Filter Assombly & Magnetic Stirrer. CHEMICALS: “ Ammonis dichromate, ammonium acetate, Ammonium Hydroxtle(Ammonia Solution), Potasium iodide Sodium thiosulphate, Hydrochloric Acid & Ammonium chloride, a a a REAGENTS: 5. Ammonium dichromate solution. Dissolved 25g of ammonium dichromate and make up to 250ml with distilled water 2, Ammonium acelate solution: Dissolved 75, of ammonium acetate in 150ml of distilled adjust the pHI of this solution to 7.00 using ammonia solution then make up to 250ml with distilled water, 3. Dilute ammonium acetate wash solution Take 10tnl of Ammonium acetate solution make up to $00m! with distibied water, 4. Potassium wile solution (10%) Dissolved 25g of Potassium lodide and make up to 250 mi with distilled waver. 5, Sodiuma Thio sulphate (0-1N): Take 12.5 g of Sodium Thio sulphate dissolved and mnake up to 500 with distilled water 6. Sodium Thio sulphate (0.01N) Take 56 ini af Sodiura Thio sulphate (0 IN) make up to 500 ml vith distlled water: PROCEDURE: mn Beaker add few drops of 111 (1:1) reduse the volume to about 200 mf by heptn ‘Take 000m of samy hot plate at 90°C Note (1 10H0ml Beaker not available eke SiN ml beaker ist add 400m sane relat 4m ad 1a in the same redice to 100% again ad 300m] sample in the same then finaly reduce to 200ral) ‘Add 0 Sgemmontum Chlonde and }Oma! Arimonia sotation Kept to boiling. Then Ger the solution sng acinar fikor (ee ‘ “Take tae fate ada’ 0m! of ammonium acetate solution (Excess) Bol ths solution ad Smal of AmmoblutaSilionmnts solution with continous stirring ustig gIEE rod. Coohthe solution atroom temperature Then Ble the soution using Whatren fier paper. Wesh the Filter paper with dilute a paper decolorized “Faeon the fker paper in iodine fask add 10 rl (1:1) HCI. and 100mt hot water (dsilek water) Shake well and add SOml of potassium Iodide + lml of Stach solution. . “Ttvate the solution against sodium thio sulphate (.01N) unl the blue colour disappess (ate solution unil filter Note -( after adding starch ifn blue colour present mean bartam will be a BDL range) CALCULATION: Banum, Mg = Litration value X-0.04 5 65.78 X 1040 Wate oA e oF ample taken (10nd Vols RPSULT: Hains ome dCOPPER . METHOD: | NEOCUPROINE + 18:3025 (PART—42) | APPARATUS: Specttophotometer (457M), Hot Plate & Separating funnel. CHEMICALS: Chloroform, Hydrochloric acid, Hydroxylamine hydrochloride, Isopropyl alcohol, Neceuproine, Nitric acid, Sulphuric acid, Sodium ciate, copper metal powder, Hydrogen peroxide, Anunonium Fydroxide(Ammonia Solution), REAGENTS: 1. Hydroxylamine hydrochloride solution: Dissolved 20g of Hydroxylamine hydrochloride and make up to 10m with distilled water. 2. Neocupromne solution: Dissolved 0 1g of Neocuproine in 50ml of Isopropyl alcohol then make up to 100ml with distilled water distilled water Sodium extrate solution: Dissolved 25 g of Sodium citrate and make up t9 100ml with distilled water. AV 4 Stock Copper (In solution: (1m =0.2mg) Dissolved 0p pure copper metal powder in 100ml beaker ad nl of (1:1) Nit aidan Suc of Con, Su A acid evaporate the solution to dryness. Then dissolved the residue using distilled water then make up to 500ml with di So) water, 5 