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Organic Pharmacy Sessional -Pharm-1004 Exp-1: Determination of Sulphur by Sodium fusion method. Exp-2: Determination of Nitrogen by Sodium fusion method. Exp-3: Determination of Chloride by fusion Extracts method. Exp-4: Determination of Bromide by fusion Extracts method. Exp-5: Determination of Iodide by fusion Extracts method. Exp-6: Solubility test of Class S1 compound. Exp-7: Solubility test of Class S2 compound. Exp-8: Solubility test of Division A1 compound. Exp-9: Solubility test of Division A2 compound. Exp-10: Solubility test of Division B compound. Exp-11: Solubility test of Division N1 & N2compound Exp-12: Determination of Functional group –Alcohol Exp-13: Determination of Functional group –Hydrocarbon Exp-14: Determination of Functional group –Amine Southeast University Department of Pharmacy Exp: 1 Course code: Pharm 1004 Course Title: Prnanic Pharmacy I (Sessional) Name of the Exp: Determination of Sulphar by Sodium fusion method. Procedure: Sodium Fusion Method: Add dry piece of metallic sodium to the test tube, shake the bottom of the tube slightly and gradually apply heat to the bottom of the tube until the sodium has melted. Being careful not to heat the side of the tube with the sample, drop a few mg of the substance being tested directly onto the melted sodium. Heat the bottom of the tube until the glass is red hot, and continues heating for 2 minutes. Allow the tube for stand, add 5 drops of methanol. If the residue is a globular mass, break it up with a clean glass rod. If gas bubbles are produced wait until the reaction is completed, then add 3.0 ml of distilled water. Boil the mixture and filter it. If at this points the solution is dark colored so as to obscure further tests it is probable that the amount of sample was too large or that the fused mass was too large or that the fused was not heated to a sufficient high temperature. The fusion procedure should be repeated .The selection obtained by the above procedure is to be used in the test for N, X, S and other elements. Detection of Sulfur: a) Lead acetate test: About 0.2ml of the alkaline filtrate or centrifuged from the sodium fusion is place in a 3 inch test tube.1 drop of lead acetate solution is added followed by dilute acetic acid until the solution is acidic. A brown to black precipitate or coloration indicates the formation of lead sulphide. b) Sodium Nitropruside Test: Place 0.2 ml of filtrate from sodium fusion in a 3 inch test tube and add 1.0 drop of a 0.1% solution of sodium nitropruside. A deep red or purple color indicates the presence of the sulphide ion. Southeast University Department of Pharmacy Exp: 2 Course code: Pharm 1004 Course Title: Prnanic Pharmacy I (Sessional) Name of the Exp: Determination of Nitrogen by Sodium fusion method. Procedure: Sodium Fusion Method: Add dry piece of metallic sodium to the test tube, shake the bottom of the tube slightly and gradually apply heat to the bottom of the tube until the sodium has melted. Being careful not to heat the side of the tube with the sample, drop a few mg of the substance being tested directly onto the melted sodium. Heat the bottom of the tube until the glass is red hot, and continues heating for 2 minutes. Allow the tube for stand, add 5 drops of methanol. If the residue is a globular mass, break it up with a clean glass rod. If gas bubbles are produced wait until the reaction is completed, then add 3.0 ml of distilled water. Boil the mixture and filter it. If at this points the solution is dark colored so as to obscure further tests it is probable that the amount of sample was too large or that the fused mass was too large or that the fused was not heated to a sufficient high temperature. The fusion procedure should be repeated .The selection obtained by the above procedure is to be used in the test for N, X, S and other elements. Detection of Nitrogen: a) Prussian blue test: About 0.8ml of the sodium fusion filtrate in a 4 inch test tube and add 1.0 drop of 3% potassium fluride, 1.0 drop of 10% NaOH and 15.20 mg of a ferrous sulphate crystals of ferrous ammonium sulphate crystals. Boil the mixture gently for 1.0 min. If a bluish ppt does not exist at this point, add 2 drops more of the 10 % NaOH solution and reboil the mixture .Add a small drop of 1% ferric chloride and again bring the mixture to boiling. Add dilute sulfuric acid ( dropwise and shaking ) until the oxides of the iron have just dissolved. Allow the tube to stand for 2 to 5 mins. A blue color or blue ppt is a positive test for nitrogen A green or greenish – blue