Marwadi University Chemistry Lab Manual PDF

CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT LABORATORY MANUAL Course Code: 01CH1306 Course Name: Engineering Chemistry-II Prepared By: Dr. Swati Dubey Department of Chemical Engineering...

CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT LABORATORY MANUAL Course Code: 01CH1306 Course Name: Engineering Chemistry-II Prepared By: Dr. Swati Dubey Department of Chemical Engineering Marwadi University, Rajkot, Gujarat CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT INDEX Page Date Signature S. No. Title of Experiment Number Qualitative analysis of Primary and secondary alcohol. 1 2 Qualitative analysis of carboxylic acid group Qualitative analysis of halides 3 4 Determination of unsaturated aliphatic hydrocarbon Determination of aldehydes and ketones. 5 Qualitative analysis of phenol. 6 Analysis of oils. 7 8 Analysis of fats 9 Preparation of any dye 10 Separation of volatile liquid components by distillation Separation of two immiscible liquid by separating 11 funnel. 12 Determination of sulfur content in organic compound 13 Determination of nitrogen content in organic compound Determination of distribution coefficient of benzoic 14 acid between water and toluene. 1|Page  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT GENERAL SAFETY AWARENESS AND PRACTICES  Know all the safety rules and procedures that apply to your work. IF YOU DO NOT UNDERSTAND - ASK!  Determine the potential hazards, appropriate safety precautions and proper waste disposal techniques before beginning any new operation.  Know the location and proper use of emergency equipment (safety showers, eye baths, fire extinguisher, and first aid kits)  Be familiar with emergency procedures (exits, alarm stations, and evacuation routes)  Do not eat, drink, smoke or apply cosmetics in any laboratory.  Do not pipette or start siphons by mouth.  Wash hands with soap and water before leaving the work area. This applies even if one has been wearing gloves  Know what protective equipment is available and use the proper type for each experiment  Ensure that all chemicals are correctly and clearly labeled.  Use laboratory equipment only for its designated purpose.  Combine reagents in appropriate order. (i.e., pour water first and then acid; and avoid adding solids to hot liquids)  Wipe up spills immediately.  Keep sinks clean. Practice good housekeeping and clean up at the end lab work.  Keep aisles free of obstructions (chairs, stools, boxes, etc.). Apparatus set up should be as far back on bench as conveniently possible so it will not tip onto floor.  Do not set up apparatus so that it is necessary to reach through the assembly to turn water, gas, or electricity on or off. Assemble apparatus so that control valves and switches will remain accessible if a fire should occur.  Confine long hair and loose clothing or jewelry when in the laboratory  Avoid exposures to gases, vapors, and aerosols (USE FUME HOODS)  Do not leave experiments in process unattended. (If you must leave equipment running over night please post contact information near experiment)  Identify shut off switches and ensure they are easily accessible.  Children should not be allowed in the laboratory.  Avoid working alone at night.  Keep laboratories locked when unoccupied. (Leave doors unlocked while working in laboratory in case assistance is needed)  Do NOT wear protective gloves outside the lab area, to avoid contamination on door handles, water fountains, etc. If you are not already fully knowledgeable of the following, please learn about the following:  emergency telephone numbers  proper use of fire extinguishers  proper means of disposing of broken glassware  proper disposal of “sharps”  proper use of safety showers and eye-wash fountains 2|Page  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT  correct storage and handling or dispensing of flammable liquids  proper procedures for radiation monitoring and control, if applicable  proper procedures for chemical or biological spill clean-up and disposal  correct operation of fume hoods or biological safety cabinets, if applicable A departmental safety representative or the Director of Safety (see p. iv) can advise you on all health and safety practices, including those mentioned above. In the laboratory areas where you work, find and remember the location of:  telephones  exits, especially emergency exit routes should be planned in advance  fire extinguishers  fire alarm stations  safety showers  eye-wash stations  first-aid kit  designated building door for ambulance arrival 3|Page  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT Experiment 1 AIM : Qualitative analysis of Primary and secondary alcohol. THEORY: Alcohols are those organic compounds which are characterized by