Intermediate Copper (1) solution: (Imi = 0.02mg) Take 10 ml of Stock Copper (ID solution and make up to 100 ra distilled water. PROCEDURE: Take 6 No's of Separating tunnel ey Funnel 1(250mN Take 50m! of sample Funnel £112Simb Take 50m! of Blark (Distilled Water) Svea ILC 2Smty os ml intermediate Copper Solution (Ten = 9 oF Copper: Funnel (V/12Simle Fake 2ml Intermediate Copper Solunion Funnel V (125ml ‘Take 3iml Intermediate Copper Soluion annnel VI( 25m) ‘Take dm Intemmediate Copper Sotaton ‘Add all separating funnel Sml of hydroxylamine Hydrochloride Solution + {Oml of sodiumn citrate solution + 1W-al of Neosupsine Solution shake well for few sects, ‘Add 20mi chloroform shake for | minute vigorously. Then allow I minute settling the layers. Separate the chloroform layer is nesslere oylinder. ‘Take the OD value of standards and sample using chloroform layer in spestrophotometer at 433NM. Draw the graph Mg of Copper Vs OD Valves of Standards, : 451 : . CALCULATION: Copper.Mg = ‘Graph Value X 10k Volume of saraple taken, RESULT: Capper 0S mg/ 3IRON METHOD: 1, 10 PHENONTROLINE. - TS 3025 (P-S3) APPARATUS: Spectrophotometer (510 NM), Tot Plate & Conia! Ask 250m, citeicats: Hyerochlorie Acid, Hydiox) lamine Hydrochloride, Ammonium Acetate, Sodium Acetate, 1,10 Pehnathroline Sulphuric Acid, Ferrous Ammonium sulphate, Di leo propyl Ether, Potassium permanganate REAGENTS: 1. Stock eon Solution: ‘Add 10 mil Cone.412so4 to 2Smul water contained 250 mi beaker and Dissolve 0.702 gan ferrous aramoniam Sulphate Add potassium permanganate drop wise until «faint pm color persist. Make up to SOC ml dishlled water Hani = *n0ug of Fed 2. Mandate on solution peue ml stock ZEA efution nto a SO0ra standard Ns imix well (1 Ol = J0.mg of Fe 3. Hydroxylamine Hydrochloride 10g of hydroxylammne Hydrochiorsde in 100m! water 4. Ammonium Acetate buffer solution, Dissolve 25 gm ammoniuan acetate in Sun distilled water and 70m! glacial aceue az. 5.1, 10 Phenonthroline Solution: Dissolve 0.1mg of 1,10 Phenonthrolins in 100ml of distilled water, Boil slishdy fox cisolvation. monet Puno Comical Flask 1 Take 50m of sample Conseal Flask I ~ Take 50ml of Blank (Distilled Wate Comical Flask 117 Take 1m Standard fon Solution (Im! =0.02Mg of ron} + 49 aii Pastiled water Conical Flask TV = Take ml Standard Iron/Solution + 48 mi Distilled wate Conscal Flask V ake 3ml Standard Iron Solution +47 mil Distilled water ~ Conical Flask V1 Take 4ml Standard ron Solution + 46 ml Distilled water ‘Add all Conical Flasks Iml of Hydroxylamnine Hyarochloride Solution + 2ml of Con. HCL, Then Ke>¢ the all flask im hot plate and reduce the value about 20m ‘After cooling add all flasks 10ml of Ammonium Acetate Guffer Solution + 10ml of 1,10 Phenontrols>: solution then make up 'o 100mm) with distilled water using nessler eylinder respostively. 12 oF ron Vs OD Vanes of ope Take the OD vahue of standards and semple in spectrophotometer at SIONM, Draw the grap Standards CALCULATION: t Iron. Mei = Graph Vi Volume of sample taken ($0ml) ron O ImgMANGANESE METHOD: i POTASSIUM PERIODATE + 18:3025 (PART-59) APPARATUS: Hot Piste, Distillation Apparatus, Gibbs Apparatus (SOz Generator) & Nessler Cylinders (100m). CHEMIGgLS: Sulphuric aeid, Hydrogen peroxide, Nitric acid, Potassium Permangunate, Ortho Phosphoric acid, Potassium Periodate REAGENTS: AF B51 oe Sophie cid) we Take 30m of Distled water in 250m bskar ad Som of Con Suhre Acid slowly with continuous ting ose gf 2/5 2 tydtogen peroxide: Nini cid Mixa Ke Dissolved 0. 