Lab Manual

Inorganic and organic chemistry

Name: Sajjad razzaq Registration No. 2019-CH-409
Group 2 Class Instructors: Dr.Sajjad Ahmad
Index/Marks Sheet
Sr. Date Week Content List / Name of Experiment Pg. Grade Signature
# # #
01 6-10- 1. Safety Symbols Obtained Marks/
2020 Total
01 6-10- 1. MSDS/Health Hazard Codes
2020
02 13-10- 2 How to do the preliminary examination for unknown
2020 organic compound.
03 20-10- 3. Detection of Nitrogen, Sulphur and Halogen by using
2020 Lassaigne test.(as per standard format)
04 27-10- 4. How to do solubility test for the give unknown organic
2020 compound.
Lab Assignment
5 Determination of various functional groups in given
unknown organic compound
6 Determination of Aldehydes and ketone functional
groups.
7 Determination of Benzophenone/succinic acid/Benzoic
acid/sucrose
8 Detection of starch /Glucose /fructose.
Viva ,copy etc.
9 Detection of urea/ a-Naphthol/B-Naphthol
10 Detection Thiourea /catechol/Diphenyl amine
11 Detection of salicylic acid/Benz aldehyde
12 Preparation of Ethyl Benzoate or nitrobenzene and
determination of its %age yield.
Quiz
13 Open end lab performance (idea, principle,
performance, result &conclusion)
Final Manual Checking
Viva 2
Total 100
Grade/Marks Average:

Teacher Signature:

Teacher Name: Dr.Sajjad Ahmad

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Experiment No # 2
How to do the preliminary examination of unknown
organic compound.
Preliminary examination includes:

o Physical state
o Color
o Odour
o Ignition
o Physical constant

2.1 Physical state:

The compound may be solid or liquid; the former is somewhat easier to handle than
the latter. A solid sometimes becomes wet on keeping due to its hygroscopic character.

2.2 Color:
The color of a compound is due to the presence of chromophoric groups such as nitro,
amino, azo, nitroso, quinonoid etc. When such groups are introduced into a molecule
absorption maxima are shifted towards the visible region and the substance appears coloured.

Color of the compound Possible class of the compound

Pale yellow and deep yellow Nitro compounds, iodoform, picric acid, nitro
phenol, benzyl, Quinone’s.
Greenish Anthrancene.
Greenish Nitrobenzaldehyde.
Red 1, 2-Naphthoquinone.
Orange O-Nitro aniline, phenols azo compounds.
White/colorless Hydrocarbons, alcohols, Ketones, aldehydes,
acids, ethers.

2.3 Odour:
A large number of organic compounds possess characteristic Odour and with
experience this property can be of great assistance in identification.

Smell of the compound Possible class of the compound

Pleasant fruity Ester
Sweet and pleasant Ether, aromatic hydrocarbon, benzene.
Pungent Lower aliphatic acid, pyridine, acid halides.
Bitter almond Aromatic aldehydes, benzonitrile,
nitrobenzene
Phecolic Phenols, Naphthol, some derivatives of

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 salicylic acid
Fishy Amines

2.4 Ignition:
A small quantity of the given compound is heated on a crucible lid or on the tip of a
spatula until it burns, and its behavior on combustion is observed as.

Flame on burning of the compound Possible class of the compound

Smoky Aromatic or aliphatic compounds having
more than four carbon atoms.
Non-smoky Aliphatic compounds containing low
percentage of carbon.
Violet vapors Iodoform.
No flame Poly halogenated compounds
Acid vapors Phenols
Irritating Odour Carboxylic acids
Alkaline vapors Urea, amides etc.
Swelling, burnt sugar Odour along with Carbohydrates, citrates, tartrates and lactates.
charring
Residue after ignition Compounds containing metals such as the
salts of carboxylic sulphunic acids etc.

2.5 Physical constant:

Physical constants such as melting point, boiling point etc, of the unknown organic
compounds is very important to establish their identity. Both these constants are said to be the
criterion of purity of the substance.

2.5.1 Melting point:

The temperature at which the liquid and solid phases co-exist in equilibrium without
change in temperature is defined as melting point.

2.5.2 Boiling point:

Boiling point of a liquid may be defined as the temperature at which the vapors
pressure of a liquid becomes equal to the external pressure

2.6 conclusion
We can easily detect some organic compounds by using our knowledge about the physical
state, color, Odour, type of ignition and melting &boiling points of different organic
compounds.

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 Dated: 24/09/19

Experiment No. 3

Detection of elements (Nitrogen, Sulphur & halogens)

by using Lassaigne test or sodium fusion test.
3.1 Objective:
To detect the presence of nitrogen, Sulphur and halogens in organic
compounds.

3.2 Principle:
In doing so, Na converts all the elements present into ionic form.

o Na + C + N → NaCN
o 2Na + S → Na2S
o Na + X → NaX ( X= Cl, Br, or I)
The formed ionic salts are extracted from the fused mass by boiling it with
distilled water. This is called sodium fusion extract.

3.3 Apparatus:
Test tubes, Pipette, Dropper, Funnel, Beaker, Bunsen burner, Tripod stand,
China dish, Wire gauze, Glass rod, Filter paper, Fusion tube, Test tube stand, Test tube
holder, Burette stand and Measuring cylinder.

3.4 Chemicals Required:

Sr.No. Name MSDS
01 Distill water -----
02 5% H2SO4 Hazardous, corrosive, irritant & permeator.
03 Na- metal Hazardous, corrosive & skin inflammatory.
04 5% NaOH Hazardous, corrosive & irritant.
05 FeSO4 Hazardous, toxic & irritant.
07 Sodium -----
Nitropruside
.

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3.5 Chemical equations:
2Na + 2X2 2NaX 2Na+ + 2X-

Na + C + N NaCN Na+ + CN-

2Na + S Na2S 2Na+ + S2-

3.6 Procedure:

1. All the equipment was washed before using.

2. 3mm or small amount of sodium metal was taken in a fusion tube and melted at
Bunsen burner.
3. Small amount of given organic sample was added in the melted sodium metal and
again heated till red hot.
4. 15 mL distill water in a china dish was taken by the help of measuring cylinder and
the red hot fusion tube was put inside it.
5. Once the fusion tube was broken, it was further smashed to get small pieces.
6. China dish was put over the flame for 10 minutes or till water boils.
7. Solution in the china dish was filtered with the help of filter paper attached to the
funnel to the beaker.
8. Alkalinity of the solution with the help of litmus paper was checked; if it was not
alkaline then NaOH was added.
9. Small amount of filtered solution was taken from the beaker with the help of pipette
in 3 different test tubes.
10. Nitrogen and Sulphur detection tests were performed and the observations were
recorded.
11. This procedure was repeated for all the given samples.

3.6.1 Detection of Nitrogen:

Add about 5-6 drops of freshly prepared saturated solution of ferrous sulphate (or 0.2g
of ferrous sulphate crystals) to 5mL of the solution extract taken in a test tube. Boiled the
mixture for 30 seconds cooled and acidified with diluted sulphuric acid. A Prussian blue or
greenish coloration sometimes followed slowly by an actual precipitation of Prussian blue,
indicates the presence of cyanide in the filtrate and, therefore, of nitrogen in the given organic
compound. If only a green colorations is obtained it often indicates insufficient reaction with
the sodium or small percentage of nitrogen in the organic compound.

Chemical reactions:

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 FeSO4 + 2NaOH Fe (OH) 2 + Na2SO4

Green ppt.

