INDEX

SR. NO.
1.

TITLE

PAGE NO.

DETERMINATION OF DISSOLVED OXYGEN CONTENT. DETERMINATION OF BIOCHEMICAL OXYGEN DEMAND DETERMINATION OF CHEMICAL OXYGEN DEMAND (C O D) DETERMINATION OF TOTAL,DISSOLVED,VOLATILE,SUSPENDED AND FIXED SOUND SLUDGE VOLUME INDEX CONDUCTIVITY

2.

3.

4.

5. 6. STUDY OF WASTE WATER ORGANISMS 7. PHOSPHATE CONTENT 8.

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1.Determination Of Dissolved Oxygen Content of wastewater Sample

AIM: To determine the dissolved oxygen content in given sample of water (waste water). APPARATUS: Burette, pipette, volumetric flask, 300ml bottles, measuring cylinder etc. REAGENTS; 1.Manganous sulphate solution. 2.Alkali iodide azide reagent. 3.Concentrated sulphuric acid. 4.Starch indicator. 5.Sodium thiosuphate solution (N/40). 6.Potassium dichromate solution(0.025N).

THEORY: General; Oxygen is poorly soluble in water and its solubility is directly proportional to its partial pressure.[For example, at a specific temperature such as 20C, with Henry's law constant being 43.8(mg/lx atmosphere) and partial pressure of oxygen being 0.2094 atmosphere at 1 atmosphere of air; DO saturation value =43.8(mg/lx atm.) x 0.2094(atm) =9.17 mg/l] (DO saturation decreases with rise in temperature, and decreases with rise in salt concentration, decreases with rise in altitude and decreases with rise in organic concentration.) the solubility of atmospheric oxygen in fresh water range from14.6mg/l at C to about 7 mg/l at 35C under 1 atm. Of pressure. Variation of DO with temperature (clean water at zero altitude or 1atm pressure) Temperature, 0 5 10 15 20 C DO saturation, Mg/l 14.62 12.8 11.33 10.15 9.17

25 8.38

30 7.63

35 7.0

40 6.6

45 6.1

50 5.6

1) Environmental significance: a) Dissolved oxygen measurement is required to ensure that aerobic Conditions are maintained in natural waters that receive pollutional matter. The minimum DO content should be 4mg/l in natural waters as per standards. b) It forms the basis of BOD test. c) All aerobic treatment process for waste water depend on presence of dissolved oxygen and therefore measurement of D.O. is a means of controlling rate of aeration to make sure that adequate amounts of air is supplied and to prevent use of excess air which will increase cost.

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d) Oxygen is a significant factor in corrosion of iron and steel in water distribution system by boilers. The D.O. measurement controls the removal of oxygen by physical and chemical means in boiler feed water. 2) Collection and preservation of samples: Since oxygen value may change radically with time because of biological activity, it is customary to fix the field sample collected in 250ml to 300ml ground glass stoppered bottles. Fixation is done by addition 0-7ml con. H2SO4 and 1ml of 2% sodium azid to arrest the biological activity. The fixed samples are stored in the dark at 0C.the test should be carried out within 6 hours of fixation. 3) Winkler method: the winkler and iodometric method is based upon the principle that +2 oxygen Mn from manganous sulphate to a higher state of valence under alkaline conditions and that manganese in higher state of valence is capable of oxidizing I to I2 under acid conditions.thus the amount of free iodine released is equivalent to the dissolved oxygen originally present. The free iodine is measured by titratig with standard reducing agent viz. sodium thio sulphate using starch as indicator. The reaction involved are: Mn2 +2OHMn(OI)2 white precipitate. If no oxygen is present a white precipitet is formed when MnSO4 and alkali iodide (NAOH) KI2 + reagent are added to sample. If oxygen is present, Mn is oxidized to Mn+4 and precipitate as brown hydrate oxide. Mn2+ 2OH Mn+2 + 2OH- + 1/2O2=MnO2 + H2O,or Mn(OH)2 + O2=MnO2 + H2O This is called fixation of oxygen. The process is slow and vigorous shaking is needed for all the oxygen to react. Under low PH condition MnO2 oxidise I to produce I2. MnO2+ 2I + 4H+ Mn2+ + I2 +2H2O (4) Azide modification: The nitrite ion is one of the frequent interference encountered in the D.O. Determination. It occurs in effluents from sewage treatment plants in river water etc. it does not oxidize Mn+2but does oxidize to I2 under acid conditions. It reduced from N2O2 which enters the sample during titration is oxidized and converted to NO_2 again , establishing a cyclic reaction,thus making it impossible to obtain permanent end point as soon as blue colour of starch indicator disappears, the nitrites formed by oxidation of N2O2 will react with more I- to produce I2 and blue colour again appears. The reaction can be shown as 2NO2+2I-+4H+ .I2+N2O2+2H20 N2O2 +1/2O2 ..2NO2+2H

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Nitrite in interference may be early overcome by the use of sodium azide . It is convenient to incorporate the azide in the alkali KI reagent. PROCEDURE: A. Selection of normality :normality is so adjusted such a way that each ml of titrant to 1mg of measured material. In DO determination , it has become standard practice to use 200 ml sample for titration, which is 1/5th of litre by using titrant which is 1/5th as strong as conventionally used ,the results obtained on 200ml of samples in terms of ml of titrant used are same as 1 litre ,sample has been titrated with N/8 reagent. Thus when a N/40(N/8x1/5) solution of sodium thiosulphate is used to titrate 200 ml of sample the DO value in mg/l is equal to titration. B. Standardization of sodium thiosulphate solution : because of this nature of hydration sodium thiosulphate cannot be dried to a compound of definite composition and even loses water at room temperature under conditions of low humidity. It is necessary therefore to prepare solution that is slightly stronger than desired. Potassium dichromate is used as primary a standard. For this following procedure is adopted. (a) 2 gm of potassium iodide is placed in a flask. (b) 100 ml-distilled water is added. (c) 10 ml of H2SO4 is added. (d) 10 ml of standard potassium dichromate (0.25N) is added. (e) 100ml distilled water is added again. (f) Mixture is titrated against a given sodium thiosulphate using starch indicator. Normality of sodium thiosulphate is N =(0.025x10) x quantity of titrant used in ml. C. Procedure for calculation of DO: (a) The sample is filled in 300ml capacity BOD bottle. (b) 2 ml of MnSO4 solution is added by means of graduated pipette depending the end of pipette below liquid surface. (c) 2 ml of alkali iodide azide reagent is also added to same manner. The bottle is stopped and mixed thoroughly. (d) When brown ppt. is formed, 2 ml of conc. H2SO4 is added and mixed thoroughly. (e) From the bottle, 203 ml of content is taken out and used for titration, which will give 200 ml for the original sample for titration.As 2 ml of each magnesium sulphate and alkali iodide azide reagents have been added , the proportionate quantity corresponding to 200ml is obtained as below: 200 x exact capacity of bottle =208ml. (f) This is titrated against sodium thiosuphate taken in burette, using starch indicator, till the blue colour disappears and volume of titrant is noted. The ml of thiosulphate used is equivalent to mg/l of DO

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PRECAUTIONS: (a) MnSO4 and alkaline iodide azide reagent should be added very quickly after the sampling so that sample is preserved. (b) Freshly prepared starch solution should be used. (c) Sodium thiosulphate solution should always be standardized at the time of titration.