1g of Neocuproine in 50m of Isopropyl alcohol then make up to 10(ral with distilled water distilled water 3 §. & Stock Manganese solution og Measures 45.5ml of 0 IN Potassium permanganate solution into a 250m! beaker add $ drops of Dilute Sulphuric > 53 © Acid (1°, bol the solution then add con. Sulphur dieside drop by drop until the solution decolorize, Boil dhe solution tor gj % !Sammutes thon make upto 500ml with distilled water 4, Standard Manganese solution Take 50 ml of Stock manganese solution listlled water. | Sm of Dilute Sulphuric Acid (1.1) then make up to 500m! with 5. Potassium permanganate 0.1N solution: “Take 0.316g of potassium permanganate dissolved and make up to 100rnl with distilled water nical Flask 1 Take 10ml of sample Comeal Flask TL = Take 100m! of Blank (Prsntlet Water) Conical Flask 1) Jake t mi Standard Manganese Solutions. (Imt=() 02Mg of Mr)#-99 mi Dislices water Conical Flask IV Toke 2ml Standard Manganese Solution + 98 mi iDisilled water Conical Flask V ‘Take 3ml Standard Manganese Solution + 97 ml Distilled se: Conical Flask ¥¥ E ‘Take 4ml Standaré Manganese Solution + 96 ml Distilled water ‘Add all conical flasks 4m! of sulphuric acid (1:1) and evaporate to farming using hot plate, Cool for few minutes ‘Add 4 drops wi hydrogen peroxide- Nitne acid Mixture and Bciled for 5 mutes. Then Coot 3 ‘Add 50m of distilled water + 2m] of ortho Phosphoric acid + ().2g of Potassium Periodate kept all flasks for vigorous boiling for! 3 hour in hotplate at 90° C a ‘After that the covcur will developed then transfer the solution to nessler cylinders and make up to 100ml with éistlled water. Compare the colors ofthe sample with standards. CALCULATION: Magamese Mail = Matched exlied al Volume of sample taken ( RESULT Manganese U tmgt IsNITRATE (NO3) METHOD: DEVARDASS ALLOY -3S 3025 (PART34) APPARATUS: Kjeldhal flask apparatus, Ph Meter, Heating Mantle cHEMica} Devardas allay, Borie Acid, Sulphrurie Acid, Sodium Hydsoxide, Sodium Tet borate, Methylene Blue Ethanol, Isopropyl Alcohol, Methyl red indicator, Mercurie ledite Potassium Iodide, Ammonium Chiorics. ‘REAGENTS: } Borate buffer solution Take 44ml of 0.1 N NaOH in 250ml of standard flask make up to the mark using (0.025 M) sodium tetra borate (2.368¢m sodium tetra borate(Borax) in 250m: distilled Water) and made up to 500ml with distilled water Mixed Indicator solution 11g of methyl ted dissolved in 50m of isopronv alcohol. 