rie Where: ‘A= weight of residue + dish before ignition, me, Be weight of residue + dish or filter after ignition, mg and (C= weight of dish or filter, mg. 6) Precision ‘The standard deviation was 11 mg/ at 170 m/l volatile total solids in studies by three laboratories on four samples and 10 replicate. Bias data on actual sample cannot be obtained. F)_Setteable Solids 1) General Discussion Setteable solids in surface and saline waters as well as domestic and industrial waste may be determined and reported on either a volume (mi/)) or a weight (mg/!) basis. 2) Apparatus ‘The volumetric test requires only an Imhoff cone. a) Evaporating dishes: - Dishes ‘of 100 ml capacity made of one of the following materials; 1) Porcelain, 90mm diameter. 2) Platinum: Generally satisfactory for all purpose. 3) High- silica glass. bb). Mufle furnace for operation at 530% ©) Steam bath d) Desiccators, provided wi concentration or an industrial indicator. €) Drying oven, for operation at 103 to 105% 1) Analytical balance, capable of weighting 10 0.1 mg 2) Magnetic stirrer with TFE stirrer bar. -bore pipets. ’) Glass-fiber filter disks without organic binder. |) Filtration apparatus: One of the following suit ith a desiccant containing a color indicator of moisture able for the filter disk selected: 1) Membrane filter funnel. 2) Gooch crucible, 25 ml to 40 ml capacity, with gooch crucible adapter 11 @ Scanned with OKEN Scannerwo 40 pm) Hite disk a We fi 4) Filtration apparatus with are mple si selected ky Suction ‘ask of sufficient CP 1). Drying oven for operat rm) Aluminum weight : rn) Aglass wessel with a cat k with a well mixed sample. Settle fo, 1) Volumetric: Fill a7 Inf come 10 ofthe cone WIEN 2 rod or by spinning, sete rnin. penly agitate same near the side ceo by sini ty rin longer and record VOlUM® of sta ce rc pares = le ‘contains pockets of Haul ean ese me tat volume of settled solids. The practical lower lng, measurement depends 0 sample composition and generally is inthe range of 0x16) if. Where a separation of settleable and floating material occurs, do not estimateg ally are not required. floating materials secTeable matte Replicates Us b) Gravimetric E 1) Determine tot 2) Pour a well mixed sample into @ less than 1L and sufficient samp! ection D- sel of not less than gem diameter Using, e to give a depth of 20 cm. alternatively use agi vessel of greater diameter and 2 larger volume of sample. Let stand quiescent fy, hand without disturbing the settled or fl0atinB material, siphon 250 mil from cen: crcontainer ata point halfway between the surface of the settled material andi liquid surface. Determine total suspended solids (mg/l) of this supernatant Iga— ‘These are the nonsettleable solids. al suspended solids as in 5 glass ves 4) Calculation mg settleable solids/L= mg total suspended solids/L - mg nonsettleable — Solids/L 21057 -43+g mgt S = VIS to math r 5) Precision and Bias - i recision and Bias data are not availabl: le. lll @ Scanned with OKEN Scannerhe, 7 Conclusien a 7 - @ toral_svtidg = 1999-8 mglt | @ -total pissolved _Seltds = 42+? _mgld as lest malt _ eis |@ _Tatol__suspended__sofids nate @_Nolasile __Soltds = isaey maglt i of ©. Fined _Gotids _ aus-y mgt > 1, the |©__sesrerwe solid elisha ter Z the @ Scanned with OKEN ScannerExperimental no. 2 SLUDGE VOLUME INDEX (SVI) et | @ Scanned with OKEN ScannerSLUDGE VOLUME INDEX (SVI) Object: Determination of Sludge Volume Index (SVI) of aerated MLSS Apparatus: 2 liter eane, Inhofe cone (I liter), china elay evaporating dish, beaker, filter papers, oven. Theory: The SV1 is the volume in milliliters occupied by 1gm of a suspension after 30 minutes Yeading. SVI typically is used to monitor setling characteristics of activated sludge and ther biological suspension. Although SVI is not supported theoretically, experience has shown it to be useful in routine process control. Procedure: 1) To determine the suspended solids concentration of a well-mixed sample of the suspension. ‘A well-mixed sample is filtered through a weighed standard glass-fibre filter and the yesiduc retained on the filter is dried to