OBSERVATIONS: SR.NO. DESCRIPTION TEMP. OF OF SAMPLE SAMPLE DO mg/l REMARK

RESULT:

CONCLUSION:

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2. Determination of Biochemical Oxygen Demand of wastewater Sample

Aim: To determine BOD of a given waste water sample. Apparatus: BOD incubator (range 5 to 50C) BOD bottles, burette, pipette, measuring cylinder, air compressor, mixing apparatus etc. Reagents: 1. Distilled water. 2. Phosphate buffer solution 3. Magnesium sulphate solution 4. Ferric chloride solution 5. MnSO4 solution 6. Alkali, iodide azide solution 7. Calcium chloride solution 8. Conc. H2SO4 9. Standard sodium thiosulphate solution (N/40) 10. Starch indicator SIGNIFICANCE: The BOD test is widely is used to determine the pollutional strength of sewage and industrial waste in terms of the oxygen that they will require if condition exists. The test is most important in stream pollution control activities and by its use, it is possible to determine the degree of pollution of streams at any time. This test is of importance in regulatory works and in designing, evaluating the performance & efficiency of sewage treatment units. THEORY: 1. General: - BOD is defined as the amount of oxygen required by bacteria while stabilizing decomposable organic matter under aerobic condition. BOD test is an oxidation process in which diverse groups of living organisms serve as the medium for oxidation of the organic matter to CO2 and water. Therefore, it is important that a mixed grouped of organisms commonly seed be present in the test. The rate of reaction depends upon the population number of microorganisms and temperature. 2. Nature of BOD reaction: studies of the kinematics of BOD reactions have established that they are first order in character, i.e. the rate of reaction is proportional to th e amount of oxidisable organic matter remaining at any time which can be represented by the equation , -dL = dL dt K-1L -dL /dt = K-1L Where, L=concentration of oxidizable organic matter (pollutant) at the start of the time interval t or ultimate or total BOD. K =rate constant for the reaction in per day where k = kL/2, 0.303
Lt =BOD at any time t

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Y= total or ultimate BOD in mg/l L = BOD at any time mg/l BOD exerted = Y = L = Lt = L(1-1O-kt)

Draw Graph BOD Vs time in days 3. Conditions under which test should be performed: As the test is of arbitrary nature, it is essential that test is performed under standard conditions. These are: a) Temperature should be constant through out the test (20C) b) There should not be nitrification. c) Sufficient nutrients should be present for the growth of microorganisms. d) PH should be maintained in the range of 6.5 to 8.5. e) Proper osmotic conditions should be maintained. f) D.O. content should be sufficient to complete the test.

4. Use of different reagents: Though, theoretically, the time taken for complete biological oxidation of organic matters is infinite, a 5 day period at 20c incubation temperature has been considered ideal, as about 2/3 of the total BOD is stabilized in this period. The oxygen demand is essentially due to carbonaceous matter and no interference by nitrites. (i.e. oxidation of ammonia) are absorbed in this period . Domestic waste water has an ample supply of nutrient element such as nitrogen and phosphorus, but many industrial wastes are deficient in one and sometimes both of these elements because of these limitations. Phosphate buffer is used in dilution water to maintain the favorable pH conditions at all

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times as the saprophytic bacteria acts in the ph ranges of 6.5 to8.5. The potassium, sodium, magnesium and calcium salts are added to give buffering capacity and proper osmotic conditions, also serve to provide the micro-organisms with any of these elements that are needed in growth. ferric chloride , magnesium sulphate and ammonium chloride supply the requirements for iron, sulphur and nitrogen in dilution water. Domestic waste water ,particularly from combined sewer systems, provides balanced population of mixed organisms for seeding purpose. Nitrification control in the test: The mixed culture of organisms (seed), when derived from the soil or domestic waste water, contain large number of saprophytic bacteria and other organisms that utilize the carbonaceous matters present in the samples subjected to BOD analysis and use oxygen in corresponding amount. In they normally contain nitrifying bacteria. The nitrifying bacteria are usually present in relatively small numbers in untreated domestic waste water and their reproductive rate at 20c,in such that, their populations do not became sufficiently large to exert an appreciable demand for oxygen un2til about 8 to 10 days have elapsed in the regular BOD test. Once the organisms become established they oxidized nitrogen in the form of ammonia to nitrous and nitric acids in amounts that introduce serious error into BOD work. 2NH3+3O2 Nitrite forming/bacteria=2NO-2 + 2H+ +2H2O 2NO-2 + O2 +2H+nitrite forming/bacteria= 2NO3 +2H+

The effluent from biological treatment units, such as trickling filters and activated sludge, often contain populations of nitrifying organisms sufficient to utilize significant amount of oxygen during the 5 days incubation period. The action of the nitrifying acteria can be arrested by the use of inhibiting agents such as methyelene blue allylthiourea (ATW) or nitrifying populations can be reduced to insignificant levels by pretreatment of the samples by pasteurization, chlorination and acid treatments. 6. Dilution of sample: A wide variety of waste material is subjected to the BOD test. These range from industrial wastes that may be free from micro organisms to domestic waste water with and abundance of organisms. Many industrial waste have extremely high BOD values. Water about 9 mg/l at 20C must be diluted to the levels of demand to ensure that dissolved oxygen will be present through out the periodof the test.dilution that results in a residual D.O. of test 1mg/1after 5 days incubation produces the most reliable results. 7. Use of blanks: In the determination of BOD by dilution technique.it is safe to assume that the dilution water containing the seeding material will contain organic matter and that the addition of the diluting water to the sample will increase the amount of oxidisable organic matter. Hence a correction is applied. Usually the correction is made without special consideration by letting days dissolved oxygen value of the blank represent the zero day corrected value.