the presence of one, two or more hydroxyl groups (−OH) that are attached to the carbon atom in an alkyl group or hydrocarbon chain.Alcohols are classified as primary alcohols secondary alcohol and tertiary alcohol, as accordingly where the carbon atom of an alkyl group is attached to the hydroxyl group. Primary alcohol Primary alcohols are those alcohols where the carbon atom of the hydroxyl group(OH) is attached to only one single alkyl group. Eg : Methanol,ethanol,propanol Secondary alcohol Secondary alcohols are those where the carbon atom of the hydroxyl group is attached to two alkyl groups on the either sides. The two alkyl groups present may be either structurally identical or even different. Tertiary alcohol Tertiary alcohols are those which feature hydroxyl group attached to the carbon atom which is connected to 3- alkyl groups. The physical properties of these alcohols mainly depend on their structure. 4|Page  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT CHEMICALS REQUIRED  Potassium Permaganate  Glacial Acetic Acid  Alcohol GLASSWARES  Test tubes  Beakers  Petridish  Dropper PROCEDURE 1. To a large test tube, add about 2 mL of glacial acetic acid followed by 3 drops of unknown alcohol. 2. To the test tube, add dropwise, with the swirling to mix contents for each addition, a saturated solution of KMnO4. 3. Note if there is any change in color 4. Primary and secondary alcohol decolorizes purple permanganate color. OBSERVATION Solution 1: Solution 2: RESULTS 5|Page  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT CONCLUSION 6|Page  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT Experiment 2 AIM: Qualitative analysis of carboxylic acid group THEORY: Carboxylic acids are versatile organic compounds. It has excellent physical and chemical properties. The chemical structure of carboxylic acid contains a carbonyl functional group and hydroxyl group. It interact easily with polar compounds and contributes to many important chemical reactions. The carboxylic acids are the most important functional group that contains C=O. Carboxylic acids have a tendency to donate protons and act as acids. It is this property which is helpful in the identification of a -COOH group. When carboxylic acid reacts with sodium bicarbonate solution carbon dioxide is evolved with a brisk effervescence along with sodium acetate is formed. The chemical reaction is given below. RCOOH + NaHCO3 → RCOONa + H2O + CO2↑ (brisk effervescence) CHEMICALS REQUIRED  Sodium bicarbonate  Carboxylic acid compound GLASSWARES  Test tubes  Beakers  Petridish  Dropper  Spatula PROCEDURE 1. Prepare a saturated solution of sodium bicarbonate by dissolving sodium bicarbonate in 1ml of water. 2. Add the given organic compound to the saturated solution of sodium bicarbonate solution. 7|Page  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT 3. Shake the solution well. 4. If there is an evolution of brisk effervescence then it indicates the presence of carboxylic acid. OBSERVATION Evolution of brisk effervescence was observed RESULTS CONCLUSION 8|Page  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT Experiment 3 AIM: Qualitative analysis of halides. THEORY A halide (rarely halogenide) is a binary chemical compound, of which one part is a halogen atom and the other part is an element or radical that is less electronegative (or more electropositive) than the halogen, to make a fluoride, chloride, bromide, iodide, astatide, or theoretically tennesside compound. The alkali metals combine directly with halogens under appropriate conditions forming halides of the general formula, MX (X = F, Cl, Br or I). Many salts are halides; the hal- syllable in halide and halite reflects this correlation. All Group 1 metals form halides that are white solids at room temperature. A halide ion is a halogen atom bearing a negative charge. The halide anions are fluoride (F−), chloride (Cl−), bromide (Br−), iodide (I−) and astatide (At−).[clarification needed] Such ions are present in all ionic halide salts. Halide minerals contain halides. All these halides are colourless, high melting crystalline solids having high negative enthalpies of formation. Metal halides are used in high-intensity discharge lamps called metal halide lamps, such as those used in modern street lights. These are more energy-efficient than mercury-vapor lamps, and have much better colour rendition than orange high-pressure sodium lamps. Metal halide lamps are also commonly used in greenhouses or in rainy climates to supplement natural sunlight. Silver halides are used in photographic films and papers. When the film is developed, the silver halides which have been exposed to light are reduced to metallic silver, forming an image. Halides are also used in solder paste, commonly as a Cl or Br equivalent. Synthetic organic chemistry often incorporates halogens into organohalide compounds. CHEMICALS REQUIRED  Sodium chloride  Silver Nitrate  Nitric acid GLASSWARES 9|Page  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT  Test tubes  Beakers  Petridish  Dropper  Spatula PROCEDURE 1. Prepare a saturated solution of sodium chloride by dissolving sodium chloride in 10ml of water. 