Fe (OH) 2 + 6NaCN Na4 [Fe (CN) 6] + 2NaOH

Sodium Ferro cyanide

3Na4 [Fe (CN) 6] + 2Fe2 (SO4)3 Fe4 [Fe (CN) 6]3 + 6Na2SO4

Ferriferrocynaide

3.6.2 Detection of Sulphur:

To about 5mL of sodium extract added a few drops of freshly prepared sodium
Nitropruside solution a brilliant purple coloration (resembling permanganate) indicates the
presence of sulphide in the filtrate and, therefore that of Sulphur in the given organic
compound; the coloration slowly fades in standing. As sodium Nitropruside on each
occasion.

Chemical reaction:
Na2S + Na2 [Fe (CN) 5NO] Na4 [Fe (CN) 5NOS]

3.6.3 Detection of Sulphur and Nitrogen together:

Acidify 1mL of sodium extract with dilute HCl and 1-2 drops of FeCl3, a blood red
color indicates the presence of both Sulphur and nitrogen.

Chemical reaction:
Na
C +N+S Na CNS

Sodium sulphocyanide

3NaCNS + FeCl3 Fe (CNS) 3 + 3NaCl

Ferric sulphocyanide

3.6.4 Detection of Halogen:

AgNO3 test:
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 Acidify about 5 mL of sodium extract with dilute nitric acid, boil it and then add silver
nitrate solution. A flocculent white or yellow precipitate which darkens on exposure to light
indicates the presence of halogen.

Chemical reaction:
Na+X- + AgNO3 dil. HNO3
AgX + NaNO3

Since, all the halogens precipitate in this test; therefore, the presence of individual
halogen has to be made. Fluorine is not detected in this test, since silver fluoride is soluble in
water. In order to detect the individual halogens proceed as follows:

(a) A white precipitate soluble in NH4OH shows the presence of chloride.

(b) Pale yellow precipitate soluble in excess of NH4OH indicates bromine.
(c) Yellow precipitate insoluble in NH4OH indicates the presence of iodine.

2 Na + X2 2 NaX

AgCl (white)

AgNO3 + NaX AgBr (pale yellow)

AgI (yellow)

3.7 Observation Table:

Sr#. Test Sample A Sample B
1. Test for Nitrogen Present Present
2. Test for Sulphur Not present Present
3. Test for Nitrogen & Sulphur Not present Present

3.8 Conclusion:
With the help of Lassaigne test, presence of Sulphur, nitrogen and some halogens can
be easily detected in organic compounds.

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 Dated: /09/19

Experiment No. 4
How to do the solubility tests for the given unknown organic
compounds.
4.1 Objective:

Detection of organic compounds by using their solubility.

4.2 principles

Organic compounds tend to dissolve well in solvents that have similar

properties to themselves. Like dissolves like.

4.3 Chemicals required

Sr# chemicals MSDS

1 Distill water

2 5% NaOH Hazardous, corrosive & irritant

3 5%HCl Irritant, corrosive, coughing

4 5%NaHCO3 Irritant, fatal to inhale

6 Con.H2SO4 Causes severe skin burns and eye damage.

4.4 Procedure:

Determine the solubility in water first. If an unknown dissolves in water then no

need to test it in 5% NaOH or any other solvent. If an unknown substance is insoluble in
water, test it in 5% NaOH solution. To check whether the compound is soluble in 5% NaOH,
shake the compound with 5% NaOH solution, filter it from undissolved sample and make the
filtrate acidic with few drops of 5% HCl, the formation of a precipitate or turbidity indicates
significant solubility of the compound in 5% NaOH. Solubility of a water insoluble sample in
5% NaOH shows the presence of an acidic functional group in the unknown organic
compound. Then diluted base soluble samples are tested foer solubility in 5% NaHCO3
solution. If the sample is insoluble in both water and dilute base then it is tested for solubility
in 5% HCl. The compounds that are weakly basic to dissolve in 5% HCl are soluble in

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concentrated H2SO4. Any detectable reaction such as evolution of a gas or formation of a
particle is considered soluble in concentrated H2SO4.

4.5 Observation table

Class Nature of Class Compounds

W1 Acid class Aliphatic carboxylic acids, nitro phenols etc.
W2 Basis class Lower aliphatic amines
W3 Neutral class Carbohydrates, amines, alcohols, low molecular weight
aldehydes, and ketones, alkyl halides, thio-alcohols,
amides, thio-urea etc.
E1 Strong Acid class Aromatic or higher carboxylic acids and nitro-phenols
E2 Weak Acid class Weak acids and phenols.
E3 Basis Class Aromatic amines (secondary amines are usually not soluble
in HCl), hydrazine’s.

4.6 Conclusion

On the basis of solubility of organic compounds in different chemicals many organic

compound can be detected.

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 Dated: /10/10

Experiment No. 5
Determination of different functional groups in the given
unknown organic compounds.
Objective
To find presence of different functional groups in given organic compound.

5.1 Chemicals Required:

Sr.No. Name MSDS

01 Distill water -----
02 H2SO4 Causes severe skin burns and eye damage.
03 FeCl3 Hazardous, corrosive & irritant.
04 NaHCO3 Flammable, corrosive & toxic.
05 30% NaOH Hazardous, corrosive & irritant.
06 KMnO4 ------

5.2 Apparatus Required:

Test tubes, Pipette, Dropper, Beaker, Bunsen burner, Test tube stand, Test tube
holder and measuring cylinder.

5.3 Soda Lime test or NaOH test:

5.3.1 Objective:

To determine the presence of various water soluble compounds.

5.3.2Procedure:

Mix thoroughly one part of organic compound (0.3g) and four to five parts of
soda lime (NaOH + CaO) or 5 mL 30% NaOH. Then heat the mixture in dry test tube.

Observation Inference
NH3 evolved Amides, and ammonium salts are indicated,
e.g., acetamide, benzamide, ammonium acetate

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 etc.
Smell of caramel Carbohydrates, citric acid, tartaric acid
indicated.
Smell of aniline Anilides indicated
Smell of benzene Benzoic acid; phthalic acid which requires
longer heating than benzoic acid.
Chloroform evolved with characteristic Chloral hydrate (CCL3 CH (OH)2 ) is indicated
smell

5.4 Sodium Bicarbonate test:

5.4.1 Objective:

To determine the presence of Carboxylic acid and sulphunic acid.

5.4.2 Procedure:

Add few crystals of organic compound to the cold solution of 5% NaHCO3 and
watch very carefully if there is any effervescence from the NaHCO3 solution. Carboxylic
acids and sulphunic acids are indicated if bubbles are evolved from NaHCO3 solution.
Phenols do not give this test; however, nitro phenols being stronger acid may evolve CO2 in
this reaction.

5.4.3 Chemical reaction :

RCOOH + NaHCO3 RCOONa + CO2 + H2O

5.5 Neutral Ferric Chloride test:

5.5.1 Objective:

To determine the presence of phenols and hydroxyl acids.

5.5.2Procedure:

Ferric chloride solution sometimes contains a large excess of HCl which would
interfered with the following reactions. If it is very markedly acidic add dilute NaOH or
NH4OH solution, drop by drop, to the ferric chloride solution until a small but permanent
precipitate of ferric hydroxide is obtained. Filter this off through a small fluted filter paper,
and use the clear filtrate which becomes neutral. To this neutral ferric chloride solution add
an aqueous or ethanolic solution of phenol or hydroxyl aromatic acids, coloration indicates
phenols or hydroxyl aromatic acids. All phenols and hydroxyl acids show this test. The color
is due to formation of a complex ion [Fe (Oar) 6]3-.