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PROCEDURE: 1. Prepare the dilution water by aeration of distilled water with compressed air up to saturation and by adding 1ml each of phosphate buffer solution, magnesium sulphate solution, calcium chloride, ferric chloride, Mgo4 solution. 2. Add 2ml of settled sewage in dilution water.(for seeding if necessary) 3. Aerate the dilution water with the help of air compressor for about 10 to 15 minutes. 4. Find the dissolved oxygen of sample and designate as Dos. 5. Prepare the desired percent mixture by adding sample in dilution water. 6. Find BOD bottles with desired mixture with different dilution factor and another with dilution water (blank). 7. Put all these bottles in a incubator at 20c for 5 days. 8. \Find out the dissolve oxygen of both the bottles after incubation. Designate mixer as DOi and blank as DOb.

Precautions:
i. ii. iii. At least three dilutions should be prepared. The distilled water should be aerated and significant amount of nutrients should be added. The sample should be seeded with domestic settled sewage if necessary.

Observation table:
Sr. no. Description of sample Initial D O Mg/lit Final D O Mg/lit Dilution ratio Result

Calculation of B O D mg/l @ 20c for 5 days = (DOb - DOi) 100% - (DOb - DOs) X dilution factor.

RESULT:

CONCLUSION:

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3. Determination of Chemical Oxygen Demand COD of wastewater Sample

AIM: To estimate oxygen demand (COD) of a given waste water sample. APARATUS: Burette with stand, pipette, 250 ml capacity beakers, measuring cylinder, digestion and reflux apparatus, hot plate etc. REAGENTS; Con. Sulphuric acid.36N 0.25N potassium dichromate solution. 0.1 N ferrous ammonium sulphatesolution. Ferroin indicator. Silver sulphate. Mercuric sulphate. Glass beads. SIGNIFICANCE: The chemical oxygen demand is a measure of the oxygen equivalent of the organic matter content of a sample that is subjected to oxidation by strong chemical oxidant. The COD test data is used for the following:1. it is used in the analysis of industrial wastes. 2. Results may be obtained with in a relatively short time and measures taken to correct errors on the day they occur. 3. In conjuction with BOD test, the COD test is helpful in indicating the presence of biologically resistant organic substances. 4. The test is widely used in the preparation of treatment facilities because of the speed with which results can be obtained. THEORY: 1. General: The chemical oxygen demand (COD) test is widely used as a means of measuring the pollutional strength of domestic and industrial wastes. It is the measurement of waste in terms of the total quantity of oxygen requirement for oxidation to carbon dioxide and water according to the following. Cn Ha Ob Nc + (n+a/4 b/2 3c/4)O2 nCO2 + (a/2 3c/2) H2 O=CNH3 It is based upon the fact that all organic compounds with a few exceptions, can be oxidized by the action of strong oxidizing agents under acid conditions. The reaction involved may be represented as follows with dichromate ion. Cn Ha Ob + C Cr2 O7 + 8CH+Heat nCO2+(a+8C) /2 x H2O+2C Cr3+ Environmental Engineering-II Civil Engg. Deptt. C O E P. 10

Where C= 2/3 n + a/6 b/3

2. Relation between BOD and COD : During the determination of COD organic matters are oxidize completely regardless of their biological assimilability. Hence, COD values are greater than BOD. Ratio of COD BOD to BOD is called treatment ability index. It ranges from 0.4to0.8 for untreated domestic waste. 3. Condition for test: a) The solution must be strongly acidic. b) Temperature should be high @ 150oc for oxidizing the organic matter by K2 Cr2O7, Completely. c) Volatile matters, (organically present and those formed during digestion period) should not get lost during digestion, hence reflux condenser is used. d) K2Cr2O7 should be in excess. 4. Use of potassium Dichromate:Potassium permanganate, potassium iodide and potassium dichromate are the oxidizing agents that have been studied extensively for the determination of COD potassium dichromate has been found to be the most practical of all because a) It is capable of oxidizing a wide variety of organic substances almost completely to carbon dioxide and water. b) It is relatively easy to measure any excess of potassium dichromate,in order to calculate the amount actually used in the oxidization of organic matter. c) It is relatively cheap compound and can be obtained in a high state of purity. d) After drying at 1030C, it can be used to prepare solutions of an exact normality by direct weighing and dilution to the proper volume. 5. Use of silver sulphate:Certain organic compounds, particularly low molecular weight fatty acids, are not oxidized by dichromate hence silver ions act as catalyst in the test. Aromatic hydrocarbons and pyridine are not oxidized under any circumstances. 6. Selection of normality of K2Cr2O2:Since the equivalent weight of oxygen is 8, hence N/8 or 0.125N solution of oxidizing agent should be used in determination, so that results can be calculated easily. Experience with test has shown that it has sufficient sensitivity to allow the use of stronger solution of dichromate, and a 0.25N solution is recommended, doubles the rang of COD that can be measured in the test procedure.

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7. Necessity of ferrous ammonium sulphate;A solution of reducing agent is used for the measurement of excess oxidizing agent remained after oxidizing all organic matter, ferrous ion is an excellent reducing agent for dichromate. Solution it can be best prepared from ferrous ammonium sulphate which is obtainable in rather pure and stable form. In solution it is slowly oxidized by oxygen dissolved from the air(as the other reducing agents oxidized), and standardization is required each time the reagent is to be used. The reaction occurs as follows;6Fe2+ + Cr2O72- + 14H.. 5Fe3+ + 2Cr3+ + 7H2O. 8. Use of Blank:It is important that no organic matter from outside source be present if a true measure of the amount present in the sample is to be obtained. Since it is impossible to exclude extraneous organic matter in the COD test, blank sample is required. Ferroin (ferrous 1, 10- phenanthroline sulphate) is an excellent oxidization reduction indicator indicates when all dichromate is reduced by ferrous ion. It gives a sharp colour change in spite of the green colour produced by the Cr+3 formed on the reduction of the dichromate. Although an oxidizing agent is used in the measurement of COD. It does not figure directly in the calculation of COD, through reducing agent. The COD test is precise and accurate for samples with a COD of 50mg/l or greater. 9. Interference of inorganic matter:Certain reduced inorganic ions can be oxidized under the condition of the COD test and thus can erroneously, high results. Chlorides cost the most serious problem because of their high concentration in most waste waters. This interference can be eliminated by addition of the other reagent. Nitrites are oxidized to nitrates. This interference can be overcome by the addition of H2SO4 to the dichromate solution. PROCEDURE: 1. ferrous ammonium sulphate is standardized as follows; a) 10 ml of .25KN K2CR2O7 solution is diluted to 100 ml with distilled water. b) 30 ml of conc.H2SO4 is added and cooled to room temperature. c) it is titrated against given ferrous ammonium sulphate using pheroin as indicator. d) Normality of ferrous ammonium sulphate is determined as N= .25 x 10/(Volume of titrant used). 2. Two COD flasks A and B are taken. 3. About 0.4 gm of mercuric sulphate is placed in each flask to suppress the interference of chloride ion. 4. 20 ml of distilled water is added to in flask A and 20 ml sample in flask B.