2. Put a diluted solution of nitric acid followed by addition of silver nitrate solution to it. 3. Salt solution acidified with dilute HNO3 on addition of silver nitrate solution gives a curdy white precipitate soluble in ammonium hydroxide solution. This indicates the presence of Cl – ions in the salt. OBSERVATION Color of the precipitate formed is RESULTS CONCLUSION 10 | P a g e  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT Experiment 4 AIM: Determination of unsaturated aliphatic hydrocarbon THEORY An aliphatic compound or aliphatic hydrocarbon is an organic compound containing hydrogen and carbon atoms that are usually linked together in chains via single, double or triple bonds. Sometimes the chains are also in branched trains or in the form of non-aromatic structures. Notably, apart from hydrogen some other elements like oxygen, nitrogen, chlorine, and sulphur may be bound to the carbon atoms in the chain. Aliphatic compounds may be saturated or unsaturated. Saturated hydrocarbon contains mainly alkanes which are open chain hydrocarbons containing a carbon-carbon single bond. Most of the time the bond exists in the form of a covalent bond. These compounds are inert in nature and do not readily react with acid, bases or other reagents. Hydrocarbon molecules with at least one double bond are called unsaturated meaning that more hydrogen atoms can be added to these molecules. Such molecules are much more reactive than saturated.. This is because the double bond is less than twice as strong as a single bond, making it easier to break one part of the double bond apart than it would be to break a single bond. CHEMICALS REQUIRED  Hydrogen Bromide or any bromine compound  Aliphatic unsaturated hydrocarbon GLASSWARES  Test tubes  Beakers  Petridish  Dropper  Spatula 11 | P a g e  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT PROCEDURE: 1. The organic compound to be tested is taken in a test tube. 2. Dissolve it in 2ml of distilled water. 3. Add bromine water drop wise with constant shaking. 4. If the orange red colour of bromine disappears then the given organic compound is unsaturated. When all the pi bonds are broken then the colour persists. 5. If the colour of bromine persists then the given organic compound is saturated OBSERVATION The final color of the solution is RESULTS CONCLUSION 12 | P a g e  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT Experiment 5 AIM : Determination of aldehydes and ketones. THEORY Aldehydes and ketones have a carbonyl group (C=O) as a functional group. A ketone has two alkyl or aryl groups attached to the carbonyl carbon (RCOR’). The simplest ketone is acetone, which has two methyl groups attached to the carbonyl carbon (CH3COCH3). An aldehyde is similar to a ketone, except that instead of two side groups connected to the carbonyl carbon, they have at least one hydrogen (RCOH). The simplest aldehyde is formaldehyde (HCOH), as it has two hydrogens connected to the carbonyl group. All other aldehydes have one hydrogen bonded to the carbonyl group, like the simple molecule acetaldehyde, which has one hydrogen and one methyl group (HCOCH3). The carbonyl carbon in both aldehydes and ketones is electrophilic, meaning that it has a dipole due to the electronegativity of the attached oxygen atom. This makes the carbonyl carbon an ideal target for nucleophiles in a nucleophilic addition reaction. During this reaction, the nucleophile, or electron donor, attacks the carbonyl to form the tetrahedral intermediate. The negatively charged oxygen accepts a hydrogen ion to form a hydroxyl group. CHEMICALS REQUIRED  Sodium bisulphite  Formaldehyde GLASSWARES  Test tubes  Beakers  Petridish  Dropper  Spatula 13 | P a g e  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT PROCEDURE 1. Take a saturated solution of sodium bisulphite in a clean test tube. 2. Add 1ml of the given organic compound to be tested. 3. Shake well and leave it for 15-20 minutes. 