CROSS CURRENT LEACHING Aim: To study the principle governing leaching and compare the result obtained by conducting

test on a mixture of Sodium Carbonate and sand. Apparatus Required: 500 ml Beaker Funnel Pipette Burette Glass Rod Filter paper

Chemicals required: Principle: The process of leaching deals with removal of solvent constituent from solid by means of liquid solvent. It is generally necessary to recover or separate either by evaporation or any other means the component of new system i.e., solute and solvent which was extracted. It is important because it is generally necessary for product the most economical scheme for leaching process. Leaching differs very little from the washing of filtered solids as discussed and leaching equipment strongly resembles the washing section of various filters. In leaching the amount of solute material removed is often greater than in ordinary filtration washing and the properties of the solids may change considerably during the leaching operation. Coarse, hard or granular feed solids may disintegrate into pulp when their content of soluble material is removed. Procedure: Cleaned and dried 500 ml beakers were taken and then numbered. Weigh a quantity of 50 g of sand and 20 g of Na2Co3. Add 100 ml of distilled water and stirred well. Sodium Carbonate (20 g) Sand (50 g) Hcl (0.5 N) Phenolphthalein Indicator

Filter the solution using the filter paper and the filtered off. 10 ml of the raffinate is taken and titrated against 0.5 N HCl Solution using Phenolphthalein as indicator and note the titre value. Then add 100 ml of distilled water again to the titrate and the above procedure was repeated. The same procedure was repeated for three stages.

Examples of leaching operation: o o o o o Extraction of gold from its ores by using sodium cyanide solution. Extraction of sugar from sugar beats using hot water Extraction of tannin from tree bark using H2O Extraction of perfumes from flowers Preparation of tee and coffee

Result: The stage efficiency using cross current leaching was found to be Stage I Stage II Stage III = = =

Extract

Extract

Extract

50 g sand +

Raffinate

Raffinate

Raffinate

20 g Na2CO3

S.No

No. of Stage

Volume of extract Collected (ml)

Volume of extract taken for filtration against Hcl (ml)

Titre Value (ml)

100 ml Water

100 ml Water

100 ml Water

DETERMINATION OF STAGE EFFICIENCY USING COUNTER CURRENT LEACHING

AIM:
To verify the properties of counter current leaching of a mixture of oxalic acid and sand using water by a three stage process.

APPARATUS REQUIRED:
Conical flask-6 nos (500 ml) Burette-50ml Pipette-25ml,10ml Beaker- 200ml (2 nos) Measuring jar-500ml Conical flash-250ml(2 nos)

PROCEDURE:
1) 250g of sand, 2.5g of oxalic acid and 100 ml of water are taken in each of 6 conical flasks. 2) Another 100 ml of fresh water is added to the flask one, content are mixed well for 5 min and allowed to settle. 3) 100ml of leached solution is transferred from flask one to flask two, agitated well and allowed to settle. 4) 100ml of leached solution is transferred from flask 2 to flask 3, agitated well and allowed to settle.

5) 100ml of leached solution from flask 3 is discarded; flask 1 is removed after this trial. 6) Next 100ml of fresh water is once again added to flask 2. 7) Once again the above procedure is repeated with flask 2, 3, 4 with flask 2 removed after this trial. 8) Then with 3, 4,5 with flask 3 is removed and finally with 4,5,6. 9) From the last of trial 4, 5,6 leached solution from these are titrated against standard NaOH solution when phenolphthalein as indicator (colour changes from colourless to pale pink). 10) Readings are tabulated; calculation as done and graph are plotted.

TABULATION: FLASK NO STAGE NO TITRE VALUE OXALIC ACID IN EXTRACT % EXTRACT

CALCULATION: STANDARDISATION OF SODIUM HYDROXIDE (NaOH): Volume of oxalic acid, V1 = Normality of oxalic acid, N1 = ml N ml N

Volume of sodium hydroxide, V2 = Normality of sodium hydroxide,N2 = V1N1 = V2N2 N2 = V1N1/V2 N2 = N

STAGE 1: Volume of oxalic acid, V1 = Normality of oxalic acid, N1 = Volume of NaoH, V2 = Normality of NaoH, N2 = V1N1 = V2N2 N1 = N ml N ml N

Amount of oxalic acid present in extract = (volume * normality * equivalent weight)/1000 = g