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5. 10 ml of standard (0.25N) K2Cr2O7 is added to each flask. 6. 30 ml of conc. H2SO4 is added to each flask. 7. about 0.2 gm of silver sulphate is added to each flask. 8. There are 4 glass leads are added to each flaskto prevent bumping during boiling. 9. the contents of each flask are boiled for 2 hours. 10. Each condenser is cooled and washed down with 20 ml of distilled water. 11. 80 ml of distilled water is added to each flask and cooled to room temperature. 12. The content of each flask is titrated against ferrous ammonium sulphate using ferrion as indicator. Colour change is blue green to reddish brown at the end. 13. COD of the sample is determined as Eq. wt. of oxygen = 8. Where: a =amount of titrant used for blank flask A. b = amount of titrant used for sample flask B. N= normality of ferrous ammonium sulphate solution (equivalent wt. of oxygen =8) PRECAUTIONS: A) strong waste should be diluted . B) mixing of conc. H2SO4 should be done carefully. C) Reflux apparatus should be assembled properly. D) Ferrous ammonium sulphate solution should be standardized at the time of titration.

Sr. No.

OBSERVATION TABLE: Description Normality of sample of ferrous ammonium sulphate

a ml

b ml

Dilution Ratio/factor

COD results

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COD mg/l =[(a-b) x N x 8 x 100] x dilution factor ... Ml of sample taken . CALCULATION:

RESULTS:

CONCLUSION:

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4.Determination of total, dissolved, volatile, suspended and fixed solids of wastewater Sample
AIM: To determine the amount of total, volatile, fixed, suspended and dissolved solids in the given sewage sample. APPARATUS: Evaporation porceline dishes or crucible, drying with thermostat, chemical balance, desiccators, filter paper, water bath, muffle furnace , measuring cylinder, conical flask etc. SIGNIFICANCE: Application of solids data : Following are the application of total solids determination; a) In public and industrial water supply the total solids determination is of importance. b) The total solids content may dictate the type of water softening procedure used. c) Corrosion control is frequently accomplished by the production of stabilized water through PH adjustment. The PH at stabilization depends to some extent upon solids present. The settlement solids determination has two very important applications: 1. It is used in the analysis of industrial wastes to determine the need for the design of primary settling tank in plants employing biological treatment processes. 2. It is widely used in waste treatment plant operation to determine the efficiency of sedimentation units. The suspended solids determination is used for following : 1 It is valuable in determining the amount of suspended solids remaining after the settlement solids have been removed in primary settling unit, for the purpose of determining the loading of remaining materials on secondary biological treatment units. 2. from the viewpoint of stream pollution control , the removal of suspended solids usually as important as BOD removal. 3. It is used to control the aeration solids in the activated sludge process.

Principle:
The principle consists of evaporating a measured waste water sample and weighting the dry residue. Volatile solids are determined by igniting the dry residue till the volatile portion is burnt off .The loss on ignition represents the amount of organic solids . The final residue remaining is the fixed or inorganic solids. Environmental Engineering-II Civil Engg. Deptt. C O E P. 15

THEORY:
All matter except the water contained in liquid materials should be classed as solid matter, However the definition of solids, refers to the matter that remains as residue upon evaporation and drying at 103 to 105 C. Thus, excluding the materials that exert significant vapour pressure at this temperature are lost. Solids in Env. Engg. Practices are organic in nature. At this temperature they will not be volatized due at 103C all free water is removed. Gravimetric methods are used to gain the information on the amount of various kinds of solids present e.g. dissolved, suspended, volatile and fixed. Dissolved and non dissolved solids : In potable water, most of the matter is in dissolved form and consists of mainly, inorganic salts , small amount of organic matter and dissolved gases. The total solid contents of potable water usually ranges from 20 to 1000 mg/l and as rule hardness increases with total solids. In all other liquid materials, the amount of non-dissolved solids, colloidal and suspended matter increases with degree of pollution. Sludge represents an extreme case in which most of the solids matter is non dissolved solids and dissolved fraction is of minor importance. Volatile and fixed solids: One of the major objective of performing solid determination upon domestic wastes, industrial wastes and sludge sample is to obtain a measure of the amount the organic matter present. This test is accomplished by a combination procedure in which organic matter is converted to carbondioxide and water, while the temperature is controlled to prevent decomposition and volatisation of inorganic substances, as much as is consistent with complete oxidation of the organic matter. The loss in weight is interpreted in terms of organic matter. The standard procedure is to conduct ignition 550C +/_ 50C at this temperature decomposition of inorganic salts is minimized, but most other inorganic salts are relatively small, with the exception of magnesium carbonate as given below; MgCO3..250C..MgO + CO2 In sludge analysis, the ammonium compound exists mainly as ammonium bicarbonate are completely volatilized during the evaporation and drying procedure and are not present in to interfere in volatile solids determination. NH4HCO3 ..NH3+ CO2 + H2O Serious errors can be introduced in volatile solids determination by conducting ignition at uncontrolled temperature. Therefore combustion is done in muffle furnace where the temperature can be accurately controlled. Calcium carbonate, which is a major component of the inorganic salts normally present in the samples subjected to volatile solids analysis is decomposed at 825C

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The determination of volatile solids in sludge is often subject to serious error because of losses due to decrepitation during the procedure. Decrepitation may be eliminated by a preliminary controlled firing of samples with a Bunsen burner to destroy all flammable materials before placing the sample in the muffle furnace. Settleable solids :sludge are accumulation of settleable solids. The measurement of settleable solids is important to determine the need for sedimentation units and the physical behavior of waste streams entering bodies of water. The test is conducted in imhoff cone allowing sufficient settling time at room temperature.

Procedure :1. A Dry constant weight empty crucible is taken and weighed accurately ( W I). 2. A measured quantity of sample is transferred to the crucible and the contents evaporated to dryness in a water bath and then put in oven ofr one hour at 103 to 105 C 3. It is allowed to cool in dessicator and then weighed accurately ( W2 ) 4. The same crucible is kept in muffle furnace and ignited at 500+_ 50 C for 15 minutes. 5. The crucible is taken out from the furnace and allowed to cool in dessicator and weighed accurately ( W3 ). 6. For determining dissolved solids, same amount of sample is filtered thorough filter paper and filtrate is collected in another pre weighed ( W4 ) crucible. 7. The filtrate is also evaporated to dryness in water bath and then hot air oven for about one hour 103 to 105 C. It is then allowed to cool and weighed accurately ( W5 ).