4. If there is a formation of white precipitate, then the presence of the carbonyl group is confirmed. Aldehydes and ketones combine with sodium bisulphite to for well-crystallized water-soluble products known as “aldehyde bisulphite” and “ketone bisulphite”. The chemical reaction is given below. OBSERVATION RESULTS CONCLUSION 14 | P a g e  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT Experiment 6 AIM: Qualitative analysis of phenol THEORY Phenol is a hydroxyl group (-OH) on an aromatic ring or simply the hydroxy derivatives of aromatic compounds are known as phenols. Phenols are weaker acids than carboxylic acids. It undergoes substitution reaction easily. Phenol is one of the most versatile and important industrial organic chemicals. Phenols are similar to alcohols but form stronger hydrogen bonds. Thus, they are more soluble in water than are alcohols and have higher boiling points. Phenols occur either as colourless liquids or white solids at room temperature and may be highly toxic and caustic. CHEMICALS REQUIRED  Phenol  Iron Chloride GLASSWARES  Test tubes  Beakers  Petridish  Dropper  Spatula PROCEDURE Aqueous solution of phenol reacts with freshly prepared ferric chloride solution gives coloured complex. Most phenols give dark coloured solutions. The chemical reaction is given below. 1. Dissolve the given organic compounds in water. 2. Add a neutral solution of ferric chloride slowly dropwise. 15 | P a g e  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT 3. Observe the change in colour. A red, blue, green or purple colouration indicates the presence of phenol. OBSERVATION The color of the resulting solution is RESULTS CONCLUSION 16 | P a g e  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT Experiment 7 AIM: Analysis of oils THEORY An oil is any nonpolar chemical substance that is composed primarily of hydrocarbons and is hydrophobic (does not mix with water) & lipophilic (mixes with other oils). Oils are usually flammable and surface active. Most oils are unsaturated lipids that are liquid at room temperature. The general definition of oil includes classes of chemical compounds that may be otherwise unrelated in structure, properties, and uses. Oils may be animal, vegetable, or petrochemical in origin, and may be volatile or non-volatile. They are used for food (e.g., olive oil), fuel (e.g., heating oil), medical purposes (e.g., mineral oil), lubrication (e.g. motor oil), and the manufacture of many types of paints, plastics, and other materials. Specially prepared oils are used in some religious ceremonies and rituals as purifying agents. Organic oils are produced in remarkable diversity by plants, animals, and other organisms through natural metabolic processes. Lipid is the scientific term for the fatty acids, steroids and similar chemicals often found in the oils produced by living things, while oil refers to an overall mixture of chemicals. Organic oils may also contain chemicals other than lipids, including proteins, waxes (class of compounds with oil-like properties that are solid at common temperatures) and alkaloids. Lipids can be classified by the way that they are made by an organism, their chemical structure and their limited solubility in water compared to oils. They have a high carbon and hydrogen content and are considerably lacking in oxygen compared to other organic compounds and minerals; they tend to be relatively nonpolar molecules, but may include both polar and nonpolar regions as in the case of phospholipids and steroids. CHEMICALS REQUIRED  Potassium bisulfate  Oil sample GLASSWARES  Test tubes 17 | P a g e  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT  Beakers  Petridish  Dropper  Spatula  Burner PROCEDURE 1. Take the sample to be tested in a test tube. 2. Add few crystals of potassium bisulfate to it. 3. Heat the mixture and observe the change in odour. 4. If there is pungent irritating odour then the presence of fate or oil is confirmed. Fats and oils when heated with some crystals of potassium bisulfite KHSO 4 in a test tube. A pungent irritating odour or smell of acrolein confirms the presence of fat or oil. The chemical reaction is given below. OBSERVATION Type of odor RESULTS CONCLUSION 18 | P a g e  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT Experiment 8 AIM : Analysis of fats THEORY Fat usually means any ester of fatty acids, or a mixture of such compounds, most commonly those that occur in living beings or in food. They are solid at room temperature. There are two types of fats that are solid at room temperature. They are saturated fats and trans fats. Saturated fat is also known as solid fat. Saturated fat in fish and poultry is less when compared to animal fat or red meat. This fat can increase your cholesterol levels. Tropical oils such as cocoa butter, coconut oil, and palm oil also have saturated fats. It is mostly found in non-dairy products and snacks in large quantities. Cakes, butter, and cookies are some examples of food containing maximum saturated fats. A fat is changed to increase its shelf life. The process to make this change happen is called hydrogenation. This fat is harder at room temperature. The importance of trans fat is that it makes flakier pie crusts and crispier crankers. It is found in cookies, chips, processed food etc. CHEMICALS REQUIRED  Potassium bisulfate  Fat sample GLASSWARES  Test tubes  Beakers  Petridish  Dropper  Spatula  Burner PROCEDURE 1. Take the sample to be tested in a test tube. 2. Add few crystals of potassium bisulfate to it. 3. Heat the mixture and observe the change in odour. 