coloration indicates a weak test for nitrogen [ perhaps due to poor fusion]. The addition of a drop of dilute phosphoric acid to such a greenish mixture will, usually because the blue color to show up, since the yellow color is due to ferric chloride and ferric ions are largely removed by the phosphoric acid. A yellow colored solution after acidification by the sulphuric acid indicates a negative test for nitrogen. Southeast University Department of Pharmacy Course code: Pharm-1004 Exp. No. – 03& 04 Name of the Exp: Determination of Iodine & Chlorine by fusion Extracts method. Procedure: Sodium Fusion Method: Add dry piece of metallic sodium to the test tube, shake the bottom of the tube slightly and gradually apply heat to the bottom of the tube until the sodium has melted. Being careful not to heat the side of the tube with the sample, drop a few mg of the substance being tested directly onto the melted sodium. Heat the bottom of the tube until the glass is red hot, and continues heating for 2 minutes. Allow the tube for stand, add 5 drops of methanol. If the residue is a globular mass, break it up with a clean glass rod. If gas bubbles are produced wait until the reaction is completed, then add 3.0 ml of distilled water. Boil the mixture and filter it. If at this points the solution is dark colored so as to obscure further tests it is probable that the amount of sample was too large or that the fused mass was too large or that the fused was not heated to a sufficient high temperature. The fusion procedure should be repeated .The selection obtained by the above procedure is to be used in the test for N, X, S and other elements. Detection of Iodine: 1. 0.5ml of sodium fusion filtrate into a 4.0 inch test tube. Add 0.5 ml of carbon tetrachloride (CCl4) and 3.0 drops of concentrated nitric acid (HNO3). Shake the tube and allow the liquid to stratify. The presence of Iodine is indicated by a Violet color in the carbon tetrachloride layer. 2. Iodine is present, remove the carbon tetrachloride layer by a pipette and add 0.5 ml of carbon tetrachloride to the same original test solution. Add 1.0 drop of concentrated nitric acid, shake the mixture and allow it to stratify. If the violet color is still shows, remove the lower layer by means of pipette and without adding more nitric acid repeat the extraction of iodine by CCl4 until the lower layer remains essentially colorless. Now add 2.0 ml of concentrated HNO3 to mixture being tested. Shake the solution and allow to stratify. The presence of bromine is indicated by a Tan or Tan-Red color in the CCl4. Layer. Repeat the extraction of the bromine, if present until the lower layer becomes colorless. Add 3.0 drops of silver nitrate to the aqueous layer. The immediate formation of a white precipitate indicates Chlorine. Southeast University Banani Dhaka Course code: Pharm-1004 Exp. No. - 05 Exp-5: Determination of Bromine by fusion Extracts method. Procedure: Sodium Fusion Method: Add dry piece of metallic sodium to the test tube, shake the bottom of the tube slightly and gradually apply heat to the bottom of the tube until the sodium has melted. Being careful not to heat the side of the tube with the sample, drop a few mg of the substance being tested directly onto the melted sodium. Heat the bottom of the tube until the glass is red hot, and continues heating for 2 minutes. Allow the tube for stand, add 5 drops of methanol. If the residue is a globular mass, break it up with a clean glass rod. If gas bubbles are produced wait until the reaction is completed, then add 3.0 ml of distilled water. Boil the mixture and filter it. If at this points the solution is dark colored so as to obscure further tests it is probable that the amount of sample was too large or that the fused mass was too large or that the fused was not heated to a sufficient high temperature. The fusion procedure should be repeated .The selection obtained by the above procedure is to be used in the test for N, X, S and other elements. Detection of Bromine: About 0.2 ml of the filtrate is placed in a microtube with 1.0 to 2.0 drops of chloroform and 1.0 drop of dilute sulphuric acid. A drop of freshly prepared Chlorine solution or 2.0 to 3.0 drops of 3% hydrogen peroxide are added and the mixture is shaken. The chloroform layer becomes almost colorless if the halogen is a Chloride. Brown or Tan if it is Bromine and Violet if it is Iodine Southeast University Banani Dhaka Course code: Pharm-1004 Exp. No. – 06 & 07 Exp-6 & 7: Solubility test of Class S1 and S2 compound. A compound is considered soluble in a solvent if 30mg of it dissolve