5.5.3 Chemical reaction :

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 6 ArOH + FeCl3 3H+ + [Fe (Oar) 6]3- + 3HCl

Color Inference
Violet Phenol; vanillin with vanilla, smell; cresols;
phloroglucinol and resorcinol without any
odour; p-anisidine
Green Catechol
Blue violet Resorcinol
Purple Salicylic acid, p-amino phenol
White ppt. if the solution prepared was in α ‒ and β ‒ Naphthol
H2O
Violet in ethanolic solution α ‒ Naphthol
Red in ethanolic solution β ‒ Naphthol
Red coloration Formic and acetic acid
Buff precipitate Succinic, benzoic and adipic acids
Yellow coloration Tartaric and citric acids

5.6 Concentrated H2SO4 Test:

5.6.1 Objective:

To determine the type of acids.

5.6.2 Procedure:

Place a small amount of the substance in a dry test tube and add 1 mL of conc.
H2SO4 in it. Note any reaction in the cold and then warm gently.

Observations Inferences
CO & CO2 evolve in cold, no charring Oxalic acid
CO & CO2 evolve in cold, no charring but Citric acid
the solution becomes yellow
CO & CO2 evolve in cold with charring Hydroxyl aliphatic acids
Blackening without effervescence Resorcinol or polyhydric alcohols
Blackening with effervescence of CO/CO2 Carbohydrates, tartaric acid , lactic acid
or SO2
No blackening but pungent odour Simple phenol, succinic acid, benzoic acid

5.7 Potassium Permanganate test (Baeyer test):

5.7.1 Objective:

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 To determine the unsaturation of organic compound.

5.7.3 Procedure:

Dissolve 0.1g (or 0.2 mL) of the unknown in water or acetone/ethanol. Then
add 1-2 drops of 1% aqueous solution of KMnO4 and shake. The disappearance of purple
color and appearance of a sparingly soluble brown MnO2 is a positive test for unsaturation.

5.7.4 Chemical reaction :

3 C C + 2 KMnO 4 + 4H2O 3 C C + 2MnO 2 +

2KOH

OH OH

Further Oxidation

C O+O C

5.8 Bromine Water test:

5.8.1 Objective:

To determine the saturation and unsaturation in organic compound.

5.8.2 Principle :

On the addition of few drops of bromine water into the solution of organic
compound. The bromine water disappears. Decolourizatio is due to reduction of elemental
bromine (reddish brown) into a colourless brome derivative.

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5.8.3Procedure:

Dissolve 50 mg (or 2 drops) of unknown in 1mL of carbon tetra chloride/acetic

acid. To this add drop wise a 2% solution of bromine in CCl4. Decolourization shows
unsaturation, like KMnO4 a white precipitate indicates phenol or an aromatic amine.

5.8.3 Chemical reaction :

Br2 2 Br1
coloured colourless

Br
CCl 4
3 C C + Br2 3 C C

Br

5.9 Molish Test:

5.9.1 Objective:

Detection of presence of carbohydrates in given organic compound.

5.9.2 Procedure:

Place about 0.1 g of the compound in a test tube containing 2mL of water. Mix
with 2-4 drops of Molish reagent (1% I-Naphthol in ethanol). Allow 1mL of conc. H2SO4 to
flow along the sides of the inclined test tube so that the acid may from a layer under the
aqueous solution. A red ring changing to violet at the interference of the two liquids indicates
the presence of carbohydrates.

Note:

i. Perform this test when the substance is neutral and contains no

nitrogen.
ii. Carbohydrates on hydrolysis in the presence of conc. H2SO4 are
converted to furfural, which forms an unstable condensation product
with 1- Naphthol.

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5.10 2, 4 – Dinitrophenyl Hydrazine Test:
5.10.1 Objective:

Detection of presence of aldehyde and ketones.

5.10.2 Procedure:

Dissolve 0.2 g of the carbonyl compound in 3-4 mL of shake the mixture

vigorously. Observe the formation of orange or yellow precipitate which indicates the
presence of an aldehyde or a ketone. Sometimes the solution has to be left over for about 10
minutes to get the precipitate e.g. Benzophenone.

5.10.3 Chemical reactions:

The following chemical reaction takes place in which hydrazine is converted to

hydrazine. Yellow ppt. from isolated carbonyl compound, Orange red ppt. from carbonyl
compounds conjugated with double or aromatic rings

+
H2O

5.11 Tollen Test or Silver Mirror Test:

5.11.1 Objective:

To detect the presence of aldehyde.

5.11.2 Procedure:

Add dilute NH4OH solution dropwise to about 3mL of 10% AgNO3 solution
until a precipitate produced just re-dissolves. Add small quantity of organic compound to the
above ammoniacal silver nitrate solution [Ag (NH3)2]+ and place the test tube in water bath

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for 5-7 minutes. A metallic silver mirror deposit or silver mirror formation indicates the
presence of aldehydes.

5.11.3 Chemical reaction:

AgNO3 + NH4OH [Ag(NH3)2]+OH-

2[Ag (NH3)2] + + 2OH- + RCHO 2Ag + RCOO-NH4+ + H2O +

3NH3

5.11.4 Limitations:

Ketones do not respond to this rest because like aldehydes they cannot be
oxidized to carboxylic acids. However glucose and fructose both give reaction as the keto
group of fructose is easily oxidizable.

5.12 Fehling Solution Test:

5.12.1 Objective:

To detect of presence of glucose, fructose, aldehydes and phenols.

5.12.2 Procedure:

Mix equal volume of Fehling A (CuSO4 in H2O) and Fehling B (Na, K

tartarate-Rochelle salt and NaOH in H2O). Add organic compound to it and boil it. Formation
of a red or brown precipitate indicates the presence of glucose, fructose, aldehydes, some
phenols. Uric acid at first gives a white precipitate but on prolonged heating it gives red
precipitate because of reduction of cupric form to cuprous form.

5.12.3 Chemical reaction:

CuSo4 + 2NaOH Cu (OH)2 + Na2SO4

Cu (OH)2 CuO + H2O

2CuO + CH3CHO CH3COOH + Cu2O (red ppt.)

5.13 Schiff Test:

5.13.1 Objective:

To detect the presence of aliphatic and aromatic aldehydes.

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5.13.2 Theory:

Schiff reagent consists of 0.1% aqueous solution of fuchsia (p-rosaniline

hydrochloride) decolorized by passing SO2 gas or sodium sulphite. This test is utilized to
check the presence of aliphatic as well as aromatic aldehydes.

5.13.3 Procedure:

Treat 0.2g of the given compound with 4-5mL of the Schiff reagent in cold,
(never warm the mixture as It may result to wrong indication). Pink or violet coloration
indicates aldehydes (salicyl aldehyde and Vaniline do not give this test).

Note: The aliphatic aldehydes give coloration after sometime. However, the
presence of aldehyde must be confirmed by (a) Tollen reagent and (b) Fehling
solution. When treated with aldehyde, Schiff reagent ( 1% p-rosaniline +excess
SO2) is reoxidezed to give purple color.

5.13.4 Chemical reactions:

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5.14 Hinsberg Test:
5.14.1 Objective:

To distinguish primary, secondary and tertiary amines.

5.14.2 Procedure:

Add 5-10mL 10% NaOH solution to about 0.5g of amino compound in a test
tube. Then add 0.6mL of benzene sulphonyl chloride and mix vigorously for 5 minutes. If no
reaction appears to occur, warm the reaction mixture on a water bath for 1 minute and cool in
ice. On cooling, if no solid separates out then the substance is probably a tertiary amine. If a
precipitate appears in the alkaline medium, add 5mL of water and shake precipitate does not
dissolve indicates a secondary amine. If the solution is clear, acidify with dilute HCl
appearance of a precipitate indicates a primary amine.