a constant weight at 103°C to 105°C. Day the crucible, filter paper and suspended solids in an oven at 103°C to 105°C for} hour cool in desiceators to room temperature and weigh. Repeat cycle of drying, tooling, desiceating and weighing until a constant weight is obtained or until weight change is less than 4% of previous weight or 0.5mg whichever is less ‘A= wt. of crucible + filter paper + dried residue (mg) wt, of erucible + filter paper (mg). Total suspended solids in mg/L = (A-B) * 1000 Sample volume in mal Note: Usually a erucible of 25 to 40 ml capacity is used. Sample size should be such that it will be such that it will yield between 10 to 200 mg dried residue, 2) To determine 30 minutes settled sludge volume. Place 1.0 L sample in settling Imhoff cone and distribute solids by cov and inverting eylinder three times. Let the suspension settle for 30 amin. in m ing the top L. Observations: Time of collection= 30 min Volume of settled sludge = 41 mglt Wt of suspended solids= 630 mal @ Scanned with OKEN ScannerCalculation: = (ml/gm) svi= Soe sds womens (wD) ed 0 103°C 10 105°C for 24 In (mg/L) Wi oF suspended sol AL 4 1000 S09 mglam Sludge Volume Index (SVI) ‘of given sample = Es.of mgm ig in Aonge gosd SaHing sk pie used is Ft avi fot cisd melgm - hence dhe Som SetHing sludge copacetyExperimental no.3 DISSOLVE OXYGEN @ Scanned with OKEN ScannerDISSOLVE OXYGEN 1. O.level in wastewater sample by wrinkler or iodometnic Object: - To determi method, it’s modification as Azide modification method. Apparatus: Beaker, 300ml BOD test bowls with rounded glass stopper, Burette, inders. Volumetric Mash, Pipette, Measuring cy ic method or procedure based on the iodizing f divalent manganese solution, followed by 5 an equivalent -lodometric method It is a ttrimetri It is based on the addition of sample in a glass-Stoppard bottle. DO rapidly oxi the dispersed divalent manganous hydroxide precipate to hydroxide of higher iodine reverts to the divalent state, with the liberation of trating with a standard Introduction: property of DO. strong, alkali, (0 the amount of valance state. In the presence of jodine equivalent to the original DO content, The iodine is then « solution of thiosulphate. “The tation end point can be detected visually, with a starch indicator. Most organic matter is oxidized partially when the oxidized manganese precipate is acidified, thus eausing neg: ¢ errors, is adopted to minimize the effect of interfering Modification of the iodometric method ly removes interference in biologically treated materials. The azide modification effectiv effluent and incubated BOD samples. Reagent:- 1) Manganous Sulphate Solution: Mn$OsH1,0 -364gm ~ Diluted to | liter i.e, 36.4 gm diluted to 100 ml distilled water. 2) Alkaline Potassium Todide-(Alkali-lodide-Azide reagent) 500 gm NaOH + 150 gm KI+ 20 gm NaNs ~1 Liter distilled water ie, 50 gin NaOH + 15 gm KI +2 gm NaNs ~ 100 ml distilled water 3) N/40 Sodium Thiosulphate Solution:- 40510 in distilled water and dilute to | liter. 6.205 gm Nox 44) Cone. Sulphuric Aci. 55) Starch Indicator: 16 a @ Scanned with OKEN Scanner22pm starch + 100m! hot distilled water, ‘Standradization yjesolve approximately 2gm KI, fee from Hoda, in a Mask: with 100 v0 150 ml oieetce Add Ural 6N HeSO, or 0 fe drops of concentrated 1HS04 and 20a, a bridle solution, Dilute 4 200 and trate [berated iodine wil os ini anda ling strch toad end of ration, when pale sass enfour is reached when te sear are of equal stent, 20m 0,0021M Nas should be required if mot ads he Nay8;0 solution to 0.0021M. ‘i ree 1) 300m BOD bottle filled ful with sample. 3) Add Im! Manganous Sulphate (MnSO3) solution. 53) Adkd Im! alkaline Potassium lodide solution. $) te pipes ste dipped into sample, they should be rinsed before returning them to reagen! bottles, or hold pipet tips just above liquid surface while adding reagent | 5) Stopper eatefully to exclude air bubbles. Gain by inverting. butte few times, when precipate has settled sufficiently ( 19 Rpmovimately half the Bote volume) to lave a clear superatant above the manganese hydroxide floc 7) Add 2 concentrated Sulphuric Acid (HeSO0) 8) Restopper and dissolve precipate by vigorous shaking. 