Precautions:1. The weight measurement must be very accurate. 2. The crucible should never be touched with hands they should be handled with tongs. 3. The crucible must always be cooled in dessicator. 4. The oven, muffle furnace be kept at proper temperature.

Observation:
1. wt. of first empty crucible 2. wt. of crucible + total solids after dry 3. wt of crucible + fixed solids 4. wt. of second empty crucible 5. wt of crucible + dissolved solids W1mg W2mg W3 mg W4 mg W5 mg

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CALCULATIONS: Total solids = [(W2-W1)/ V] x 1000 Fixed solids =[(W3-W1)/V] x 1000 Dissolved solids = [(W5-W4) x 1000 mg/l mg/l mg/l

Suspended solids (mg/l) = total solids dissolved solids Volatile solids (mg/l) = total solids fixed solids

Result :

Conclusion:

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5. Sludge volume index (SVI) 5.1 INTRODUCTION:

SVI an important parameter, used for monitoring efficient operation of aerated systems. SVI is the volume in ml, occupied by 1g of mixed liquor suspended solids (MLSS). Settled in 30 minutes. Mixed liquor sample for SVI test is drawn from the outlet of an aeration tank of an Aeration tank of an activated sludge process-conventional or modified. 5.2 Importance of SVI determination: 1. SVI is used for determining the quality of sludge produced in a biological aeration unit and hence its efficiency. 2. Specified MLSS concentration in the aerator. 3. It is also used for estimating suspended solids concentration in recirculated sludge.

5.3 Discussion:
An Imhoff cone is used for determination of SVI. This represents , effectively the principle and working of a secondary settling tank in an aerobic biological system.(In the absence and working of a Imhoff cone,a 1000 ml graduated cylinder may be used particularly for field tests) The volume of sludge (ml),settled in 30 min./gram MLSS varies from 25 to 200 depending upon the quality of sludge produced. As the purpose of biological aeration is to convert non-settleable organic suspended solids into settleable cell mass, low SVI values indicate high quality of sludge produced and high efficiencies of BOD removal.

Associated Operational Parameters For Biological Aeration Process

SVI mg/l Process MLSS, Mg/l F/M d-1 Aeration Time, h Average sludge age , d 5 10 BOD Quality removal of sludge Efficienc y% 60-75 Poor 80-90 Good as indicated by the median value 100 ml/g

150-200 High rate 50(100)150

5001000

0.5-1 0.2-0.5

3-4 6-10

conventional 20003000

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25-50

Extended aeration

40006000

0.050.2

24-36

25

90-98

Excellent

Sludge produced in an aeration system is considered excellent1. if it settles easily. 2. it occupies minimum volume. 3. it is granular and highly mineralized. 4. it dewaters and dries easily without odour nuisance. Sludge to be wasted from extended aeration systems, with SVI in the range of 25 to 50 ml/g, can be discharged to sludge drying beds directly, without the need of aeration in anaerobic digesters. Sludge from the aerator of a conventional or standard rate ASP, with SVI around ml/g, is good in quality but inferior to sludge produced by an extended aeration process. It has pollutional load and requires stabilization in a digester before drying. Sludge from an aerator of a high rate process, with SVI in the range of 150 to 200 ml/g, is poor in quality, odourous high in volume, sticky and highly pollutional. it is unfit for disposal without proper digestion.

5.3.2 Sludge bulking:

If SVI IS more than 200 ml/g, sludge produced in a biological aeration system is said to be bulked. Bulked sludge indicates failure of the process. Sludge bulking is a major operational problem, which increases effluent BOD and decreases process efficiency.

Causes of sludge bulking:

A) Poor characteristics of influent water:1) Frequent variation in quality and quantity of influent. 2) Low PH (filamentous organisms such as Beggiatoa and Sphaerotilus grow below PH 5, these multi-cellular organisms get water entrained and remained suspended without settling down in SST). 3) Low temperature resulting in decreased bacterial activity. 4) Staleness or septicity of influent. 5) Low nutrients (the common BOD: N :P weight ratio required for biological treatment is 100:5:1). 6) High carbohydrates B) Poor plant design and operation; 1) In sufficient aeration 2) Insufficient mixing (of recirculated sludge and influent waste water) in the aerator. 3) Organic-overloading (high F/M) 4) Insufficient hydraulic retention time or aeration time. 5) Insufficient sludge retention time 6) Improper recirculation of sludge resulting in fluctuating MLSS in the aerator. 7) Retention of sludge in SST for too long promoting anaerobic conditions. Environmental Engineering-II Civil Engg. Deptt. C O E P. 20

C)1. Emergency control measures a) controlled Chlorination of bulked sludge to kill filamentous organisms. b) Reaeration of return sludge on the recycle line. 2. Long term control measures a) modification and improvement of influent characteristics. b) modification and improvement of plant design and operational parameters.

Recirculation ratio and Concentration of return sludge in ASP

Excess Sludge Influent Aeration Tank (Settled sewage from primary sedimentati on tank) effluent Second aery clarifier Activated Sludge

Return sludge

SVI is related to the volume and concentration of return sludge V=volume of setteled sludge per litre, ml Q=average waste water flow,m3/d Qr=recirculation sludge, m3/d. Suspended solids concentration in recirculated sludge,mg/litre =100ml/l x 1000(mg/g) =106 mg/l SVI(ml/g) SVI

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5.4

Determination of SVI of wastewater Sample

5.4.1 PrincipleSVI determination is based on estimating the volume of sludge settled in 30 minutes per gram of MLSS. 5.4.2 Apparatus and equipmentImhoff cone (or 1000 ml measuring jar), 50 ml measuring cylinder, crucibles,250 ml beaker, whatman no. 40 filter paper (with funnel and stand). Hot air oven. 5.4.3 Procedure of test :A) 1. Take exactly one litre of a mixed liquor sample from in a biological aeration tank and allow it to settle in an imhoff cone. 2. Record volume of settled sludge (V ml/l) at the end of 30 minutes. B) 1 weight a clean and empty crucible (P)W1 mg 2. Stir up the imhoff cone contents well, collect 50ml of the mixed liquor in (P) (25 ml, if a high value of MLSS is expected) and evaporate to dryness in a hot air oven. 3. Cool the crucible (P) to room temperature and weight with solids residueW2 mg. 4.Weight a clean and empty crucible (Q).W3 mg. 5. Stir up the imhoff cone content again and collect 50 ml of the mixed liquor and filter through corrugated whatman no. 40 filter paper and collect the filterate in crucible (Q) and evaporate to dryness. 6. cool the crucible (Q) with dissolved solids residue and weight..W4 mg.