5.14.3 Chemical reaction:

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5.15 Nitrous Acid Test (Diazotization Test):
5.15.1 Objective:

To distinguish amino group, primary secondary and tertiary aliphatic amines.

5.15.2 Procedure:

Dissolve 0.2g of the substance in 2mL of dilute HCl (2M HCl), cool it in ice.
Add 2mL ice cold 10% NaNO3 aqueous solution. Warm gently over water bath and watch the
under given changes.

5.15.3 Observations:

i. An immediate evolution of a colorless gas (nitrogen) indicates an amido group

/a primary aliphatic amine.
ii. If nitrogen gas does not evolve then add a few drops of the cold reaction
mixture to a cold solution of 0.5g of β- Naphthol in 2mL of 2M NaOH the
formation of an orange azo dye shows the presence of primary aromatic
amine.
iii. If an insoluble yellow or orange liquid (oil mass) is separated without
evolution of nitrogen gas, the aliphatic or aromatic secondary amine is
indicated.
iv. If no reaction is observed then the unknown compound is tertiary amine.

5.16 Lucas Test:

5.16.1 Objective:

To distinguish primary secondary and tertiary alcohols.

5.16.2 Procedure:

Add 1mL of alcohol to 2mL Lucas reagent (Conc. HCl + ZnCl2). Tertiary
alcohol gives precipitate of insoluble chloride immediately, secondary alcohol gives
precipitate after about4-5 minutes and primary alcohol reacts very slowly and gives
precipitate only in boiling.

5.16.3 Limitations:

This test fails if ZnCl2 is not anhydrous or if the reagent has been on the shelf
for a long time. In case of doubt whether the alcohol is tertiary or secondary, conc. HCl may
be added.

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5.17 Hydroxamic Acid Test:
5.17.1 Objective:

To detect the presence of ester acid chloride, amide, nitrile and anhydride.

5.17.2 Procedure:

Place 100 mg of the unknown in a test tube and add 1-2 mL of hydroxylamine
hydrochloride solution in ethanol. Make the solution alkaline with 10% NaOH. Heat the
mixture just to boiling then cool and just acidify the solution with dilute HCl. Add 1-2 drops
of 10% FeCl3. Development of a red color (due to the formation of a complex ferric hydroxy
mate from hydroxamic acid and ferric ions) indicates the presence if an ester, acid chloride,
amide nitrile and anhydride.

5.17.3 Limitation:

Benzene fails to give this test.

5.17.4 Chemical reaction:

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5.18 conclusions

By using different test, we can determine different functional groups present in an organic
sample.

Experiment no# 6
Determination of aldehydes and ketone functional groups by
using systematic analysis approach.
6.1 objectives
To find the nature of an unknown organic compound

6.2 Apparatus:
Test tubes, Pipette, Dropper, Funnel, Beaker, Bunsen burner, Tripod stand, China
dish, Wire gauze, Glass rod, Filter paper, Fusion tube, Test tube stand, Test tube holder,
Burette stand and Measuring cylinder.

6.3 Chemicals Required:

Sr. # Chemicals MSDS

1. NaOH It is an irritant very hazardous in case of skin

contact and eye contact

2. NaHCO3 Slightly hazardous in case of eye contact and

also in case of inhalation

3. Distilled water -----------------------------------------

4. Bromine water May Causes eye injury, cause irritation

5. Acetic Acid Damaging internal organs cause inhalation

6. HCl Irritative,hazardous to eyes

7. CuSO4 Poisoning,Irritative

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 8. FeCl3 May cause an allergic skin reaction.

9 Sodium metal Irritant.

10 Potassium Irritant. Hazardous

11 Rochelle salt

12 H2SO4 irritant
13 KMnO4 Toxic to kidney, liver, etc
14 DNP Toxic for inhalation
Sample A

6.4 Observation table:

Sr. Tests Observation inference
#
1. Physical test:
i) Color. White. Alcohols, aldehydes, acids,
ii) State. crystals ketones and ethers may be
iii) Odor. Odorless. present

2. Ignition.
Small quantity of compounds Non smoky flame Aliphatic compounds may be
heated on tip of spatula. present
3. Solubility:
Add a little amount of Insoluble in water. Monofunctional compounds,
compound in water. alcohols , aldehydes,
ketones,amides, esters,
Add little amount of insoluble Anilides, olefins etc may be
compound in NaOH. present
Now add the compound in Insoluble.
NaHCO3.
Add little amount of HCl. insoluble
Add little amount of soluble without charring
con.H2SO4.
4. Litmus test: Base is present, ketones,
Use litmus paper to test the Red litmus paper turns aldehydes, amides may be
solution. blue. present.
6. KMnO4 No change in color Unsaturated compounds are
Treat the solution with present
KMnO4 solution.
7. Lassaigne test:
i) Sodium extract No Prussian blue color. Nitrogen is absent.
added in ferrous
sulphate and
boiled it for 30
seconds cool and No black ppt. Sulphur is absent.
acidify it

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 ii) Added sodium
extracts in lead
acetate and
acidifies by acetic
acid.
iii) Sodium extract No ppt Halogens are absent
+HNO3 +AgNO3
8. 2,4-Dinitophenyle Orange or yellow Ketones or aldehydes indicated.
Hydrazine test precipitates.
Treat the solution with
DNP+alcohol+con. H2SO4
9. Melting point:
Add small amount of organic 48degree Ketone functional group may be
compound in capillary tube. present
And place it in apparatus.

10 Fehling solution test No red color precipitates Aldehyde is absent, so

Mix equal volume Fehling confirmed ketone is present
solution A (CuSO4 in water)
and solution B (Na, K,
tartrate, Rochelle salt and
NaOH in water) and add
organic compound in it and
boil it.
11 Compound +sodium Red coloration Ketone group confirmed.
nitroprusside+NaOH

6.5 conclusions
So from above tests it is confirmed that sample A is a ketone.

Sample B

6.6 Observation table:

Sr. Tests Observation inference
#
1. Physical test:
Color. White. Alcohols, aldehydes, acids,
State. crystals ketones and ethers may be
Odor. Odorless. present

29
2. Ignition.
Small quantity of compounds Non smoky flame Aliphatic compound is present
heated on tip of spatula.
3. Solubility:
Add a little amount of Insoluble in water. Monofunctional compounds,
compound in water. alcohols , aldehydes,
ketones,amides, esters,
Add little amount of insoluble Anilides, olefins etc may be
compound in NaOH. present
Now add the compound in Insoluble.
NaHCO3.
Add little amount of HCl. insoluble
Add little amount of soluble without charring
con.H2SO4.
4. Litmus test: Base is present, ketones,
Use litmus paper to test the Red litmus paper turns aldehydes, amides may be
solution. blue. present.
6. KMnO4 No change in color Unsaturated compounds are
Treat the solution with present
KMnO4 solution.
7. Lassaigne test:
(1)Sodium extract added in No Prussian blue color. Nitrogen is absent.
ferrous sulphate and boiled it
for 30 seconds cool and
acidify it
No black ppt. Sulphur is absent.
(2)Added sodium extracts in
lead acetate and acidifies by
acetic acid.
(3)Sodium extract +HNO3
+AgNO3

No ppt Halogens are absent

8. 2,4-Dinitophenyle Orange or yellow Ketones or aldehydes indicated.
Hydrazine test precipitates.
Treat the solution with
DNP+alcohol+con. H2SO4
9. Melting point:
Add small amount of organic -123.5 degree Aldehyde is confirmed
compound in capillary tube.
And place it in apparatus.