19 | P a g e  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT 4. If there is pungent irritating odour then the presence of fate or oil is confirmed. Fats and oils when heated with some crystals of potassium bisulfite KHSO4 in a test tube. A pungent irritating odour or smell of acrolein confirms the presence of fat or oil. The chemical reaction is given below. OBSERVATION RESULTS CONCLUSION 20 | P a g e  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT Experiment 9 AIM : Preparation of any dye. THEORY: A dye is a colored organic compound that is used to impart color to an object or a fabric. Azo dyes, colored compounds containing the -N=N- group, are the largest and more important class of dyes. In azo-dyeing, the fabric is first impregnated with an aromatic compound activated toward electrophilic substitution, then is treated with a diazonium salt to form the dye. Azo compounds are prepared by the reaction of diazonium salts with phenol under alkaline conditions. Primary aromatic amines react with nitrous acid at 0 oC to give a diazonium salt. Nitrous acid is in turn formed by the reaction of sodium nitrite with hydrochloric acid. The active reagent is nitrous anhydride or dinitrogen trioxide. Nitrous anhydride reacts with aniline to give a nitroamine derivative which is unstable and isomerizes to form a diacetic acid which in turn is converted to a diazonium salt. Finally, this diazonium salt reacts with 2-naphthol in the presence of sodium hydroxide to give 2-naphthol aniline which is an aniline dye. 2- Naphthol aniline dye is a scarlet dye that can be prepared by coupling reaction. Aniline reacts with sodium nitrite in the presence of hydrochloric acid to form benzene diazonium chloride. Further benzene diazonium chloride reacts with 2-naphthol forms a bright orange colour 2-naphthol and forms aniline dye. 21 | P a g e  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT CHEMICALS REQUIRED  Aniline  Sodium nitrite  Hydrochloric acid  2-Naphthol  Sodium hydroxide solution GLASSWARES  Test tubes  Beakers  Petridish  Dropper  Spatula PROCEDURE 1. Dissolve 5 ml of aniline in a mixture of concentrated hydrochloric acid and water. 2. Cool the solution in an ice bath between 0-5 oC. 3. Add a solution of 4 gm sodium nitrite in 15 ml of water dropwise with continuous shaking. 4. Take another flask to dissolve 8 gm of 2-naphthol in a solution of 5 gm sodium hydroxide solution in 50ml of water. 5. Cool the solution in the ice bath to 0-5oC. 6. Now mix the two cold solutions slowly dropwise with constant stirring. 7. Continue the stirring for at least half an hour without allowing the temperature to rise above 10oC. 8. An orange colour azo dye called 2-naphthol aniline separates out. 9. Filter the crude sample and wash it with cold water. 10. Dry and recrystallise it from ethyl alcohol or glacial acetic acid. OBSERVATION Color of the crystals = Weight of the crystals = RESULTS CONCLUSION 22 | P a g e  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT Experiment 10 AIM: Separation of volatile liquid components by distillation THEORY: Distillation is a unit operation in which the constituents of a liquid mixture are separated using thermal energy. Basically the difference in vapour pressure of different constituents at the same temperature is responsible for the separation. Distillation is used in chemical and petroleum industries as a means of separating the liquid mixture into its component parts. Theoretical Background: Distillation is a unit operation in which the constituents of a liquid mixture are separated using thermal energy. With this technique it is possible to separate the liquid mixture into its components in almost pure form and due to this, distillation is the most important of all the mass transfer operations. In distillation, the phases involved are liquid and vapour and mass is transferred from both the phases to one another by vaporization from the liquid phase and by condensation from the vapour phase. The net effect is an increase in composition of the more volatile component in the vapour and that of the less volatile component in the liquid. The basic requirement for the separation of components by distillation is that the composition of the vapour be different from the composition of the liquid with which it is in equilibrium. The vapour is always richer in more volatile component than the liquid from which it is formed. If the vapour composition is the same as the liquid composition, distillation technique will not affect a separation. 