Cpd_analysis Procedure 2011 Final

8/3/2019 Cpd_analysis Procedure 2011 Final

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Experiment No:--------------------

Date: --------------------

Aim: To analyse the given organic compound systematically and prepare a suitable crystalline derivative ofthe same.

EXPERIMENT OBSERVATION INFERENCE

1) Physical State

Solid / liquid

Colored/colourlessOdour;Pleasant/offensive

Crystalline/Amorphous

2) Solubility Test

Tested the solubility of the

compound.

IN WATER,COLD/HOT ------------

IN dil HCl -------------

IN dil NaOH -------------

IN Conc.H2SO4 -------------

3)

a)Flame Test: Carried out the flame test.

b) Charring Test:

Sooty, luminous flame/

Non sooty flame

Observed: --------------

b)Smell of burning sugar

observed--------------------.

Black bead formationObserved:---------------

4) Test for Unsaturation: Carried out the

test for unsaturation.

i)Cold Aq. KMnO4 Test:

ii)Bromine water test:

i) Dischargeof pink colour.

Observed:------------------

ii)Discharge of brown colour.

Observed:-------------------

5) M.P/ B.P. :Determined the M.P./ B.Pof the compound.

M.P=.------------

B.P.= -------------

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6)Extra Element Tests:

a)FeSO4/H2SO4 test for

Nitrogen

b)AcOH/Pb(OAC)2 test for sulphur:

c)Nitroprusside test for sulphur

d) N+S combination test

e) Silver nitrate test for halogens:

f)Layer Test for Halogens:

g)Side chain halogen test:

a)Prussian blue colourationobserved:-----------------------

b)black ppt.

Observed:--------------------

c)Violet/pink colour

Observed:----------------------

d)blood red colourationobserved:-----------------------

e)White/yellow ppt.

Observed:---------------------.

F)Brown/violet colour in organic layerObserved:------------

g)white ppt.

Observed:------------------

Functional Group Analysis (forFUNCTIONALGROUPSNOTCONTAININGNITROGEN)

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6) Test for Carboxylic group:

a) Litmus test: To the soln of the comp.

added blue litmus paper.

b)Sodium bicarbonate test:To about 2ml

of cold saturated soln of sodiumbicarbonate in a test tube added a

small amount of O.C./aq. Solution of the

compound.

c) Distinction between mono and

dicarboxylic

acid(phenolphthalein/fluorescein

test):Took equal amounts of recorsinoland O.C. in a dry tt and and 1 drop of

conc. H2SO4 (to just moisten), fused

,cooled and transfered the contents to

exess of 10% NaOH in a beaker.

d) Special test for oxalic acid: Acidified

1ml soln.of OC with 2N H2SO4 then

warmed and added 2 drops of dil. KMnO4soln.

a)Blue Litmus to Red.

Observed:-----------------

b)Brisk effervescence due to evolution

Of CO2 gas.

Observed:---------------------

C)Green Fluorescence

Observed:-------------------

d)Discharge of pink colour.Observed:------------

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7) Test for the Carbonyl group:

a) DNP Test: TO~0.2mlof the organic

compound( or its solution in alc.) added 3

4ml of the DNP reagent( in water or alc.

depending upon the solubility of thecpd.)and allowed to stand for 5-10min.If

no ppt formed on standing then warmed

on the boiling water bath. Then, cooled.

b)Tollens test: To 0.2ml(or 2 drops) of

the organic cpd. added 2ml of Tollens

reagent in a clean t.t.(cleaned with conc.

HNO3 )If no reaction occured in cold then

warmed on the boiling water bath for `10min.

c)Fehlings solution test:To 0.2ml of cpd

added 3ml of fehling soln. And heated on

the boiling water bath for~5- 10 min.

d) Schiffs reagent test: To

2ml of the Schiffs reagent added 2 drops

of the organic compound

e) Iodoform test: In 2ml of water added a

pinch of KI then added Iodine (solid)toget

a saturated solns.,decantedAdded 2-3drops of the OC (if insoluble in water add

alc. to make it homogeneous.) Added 5%

of NaOH soln. Until,dark brown colour is

discharged.Allowed to stand for 3-4min.If

no ppt forms in cold, warmed on water

bath at 60.(removed excess of iodine by

adding dil NaOH soln).

8) TEST FOR PHENOLS:

a)Ferric chloride test: Took the OC or

soln.of 0.05g of the organic cpd.in 5ml of

water( if cpd is sparingly soluble ,preparedhot saturated aq. Solution and use 1ml of

the cold filtrate) added 1- 2 drops of

neutral 1%FeCl3 and shook the contents.

(If no ppt is obtained,repeated the sametest with ethanol as solvent in place of

water)

a)Yellow /Orange ppt.

Observed:------------------

b)Silver mirror along the walls of the test

tube.

Observed:------------------.

c)Red ppt

Observed:-----------------

d)i) instant pink colour.

Observed:-----------------

ii) pink colour on standing. 5min

observed:-----------------

e)Yellow ppt.in cold or on heating on a

water bath.