10 Fehling solution test red color precipitates Aldehyde is confirmed.

Mix equal volume Fehling
solution A (CuSO4 in water)
and solution B (Na, K,
tartrate, Rochelle salt and
NaOH in water) and add
organic compound in it and

30
 boil it.

6.7 conclusions
So from above tests it is confirmed that sample B is an aldehyde.

Experiment no 7
Detection of Benzophenone/Succinic acid/Benzoic acid/sucrose.
7.1 Objective:
To find the nature of unknown organic compound.

7.2 Apparatus:
Test tubes, Pipette, Dropper, Funnel, Beaker, Bunsen burner, Tripod stand, China
dish, Wire gauze, Glass rod, Filter paper, Fusion tube, Test tube stand, Test tube holder,
Burette stand and Measuring cylinder.

7.3 Chemicals Required:

Sr. # Chemicals MSDS

1. NaOH It is an irritant very hazardous in case of skin

contact and eye contact

2. NaHCO3 Slightly hazardous in case of eye contact and

also in case of inhalation

3. Distilled water -----------------------------------------

4. Bromine water May Causes eye injury, cause irritation

31
 5. Acetic Acid Damaging internal organs cause inhalation

6. Fecl3 Irritative,hazardous to eyes

7. Cu metal Poisoning,Irritative

8. Phthalic Anhydride May cause an allergic skin reaction.

Sample A

7.4 Observation table:

Sr. Tests Observation inference
#
1. Physical test:
iv) Color. White. Alcohols, aldehydes, acids,
v) State. crystals ketones and ethers may be
vi) Odor. Odorless. present

2. Ignition.
Small quantity of compounds Smoky flame. Aromatic compound may be
heated on tip of spatula. present.
3. Solubility:
Add a little amount of Sparingly soluble in water
compound in water. and more soluble in hot
water. Aromatic, Phenols or amines
may be present.
Add little amount of
compound in NaOH. Soluble.
Now add the compound in
NaHCO3. Soluble.

4. Litmus test: Red color changes to blue. It may be acid or Phenol

.
5. Alkaline KMnO4: No change in color. Aromatic, saturated acid is
present.

6. FeCl3 test:
Add neutral FeCl3 in Buff precipitate. Benzoic and adipic acid,
compound. succinic acid
7. Lassaigne test:
iv) Sodium extract Prussian blue color. Nitrogen is absent.
added in ferrous
sulphate and
boiled it for 30
seconds cool and No black ppt. Sulphur is absent.
acidify it
v) Added sodium

32
 extract in lead
acetate and
acidify by acetic
acid
vi) Sodium
extract+AgNO3+ No ppt Halogen is absent.
HNO3.
8. Sodium bicarbonate test: Bubbles are evolved.
Introduce few crystals of Carboxylic acids and sulphunic
compound in solution of 5% acids may be present.
NaHCO3.
9. Concentrated H2SO4:
Organic compound adds in No blackening but Simple phenol, succinic acid
concentrated H2SO4. pungent odor. and benzoic acid may be
present.
10. Melting point:
Add small amount of organic 121○ Benzoic acid may be present.
compound in capillary tube.
And place it in apparatus.
11. Confirmatory test:
Heat small quantity with Fruity smell, M.P 130○ Benzoic acid is confirmed.
ethanol and H2SO4 on water
bath, Amide formation

7.5 Conclusion:
So, from the above tests performed it is confirmed that the unknown compound is
Benzoic acid.

Sample B

7.6 Observation table:

Sr. Tests Observation inference
#
1. Physical test:
Color. White. Coloured compounds are
State crystal absent.
Odor. pleasant
2. Ignition.
Small quantity of compounds Smoky flame. Aromatic compound may be
heated on tip of spatula. present.
3. Solubility: Monofunctional compounds,

33
 Add a little amount of compound insoluble alcohols , aldehydes,
in water. ketones,amides, esters,
Anilides, olefins etc may be
present
Add little amount of compound Insoluble.
in NaOH.
Now add the compound in insoluble
NaHCO3.
Add little amount of HCl. insoluble
Add little amount of con.H2SO4. soluble
4. Litmus test: No action on blue or Acid , phenols and amines
. red litmus paper. are absent
5. Alkaline KMnO4: No change in color. Saturated compound is
present.

6. Compound +Bromine water No decolourization A saturated compound is

present.
7. Lassaigne test:
(1)Sodium extract added in No Prussian blue color. Nitrogen is absent.
ferrous sulphate and boiled it for
30 seconds cool and acidify it
(2)Added sodium extracts in lead
acetate and acidifies by acetic No black ppt. Sulphur is absent.
acid.
(3)Sodium extract +HNO3
+AgNO3 No ppt Halogen absent
8. compound+2,4-dinytrophenyle Orange ppt A ketone or aldehyde is
hydrazine+methanol+con.H2SO4 present.

9 Silver mirror test; No red ppt An aldehyde is absent, a

Compound+ammonical silver ketone is present.
nitrate solution.

9. Concentrated H2SO4: Yellow solution Benzophenone indicated.

Organic compound adds in
concentrated H2SO4.

10. Melting point: Benzophenone indicated

Add small amount of organic 48 degree
compound in capillary tube. And
place it in apparatus.

11. Confirmatory test: Benzophenone is confirmed.

Fused the compound with Deep blue color is
sodium metal obtained

7.7 Conclusion:

34
 So, from the above tests performed it is confirmed that the unknown compound is
Benzophenone.

Sample C

7.8 Observation table:

Sr. Tests Observation inference
#
1. Physical test: acids, carbohydrates, phenols
vii) Color. White. and amides may be present
viii) State. crystals
ix) Odor. Odorless solids.
2. Ignition.
Small quantity of compounds No Smoky flame. Aromatic compound absent.
heated on tip of spatula.
3. Solubility: An aliphatic compound may be
Add a little amount of Sparingly soluble in water present.
compound in water. and more soluble in hot
water

4. Litmus test: No action on blue or red A neutral compound may be

. litmus paper. present.
5. Lassaigne test:
vii) Sodium extract Prussian blue color. Nitrogen is absent.
added in ferrous
sulphate and
boiled it for 30
seconds cool and No black ppt. Sulphur is absent.
acidify it
viii) Added sodium
extracts in lead
acetate and
acidifies by acetic
acid.
ix) Sodium extract No ppt Halogens are absent
+HNO3 +AgNO3
6 Compound +KMnO4 No decolourization Saturated compound may be
present.
7. Concentrated H2SO4:
Organic compound adds in Blackening occurred. A carbohydrate may present.
concentrated H2SO4.
8 Heated the compound with Smell of burnt sugar A carbohydrate may be
soda lime present.

35
9 Molish test; Reddish violet ring is A carbohydrate is indicated.
Compound +1% a- formed at the junction.
naphthol+con.H2SO4
10 Melting point:
Add small amount of organic Sucrose is present
compound in capillary tube.
And place it in apparatus.
11 Confirmatory test: Sucrose is confirmed.

7.9 conclusions
So from above experiment it is confirmed that given simple is sucrose.

Sample D

7.10 Observation table:

Sr. Tests Observation inference
#
1. Physical test:
x) Color. White. Alcohols, aldehydes, acids,
xi) State. crystals ketones and ethers may be
xii) Odor. Odorless. present

2. Ignition.
Small quantity of compounds No Smoky flame. Aromatic compound may be
heated on tip of spatula. absent.
3. Solubility:
Add a little amount of Sparingly soluble in water Aliphatic acid may be present.
compound in water. and more soluble in hot
water.