Calculation:
Mixed liquor total solids (MLTS), mg/l = (W2-W1) mg x sample taken (ml) 1000 (ml/l) Mixed liquor dissolved total solids (MLDS), mg/l =(W2-W1) mg x original sample Taken (ml)

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Mixed liquor suspended solids (MLSS), mg/l =MLTS - MLDS SVI, ml/g = V(ml/l) x 1000 (mg/g) MLSS (mg/l)

Observation table:

Sample no.

Description of sample

Volume of settled sludge, ml/l

MLSS, mg/l

SVI, ml/g

Remarks

Result:
Note: SVI value has no practical significance, if the corresponding MLSS value is not satisfactory.

Conclusion:

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6. Determination of Conductivity of wastewater Sample Introduction:Irrigation water, which may be river water, lake water, well water or treated waste water, is evaluated by its total salt concentration excessive salts in water reduce the osmotic activity of plants and diminish the absorption nutrients from soil, affecting plant growth & crop yield. A salt solutions conduct electricity, the concentration of salts in irrigation water is evaluated by determining its electrical conductivity. Low salinity (EC <3000 micromhos/cm) in irrigation water is generally caused by Ca+2, Mg+2 & HCO-3 ions.High salinity (EC 3000 10,000 micromhos/cm) is caused by a combination of Ca+2, Mg+2, Na+ and rarely K+ cations with HCO-3, SO_24 and Cl- anions . Very high salinity (EC > 10,000 micromhos/cm) is caused by Na+ (seldom K+) and Clions.(Bicarbonates ions in combination with the above cation can push the PH upto 8.3 but when carbonate ions are present, PHmay go above 9.0 making water unsuitable for irrigation.) Electrical conductivity is proportional to the ionizablefraction of dissolved solids concentrations. Therefore measurement of conductivity may be used to obtain a quick measure of dissolved salts in water.For water with (PH 5 to 9 & temperature TC ) between 10 to 40 C an empirical expression is , Total dissolved (inorganic) = K1 x (1.02)T_25x conductivity (microm/cm) Solids (mg/l) K is a factor depending on the electrolytic character of water. K= 0.7 , if dissolved solids in irrigation of water contain 83% (generally maximum) salts which conduct current. K = 0.58, if only the electrolytic component of irrigate is required. Salinity problem, related to water quality occurs; if the total quantity of water of salts in irrigation water is high enough to accumulate in the soil which is influenced by drainage characteristics of soil. Light textured soils having a clay content of less than 10% , have excellent internal and surface drainage. EC of irrigation water from 6000-8000 micromhos/cm may be considered safe for semi-tolerant crops, because of effective leaching action. Medium textured soils, having a clay content of 20 to 30 % have moderate drainage characteristics restricting EC of irrigation water to a safe maximum limit of 2000 micromhos/cm Salt tolerance levels of crops,as determined by maximum EC values, beyond which normal crop-yield starts dropping:Crop variety EC of saturated soil extract EC of irrigation water micromhos/cm micromhos/cm Field crops:1.corn 1,700 1,100 2.wheat 6000 4000 3.cotton 7,700 5100 Forage crops:1,500_7500 1000_5000

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Different types of grasses. Vegetables crops:1.Beans and carrots 2.lettuce 3.potato and sweet potato Fruit crops:1. apple, orange, grape & lemon 2. pomegranates 3. date palm.

1000 1300 1600 1700 2700 4000

700 900 1100 1000 1,800 2700

Although many crops have high salt tolerance levels. it is imperative to supply irrigation water with a low concentration , to allow for possible build up of salinity at the plant root zone in the soil especially in arid regions. EC at 25C micromhos/cm < 250 Salinity Low Application Suitable for all crops-field crops; forage crops; vegetables & fruit crops on all soils. Suitable for field crops; forage crops; fruit crops & vegetables crops on soils with moderate drainage. Suitable for some salt tolerant field crops (cotton wheat) some varieties of grasses and some varieties of fruit crops (pomegranates, date palm) on soils with good drainage. Suitable for a very few salt tolerant field crops (cotton wheat) and a few varieties of grasses only on soils with excellent drainage.

250-750

Medium

750-2250

High

2250-3000

Very high

In addition to affecting plant growth, salinity in water also affects fish culture. Salinity reduces solubility of oxygen and results in diminished intake of oxygen through the gills of fish. Standards recommended :1. Tolerance limits for inland surface water for irrigation_ a) electrical conductance at 25C max.3000 micromhos/cm (IS 2296)

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b) TDS (inorganic) , max. 2,100 mg/l (IS 2296) 2. tolerance limit for inland surface water for fish culture electrical conductance at 25 C, max1000 micromhos/cm (IS 2296) Determination of conductivity :Principle:Determination of conductivity is based on measuring the resistance of a column of solution of area A cm2 and length 1 cm. Specific conductance = (1/A) X (1/R), where R is the resistance offered by the soluti & (1/A) denotes the cell constant. Equipment and glass-ware:Conductivity meter 100 ml beakers, 100 ml measuring cylinder (and blotting paper). Chemicals:1. 0.1 N potassium chloride 2. Standard salt solution. Procedure:(The direct reading conductivity meter is one of the types of instrument used for measuring specific conductance of any solution, using a conductivity cell. The cell consists of two electrodes spaced 1 cm apart. Which isolates 1cm3of the sample solution. This design makes the measured resistance independent of sample volume, once the cell is immersed up to the specified mark) 1. 2. 3. 4. 5. Switch on (A) the indicator lamp (B) glows. Put switch (C) on caliberation. Adjust caliberation knob (D) to read 100/300 on the indicator panel. Turn range selector E to extreme right position. Immerse the conductivity cell in 0.1 KCL solution the specific conductance of which is known for the temperature of test,(refer to the conductivity chart of 0.1N KCL). 6. Put C to read position. 7. Turn range selector (E) to get a range (0-30micromhos in this case) in which the needle shows max. Deflection. 8. Adjust cell constant knob (F) so that the indicator reads the right value of conductivity at the temperature of experiment (say 12.88 micromhos/cm at 25C). the instrument is now calibrated . 9. Put (C) on calibration. 10. Clean the cell with distilled water and dry it using a blotting paper. 11. Put range switch (E) to extreme right position (this is important to prevent damage, if the meter deflects beyond the full scale in the wrong range). 12. Dip the cell in the given sample solution (a minimum of 60 ml is required in a 100mlbeaker to immerse the electrodes upto the mark). 13. Put (C) to read position.