STAGE 2: Volume of oxalic acid, V1 = Normality of oxalic acid, N1 = Volume of NaoH, V2 = Normality of NaoH, N2 = V1N1 = V2N2 N1 = N g ml N ml N

Amount of oxalic acid present in extract = (Volume* Normality * Equivalent weight)/1000 =

STAGE 3: Volume of oxalic acid, V1 = Normality of oxalic acid, N1 = Volume of NaoH, V2 = Normality of NaoH, N2 = V1 N1 = V2N2 N2 = N ml N ml N

Amount of oxalic acid present in extract = (volume * normality * equivalent weight)/1000 = Overall percentage extract = (stage 1 + stage 2 + stage 3)*100*(1/2.5) = %

RESULT:

Overall percentage extracted by three stages process = Amount of oxalic acid in

1) I stage = 2) II stage = 3) III stage =

% % %

LIQUID - LIQUID EXTRACTION

Aim: To determine the extraction characteristics of the solvent at various volume. Apparatus required: Beaker. Burette. Funnel. Separating funnel column.

Chemicals required: 15% Acetic Acid solution. Ethyl Acetate. Sodium Hydroxide 0.5N. Phenolphthalein Indicator.

Theory: Liquidliquid extraction, also known as solvent extraction and partitioning, is a method to separate compounds based on their relative solubilities in two different immiscible liquids, usually water and an organic solvent. It is an extraction of a substance from one liquid phase into another liquid phase. Liquid extraction is one of the main alternatives to consider. Close boiling mixture or substance cannot withstand the temperature of distillation. Even under a vacuum may often be separated from impurities by extraction which utilises chemical differences instead of vapour pressure differences.

When either distillation or extraction may be used the choice is usually distillation in spite of the fact that heating and cooling are needed. In extraction the solvent must be recovered for reuse usually by distillate and combined operations is more complicated and often more expensive then ordinary distillation without extraction. However, extraction does offer greater flexibility in choice of operating conditions, since the type and amount of solvent can be valid as well as the operating temperatures.

Procedure: 1. 50ml of 15% acetic acid is taken in four conical flasks. 2. Ethyl acetate solvent of different volume (say 25, 50, 75 & 100) in ml added to each conical flask. 3. After thorough mixing, ethyl acetate will extract the acetic acid and form two layers. 4. The two layers can be separated by using separating funnel and the raffinate was taken in the burette. 5. A standard solution of NaOH was titrated against the burette solution with the help of phenolphthalein indicator and calculations were made. Applications: Long chain fatty acid can be separated from vegetable oils by high vacuum - distillation but more economically by extraction with liquid propane. Liquid extraction which incurs no chemical consumption or by product can be less costly. Metal separation such as Uranium Vanadium, Tungsten molybdenum and the fission products of atomic energy process are more economical by liquid extraction.

Result: The extraction characteristics of the solvent at various volumes can be determined.

S.No

Solvent amount

% of Extraction

Distillation co-efficient

Feed 5o ml Acetic Acid Solvent Ethyl Acetate Raffinate

1
Extract

Feed 5o ml Acetic Acid Solvent Ethyl Acetate

Raffinate

2
Extract

Feed 5o ml Acetic Acid Solvent Ethyl Acetate Raffinate

3
Extract

Feed 5o ml Raffinate Acetic Acid Solvent Ethyl Acetate

4
Extract

Tabulation: S.No 15% Acetic Acid solution (ml) Solvent solution (ml) Titre Value (NaOH) (ml) % of Extraction Distribution Co-efficient

MOLECULAR DIFFUSIVITY AT CONSTANT PRESSURE AND DIFFERENT TEMPERATURE Aim: To determine the diffusivity of acetone air system at a known temperature. Apparatus Required: Diffusivity measurement Thermometer Stop Clock

Formula Used: 1) Diffusivity, DAB = NA*x (RTZ) x PBM / PT x (PA1-PA2)

Where, NA*- Molar flux of acetone = moles/ time x area R - Universal gas constant T - Temperature, K Z - Distance between the maximum and minimum concentration point PT - Total pressure PA1- Partial pressure of acetone at section 1 PA2- Partial pressure of acetone at section 2 2) PBM = PB2-PB1 / ln( PB2/PB1 ) Where, PBM log mean pressure of B (mm of Hg) PB1 - pressure of area of section 1 PB2 pressure of area of section 2 3) NA = V x / MA x T x A Where, V- Volume of acetone used Density of acetone and the temperature of water bath MA molecular weight of acetone T- Time taken for diffusion

A Area Procedure: Acetone was added to the diffusivity cell surrounded by water and the heater blower was turned on. When the temperature attained the constant value, initial distance of acetone level in the diffusivity cell from the top was noted down and the stop watch was started. The final distance of acetone level from the top after the decrease of 1cm level from the initial value was noted down and the total time taken for the decrease in 1 cm in acetone level was recorded. The temperature was noted down. Readings were tabulated and diffusivity of acetone vapour in air was calculated.