0.05g of methylene blue dissolved is 25m! of sopropy! alcohol Combine these two, 3 Rorie acid solution Dissolved Spi of boric acid in 300ml of distilled water add Sm mixed indicator then make up to SO0mt with, distilled water PROCEDURE: Take 250m! of saraple in Beaker (250m!) add 12.Sml of Borate huier solution then adjust the pT ofthe solution to above 9.5 using INNIOH, ‘After that transfer the solution to Kjeldhal apparatus then start the distillation. Collect at leas! (50m! of dis ‘Then stop the distillation, Discard the distillate which was collected ate Then add 1g of devardass alloy powes + 10m of distilled water round bottom flask. impress tke ed ofthe condenser Indicsting bore acid solution which is taken in Beaker. Star the distillation and collect 75m of distillate in the same beaker. Titrate the solution wash 0 2 Sulphune Acid. [’nd point presence of Bie colonr (Tavender Blue) CALCULATION: x Nutrate, Mel = Tiration Val 0 = ‘ Volume of sample (250m!) RESULT: Nitrate 45Mg/ITRITE (NO2) METHOD: SPECTROPHOMETRIC - % 18:3025 (PART 34) APPARATUS: ‘Spectrophotometer (543NM), Nessler tubes (50m) & Distillation apparatus, CHEMICALS: Potassium Permanganate, Calsium hydroxide, Sulphanilamide, Hydrcchlorie acid, NED dihydrochlorie. acid, Sodium Nitrite, Chloroform REAGENTS: 1. Sulphanilamide Sohuton: Dissolved 2.5g of the sulphanilamide in 25ml of con. Hydrochloric acid and 150ml of distilled water then make tp to 250ml with distilled water 2 NED diltydrochlonde Solution: Dissolved 0 25mg of the NED dihycrochtorie and make up to 250m with distilled water, Stores mn dark bole 5. Stock Nitrite solution. (Lil = 0.25Mg of NO3) Dissolve 1616p of sodium nitrite and make up to 500ml with distilled water. 4. Intermediate inte solution: (Iml= 0,05Mg of NO2) Take 50 ml of Stock nitrite solutien and up to 250ml with distilled water 5. Standard Nitnte solution: (1ml = 0,005Mg of NO Take Sil Intermediate nitrite solution and meke up to 500ml with distilled water Take 6 No's of SOml Nessler’s Cylinders) Nessler's Cylinder 1 -—~ Take 25m of sample Nessler’s Cylinder Tl Take 25m! of Blank (Distilled Water) Nessier's Cylinder Ill Take | nel Standard Nitrite Solutton + |sel = d.005Mg of O Newsler’s Culider 1V Jake 2m standard Nitnte Solution | ake Il Standard Nitrite Solution Nessler » Cylinder V Nessler’s Cylinder VI ‘Take 4m Standard Nitrite Solution PROCEDURE: x Then ad each cylinder Imi of Sulphanailamide Solution and wait for 3 minutes, Then add I ml of®ED dihydrochlyride and ‘want for $ minutes, Then make up to 50 ml with distilled water . ‘Toke the OD valuc of standards and sample in specirophotometer al 540 NM, Draw the graph Mg of Mitnte Vs OF Vaies of Standards, : CALCULATION: Nutnte, Mev! RESULT. Niante omALUMINIUM ‘METHOD: ERICHROME CYANINE R DYE : 15 3025 (P-55) APPARATUS: Spectro photometer (835M), Nessler thes (50m) & pli meter CHEMICALS: Ascorbic Acid, Sodium Acetate, Acctic Acid, Sulphuric Acid, Sodium Hydroxide, Eriochrame Aluminimum Potassium Sulphate, Methyl Orange, Di-Sodium EDTA dehydrate REAGENTS Stock Entchrome Cyanine R Dye Sniuton: Dissolve 0.3g of dye in to 50 ml water. Adjust the pH 2.9, with the help of 1:1 acetic acid dilute to L0Omt with distilled water. 