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14. Turn the range switch (E) to obtain maximum deflection. 15. Read the specific conductance of the sample on the proper scale [(0-100) if the range selector shows 1, 10 or 100 and (0-300) if the range selector shows 3, 30 or 300].

Reference chart of conductivity of 0.1 N KCL: Temperature C 15 16 17 18 19 20 Temperature C 27 28 29 30 31 32 EC mmhos/cm 10.48 10.72 10.95 11.15 11.43 11.67 Temperature C 21 22 23 24 25 26 EC, mmhos/cm 12.01 12.15 12.39 12.64 12.88 13.13

EC,mmhos/cm 13.37 13.62 13.87 14.12 14.37 14.62

Preparation of caliberation chart of the instrument used :1.Prepare standard dilutions of known salt concentration using 3000 mg/l of KCL solution (S). 2.Determine conductivity of each diluted standard. 3. Plot conductivity (X-axis) Vs salt concentration (Y-axis). 4.Drop on ordinate corresponding to the conductivity of the sample and read out the equivalent total salts concentrations on the (Y-axis).

Note: the calibration graph will be a straight line, passing through the origin, if the distilled water used for preparation of standard solutions is very good in quality, and KCL salt is used is 100% pure. An intercept on the X-axis indicates ionized salts present in distilled water. An intercept on the Y-axis indicates non ionizable salts or solids (impurities)

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Present in KCL salts.

Observation table:

Salt concentration mg/l

Dilution

Volume of Volume of Conductivity, standard diluted micromhos/cm solution (S) ml standard, ml x103

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7) Study of waste water micro-organisms of wastewater Sample

Biological characteristics ; These are due to the presence of microorganisms, which includes bacteria, fungi, algae, protozoa, rotifers, crustaceans and viruses. A brief description of there characteristics and the role played by them in stabilizing organic matter as in sewage treatment and in influencing human environment is given below.

Bacteria ; They are the simplest form of plant life, are single cell organtsms, which use soluble food and are capable of reproduction. Bacterias are the fundamental organisms in the stabilization of organic wastes and therefore are much important in biological treatment. They are present in vast numbers in sewage. One liter of sewage may contain 22 to 55 million bacteria. Most of these bacteria are harmless to man and are largely engaged in the beneficial process of converting the complex organic compounds of sewage into simpler, stable organic and mineral compounds resulting in the purification of sewage. Some of the bacteria may however be harmful, particularly the disease producing or pathogenic type and may constitute a real danger to the health of the public. Based on nutritive requirements, bacteria are classified as heterotroph ic bacteria and autotrophic bacteria. Heterotrophic bacteria use organic compounds and carbon source for synthesis. They can be broken up into three groups based upon the manner of satisfying there oxygen requirements. These are aerobic, anaerobic and facultative. Aerobic bacteria require free dissolved oxygen to live and multiply. Anaerobic bacteria live and develop in the absence of free dissolved oxygen and there oxygen requirements come from the oxygen radicals of organic compounds and mineral substances as nitrates and sulphates. Facultative bacteria e.g. Escherichia Coli are common to either of the aforesaid types-they use free dissolved oxygen when available but also can respireand multiply in its absence. Besides, there is a particular heterotroph called saprophytic bacteria, which abounds in the upper layers of the soil and lives on the dead organic matter into stable humus-like products. Autotrophic bacteria use CO as a carbon source and oxidize inorganic compounds for energy. As nitrifying, sulphur and iron bacteria, there importance is principally in the corrosion of pipe sewers as well as in pipes conveying water containing dissolved iron. They can also be further classified as aerobic, anaerobic, and facultative depending upon there need for oxygen.

Fungi: They are multi-cellular, non-photosynthetic plants and include yeasts, molds and bacteria. Though bacteria are aclass of fungi, because of its importance bacteria are considered separately. Most fungi are strict aerobes, they have the ability to grow under low moisture conditions and low ph environments in the range 2 to 9. Fungi also have low nitrogen requirement. The ability of fungi to survive under low ph and nitrogen limiting conditions make them very important in the biological treatment of waste and in the composting of solid organic waste. Algae: They are uni-cellular or multi-cellular autrophic photosynthetic plants. In the presence of sunlight, algae convert the inorganic materials in the water into inorganic matter in the form of protoplasm through the process of photosynthesis. This is represented by the following equation;

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CO2 + H2O SUNLIGHT

CH2O + O2 +H2
( new algae cells)

The ability of algae to produce oxygen is extremely important to ecology of water environment. Algae are autrophic- using CO2 (or bicarbonates in solution) as a carbon source. Algae grow in abundance in oxidation ponds rich in inorganic nutrients and CO2 released from bacterial decomposition of organic wastes. Green algae chlorellas are commonly found in oxidation ponds. Protozoa: They are single cellular animals, which reproduce by binary fission and live mainly by eating bacteria. The common types are rhizopoda, flagellate and cilliate. The protozoa, which are of importance in biological treatment, are strictly aerobic, non photosynthesis organisms generally found in oxidation ponds, trickling filter and and in activated sludge. These microscopic animals have complex digestive systems, which use solid organic matter as an energy and carbon source. Protozoa form a vital link in aquatic food chain since they ingest bacteria and algae. Rotifers: They are the simplest multi-cellular animals. They are also strictly aerobic and metabolize solid food from bacteria. They can ingest only small organic particles. Because of their metabolic habits rotifers are found only in water of organic content. They act as good indicatos of low pollutional water and are regularly found in streams and lakes. A typical rotifer philodina is distinguished from the cilia around its head which it uses to catch food through a rotary action which probably is the source of its name. Crustaceans: They are multi-cellular animals having rigid shell structure e.g. daphnia and Cyclops. The crustaceans are strict aerobes, which feed on bacteria and algae. They are important as a source of food for fish. Crustaceans have been used to settle algae laden effluents from oxidation ponds. They are generally found in relatively stable streams and lakes. Viruses: they are the smallest plant cells known at present. These are inter-cellular parasites, which derive their nutrients from the host organisms in which they also reproduce. Viruses are highly specific in their reactions, with some parasitic to plants while some parasitic to animals. Many viruses are pathogenic i.e. disease producing in man and are known to be excreted in the feces of humans. In waste treatment, viruses need to be effectively controlled which is usually done by chlorination through concentration of free available chlorine and by proper disposal of plant effluent. Growth pattern of biological microorganisms: Generally bacteria reproduce by binary fission i.e. by dividing. The original cell begins two new organisms. The time required for each fission, which is termed as generation time can vary from days to less than 20 minutes. The general growth pattern in a batch culture has three phases; 1. logarithmic growth phase: It starts as the microorganisms come in contact with substance i.e. food which is organic matter. The microorganisms start to reproduce by binary fission. The number and mass of microorganisms rapidly increase but the increase in the rate of metabolism is limited by the microorganisms ability to process the substrate. Declining growth phase: it occurs due to the limitation of the available food. As the microorganisms lower the food concentration, the rate of growth becomes less and less. As the food gets exhausted, the growth of new cells is offset by the death of old cells, so that population remains stationary.