23 | P a g e  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT PROCEDURE: 1. Plot the graph between density of mixture and volume % of methanol 2. Take a known volume of methanol-water mixture in reboiler (1000 ml for a reboiler capacity of 3000 ml), find out its density using specific gravity bottle and note down the value. 3. Allow cooling water to pass through the condenser. Do not start the heater before starting the cooling water circulation. 4. Start heating and carry out distillation till sufficient distillate (about 100 ml) is collected in the receiver. 5. Stop heating, wait till all the distillate get collected in the receiver 6. Now stop cooling water supply. 7. Collect distillate, measure its volume and density OBSERVATION: Volume of methanol = …….. ml Volume of water =……..ml Volume of feed = ……… ml Volume of distillate = ………. ml Volume of residue =………ml RESULTS CONCLUSION 24 | P a g e  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT Experiment 11 AIM: Separation of two immiscible liquid by separating funnel THEORY: Two immiscible liquids are separated by using separating funnel. The mixture of oil and water forms two separate layer because they are completely insoluble in each other oil forms upper layer while water forms lower.in separating funnel they are kept for resting , when two layers become stable by using separating funnel they are filtered one by one. A separating funnel is funnel that is used to separate immiscible liquids. Liquids that do not mix with each other are said to be immiscible. Two immiscible liquids, such as oil and water, can be separated by using a separating funnel. CHEMICALS REQUIRED  Oil  Water GLASSWARES  Separating funnel  Stand PROCEDURE 1. The immiscible liquid, oil and water are taken in a separating funnel. 2. The immiscible liquid forms two clear layers. 3. The lighter liquid that is oil forms the upper layer and the heavier liquid that is water forms the lower layer. 4. When the stopper of the funnel is opened gradually the water comes out first and is collected in a beaker. 5. When the lower layer is shipped completely, the stopper of the funnel is closed. 6. The lighter liquid is left in the separating funnel. OBSERVATION Density of water = Density of oil = Volume of water after separation = 25 | P a g e  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT Volume of oil after separation = RESULTS CONCLUSION 26 | P a g e  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT Experiment 12 AIM : Determination of sulfur content in organic compound THEORY: Organosulfur compounds can be classified according to the sulfur-containing functional groups, which are listed (approximately) in decreasing order of their occurrence. Nature abounds with organosulfur compounds—sulfur is vital for life. Of the 20 common amino acids, two (cysteine and methionine) are organosulfur compounds, and the antibiotics penicillin and sulfa drugs both contain sulfur. While sulfur-containing antibiotics save many lives, sulfur mustard is a deadly chemical warfare agent. Fossil fuels, coal, petroleum, and natural gas, which are derived from ancient organisms, necessarily contain organosulfur compounds, the removal of which is a major focus of oil refineries. Sulfur shares the chalcogen group with oxygen, selenium, and tellurium, and it is expected that organosulfur compounds have similarities with carbon–oxygen, carbon–selenium, and carbon– tellurium compounds. A classical chemical test for the detection of sulfur compounds is the Carius halogen method. CHEMICALS REQUIRED  Nitric Acid  Barium Chloride GLASSWARES  Test tubes  Beakers  Petridish  Dropper  Spatula  Burner  Stand PROCEDURE 1. A known mass of the compound is heated with conc. HNO3 in the presence of BaCl2 solution 27 | P a g e  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT in the Carius tube. Sulphur is oxidised to H2SO4 and precipitated as BaSO4. 2. It is then dried and weighed. 3. Percentage of S = ((Atomic mass of S)/(Molecular mass of BaSO4)) x (( Mass of BaSO4) / (Mass of the compound)) x 100 OBSERVATION 1. Mass of organic compound = g 2. Mass of barium sulphate formed = g RESULTS CONCLUSION 28 | P a g e  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT Experiment 13 AIM: Determination of nitrogen content in organic compound THEORY Organic compounds containing nitrogen, sometimes known as amines, are created by substituting an alkyl or aryl group for one or more hydrogen atoms in ammonia. They can be found in nature in a variety of forms, including proteins, vitamins, hormones, and so on. These amines are vital for our bodies in the form of amino acids. The IUPAC system dictates that amines are named by first identifying the alkyl group and then adding amine at the end, such as methylamine. 