Tabulation: TIME ( sec) T-TUBE READING MANOMETER READING TEMPERATURE (0C)

Z1 (cm)

Z2 (cm)

L.H.S

R.H.S

Result: The diffusivity of acetone vapour in air DAB =

MOLECULAR DIFFUSIVITY AT CONSTANT TEMPERATURE AND DIFFERENT PRESSURE

Aim: To determine the diffusivity of acetone in air at constant temperature by Stephens tube method. Apparatus Required: Procedure: Acetone is taken in Stephens tube and its level Z1, is noted. A constant temperature bath is maintained with a magnetic stirrer and air is supplied at one end of the tube to ensure that there is no stagnant acetone at the tube outlet. Stop watch is stored simultaneously and time required for that active level for drop by 2ml is noted. Again the level is noted (Z2). The experiment is repeated for different temperature. The density of acetone is determined using specific gravity bottle. Stephens tube Pipette Rubber pipe Stop watch Manometer

Formula:

1) DAB = PBM x RT x ( Z22 Z11 ) acetone / PT x (PA1 PA2) x x MA 2) PBM = PB2 PB1 / ln( PB2/PB1) Where, DAB = diffusivity of acetone in air (m2/s) PBM = log mean pressure of B (mm of Hg) acetone = density of acetone (kg/m3) Z = Head of liquid column (mm) PT = Total pressure (mm of Hg) PB1 = Partial pressure of air at methyl isobutyl acetone surface PB2 = Partial pressure of air at other end PA1 = Vapour pressure of organic fluid PA2 = Vapour pressure of other fluid = Time required for decrease in level of acetone by 2mm (sec) MA = Molecular weight of acetone Tabulation: TIME ( sec) T-TUBE READING MANOMETER READING TEMPERATURE (0C)

Z1 (cm)

Z2 (cm)

L.H.S

R.H.S

Result: The diffusivity of acetone in air pressure DAB =

PAN EVAPORATOR
AIM:

To determine the rate of evaporation of varying heat. To determine the mass transfer coefficient using Himus equation.

APPARATUA REQUIRED: Water, Scale, Thermometer, Pan, Stopwatch, Electric heater, 20% NaOH solution and Beaker THEORY: Evaporation is the process of concentrating the liquid solution by evaporating a part of solvent. It is the process where atoms and molecules in a liquid state or solid state enter the gaseous state. Evaporation of a solution is an external step in the operation of a crystalline unit. The crystallizing solution is super evaporated to make it super saturated solution. FORMULA: (I) Volume of water evaporated (V)
V = /4(d2h) (m3)

Where, d= diameter h=height of head level of solution decreased (m) (II) Mass of water evaporated (m) M = V x (Kg) Where V = Volume of water evaporated (m3) = Density of water (Kg/m3) (III) Rate of mass transfer () = M/t (Kg/s) Where, t = time taken for evaporation (s) M = mass of water evaporated (Kg) (IV) Himus equation /A = K(Ps-Pw)

Where, K = Mass transfer coefficient (Kg/m2 s atm) Ps = Vapour pressure of water at operating condition (1 atm) Pw = partial pressure of water at operating condition (1 atm) PROCEDURE: Fill the pan up to 3/4th level with water and allow it to boil. Note down the time taken for reduction of 0.2 cm of water level in the pan. Measure the operating temperature of water using thermometer. Note down the time taken and temperature of water using thermometer. The readings are tabulated.

FACTORS AFFECTING: Concentration, Focusing, Temperature of substance, Scale formation, Material of construction, Flow rate of water and Air current. PRECAUTIONS: Check whether the pan evaporator is placed properly over the heater. At any time empty pan should did not be placed on the heater.

INDUSTRIAL APPLICATIONS: Evaporator is used to concentrate the organic solution. Used for concentrating pharmaceutical products. Used in large scale industries (sugar industries).