in 1.0ml of the solvent at room temperature. The solvents to be used or the solubility classifications are in the order in which they should be used, water, ether, 5% NaOH solution, 5%NaHCO3, concentrated H2SO4 and 85% H3PO4. All solubilities are to be determined at room temperature. It is permissible to warm the mixture slightly during the test but the mixture should be cooled before a decision is reached as to its solubility. If the compound is soluble in water its solubility may be tested in ether, But in no other solvent. If it is soluble then it will be Class S1 compound. Observation: Division S1: Only C, H, O present: Monofunctional alcohols, Carboxylic acids, aldehydes, Ketones and esters with five carbon or fewer. Nitrogen Present: Monofunctional amides and amines with five carbons or fewer. Halogen present: Halogen substituted C, H, O compounds. Division S2: Only C, H, O present:Dibasic and polybasic acids, hydroxyl acids, Polyhydroxy alcohols, Polyhydroxy phenols, carbohydrates. Nitrogen present: Amines, salts of organic acids, ammonium salts. Halogen present: Haloacids. Southeast University Banani Dhaka Course code: Pharm-1004 Exp. No. – 08 Exp-8: Solubility test of Class A1 compound. A compound is considered soluble in a solvent if 30mg of it dissolve in 1.0ml of the solvent at room temperature. The solvents to be used or the solubility classifications are in the order in which they should be used, water, ether, 5% NaOH solution, 5%NaHCO3, concentrated H2SO4 and 85% H3PO4. All solubilities are to be determined at room temperature. It is permissible to warm the mixture slightly during the test but the mixture should be cooled before a decision is reached as to its solubility. If the compound is soluble in water its solubility may be tested in ether, But in no other solvent. If the compound is not soluble in water, it needs not to be tested with ether. Water insoluble compounds that are soluble in sodium hydroxide should also test with sodium bicarbonate to distinguish between relatively strong acids and weakly acidic compounds. If an obvious chemical reaction occurs in any solvent, the compound may be considered as soluble in that in that solvent. Observation: Division A1: Only C, H, O present: Strong acids with more than six carbons, anhydrates, phenols with electron withdrawing groups in the ortho- and para positions and β –diketones. Nitrogen present: Amino acids, nitro acids Halogen present: Haloacids and halides Sulphur present : Sulphonic acids Sulphur and halogen present: Sulphonyl halides Southeast University Banani Dhaka Course code: Pharm-1004 Exp. No. –09 Exp-9: Solubility test of Class A2 compound. A compound is considered soluble in a solvent if 30mg of it dissolve in 1.0ml of the solvent at room temperature. The solvents to be used or the solubility classifications are in the order in which they should be used, water, ether, 5% NaOH solution, 5%NaHCO3, concentrated H2SO4 and 85% H3PO4. All solubilities are to be determined at room temperature. It is permissible to warm the mixture slightly during the test but the mixture should be cooled before a decision is reached as to its solubility. If the compound is soluble in water its solubility may be tested in ether, But in no other solvent. If the compound is not soluble in water, it needs not to be tested with ether. Water insoluble compounds that are soluble in sodium hydroxide should also test with sodium bicarbonate to distinguish between relatively strong acids and weakly acidic compounds. If an obvious chemical reaction occurs in any solvent, the compound may be considered as soluble in that in that solvent. A few of the amine hydrochlorides are slightly soluble in 5 % HCl; hence in the these cases the original amine will react when it is first added in the aqueous acid to form the amine hydrochloride and will then precipitate as that salt to determine whether the insoluble material is the original amine or a salt that has been formed, a mixed melting point determination should be made, using the washed and dried solid from the acid solution with some of the original sample. Observation: Division A2: Only C, H, O present: Weak organic acids : Phenols. Enols and anhydrites Nitrogen present: Amino acids, nitroacids Halogen present: Halophenols Southeast University Banani Dhaka Course code: Pharm-1004 Exp-10: Solubility test of Division B compound. Exp. No. – 10 Exp-11: Solubility test of Division N1 & N2compound Exp-12: Determination of Functional group –Alcohol Exp-13: Determination of Functional group –Hydrocarbon Exp-14: Determination of Functional group –Amine