.
4. Litmus test: Red color changes to blue. It may be acid or Phenol
.
5. Alkaline KMnO4: No change in color. Saturated acid is present.

6. FeCl3 test:
Add neutral FeCl3 in Buff precipitate. Benzoic and adipic acid,
compound. succinic acid
7. Lassaigne test:
x) Sodium extract Prussian blue color. Nitrogen is absent.
added in ferrous
sulphate and
boiled it for 30
seconds cool and No black ppt. Sulphur is absent.

36
 acidify it
xi) Added sodium
extract in lead
acetate and
acidify by acetic
acid
xii) Sodium
extract+AgNO3+ No ppt Halogen is absent.
HNO3.
8. Sodium bicarbonate test: Bubbles are evolved.
Introduce few crystals of Carboxylic acids and sulphunic
compound in solution of 5% acids may be present.
NaHCO3.
9. Concentrated H2SO4:
Organic compound adds in No blackening but Simple phenol, succinic acid
concentrated H2SO4. pungent odor. and benzoic acid may be
present.
10. Melting point:
Add small amount of organic Succinic acid is indicated.
compound in capillary tube.
And place it in apparatus.
11. Confirmatory test:
Succinic acid is confirmed.

7.11 Conclusion:
So, from the above tests performed it is confirmed that the unknown compound is
succinic acid.

Experiment no 8
Detection of starch/glucose/fructose.
8.1 Objective:
To find the nature of unknown organic compound.

8.2 Apparatus:
Test tubes, Pipette, Dropper, Funnel, Beaker, Bunsen burner, Tripod stand, China
dish, Wire gauze, Glass rod, Filter paper, Fusion tube, Test tube stand, Test tube holder,
Burette stand and Measuring cylinder.

37
8.3 Chemicals Required:

Sr. # Chemicals MSDS

1. NaOH It is an irritant very hazardous in case of skin

contact and eye contact

2. NaHCO3 Slightly hazardous in case of eye contact and

also in case of inhalation

3. Distilled water -----------------------------------------

4. Bromine water May Causes eye injury, cause irritation

5. Acetic Acid Damaging internal organs cause inhalation

6. Fecl3 Irritative,hazardous to eyes

7. Cu metal Poisoning,Irritative

8. Phthalic Anhydride May cause an allergic skin reaction.

Sample A

8.4 Observation table:

Sr. Tests Observation inference
#
1. Physical test: acids, carbohydrates, phenols
xiii) Color. White. and amides may be present
xiv) State. crystals
xv) Odor. Odorless solids.
2. Ignition.
Small quantity of compounds No Smoky flame. Aromatic compound absent.
heated on tip of spatula.
3. Solubility: An aliphatic compound may be
Add a little amount of Sparingly soluble in water present.
compound in water. and more soluble in hot
water

4. Litmus test: No action on blue or red A neutral compound may be

. litmus paper. present.
5. Lassaigne test:
xiii) Sodium extract Prussian blue color. Nitrogen is absent.
added in ferrous

38
 sulphate and
boiled it for 30
seconds cool and No black ppt. Sulphur is absent.
acidify it
xiv) Added sodium
extracts in lead
acetate and
acidifies by acetic
acid.
xv) Sodium extract No ppt Halogens are absent
+HNO3 +AgNO3
6 Compound +aqueous No decolourization Saturated compound may be
KMnO4 present.
7. Concentrated H2SO4:
Organic compound adds in Blackening occurred. A carbohydrate may present.
concentrated H2SO4.
8 Heated the compound with Smell of burnt sugar A carbohydrate may be
soda lime present.

9 Molish test; Reddish violet ring is A carbohydrate is indicated.

Compound +1% a- formed at the junction.
naphthol+con.H2SO4

10 Silver mirror test; Silver mirror is formed Glucose or fructose may be

Compound+ammonical silver present.
nitrate solution.
11 Fehling solution test; Reddish brown ppt. Glucose indicated.
Compound+fehling solution
10 Melting point:
Add small amount of organic 146 degree Glucose indicated
compound in capillary tube.
And place it in apparatus.
11 Furfural test; Glucose confirmed.
Glucose +1% alcoholic+1- Violet coloration
naphthol+con.HCl and boiled
8.5 conclusions
So from above experiment it is confirmed that given sample is glucose.

Sample B

8.6 Observation table:

Sr. Tests Observation inference
#
1. Physical test:
Color. White. Coloured compounds are
State crystal absent.

39
 Odor. pleasant
2. Ignition.
Small quantity of compounds No Smoky flame. Aromatic compound may be
heated on tip of spatula. absent.
3. Solubility: Polysaccharides, starch,
Add a little amount of compound insoluble hydroxide etc.
in water.

Add little amount of compound Insoluble.

in NaOH.
Now add the compound in insoluble
NaHCO3.
Add little amount of HCl. insoluble
Add little amount of con.H2SO4. soluble(with charring)
4. Litmus test: No action on blue or Acid , phenols and amines
. red litmus paper. are absent
5. Alkaline KMnO4: No change in color. Saturated compound is
present.

6. Compound +Bromine water No decolourization A saturated compound is

present.
7. Lassaigne test:
(1)Sodium extract added in No Prussian blue color. Nitrogen is absent.
ferrous sulphate and boiled it for
30 seconds cool and acidify it
(2)Added sodium extracts in lead
acetate and acidifies by acetic No black ppt. Sulphur is absent.
acid.
(3)Sodium extract +HNO3
+AgNO3 No ppt Halogen absent
8. compound+2,4-dinytrophenyle Orange ppt A ketone or aldehyde is
hydrazine+methanol+con.H2SO4 present.

9 Silver mirror test; No red ppt An aldehyde is absent, a

Compound+ammonical silver ketone is present.
nitrate solution.

9. Concentrated H2SO4: Yellow solution Benzophenone indicated.

Organic compound adds in
concentrated H2SO4.

10. Melting point: Benzophenone indicated

Add small amount of organic
compound in capillary tube. And
place it in apparatus.

11. Confirmatory test: Benzophenone is confirmed.

40
8.7 Conclusion:
So, from the above tests performed it is confirmed that the unknown compound is
starch.

Sample C

8.8 Observation table:

Sr. Tests Observation inference
#
1. Physical test: acids, carbohydrates, phenols
xvi) Color. White. and amides may be present
xvii) State. crystals
xviii) Odor. Odorless solids.
2. Ignition.
Small quantity of compounds No Smoky flame. Aromatic compound absent.
heated on tip of spatula.
3. Solubility: An aliphatic compound may be
Add a little amount of Sparingly soluble in water present.
compound in water. and more soluble in hot
water

4. Litmus test: No action on blue or red A neutral compound may be

. litmus paper. present.
5. Lassaigne test:
xvi) Sodium extract Prussian blue color. Nitrogen is absent.
added in ferrous
sulphate and
boiled it for 30
seconds cool and No black ppt. Sulphur is absent.
acidify it
xvii) Added sodium
extracts in lead
acetate and
acidifies by acetic
acid.
xviii) Sodium extract No ppt Halogens are absent
+HNO3 +AgNO3
6 Compound +aqueous No decolourization Saturated compound may be
KMnO4 present.

41
7. Concentrated H2SO4:
Organic compound adds in Blackening occurred. A carbohydrate may present.
concentrated H2SO4.
8 Heated the compound with Smell of burnt sugar A carbohydrate may be
soda lime present.