TABULATION: d = 18.3 x 10-2 m Sample Temperature Height Time (min) Rate of Evaporation 10-4 (Kg/s) Mass transfer coefficient Kg/m2 s atm

Initial Pure water

Final

20% NaOH

40% NaOH

DIAGRAM:

RESULT: The experiment has been carried out to determine the rate of evaporation and mass transfer coefficient.

Rate of Evaporation:

Pure water 20% NaOH solution 40% NaOH solution

= = =

kg/s kg/s kg/s

Mass Transfer Coefficient: Pure water 20% NaOH solution 40% NaOH solution = = = Kg/m2 s atm Kg/m2 s atm Kg/m2 s atm

SIMPLE DISTILLATION
Aim: 1. To find the relative volatility of the given liquid mixture 2. To verify Rayleigh Equation analytically and also graphically. Theory: A distillation is the process of separation of liquid mixture of a material to obtain one or more desired components present. A bath of liquid changed to a kettle or steel fitted with some heating devices such as steam jacket .The change is boiled steady and the condensate (distillate) is collected in the reservoir. The apparatus is essentially a large unit or ordinary laboratory distillation will be the most volatile substance and as distillation proceeds, the vaporized product becomes leaner. The distillate can be collected in several repeated batches called out to give a series of distilled product of various positions .Thus the simple distillation procedure as a standard for composition. Materials Required: Round bottomed flask Thermometer 25ml Beaker Condenser Beaker Measuring Jar

Glass Beads

Formula Used: 1) Rayleighs Equation (Graphically) ln (F/W) = xWxF dx/(y*-x) Where, F W y* x -Total number of moles in feed samples (gmol) -Total number of moles of residue (gmol) -Mole fraction of Vapor in equilibrium with a liquid - Mole fraction of liquid

2) Rayleighs Equation (Analytical Method) ln (F/W) = ln { (xD-xW)/(xD-xF) } Where, xD - Mole fraction of distillate. xW XF - Mole fraction of residue. - Mole fraction of feed.

3) Relative Volatility of Liquid mixture log (F xF/WxW) = log {F (1- xF) / W(1- xW)} Where, - Relative Volatility of the system. Procedure: A Calibration chart of density of liquid mixture is mole fraction of ethanol was prepared. 100 ml of CH3CH2OH and 50 ml of H2O is taken in a beaker and then the contents are transformed to round bottomed flask and heated. Water is admitted to the condenser and heater is switched on. The liquid mixture is gently until 2/3 of liquid mixture is vapourised by gradual increase of heat after regarded volume of reaction is obtained. The Heater is allowed to cool. The volume of distillate and residue is collected and measured. Composition of residue and distillate is found out using calibration chart. Rayleigh equation is verified by using the area by plotting graph for (y*-x) vs x.

Industrial Applications:

 Result:

To separate naphtha from crude oil To distill Ethanol from sugar molasses To separate Ammonia from aqueous solution of ammonia and water.

The simple distillation experiment was carried out using ethanol-water system and Rayleighs equation was verified experimentally and theoretically. Experimental Value Theoretical Value = = =

The average relative volatility was found to be Tabulation:

S.No Vol. of H20 (ml) Vol. of Wt. of H20 (ml) Wt. of

Moles of

CH3CH2OH (ml)

CH3CH2OH CH3CH2OH (ml) (ml)

Moles of H20

Relative Density

(ml)

Model Graph 1

Model Graph 2

Moles of H20

Moles of

CH3CH2OH

Mole Fraction of

CH3CH2OH

1/y*-x

SOLID IN AIR DIFFUSION

Aim: To determine the diffusivity co-efficient of the given solid in air and to determine the functional relationship among the dimensionless numbers. Introduction:
Molecular Diffusion is one of the important parameter in mass transfer studies. This is movement molecule through a substance by virtue of thermal energy. The diffusivity or diffusion coefficient DAB of constituent A in a solution B, Which is a measure of diffusive mobility and is well defined by Ficks first law. JA =DAB dCA/ dz This experimental set up is designed and developed for a case of diffusion of (A) D Camphor through non diffusing (B) air. For this we assume the following:

The air layer adjacent to Solid is saturated with the solid. The diffusion is steady and unidirectional. The vapors of the solid at the end of the cell are completely driven away and only fresh air is present.

Procedure: Switch ON the compressor and allow it reach sufficient pressure (4 kg/cm 2 ) Note down the initial weight of the solid under study state. Fix the solid to the clamp provided. Open the air inlet valve and adjust the flow rate of air. Start the stop watch. Note down the final weight of the solid after two hours. Switch OFF the compressor.