2.

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3.

Endogenous phase: when growth ceases, the food concentration is at a minimum. However, the microorganisms still complete for the remaining small quantity of organic matter in solution. As the available food is unable to satisfy the demand of the microorganisms, they are forced to metabolize on their protoplasm. As a result the total mass of microbial protoplasm decreases. And the rate of metabolism falls. The protoplasm being an energy source, the cells are starved out and ultimately die. The endogenous phase is considered important for the complete stabilization of organic waste. It may be pointed out that the aforesaid concerns the growth of a single population of microorganisms. The biological treatment processes are often composed of complex and mixed biological population with each particular microorganism having its own growth curve depending upon a variety of factors such as temperature, PH, availability of nutrients, presence of substrate, presence of toxins etc. thus it is found that the vast majority of biological systems operate best in the temperature range of 20C to 40C suitable to the growth of mesophillic bacteria, and in a neutral environment with PH around 7.2 to 7.4. such systems are adversely affected by the presence of toxic substance present in industrial wastes e.g. phenol and copper, chromium ions from metal finishing industries. In short, the growth pattern of mixed biological population shows variation of microorganism predominance with time in the aerobic stabilization of organic wastes. While bacteria are of primary importance, many other microorganisms take part in the stabilization of organic wastes.

DIAGRAMS OF DIFFERENT TYPES

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8) Determination of Phosphate content of wastewater Sample Aim: To determine the total phosphate content of given sample. Apparatus: Spectrophotometer, volumetric flask, beakers etc. Reagent: phenolphthalein indicator aqueous solution, strong acid solution (6N H2SO4), ammonium molyodate reagent (NH4)6MO7. 4H2O , stannous chloride reagent Sncl2. 2H2O. SIGNIFICANCE: 1. The main significance of phosphate data are as follows: a) it is used to control, phosphate dosage in water system for corrosion prevention and in boilers to control scaling. b) Phosphorus is essential for the growth of algae and hence growth of algae blooms natural stream receive effluents can be controlled by limiting the amount of phosphates in the effluent. c) Because of the importance if phosphorus as nutrient in biological methods of waste water treatment, its determination is necessary with many industrial wastes and in the operation of waste treatment plants. DESCRIPTION OF APPARATUS: SPECIFICATIONS: a) Make BAUSCA and LOMB (USA b) MODEL spectronic-20 c) Wavelength range 1 d) Standard photo tube340 nm to 600 nm. e) Red photo tube 600nm to 900 nm. f) Wide range photo tube600nm to 700nm. g) Spectral slit width 20nm. h) Wavelength readability 1.0nm. i) Photometric readability 0.5% j) B. OPERATION PROCEDURE: a) Turn on warm up 15 min.

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b) c) d) e) f) g)

Set zero Wavelength Insert blank Set full scale Insert unknown Read % transmission and absorbance

THEORY: In only inorganic compounds of phosphorus of significance in engineering practice are the phosphates usually referred to as polyphosphates. Domestic wastewater is relatively rich in phosphorus compounds. It contains 2 to 3 mg/l of inorganic phosphorus when phosphorus based detergent is not used. Most of the inorganic phosphorus is contained by human wastes as a result of the metabolic breakdown of proteins and elimination of the liberated phosphates in the urine. Synthetic detergent formulations designed for household market contain large amounts of polyphosphates. The use of these materials as substitutes for soap has greatly increased the phosphorus content of domestic wastewater. It has been estimated that domestic waste water probably contains form two to three times as much inorganic phosphorus at the present time as it did before synthetic detergents became widely used. Domestic waste water contains amount of phosphorus for in excess of the amount needed to stabilize the limited quantity of organic matter present. All the polyphosphates (molecularly dehydrated phosphates) gradually hydrolyse in aqueous solution and revert to the or the form from which they were derived. For the measurement, both poly and organic forms of phosphorus must be converted to orthophosphates. Phosphorus occurring as orthophosphates (H2PO4 HPO4-2 PO43-) can be measured quantitatively by gravimetric, volumetric or colorimetric methods. Gravimetric and volumetric methods are used for phosphates concentrations exceed 50 mg/l, but these methods are time consuming, hence most analysts prefer to use colorimetric method, at some sacrifice of accuracy. In colorimetric method phosphates ion combines with ammonium molybdate under acid conditions to form a complex compound known as ammonium phosphomolydate. PO43- +12(NH4)4 MOO4 +24H+(NH)4 3PO4 12MOO3 + 21 NH4 + 12 H2O The molybdenum contained in ammonium phosphomolybdate is also reduced to produce a blue colored solution that proportional to the amount of phosphate present excess ammonium molybdate is not reduced and therefore does not interfere. Stannous chlorides uses as the reducing agent. The colored compound formed has never been isolated and its formula is unknown, it is referred to as molybdenum blue. The stannous chloride reduces as below. (NH4)PO4 12MOO3 + Sn2+.molybdenum blue + Sn4+

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PROCEDURE: 1. 0.5, 1.0, 1.5, 2.0, 2.5, 3.0, 3.5, 4.0 ml of standard solution are pipetted into 100ml volumetric flask and diluted to100ml with distilled water. 2. 4ml ammonium molybdate reagent and 0.5ml stannous chloride reagent are added to each flask and mixed thoroughly. 3. Contents of each flask allowed to stand for 10 minutes. 4. Absorbance of each flask is measured in spectrophotometer against reference blank prepared by treating distilled water with specified amount of all reagents except standard phosphate solution. 5. a calibration curve is constructed for absorbance against microorganisms of phosphate. 6. To 100 ml sample containing not more than 200mgm. Phosphate free from colour and turbidity, add 1 drop of phenolphthalein indicator if sample turns pink, add strong acid solution drop wise to discharge the color, if more than 5 drops are required take a smaller samples and dilute to 100ml with distilled water after first discharging the pink colour with acid. 7. Add 4 ml of molybdate reagent and 0.5ml stannous chloride reagent with through mixing after each addition and allowed to stand for 10 minutes. 8. Absorbance is measured &corresponding micrograms of phosphate is read from calibration curve. 9. Then calculate total phosphate content using the formula; Total phosphate mg/l = (micrograms phosphate/ml of sample)

Sr. no. 1. 2 3 4 5 6 7 8 9 10

Concentration (mg/l)

Absorption (%)

Results:

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Conclusion

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