6) Tate with N/40 Sodium Thiosapate sation sil pate straw yellow cols is obiained, rane few drops of starch indicator to gel blue colour, continue tration St int disappearance of blue colour. Cateulation: Iml of N/40 Sodium Thiosulphate {itrant= Img DOYL or Ippm DO Somple © ee ce Doreys Malt oS comple D —_P29X BW _ gor-5a_ Mgt gay Sample CD 2 Bet 6B mle 7 Scanned by CamScanner @ Scanned with OKEN Scanner@ scanned with OKEN Scanner Resutk S —— somple © / : HN Soditus Thiosulphatt Hand used = 63 my 4O S rop wat Somplé D0 of Sample «ta, sample @ NM Sodium thioulphade tlttant used = S-1 mp wat wale® Sample p-o of Sample~ S-1 mq, sample GD NL Sedium Hesubphate dfttant Used = 2-0 ml Te a Masie woke Sample Mio is = 2:0 molh . xExperimental no.4 BIOCHEMICAL OXYGEN DEMAND @ Scanned with OKEN ScannerBIOCHEMICAL OXYGEN DEMAND | Object: - "To determine BOD level in wastewater sample Apparatus: - Beaker, 300m! BOD test bottles with grounded glass stopper, Burcite, Volumetric Mask, Pipette, Measuring eylin ers, Incubator, pH-meter, Mpa isa test used to determine the relative oxygen requirement of wastewater, effluent and polluted waters. The test measures the ox; ‘material (carbonaceous dem: as sulfied and ferrous inon. I nitrogen (nitrogenous deman ‘ygen required for the biochemical degradation of organic ancl) and the oxygen used to oxidize inorganic material such \ also may measure oxygen used to oxidize reduced forms of nd) unless their oxidation is prevented by an inhibator. ‘The method consists of placing @ sample in a fall, srtght bottle and incubating the bottle under specified condition for a specific time (§ days at 20°C). Dissolved os gen 1S measured initially and after incubation, The D.O. is computed from the initia and final D.O, diffe Most wastewater contain more oxyyen demanding materials than the amount of D.O. available in air-saturared water, ‘Therefore, itis necessary to dilute the sample before incubation to bring the oxygen demand and supply into approximate balance. Because bacterial growth requires nutrients such as nitrogen, phosphorous, and {tracemetal, these are added 10 the dilution water, which is buffered to ensure that the pt Of the incubated sample remain in a range suitable for bacterial growth, ‘As for BODs (carbonaceous oxygen demand) measurement, an inhibiting chemical is used to prevent ammonia oxidation (nitrogenous oxygen demand). If ammonia was oxydized, errors would result because the oxygen use would not be due exclusively to pollutants in the sample. Blank sample with dilution water ~ Analysis of these provides quality control on dilution Water at time of analysis and on cleanliness of apparatus such as BOD bottle. Reagent: - 1) Phosphate Buffer, 8.5gm KHjPO, + 21.75gm KaHPO, + 33.49gm NajHPOs.7H,0 + 17gm NILCL in 500ml distilled water & dilute to 100ml or 850mg KH;PO, + 2175mg KHPO, + 3349mg NagHPO,.7H20 + 170mg NH,CL in SOml distilled water & dilute to 100ml. 18 @ Scanned with OKEN Scanner2) Magnesium Sulphate Solution Dissolve 22.5gm MgSOx.7H20 in distilled water and dilute to 1 it oF 2250mg, MgSOs.7H:0 dissolve and dilute to 100m 3) Calcium Chloride Solution Dissolve 27.5gm CaCL> in distilled water and dite to 1 it 2750mg CaCL2 dissolve and dilute to 100ml. 4) Ferric Chloride Solution Dissolve 0.25gm FeCLs and dilute to 1 lit 25mgFeCLs dissolve and dilute to 100ml 5) Manganous Sulphate Solution:- ‘Mn$Os Hs0 -364gm ~ Diluted to 1 liter i.e. 36-4 gm diluted to 100 ml distilled water. 6) Alkaline Potassium lodide-(Alkali-lodide-Azide reagent) 300 gm NaOH + 150 gm KI-+ 20 gm NaN — 1 Liter di illed water i.e. 50 gm NaOH + 15 gm KI-+2.gm NaNs ~ 100 ml distilled water. 7) N/40 Sodium Thiosulphate Solution:- .035H,0 in distilled water and dilute to 1 iter. 8) Cone. Sulphuric Acid, 9) Starch Indicator:~ 2am starch + 100ml hot di illed water. Procedure: - 1) Preparation of Dilution water: - 1 liter aerated distilled water + Iml each of phosphate buffer, magnesium sulphate, calcium chloride and ferric chloride solution. 