9 Molish test; Reddish violet ring is A carbohydrate is indicated.

Compound +1% a- formed at the junction.
naphthol+con.H2SO4

10 Silver mirror test; Silver mirror is formed Glucose or fructose may be

Compound+ammonical silver present.
nitrate solution.
11 Fehling solution test; Reddish brown ppt. Sucrose is indicated.
Compound+fehling solution
10 Melting point: Sucrose is indicated
Add small amount of organic
compound in capillary tube.
And place it in apparatus.
11 Confirmatory test Sucrose is confirmed.

8.9 conclusions
So from above experiment it is confirmed that given sample is sucrose.

Experiment No. 9
Detection of urea/ a-Naphthol/ B-Naphthol by using
systematic analysis approach.
9.1 Objective:
To find the nature of unknown organic compound.

9.2 Apparatus:
Test tubes, Pipette, Dropper, Funnel, Beaker, Bunsen burner, Tripod stand, China
dish, Wire gauze, Glass rod, Filter paper, Fusion tube, Test tube stand, Test tube holder,
Burette stand and Measuring cylinder.

9.3 Chemicals Required:

Sr. # Chemicals MSDS

42
 1. NaOH It is an irritant very hazardous in case of skin
contact and eye contact

2. NaHCO3 Slightly hazardous in case of eye contact and

also in case of inhalation

3. Distilled water -----------------------------------------

4. Bromine water May Causes eye injury, cause irritation

5. Acetic Acid Damaging internal organs cause inhalation

6. Fecl3 Irritative,hazardous to eyes

7. Cu metal Poisoning,Irritative

8. Phthalic Anhydride May cause an allergic skin reaction.

Sample A
9.4 Observation table:
Sr.# Experiment Observation Inference
1. Physical/Primary
Test
a) State Solid Crystals ---

b) Color Black/chocolate Naphthol

c) Odour Phenolic Phenol/Naphthol

2. Ignition Test
Take a small of the Smoky flame observed. Aromatic
sample on spatula compound
and ignite it
3. Solubility Test
Add a small amount H2O 10%NaHCO3 10%NaOH Weak acids like
of the organic - - + phenols
compound in 1mL
of each of the
following
compounds.
4. Bromine water
Test
i. Add a few drops of No decolourization Unsaturated
Br-water into the compound
solution of organic

43
 compound.
ii. Add 2 drops of No decolourization Unsaturated
unknown in 1mL of compound
acetic acid and add
2% of bromine in it.
5. Neutral FeCl3 Test
i. Dissolve a little of no color appeared ---
the compound in
ethanol & add 1-2
drops of neutral
FeCl3 in it
ii. Dissolve a little of White ppt. Observed α/β-Naphthol
the compound in
water & add 1-2
drops of neutral
FeCl3 in it
6. Confirmatory Test
Gently warm the Blue color appeared α-Naphthol
sample with
dil.NaOH and CCl4
& then add Cu-
metal in it

7. Phthalic Test
To 2g of a phenol Green color observed α-Naphthol
add 2g of phthalic
anhydride. Moisten
with 2 drops of
conc. H2SO4 &
gently fuse for about
a minute. Cool a bit
& add excess NaOH
solution in it.
8. Melting Point Test
Close one side of 94ºC α-Naphthol
the capillary tube by
burning and add a
small amount of
sample in it by the
other side. Place the
tube in the device
and note the
temperature at
which the sample
burns.

9.5 Conclusion:

44
 So, from the above tests performed it is confirmed that the unknown compound
is α-Naphthol.

Sample B

9.6 Observation table:

Sr. Tests Observation inference
#
1. Physical test: Coloured compounds are
xix) Color. White. absent.
xx) State. crystals
xxi) Odor. pungent smell
2. Ignition.
Small quantity of compounds No Smoky flame. Aromatic compound absent.
heated on tip of spatula.
3. Solubility: An aliphatic compound may
Add a little amount of compound Sparingly soluble in be present.
in water. water and more soluble
in hot water

4. Litmus test: No action on blue or red A neutral compound may be

. litmus paper. present, acids, phenols,
mines are absent.
5. Lassaigne test:
xix) Sodium extract added Prussian blue color. Nitrogen is present.
in ferrous sulphate and
boiled it for 30
seconds cool and
acidify it
xx) Added sodium
extracts in lead acetate No ppt Sulphur is absent.
and acidifies by acetic
acid.
xxi) Sodium extract No ppt Halogens are absent.
+HNO3 +AgNO3

6 Compound +5% HCl Insoluble Amines are absent.

7. Compound+NaNO3+HCl+boiled. N2 evolved An amide is present.

10 Melting point: Urea indicated.

Add small amount of organic 132 degree
compound in capillary tube. And
place it in apparatus.

45
11 Confirmatory test Reddish violet Urea confirmed.
Biuret test colorization
Compound+ heats until NH3
evolved cool and dissolve the
residue in dil.NaOH+CuSO4
drop by drop.
9.7 Conclusion:
So, from the above tests performed it is confirmed that the unknown compound
is urea.

Sample C
9.8 Observation table:
Sr.# Experiment Observation Inference
1. Physical/Primary
Test
d) State Solid Crystals ---

e) Color Black/chocolate Naphthol

f) Odour Carbolic Phenol/Naphthol

2. Ignition Test
Take a small of the Smoky flame observed. Aromatic
sample on spatula compound
and ignite it
3. Solubility Test
Add a small amount H2 O 10%NaHCO3 10%NaOH Weak acids like
of the organic - - + phenols
compound in 1mL
of each of the
following
compounds.
4. Bromine water
Test
iii. Add a few drops of No decolourization Unsaturated
Br-water into the compound
solution of organic
compound.
iv. Add 2 drops of No decolourization Unsaturated
unknown in 1mL of compound
acetic acid and add
2% of bromine in it.
5. Neutral FeCl3 Test
iii. Dissolve a little of no color appeared ---
the compound in

46
 ethanol & add 1-2
drops of neutral
FeCl3 in it
iv. Dissolve a little of White ppt. Observed α/β-Naphthol
the compound in
water & add 1-2
drops of neutral
FeCl3 in it
Confirmatory test:

7. Phthalic Test
To 2g of a phenol
add 2g of phthalic
anhydride. Moisten
with 2 drops of
conc. H2SO4 &
gently fuse for about
a minute. Cool a bit
& add excess NaOH
solution in it.
8. Melting Point Test
Close one side of 94ºC α-Naphthol
the capillary tube by
burning and add a
small amount of
sample in it by the
other side. Place the
tube in the device
and note the
temperature at
which the sample
burns.

9.9 Conclusion:
So, from the above tests performed it is confirmed that the unknown compound
is α-Naphthol.

Experiment No. 11

47
 Determine the given unknown organic compound using
systematic analysis approach.
5.1 Objective :
To find the nature of unknown organic compound.

5.2 Apparatus:
Test tubes, Pipette, Dropper, Funnel, Beaker, Bunsen burner, Tripod stand, China
dish, Wire gauze, Glass rod, Filter paper, Fusion tube, Test tube stand, Test tube holder,
Burette stand and Measuring cylinder.