2-Bromoaniline is an example of an aromatic amine called after the derivative of the simplest aromatic amine, aniline. In drug production, aliphatic amines are utilized as intermediates. Aromatic amines, such as aniline and its derivatives, are used to make colours, pharmaceuticals, and photographic developers. All hair dyes contain 1,4-diaminobenzene as the major component. Herbicides made from dithiocarbonates, which are chemicals produced from primary amines, are widely used. PROCEDURE 1. Solutions Required  0.32% KMnO4 : Weigh 3.2 g KMnO4 and dissolve in 1 L of water.  2.5% NaOH : Weigh 2.5 g of NaOH pellets and dissolve in 100 ml  0.02 M NaOH: 0.16 g in 200mL  0.01 M H2SO4  0.15% methyl red indicator 2. Set up the distillation apparatus with the help of your counsellor. 3. Weigh 20 g of given sample and transfer it carefully into Kjeldahl distillation flask. 3. Moisten the sample with about 10 mL of distilled water. Wash down the soil adhering to the neck of the flask. 4. Add 100 mL of 0.32% KMnO4 solution and 100 mL of 2.5% NaOH solution and a few glass beads or broken pieces of glass rod to avoid bumping to the above sample and immediately stopper the flask. 29 | P a g e  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT 5. Take 25 mL of 0.01 M H2SO4 in a 150 mL conical flask and add 3-4 drops of methyl red to it. Dip the end of the delivery tube of the distillation apparatus into it. 6. Heat the distillation flask steadily to distill 100 mL of liquid ammonia in about 30 minutes time. 7. Titrate the excess of standard H2SO4 left in the conical flask with 0.02 M NaOH and note the volume used (X mL ) in the observation table. OBSERVATION Volume of nitrogen collected = RESULTS CONCLUSION 30 | P a g e  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT Experiment 14 AIM : Determination of distribution coefficient of benzoic acid between water and toluene. THEORY When a solute distributes itself in two immiscible sol vents than at equilibrium the ratio of the concentration of the solute remains constant at a particular temperature. This is known as Nernst distribution law. This law is valid when the solute remains in same molecular state in both the solvents. CHEMICALS REQUIRED  Benzoic acid in benzene  Benzene  NaOH  Distilled water  Phenolphthalein indicator GLASSWARE:  Separating funnel: 250 ml  Conical flask  Pipette  Burette  Stoppered bottles PROCEDURE 1. Prepare the following mixtures in separating funnels Set I: 25ml water + 25 ml of saturated solution of benzoic acid in toluene Set II: 25 ml water + 20 ml saturated solution of benzoic acid in toluene + 5 ml toluene Set III: 25ml water + 15 ml saturated solution of benzoic acid in toluene + 10 ml toluene 2. Shake the mixture in the separating funnel vigorously for about 30 minutes so that the benzoic acid gets distributed between the two solvents and the distribution equilibrium is 31 | P a g e  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT reached. 3. Allow the flasks to stand for 10 minutes to separate into two clear layers (remove the stopper of the separating funnel and keep its mouth open during this period to facilitate the separation). 4. Drain off the lower aqueous layers in 3 different stoppered dry bottles. (Discard the intermediate layer between the two phases). 5. Toluene layer remains in the separating funnels. 6. Using a dry pipette take 5 ml of organic layer (toluene) into a conical flask containing 10ml of water and titrate against 0.1 N NaOH using phenolphthalein as an indicator. End point: Colorless to pink.Pipette out 10 ml of the aqueous layer using a dry pipette and titrate it against 0.01 N NaOHsolution using phenolphthalein as an indicator. End point will be colorless to pink OBSERVATION Where; Vorg= Volume in ml of 0.1N Sodium hydroxide per 5ml of organic layer Vaq= Volume in ml of 0.01N Sodium hydroxide per 10ml of aqueous layer 32 | P a g e  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT Norg= Normality of organic layer Naq= Normality of aqueous layer Corg= Concentration of organic layer in g mole/lit = Normality (Norg) Caq= Concentration of aqueous layer in g mole/lit = Normality (Naq) K= Caq/Corg½= Partition coefficient of benzoic acid in water and benzene CALCULATIONS For Organic layer Set I Normality of Sodium hydroxide (N1= 0.1N) Volume of organic layer pipetted (V2) = 5ml N1V1 (Sodium hydroxide) = N2V2 (Organic layer) For Set II For Set III For aqueous layer Normality of Sodium hydroxide (N1= 0.01N) Volume of organic layer pipetted (V2) = 10 ml N1V1 (Sodium hydroxide) = N2V2 (Aqueous layer) For Set II For Set III 33 | P a g e  CHEMICAL ENGINEERING DEPARTMENT MARWADI UNIVERSITY GAURIDAD CAMPUS, RAJKOT Plot the graph of log CaqVs log Corg Slope = 1/n Intercept = logK K= RESULTS CONCLUSION 34 | P a g e