OBSERVATIONS AND CALCULATION: 1. Initial weight of the solid, mi (Z1) = _______Kg 2. Final weight of the solid, mf (Z2) = ________Kg 3. Air flow rate, Q = _______m3/sec 4. Molecular weight of the solid, Camphor (C10H16O) = 142 5. Total pressure = mm Hg 6. Room temperature TR = C

7. Density of organic liquid at TR = 999 Kg/m3 8. Diameter of diffusivity tube = 100 mm For diffusion of A through non-diffusing B, 9. NA = PT DAB ln[(1 Ya2)/(1 Ya1)] RTZ 10. NA = Rate of diffusion/unit area, kmol/m2-sec 11. PT = Total pressure, = mm hg = Bar = N/m2

12. R = 8.314 103 J/Kmol K 13. Z = Z1 Z2 , Kg 14. PA1 = Vapor pressure of the solid = mm Hg

Vapor pressure data for d-Camphor: Perry 6th Edition, Pg no. 3-52, Table 3-8

15. PA2

Partial pressure at the top of the cell = 0 mm Hg at 27 Deg Celsius

16. Ya1 = mole fraction of organic liquid = Pa1/PT 17. Ya2 = Pa2/PT = 0 The vapor pressure of organic liquid at certain temperature can be obtained from the above graph. 18. NA = [Volume of Solid diffused in air density of solid at T C] Molecular weight of organic liquid

Cross sectional area of Tube X Time

NA = [Q ] MA 2 ( d / 4) 20 60

(MA=Molecular wt. of organic liquid)

NA = ________________ Kg/m2-sec

Diffusivity coefficient DAB = NA RTZ ln (1 Ya1) PT (1 Ya2)

DAB = _____________ m2/sec

Sl. No.

Flow rate

Initial Level Z1 Cm

Final Level

Time Sec

Z average

NA Molar flux

DAB Cm2/Sec

Z2 Cm

1 2 3 4

Result:

The diffusivity co-efficient of the Naphthalene in air= KG = Kc =

The functional relationship was found from dimensionless numbers

Sh= Sc = Re =

SOXHLET EXTRACTION
Aim: To determine the percentage extraction of solute from the given sample using different solvent. Apparatus required: Soxhlet extraction. Electrical heater. Tea powder. Solvent Benzene, Water.

Formula used: % Extraction = Theory: Leaching is defined as the separation of soluble material dissolved from its mixture with an inlet solid by means of liquid solvent. The leaching is used in varieties of industrial applications such as metallurgical sugar pharmaceutical etc. In the soxhlet extraction the solid from an open solvent precoated through the agitated bed of solids. The solids are dispersed into the solvent and later separated from it. Procedure: 100

The known amount of solid material was weighed and taken into the soxhlet apparatus. The solvent is placed in the round bottom flask which is kept on the heater. Then the entire apparatus setup is along with condenser and the solvent is heated. The solvent vapour condensed in the condenser and it was sent down through the solid material. The condensed solvent was extracted the soluble material from the mixture and it is collected in the round bottom flask. The complete removal of soluble material from the solid material is taken into the drier.

Result: The percentage of extraction of the solute from the given samples by using soxhlet apparatus is found by, % Extraction [ for Water] % Extraction [ for Ethanol] Keq = = =

SOXHLET APPARATUS

STEAM DISTILLATION
AIM: To determine the overall efficiency of steam distillation. To determine the theoretical temperature for the same operation. APPARATUS REQURIED: Round bottom flask Steam generator Condenser Heater Measuring jar

PROCEDURE: 1) The feed is aniline (mixture of aniline and water) in the ratio 1:3 was feed to the column.

2) Then the heater was switched on to supply heat for steam generator. 3) The steam was passed into the separation vessel and packed up aniline and causes to condensate. 4) Upto 1/3 rd of the mixture is obtained as distillate water is measured after separating it into a conical flask. 5) The composition of distillate was calculated.

