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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