5.3 Chemicals Required:.

Sr. # Chemicals MSDS

1. NaOH It is an irritant very hazardous in case of skin

contact and eye contact

2. NaHCO3 Slightly hazardous in case of eye contact and

also in case of inhalation

3. Distilled water -----------------------------------------

4. Bromine water May Causes eye injury,cause irritation

5. Acetic Acid Damaging internal organs cause inhalation

6. Fecl3 Irretative,hazardous to eyes

7. Cu metal Poisoning,Irritative

8. Phthlic Anhydride May cause an allergic skin reaction.

5.4 Observation table :

Sr. Tests Observation inference
#
1. Physical test:
xxii) Color. White. Alcohols, aldehydes, acids,
xxiii) State. crystals ketones and ethers may be

48
 xxiv) Odor. Odorless. present

2. Ignition.
Small quantity of compounds Irritating odor. Carboxylic acids may be
heated on tip of spatula. present.
3. Solubility:
Add a little amount of Insoluble in water.
compound in water.
Aromatic or higher carboxylic
Add little amount of Soluble. acids and nitro-phenols may be
compound in NaOH. present.
Now add the compound in Soluble.
NaHCO3.
4. Litmus test:
Red color changes to blue. This change due to
NaHCO3. But the
compound is acid
5. Alkaline KMnO4: No change in color. Aromatic saturated acid is
present.

6. FeCl3 test:
Add neutral FeCl3 in Purple color. Salicylic acid, p-amino phenol
compound. may be present.
7. Lassainge test:
xxii) Sodium extract Prussian blue color. Nitrogen is absent.
added in ferrous
sulphate and
boiled it for 30
seconds cool and No black ppt. Sulphur is absent.
acidify it
xxiii) Added sodium
extract in lead
acetate and
acidify by acetic
acid.
8. Sodium bicarbonate test: Bubbles are evolved.
Introduce few crystals of Carboxylic acids and sulphonic
compound in solution of 5% acids may be present.
NaHCO3.
9. Melting point:
Add small amount of organic 157○ Salicylic acids may be present
compound in capillary tube. may be present.
And place it in apparatus.
10. Confirmatory test:
0.5g Organic compound add Phenol formed, M.P 142○ Salicylic acid is confirmed.
2 drops of H2SO4 and 1mL of
CH3OH heat on a bath for a
minute.

49
5.5 Conclusion:
So, from the above tests performed it is confirmed that the unknown compound is
Salicylic acid.

50
51
 Dated: 14/10/19

Experiment No. 8

Determine the given unknown organic compound using

systematic analysis approach.
.

Dated: 21/10/19

Experiment No. 9

Determine the given unknown organic compound using

systematic analysis approach.
7.1 Objective :
To find the nature of unknown organic compound.

52
7.2 Apparatus:
Test tubes, Pipette, Dropper, Funnel, Beaker, Bunsen burner, Tripod stand, China
dish, Wire gauze, Glass rod, Filter paper, Fusion tube, Test tube stand, Test tube holder,
Burette stand and Measuring cylinder.

7.3 Chemicals Required:.

Sr. # Chemicals MSDS

1. NaOH It is an irritant very hazardous in case of skin

contact and eye contact

2. NaHCO3 Slightly hazardous in case of eye contact and

also in case of inhalation

3. Distilled water -----------------------------------------

4. Bromine water May Causes eye injury,cause irritation

5. Acetic Acid Damaging internal organs cause inhalation

6. Fecl3 Irretative,hazardous to eyes

7. Cu metal Poisoning,Irritative

8. Phthlic Anhydride May cause an allergic skin reaction.

Sample A
7.4 Observation table :
Sr.# Experiment Observation Inference
1. Physical/Primary
Test
g) State Solid Crystals ---

h) Colour Black/chocolate Napthols

i) Odour Phenolic Phenol/Napthol

2. Ignition Test

53
 Take a small of the Smoky flame observed. Aromatic
sample on spatula compound
and ignite it
3. Solubility Test
Add a small amount H2 O 10%NaHCO3 10%NaOH Weak acids like
of the organic - - + phenols
compound in 1mL of
each of the following
compounds.
4. Bromine water Test
v. Add a few drops of No decolourization Unsaturated
Br-water into the compound
solution of organic
compound.
vi. Add 2 drops of No decolourization Unsaturated
unknown in 1mL of compound
acetic acid and add
2% of bromine in it.
5. Neutral FeCl3 Test
v. Dissolve a little of no colour appeared ---
the compound in
ethanol & add 1-2
drops of neutral
FeCl3 in it
vi. Dissolve a little of White ppt. Observed α/β-Naphthols
the compound in
water & add 1-2
drops of neutral
FeCl3 in it
6. Confirmatory Test
Gently warm the Blue colour appeared α-Naphthol
sample with
dil.NaOH and CCl4
& then add Cu-metal
in it

7. Phthalein Test
To 2g of a phenol Green colour observed α-Naphthol
add 2g of phthalic
anhydride. Moisten
with 2 drops of conc.
H2SO4 & gently fuse
for about a minute.
Cool a bit & add
excess NaOH
solution in it.
8. Melting Point Test
Close one side of the 94ºC α-Naphthol
capillary tube by
54
 burning and add a
small amount of
sample in it by the
other side. Place the
tube in the device
and note the
temperature at which
the sample burns.

7.5 Conclusion:
So, from the above tests performed it is confirmed that the unknown compound
is α-Naphthol.

Sample B
7.6 Observation table :
Sr. # Experiment Observation Inference
1. Physical/Primary Test
j) State Solid ---

k) Colour Brown Aromatic amines

l) Odour Carbolic Acid,phenol,amides,

anilides may be
present
2. Ignition Test
Take a small of the sample on Smoky flame observed. Aromatic compound
spatula and ignite it

3. Solubility Test
Add a small amount of the H2O 10%NaOH Aliphatic acids
organic compound in 1mL of
+ +
each of the following
compounds.
4. Litmus paper Test
Check by red litmus or blue Blue litmus red Carboxylic acid may
litmus paper be present
5. Sodium Bicarbonate Test
Add organic compound in 10% Insoluble & no An acid is absent,
NaHCO3 effervescence phenol may be
present
6. Bromine water Test
vii. Add a few drops of Br-water No decolourization but Phenolic group may
into the solution of organic white ppt. appeared be present

55
 compound.
viii. Add 2 drops of unknown in 1mL No decolourization but Phenolic group may
of acetic acid and add 2% of white ppt. appeared be present
bromine in it.
7. Neutral FeCl3 Test
Dissolve a little of the Blue Violet Resorcinol
compound in ethanol/water &
add 1-2 drops of neutral FeCl3 in
it
8. Concentrated H2SO4 test
Place small amount of the Blackening without Resorcinol or
substance in a dry test tube and effervescence polyhydric alcohols
add 1mL of conc. H2SO4.
9. Phthalein Test
To 2g of a phenol add 2g of Green colour observed α-Naphthol&
phthalic anhydride. Moisten Resorcinol
with 2 drops of conc. H2SO4 &
gently fuse for about a minute.
Cool a bit & add excess NaOH
solution in it.
10. Limbermannnitrese Test
Add organic compound in Colour change to green, Phenol
concentrated H2SO4 and few blue & violet
crystals of NaNO2

11. Add organic compound in dil. Green fluorescence Resorcinol may be

NaOH and CHCl3 present
12. Azodye Test
Add organic compound in Orange red dye is formed Resorcinol indicated
aniline reagent and conc. HCl.
Cool it and then add 20% of
NaNO2&NaOH
13. Comfirmatory Test
Add oxalic acid and H2SO4 in Blue ring is formed at Resorcinol indicated
organic compound junction
14. Melting Point Test
Close one side of the capillary 110ºC Resorcinol indicated
tube by burning and add a small
amount of sample in it by the
other side. Place the tube in the
gallenkamp and note the
temperature at which the sample
burns.

56
7.7 Conclusion:
So, from the above tests performed it is confirmed that the unknown compound
is Resorcinol.

57