2) Determine exact eapacity of three BOD bones. 3) Find out DO of diluted sample = Dume/L 4) Find out DO of diluted sample after 5 days incubation at 20°C = mg/L Di-D2 BODs, melt. —— P= Decimal volumetric fraction of sample used, 19 @ Scanned with OKEN Scannera 20.02 Ifsample used is ‘5ml, than P= 5/100 = 0.0: ise 5% dilution percentage for aN” sewage jie Sml of sewage sample Per Standards: - Wastewater sample volun me for different range of BO! | 100ml of BOD bottle capacity. 9D values to be pipetted into 3p BOD bottle Range of BOD, mglL. ml of sample 30000- 105000 7 12000-42000 . 6000-21000 0.10 3000-10500 0.20. 1200-4200 0.50 (600-2100 1.007 300- 1050, 200 120-420 5.00 60-210 10.00 30-105 20.00 6-21 100.00 es 300.00 For BOD value 120-420 ml, Wastewater sample used is Sml per BOD bottle volume. *For BOD value 60-210 ml, Wastewater sample used is 10m! per BOD bottle volume. P= Fraction of wastewater sample volume to total combined volume _ Volume of sample in mt s P= Topbottievehmme Bas oolss BOD for treated wastewater < 300mg/L Observation Table : Sr. no. Description | Dilution | D.O. D.O. BOD Factor Initi: " Zi 7 Initial S days MpLnglL. ee Bis 2S Zhe 6-2 BAe 191-45 Scanned by CamScanner @ Scanned with OKEN Scanner——7=— ” Calculation: - DF Cailudion Fact) = Nolume of BOD bottle Nolume of Sample = 34s DF a ey Somple @® s doys Gop eG ook a's. Bods = CD-0 inital - D:0 Fine ) x OF = (6 s- 254) K65 . [Bors 260 mgls somle © F doys B00 @ 2c * Boos =CD-o inital — D:o0 final) ¥ pf = (62-325) *% 65 Sf Bod's = AN. Fs mgs Reult- AVG Bods = 26e+H FT zi Avg Bods = 225 Inglt Conclusion The Untreated wotte waled fvg Bods @ 2° Valued Weate - We malt Medium - 320 molt eHeng - lo mg |e. The sample. we have 4ested 16 in dhe Range ber Were medivms, @ Scanned with OKEN ScannerExperimental no.5 CHEMICAL OXYGEN DEMAND all @ Scanned with OKEN Scannereee E- | CHEMICAL OXYGEN DEMAND Object: Determine the Chemical Oxygen Demand (COD) of waste water sample using OPS ux index. Apparat: Beaker, Pipette, Rounded bottom flask, Open reflux, Condenser, Burctte, Conical Reagent: . 1). Standard Potassium dichromate solution (0.25 N) (0.0417 M) 12.26 gm. KxCr203 ~ 1 1226 mg. KC.) 100 ml 2) Sulphuric acid reagents gm, AgiSO4 + 75 ml H;S04 3). Ferroin indicator solution 44) Standard ferrous ammonium sulphate sotution FAS. titrant (approximately 0.25 M) 98 am Fe(NI1,)2(S0.):"61130 dissolve in distilled wa Titre 9.8 pm, Fe(NHT),(S01)6H20 + 2 nil cone. 112804 - dilate 10 100 ml ‘Standardization of FAS against K:Cr0> Dilute 10 m1 KxCr:0; to 100 ml + 30 ml conc. H:SOy8 coal it Titrate with FAS using 2 3 drops of fervoin indicator Molarity of FAS solution (M) cl (nl). * 0.25 ‘Volume of 0.00417 M KzCr.02 solution ti Tn uation (mn) ser + 20 ml cone, HySOx~ dilute to Ji¥ed water before using and rinse il 1) Wash all apparatus with dist ck. TakeS0 mi sample + boiling beads + 1 sm. 2) Take 500 ml round hottom reflux fa HeS0, + $ ml acid reagent in tellus flask and cool 3) Add 25 ml 0.25 N KgCrOr in round bottom relax flask and mix it 4) Attach condenser and start cooling water 3) Add remaining 70 ml acid reagent throug! mixture 6) Apply heat and re! 7) Titrate excess dich 8). Titrate till colour changes yell fh open end of condenser and mix the reflux lux for 2 hrs. and cool. iromate with standard FAS using fervoin indicator Jou to green blue to red. Record ml of titrant used. 22 @ Scanned with OKEN ScannerObservation: St.No. | Sample] Thitial | Final] Difference | COD] Average Reading(a) | Reading(b) | e= b-a mg/L coD (ml) (cl) (ml) mg/L 1 feigue | 8 on a = 7 o 1s: 5 2 1s. PET 4og oO M24 | 607 FRY Calculation: COD (mg/L) = ml of titrant used » 8 1000 « M mil of sample somple © Cop Cmgla) = 2! ues x Bove yo = yo male Somple © Cop Cmglty = Blea % Foo xv‘ 5 344 malt J. Avg Cop (mg) = Uvet S#8-y a Result: > 4og myglA COD of given waste water sample= 1209 mg} Conclusion: Fr& UNndteated wedt? Avg. Cod Valttes Stiong — loco gle Medium - Sud mgt (ata - 25> malt Given sewage eSenable is in Aange bern Weak $ medium Zene Se it must be given Futtner entment feehte tesposing into open land 2B \ = @ Scanned with OKEN Scanner