2 Workung Erichrome Cyanine R Dye Solution Take 1Oml of stock dye solution and make up to 100 m] with distilled water. Stock alunsinrum solution: (Iml = 0 Smg of aluminiusn) Dissolve 4.3955gm aluminium potassium sulphate ann! make up to 500 ml with distilled water + Standard Aluminium solution: ( 1ml = 0.095mg of aluminium) ‘Take Sml of the stock aluminium solution and make up to 500m] with distilled water 5. Buller Solution: = Dissolve 13.6gm sodium acetate in water, Add 4 mil of IN Acetic.ccid, aad dilute te 100ml with distilled water. (IN Acetic acid: 5.4 ml of acetic acid and make up to 100m! with distilled water) 6 Ascorbic Acid: Dissolve 0.1mg of ascorbie acid in 100m] water of distilled water PROCEDURE: ‘Take 6 No’s of 501ml Nessler's Cvtinders Nessler’s Cylinder { ‘Take 251al of sample + ML of 0.02N H2S04 Consuinet for Alkalinity at 25m sample taken, Nessler's Cylinder 11 - Take 2Stal of Blank (Distilled Water) + ml EDTA (0 CM) Nessler’s Cylinder Ill ‘Take 1 ml Standard Aluminium Solution (Iml = 0.005Mg of AD) +26 ml Distilled wot Nessler's Cylinder IV -— Take 2m! Standard Aluminium Solution +23 ml Dosti-ed water Nessler’s Cylinder V ‘Take sol Standard Aluminisim Solution +22 ml Distied weter Nessler’s Cylinder V1 Take 4enl Standacd. Aluminiuin Solution + 21 ml Distilled water ‘Then add cach cylinder Iml of 0.02N H2S04 except Hank. Add each cylinder Iml of Ascorbic Acid ~ 10m! of Butter Solution + Sml of Working Erichrome Cynine R dye Then Mehe np to SOml with distilled water. Take the :°} wshic of standards and sample in spectroshotometer at 535NM. Di Vahies of Standaids raph Mg of iluminum Vs 01D CALCULATION: . Nitrate, Met = Graph Vsituc Volume of sample taker RESULT. : Aluminum OR meh > 1,Cree ZINc METHOD: ZINCON a 15 3025 (P-49) APPARATUS: Spectrophotometer (620NM), furme hood & 250ml standard flask CHEMICALS: costae Sulpinte wala Acetate, Acetic Acid, Sulphuric Acid, Sodium Hydroxide, Eriochvome Cysnine R Dye, Aluminimum Potassium Sulphate, Methyl Orange. Di-Sodium EDTA dehyesas REAGENTS: : 1 Zine Ul solution: Take 0.1372g zine sulphate and make up to 500ml with distilled water 2 Potassium eyanide solution Dissolved 1gm KCN in 50ml of distilled water and dilute to 100m 3. Cvclohexonane solution Dissolve Iml of purified cyclohexonane in 50m! of distilled water 4 orate buffer solution, Dilute 106.Sm IN NAOH make up fo 250m with dstiled water and dissolve 18.63 gm potassium chloride and 15.5 am borie acid make up to 500ml with distilled. Water. 5. Zincon sohutios 0.325¢m of zincon in 100ml of methanol by heating gently. Cool Dilute to 250m with metbano! ina 250 tml standard flask. Stored dark color bottles PROCEDURE ‘Take 6 No’s of 250m! Standard Flasks Standard Flask | Take 10ra! of sample Be Standard Flask 1 Take 10ral of Blank (Distilled Water) Standard Flask UL Take 1 ml Zine If Soluuon (ml = 0, Img of ZN) Standard Flask 1. sw> Take 2ml Zine II Solution Solution Standard Flask V ‘Take 3ml Zine Il Solution Solution Standard Flask V4 Take 4rml Zine {J Solution Solution ‘Add all asks ml of Potassium Cyanide Solution + 5inl of Borate buffer Solution + 3ml of Ziason Solution + Im of Cyclohexanone Solution, Shake well for few minutes then make up to the mark with distilled water Take the OD value of standards and sample in spectrophotometcr at 620NM, Draw the graph Ma of Zine Vs OD Values of Standards, CALCULATION: Zane, Mgll . Graph Value X 1000 . Volurae of sample taken (10m, RESULT Zine 5 Maa 6~ oe Ks CALCIUM METHOD: DTA VOLUMETRIC (TITRATION) : 1S: 3025 (PART ~ 40) APPARATUS: Hot Plate, Hot air oven digital & pH meter. CHEMICALS: Sodium Chloride, Patton & Reeder's, Hydrochloric Hydrochloric acid ‘nchrome Black T, Hydroxylamnine Hydrochloride, Methanol, Caleium Carbonate, Zine Metal id, Nitic Acid, Sodium Hydroxide, Disodium EDTA dehycrate, PotassiumBulphate & REAGENTS: 1 Sodium Hydroxide (IN NaOH) 10 gm sodium hydroxide dissolved in 250 ml of distilled water 2 Sndard EDTA solutions -0.01M: Dissolved 1,875 gm EDTA in distilled water and make up to 300m : PROCEDURE: \ Fined Take 100 ral of sample add 2mnl of NaOH (IN) and 1 fa} of Patton and Reeder indicator and titate aguinst EDTA, (©-0194) end pin presence of pre blue ealr (Vn CALCULATION: Calcium, = Titration value_< 0.0] 1000 woe: & fe ‘Volume of the Sample taken (100ml) = RESULT: Calon 75 gil 20a MAGNESIUM METHOD: EDTA VOLUMETRIC (TITRATION) ~ 18:3025 PART - 46) APPARATU Hot Plate, Hot a oven digital @ pH meter CHEMICALS: Sodium Chloride, Erichrome Black T, Hydroxylamine Hydrochloride, Methanol, Calcium Carbonate, Zine Metal Poe e seas Hsdrochlri asi, Nite Acid, Sodium Hydroxide, Disogium EDTA dehyiate, Potssans Solphers ‘Hycrochlorie acid, Ammonium Chloride, Ammonium hytoxide & ricthanol sire REAGENTS: ="5, 1 Ammonium buffer solution z Dissolve 35g ammonium chione and 285 ml ammonia sohtion and 215 ml distil ater nf iiehgome black -T (0.2gm EBTand 2.254gm hydsoxylamine hydrochloride and SOml ethanol / ethanol 5 PROCEDURE: Take 100 ml of sompie add Sm of Ammo bulfer solution and 3 to 4 drops of EBT indicator and Reeder indicator and Strate against EDTA (001M) end point presence of sky Bice coloxs (V2) vA CALCULATION: Mognessam, Mgt = Wan 01 «1000 x 2434 z ‘Volume othe Sample taken (100m) : RESULT: Magnes 30mgSULPRIDE METHOD: METHYLENE BLUE : 1s 3025 (P-29) APPARATUS: Spectrophotometer (GO0NM), Droppers & Matches Test tube. CHEMICALS: se oamattel F-Phenylene Diamine oxalate Sulphuric acd, Ferric chloride, Methyl blue, Diammonium hydrogen * ortho phosphate, Sedum Sulphide REAGENTS: 1 Amine sulphune acid reagent soliton Dosolved 0.675g of NIN Gimethylenediaming oxalate n 100ny of (1 Sulphurie acid ee Store m dark gas bot 2. Fore chloride solution: Dissolve $0gm ferric chloride in 20m! of distilled water, Z 3. Diammonium hydrogen phosphate solution Dissolve 40g of Diammonium hydrogen phosphate in 80m] of cisuilled water. 4. Methylene blue solution I: : Dissolved 0.1gm of Methylene blue in 100ml distilled water. 5. Methylene blue solution I ‘Dilute 10 ml of Methylene blue solution | to 100m! with distilled water proceyime: 7 Take 2 flo's of SOml Nessler'sCylindsr like a Tube A and Tube Is Tube & Tube B Taker sample 0'5tal ot Amine Take 7 $ sample +0.Sml of 1) Sulpure Ace -+0.15 mtor Sulphuric Acid +0.15 ml of Fernie Chprade Chloride Note (IfNo Rilue eolor m Tube A sulphide is BDI.. If biue colour developed in Tube A sulphide i presence.) Add 1.6m1 of Di ammomum Add 1.6mlof Di ammonium Hydrogen sulphate Solution Hydrogen sulphate Solution Wait for 3 minutes ‘Wait for 3 minutes ‘Adld Methylene Blue Solution | (ar) Mothvlene Blue Solaon I: drop by Drop until it tebed with tbe A, 7 Count the Number of Props CALCULATION: No uf drops Methvlene Blue oittion | #0.1 (Methylene tue Solution 