TABULATION: S.No Temperature (K) PA = PT PB (mm of Hg)

CALCULATION: Volume of aniline in distillation Volume of water in distillate Mass of aniline in distillate Mass of waterr in the distillate Volume of aniline in residue Volume of water in the residue Mass of aniline in residue Mass of water in residue Initial bioling point Final boinling point Vapor pressure of aniline PA = = = = = = = = = = =

Vapour pressure of water PB=PT-PA = 760-

TABULATION: S.No Temperature Vapour pressure of Water (PB) mm of Hg Temperature Vapour pressure of Acetone mm of Hg

FORMULA USED: 1. WA= (PA-MA)/( PB MB) = Where, MA- Molecular weight of aniline MB - Molecular weight of aniline 2. Actual amount of aniline /kg of steam used, WA= Kg of aniline / kg of steam kg of aniline/ kg of water

3. Efficiency = ( WA/ WA)*100

RESULT:

1) Theoectical amount of aniline / kg of H2O in distillation = steam 2) Actual amount of aniline/kg of steam used = 3) Vapouraisation efficiency = %
0

kg of aniline/ kg of

kg of aniline/ kg of steam

4) Theoretical temperature of steam distillation=

STERLING JACKETED PAN EVAPORATOR

AIM: To determine the mass transfer coefficient.

APPARATUA REQUIRED: Pan, Steel Pan, Stopwatch Thermometer, THEORY: Evaporation is an operation that is carried out in industry as a means of concentration of the weak liquor (or) solution by vaporising of solvent. The heat is utilised to (a) Increase the temperature of the solution to its boiling point and, (b) Supply the latent heat of vaporisation of solvent its process where the atoms and molecules in a liquid state or solid state in substance sufficient energy enter the gaseous state. FORMULA: (I) Mass of water evaporated (m) m = V x (Kg) Where V = Volume of water evaporated (m3) = Density of water (Kg/m3) (II) Rate of mass transfer or (Evaporation) () = m / t (Kg/s) Where, t = time taken for evaporation of water (s) m = mass of water evaporated (Kg) (III) Himus equation /A = K(Ps-Pw) Where, K = Mass transfer coefficient (Kg/m2 s atm) Ps = Vapour pressure of water at operating condition (1 atm)

Pw = Partial pressure of water at operating condition (1 atm) PROCEDURE: Fill the pan up to 3/4th level with water and allow it to boil. The steam is admitted in the jacket Note down the time taken for reduction of 0.5 cm of water level in the pan. Measure the operating temperature of water using thermometer. Note down the time taken and temperature of water using thermometer. The readings are tabulated. The thick liquor is then drained out from outlet. Note down the temperature of steam inlet and steam outlet.

TABULATION:

S.No

Temperature of Feed (C)

Temperature of Steam (C)

Temperature of Condensate(C)

Initial height(cm)

Final height(cm)

Time (S)

TABULATION:

S.No

Temperature (C)

Ps (atm)

Ps Pw (atm)

W/A (Kg / m3)

K = W / A / Ps Pw

(Kg/m2 s atm)

RESULT: The experiment has been carried out to determine the rate of evaporation and mass transfer coefficient by using sterling jacketed pan evaporator.

Mass Transfer Coefficient

(Kg/m2 s atm)

Rate of evaporation

TRAY DRIER
Aim: To study the characteristics of a given sample (sand) in a tray drier and to find the vapour drying zone for the above sample and drying for constant rate period and falling period. Apparatus Required: Sand, tray drier, equipment, stopwatch. Formula used: Rate of drying: N=SS/A (-dx/dt) g evaporated/m2s Where, Ss=dry weight of the sample (g) A= area of the drying surface (m2) Time of drying for constant rate period: tC= SS/A(X1 XC) s Where, tC= Rate of drying during constant rate period X1= Initial moisture content (g of moisture)/(g of dry solid) XC= Critical moisture content (g of moisture)/(g of dry solid) Time of drying for falling rate period:

tF= SS/A Where, = Area under the curve

Total time of drying: t = tF + tC (s) Where, tF= Time of drying for falling rate period (s) tC= Time of drying for constant rate period (s) Procedure: Accurately weigh the sample and it is taken. It is made to paste by adding water in a tray. It was placed inside the drier and the door was tightly closed after which the drier was balanced and heated to by switching on the heater and the temperature was made constant by switch on the blower. Time was constant for every 6 minutes. The sample was taken from the drier and weighed. The procedure was repeated and readings are noted. Industrial Applications: Preparation of organic compounds They are used to dry heat sensitive materials In pharmaceutical industry Preparation of food materials.