Observed:--------------------.

a)Blue/green/violet/brown ppt.Observed:----------------------

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b) Phthalein test: To a 0.5g of the organic

cpd.,in a dry test tube, added equal

volumes of phthalic anhydride and 1- 2

drops of conc.H2SO4 and fused. Cooled

the contents and added 4ml of 5% NaOHsolution, diluted with equal volumes of

water.

c) Libermann Test:

To a few crystals of NaNO2 in a dry test

tube added 0.5g of the

cpd. Heated gently for a few min.cool

then added 2ml of conc. H2SO4.

ii)Diluted carefully with water.

iii)Added ex.of NaOH solution.

9) Test for Ester group:

i)Hydrolysis test:

ii)Hydroxamic acid Test:(Fiegls test)

10) Test for Carbohydrates:

a) Molisch test:To ~ 1ml of very dilute

aqueous solution of the organic cpd. added

2- 3 drops of molisch reagent(10%

solution of napthol in alcohol) followedby equal volumes of conc.H2SO4 along the

sides of the test tub

b) Barfoeds Reagent test:(Distn. betn

mono/disaccharide)Heated the test tube

containing 1ml of reagent and 1ml of

dil.soln.sugar on a boiling water bath.

c)Rapid furfural test:

(distinction betn glucose and fructose)

d) TEST FOR REDUCING / NONREDUCING SUGAR:

i) Fehling solution test:

ii)Tollens Test:

i)Red colour/purple colourobserved:-----------------------

ii)Green fluorescence.

Observed:----------------------

i)Green/blue coloration.observed:-------------------------

ii)Red coloration.------------------observed:

iii)Color changes to green/ blue

observed:--------------

i)Disapperance of pink colour

Observed:---------------

ii)-----------colored ppt.

Observed:.--------------------------

Violet colouration at the junction of the

to layers.

Observed:---------------

Red ppt on heating for 2min.

Observed:------------------

Red coloured ppt.Observed:------------------------.

Silver mirror .

Observed:-------------------

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11) Test For Alcohols:a)Sodium Test:In a dry test tube

1ml of the cpd.+ CaSO4(anhy.) /Na2SO4.Decanted in another t.t. then added a

small piece of Na.

b)CerricAmmoniumNitrate test:0.5 ml

of the org. cpd.+ 2 3 drops of CAN

Brisk effervescence.

Observed:----------------------------.

Blood red colouration.

Observed:--------------

TESTS FOR NITROGEN CONTAINING FUNCTIONALGROUPS

12)T est for Primary Aromatic amine :

a)Azo Dye Test: 1ml of the cpd.in dil

HCl(t.t.-1), 2ml of 10%

aqueous solution of NaNO2( in t.t.-2) and

0.2g of - napthol in 4ml of 5% NaOH( in t.t.- 3 ) are cooled

simultaneously in ice bath(0- 5 ).

Transfered contents of t.t.-2 to t.t.- 1

dropwise with stirring allowed the

contents to stand for 3-4min,then added

those of t.t3 to the mixture.

Orange red coloured dye.

observed.:----------------------

13) Test For The Amide Group: a)To a0.5g of the organic cpd. Added 5ml of

10% NaOH solution and boiled.

Brought a rod dipped in conc. Hcl to the

mouth of the test tube.

b) Biuret Test For Urea:Heated a pinch of the organic compound

in dry china dish.

Added few ml of dilute NaOH solution

followed by a few drops of very diluteCuSO4 solution.

14) Test for Nitro group:

a)Mulliken Barker Test: Dissolved ~0.5g

of the organic cpd. in alcohol added

aqueous(2-3ml) CaCl2 or 0.5g of solid

Smell of ammonia .

Observed:-------------------

Dense white fumes.

Observed:-----------------------

Dense white fumes and smell of

ammonia.Observed:-----------------------.

Pink or violet colouration.Observed:-------------------------.

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ammonium chloride and a 0.5g of zinc

dust.

Boiled the contents and filtered.

To ~1ml of the filtrate added 2- 3 ml of the

Tollens reagent and warmed on a boiling

water bath. Grey or black ppt.or a Silver mirror.

Observed:---------------------

15) Probable Compound: The given compound contains----------------------------------------- functionalGroup/s

and has M.P./ B.P.---------------------------------, it could be

(i) ------------------------------ having Lit M.P. -----------------------.

(ii)----------------------------- having Lit M.P. -----------------------.

16) Preparation of Derivative:

Prepared a -------------------------- derivative of the compound.

Procedure of derivative prepration:

Name of the derivative is :------------------------------------------------------------ , it has M.P.=

------------------------------.Lt M.P. Of this derivative is = ---------------------------.

RESULT: The given organic compound was found to be --------------------------,it has M.P.=

--------------------------.Lit M.P. = ------------------. The M.P. of the -----------------------------

derivative is--------------------------------.Lit M.P.= ----------------------.

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Cpd_analysis Procedure 2011 Final

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