1) . RESULT, ; ‘Sulpinide DosmptANIONIC SURFACE ACTIVE AGENT METHOD: SPECTROPHOMETRIC : ANNEX K OF 1S; 13428 APPARATUS: orga Rhotowrter (650 nm).PH meter, Water bath, Gas stripping apparatus, Refhating Apparatus Evaporating dish & Au Iau with flow meter, CHEMICALS; ppdees! benzene sulphonic sodium salt, sodium chloride Ethyl acctate. Chloroform, Ethanel, Methanol Sulphorie aid, Methylene blue, Sodium bi Carbonate, Sodium hvdroxide, Sodium carbonates & phenolphthatein REAGENTS: 5 hacuy! bemytra Ja | Methvleae blue neutral Sohution Dissolve 0.035g of methylene blue i distilled water and make up to 100ml of distiiice water 2 Methylene Bing acidie solation Dissolve 0.0358 of methylene blue in SOml of distilled water ad 0,65mt of sulphur acté and ranke up to 190m! with distilled water. 3. Buffer solution: Dissolve 2.4g of sodium hydrogen carbonate and 2.7g of scxtiura carbonate in {Oi)ml vf disulled water. PROCEDURE: (CF Separation of the surfactant: AA) Take 1090! sample wth added 100g of sedi chloride in gas strigping apparatus add distilled wate thecessary tothe levei of the upper stopenck After avertlow of the test sample close the upper Stopicock artd add 130m! of ete! acetate 15) fall the wash howtle 2:3 with ethyl acetate Conneet the wash bottle with air put 7 Poss the aur through wash bottle at the flow ‘unintaining 30Vh using ai flow nigter. Stop the an flow ater tai, areca 1D) Collect the ethyl acetate layer in separating funnel remove the excess water from oraimic lay ) Transfer the ethyl acetate in evaporating dish ‘And evaporate the ethyl acetate completely using ‘water bath ¥) Dissotve the residue in Sm of methanol and. Sent oF cistlled water and make np to. 100rnt with distilled water : kona blank distiled seater) 600ml standard soliton 1. 100m! tarsiaed solution ~ I Niet suctand soliton TE 1000mt siandaee soiniton 78 also man ae same manner from aie ti ee f 8 éecadoat Fin 1 Ons Seamme Avance‘Test with the Sample Take 6 Nos of separ ing fimnels Funnel 1 250m): ~~ Take sample portion Fuonel t (250m) ‘Take Blank Distilled! Water) postion Funnel TH (125m)) ‘Take standard soluton ~ I portion “005mg Dodecyl benzene sulphonic sodium sali) port 0 01mg Dedesyl benzene sulphanic sodium sald) Funnel 1V (125m, Take standard solu Funnel V (125m) - “Take standard solutiod — {II portion ((.015mg Dodeeyl benzene sulphonic sodium salt) Farnel V1 (425m!) “Take standard solution ~ IV portion (0 02ma Dodecy! benzene sulphonic sodiam salt) Add all fannel Sr of neutral methylene blue solution, {Oma of buffer solution and 1 Smi of chlorafimn, Shake veil and altow the aver to separate, Collect the chloroform layer in nessler’s cylinder respectively ‘Wash the separating funnels and transfer the chloroform layer from nossler’seylinders respectively. Add 110ml of distilled water and Seal of acidie methylene blue solution, Shake uniformly for 1 min and allow the layer to separate Cake the OD value of standards and sample using chloroform laver in speotrophotometar at 650NM. Draw the fap Mg of Copp: (OD Values of Standards. = CALCULATION: Amen Surface anive agent. Mell = Graph Value X.1000 {Volume of sample taken (1000 RESULT: “Amonie surface active agent amg