Graph: Moisture content (X) Vs the rate of drying (N) Moisture content (X) Vs VN

Result: Drying characteristics of sample using tray drier is calculated: Time of falling rate period, Time of constant rate period, Total time for drying, Rate of drying Critical moisture content t F= t C= t= = =

Tabulation:
S.no Time (min) Weight Initial weight of sand= Moisture Content dx g of moisture/ g of solid (x) g of moisture/ g of dry solid (w) g of moisture/ g of dry solid g Evaporated/m s
2

dt (s)

dx/dt*10

-4

1/N m s/g
2

VAPOUR-LIQUID EQUILBRIUM
AIM: To determine the temperature (T), liquid composition (x) and vapor composition (y) at equilibrium and to draw the vapor-liquid equilibrium curve for the given system of liquids. PROCEDURE: 1. Preparing Calibration Chart: Mix known volumes of Water Ethanol (25:0), (20:5), (15:10), (10:15) and (5:20)ml. Determine the densities or refractive index mixtures by using specific gravity bottle or apply refractometer. Determine the density or RI of pure water and ethanol at room temperature. Convert the volume fraction into mole fraction of ethanol (more volatile component). A plot of density or RI (y-axis) Vs mole fraction of ethanol (x-axis) is the required calibration chart. If density or RI is known mole fraction can be easily obtained from the calibration chart.

2. Experimental Procedure:

Take 250ml of ethanol and 200ml of water in the RB flask and switch ON the heater and adjust for required temperature. Allow water to flow through the condenser. Once the reflux is obtained in the system, note the constant temperature. Switch OFF the heater and determine the density of the distillate and residue. Repeat the procedure for different composition of feed. Plot the equilibrium curve.

TABULATION I: Volume of Ethanol Volume of Water Weight of Ethanol Weight of Water Moles of Ethanol Moles of Water Mole fraction of Ethanol Specific Gravity

TABULATION II: Mixture I A:100ml Distillate y B:150ml Residue x Mixture II A:150ml Distillate y B:100ml Residue x Mixture-III A:50ml Distillate Y B:200ml Residue X

Weight of empty bottle

Weight of bottle + sample

Weight of sample

Volume of sample taken

Density

TABULATION III:

Volume of feed (ml) Ethanol A Water B

Temperature

Density gm/cc Distillate y Residue x

Mole fraction of A Distillate y Residue x

RESULT: The temperature of liquid composition and vapour composition at equilibrium stage was found. The vapour liquid equilibrium curve was drawn.

1. For 100ml ethanol and 150ml water Temperature = = =

Vapour composition (y) Liquid composition(x) 2. For 150ml ethanol and 100ml water Temperature Vapour composition Liquid composition 3. For 50ml ethanol and 200ml water Temperature Vapour composition

= = =

= =

Liquid composition

WETTED WALL COLUMN

Aim: To determine the mass transfer coefficient by the evaporation of liquid into steam in the wetted wall column. Apparatus required: Measuring flask Conical flask Toluene Benzene Stop watch

Formula: 1. NA = m/A x t Where, NA = Flux kg/m2s A = Cross sectional area in m2 t = Time taken for evaporation in s m = Mass of the sample evaporated 2. Cross sectional area = 3. 4. 5. 6. 7. 8. KG = NA x 2/(PA2 PA1) Total pressure = mgh NSH = 0.23(Nre)0.83(NSC) NRe = DV NSC = m/DAB NSH = kAPBmRT
2

(kg/m2s)

(m2)

Tabulation: S.no. 1. Data Sample taken from feed reservoir 2. 3. 4. Sample collected Sample evaporated Time taken Benzene

data Mol. Wt.

For benzene 78.14

For air 28.5

CT CV

562.1 k 259 m2/kg mol

132 k 86 m2/kg mol

Technical data: Density of air = 1.2 kg/m3 Length of column = 1.2 m Diameter of the column = 8.1 cm Viscosity of air = 1.90X10-5 kg/m2s Density of toluene = 862.27 kg/m3 Density of benzene at 85oC = 796.8 kg/m3 Procedure: Fill the reservoir with the measured quantity of volatile liquid. Switch on the blower. Control the rate of air entering Open the feed reservoir wall and note the time of liquid entering the wetted wall column. Liquid entering runs in a thin film inside the vertical column while air enters from the bottom. Measure the pressure difference. The inlet air will vaporize some quantity of liquid and removing liquid is collected in the measuring jar. Mass transfer co-efficient can be found from graph.

Result: Mass transfer co-efficient of benzene (experimental) Mass transfer co-efficient of benzene (theoretical) = = (kg/m2s) (kg/m2s)