|
SR NO |
EXPERIMENT |
SIGNATURE |
|
|
1 |
Identification and confirmation of unknown
compound (glucose) |
|
|
|
2 |
Identification and confirmation of unknown
compound (Sucrose) |
|
|
|
3 |
Identification and confirmation of unknown
compound (Starch) |
|
|
|
4 |
Identifications and confirmation of unknown organic
compound ( Alcohol ) |
|
|
|
5 |
Identification and conformation of unknown
organic compound Urea |
|
|
|
6 |
Identification and
Confirmation of Unknown Organic compound ( Thiourea) |
|
|
|
7 |
Identification
and Confirmation of unknown organic compound (Resorcinol) |
|
|
|
8 |
Identification
and Confirmation of unknown organic compound (Resorcinol) |
|
|
|
9 |
Determination of Carboxylic
acids (Oxalic acid) |
|
|
|
10 |
Identification
and confirmation of unknown organic Compound (CITRIC ACID) |
|
|
11 Identification and Confirmation of unknown organic
compound
Tartaric acid
DETERMINATION
OF SOLUBILITY CLASS
The
compound is said to be soluble in any solvent if it dissolve to the extent of
about 3% (0.1g/3ml). This is achieved by dissolving about 0.1g of solid
compound or 3-4 drops of liquid compound in gradual ling increasing of the
solvent up to 3ml with shaking.
FLOW CHART TO
DETERMINE THE GROUP OF SAMPLE
SAMPLE
Insoluble Soluble
|
·
Weak Acids |
· Strong Acids |
· Non Ionic |
· Ionic |
|
· Phenols |
· (C>6) |
· L5 Carbon |
· Carbon Polar Group |
|
|
· Phenols with e-with drawing group |
· Polar Group e.g: · LMW
aldehydes, ·
Ketones, ·
Aliphatic acids. |
e.g:
· Carboxylic acids, · Amines, · Carbohydrates. |
Insoluble Soluble
Cold B
Conc. Pri,
Sec,
Insoluble Soluble
I N
e.g: HMW alcohols
Aromatic aldehydes, ketones,
Aryl halides
ethers, estes
Discussion on Solvents
Water:
Water is polar solvent with a dielectric
constant equal to 80. It has the ability to form hydrogen bonding and can act
either as an acid or a base, therefore it can dissolve.
·
Salts of ammonium ion (RNH4+) or organic acid salt
with alkali metal cations (RCOO-).
·
Ionic compounds.
·
Polar compounds “like dissolves like”.
·
Organic compounds with low molecular weight (<5 carbon atoms) such as
alcohols, aldehydes, ketones and carboxylic acid.
Water is the first solvent used to determine
the solubility class of a compound. If the compound is the water solvent the
next step is to test its solubility in ether.
Ether:
Ether is a non-polar solvent having a
dielectric constant of 4.3. It cannot form hydrogen bonding, therefore it
differs from water in that it cannot dissolve ionic compound such as salts. It
dissolve most water insoluble compounds, therefore, in the determination of
solubility class, the importance of ether is for water soluble compounds only
and no further solubility tests using the remaining solvents are to be done.
According two probability is there.
1.
Compounds soluble in both water and ether.
These compounds
·
Are non-ionic.
·
Contain 5 or less carbon atoms.
·
Contain an active group that is polar and can form hydrogen bonding.
·
Contain only one strong polar group.
2.
Compounds soluble in water only ( but not in ether)
These compounds
·
Are ionic.
·
Contain two or more polar groups with no more than 4 carbon atoms for
each polar group.
This group is classified as S2
Class and includes ionic salts such as salts of Carboxylic Acid, Amines and
Compounds with more than 1 active group such as Poly Hydroxylated compounds and
Carbohydrates.
Note that solubility in ether is tested only
for water soluble compounds. For water
insoluble compounds (carboxylic acids) and phenols with electrons withdrawing
groups (e.g. NO2). Protons are weakly attached and can be given
easily.
Compounds
soluble in 5% Sodium Hydroxide solution only. This group is given class A2
and it includes Phenols, amides and Amino Acid (Weak acid).Use the left side of
the solubility classification scheme i.e. Test solubility in Sodium Hydroxide
rather than ether.
5% NaOH and 5% NaHCO3:
Water insoluble compounds must be tested first
in 5% NaOH solution which is a basic solvent. It reacts with water insoluble
compounds that are capable of donating protons such as strong and weak acids.
The stronger the acid the weaker the base. It can react with water insoluble
compounds that dissolve in 5% NaOH solution must also be tested for solubility
in 5% NaHCO3 solution. Therefore, for water insoluble acidic
compounds NaOH solution is considered as a detecting solvent whereas Sodium
Bicarbonate solution is called as Sub classified solvent since it can react
with strong acid only. That is these two solvents give an idea about the
acidity degree of the compound. Note the testing solubility in 5% NaHCO3 solution
is not needed if the compound is insoluble in 5% NaOH solution, but rather, 5%
HCl would be used two possibilities are there.
1.
Compounds soluble in both bases.
2.
This group is given class A. This class includes strong acids that have
the ability to react with the weak bases.
5% HCl:
If the compound is insoluble in water and
sodium hydroxide solution, this means that the compound is not an acid but is
either a base or a neutral compound. 5% HCl which can dissolve base such as
amines is used for such a compound. If compound is soluble in the solvent, than
it is given class B. It includes primary, secondary and tertiary amines.
Cold Concentrated H2SO4:
If compound is insoluble in water 5% NaOH and
5% HCl, Solubility in cold conc. H2SO4 should be tested.
If compound is soluble in this acid it belongs to class N which includes
neutral compounds such as hi molecular weight alcohols, aldihides, ketones,
esters and ethers and unsaturated hydrocarbons compounds that are insoluble in
cold conc. H2SO4 being to class I which includes inert
aliphatic ( saturated) hydrocarbons, aromatic hydrocarbons, hyloalkanes and
aryl halides.
Experiment
No. 1
Identification and confirmation of unknown compound
(glucose)
|
Analysis |
Observations |
Inference |
Physical state and Odour:
|
1-Physical
state 2-Odour |
Colorless
and crystalline solid. Odorless |
Carbohydrates,
Acids, Phenols and amides may be present. Carbohydrates
may be present. |
Solubility Determination:
|
3-Solubility
in water 4-Solubility
ethyl acetate |
Soluble Insoluble |
Aliphatic,
carbohydrate acids may present May be
aliphatic compound |
Ignition test:
|
5-Heat
the compound cusible lid |
Chary
and non smoky flame |
Carbohydrates
are present |
Test for saturation and
unsaturation:
|
6-Compound+
KMnO 4 7-Compound+
Bromine water solution |
No
decolourization of pink colour No
colourization |
Saturated
compounds are present Saturated
compound present |
Test for acidity and basicity:
|
8-pH
test |
pH show
neutral pH |
Aliphatic
acidic compound |
Functional group determination:
|
9-Compound + glacial acetic acid +
Conc.H2SO4 and heat 10-compounds + Alcohol + 2,4-DNPH+ heat for
few min. 11-compound + NaOH +heat 12- compounds +few drops of NaOH + few
drops of phenylalanine 13-compond+NaHCO3 14-compound+ C2H3OH +conc.H2SO4+heat 15-compound+ conc.H2SO4 + heat 16-compound + 3-4 drops of 1%
alk-d-naphthol+ conc.H2SO4 |
No fruity smell of ester formation No yellow crystals on cooling No smell of ammonia Pink colour is not discharged No differences No fruity smell of esters Charring and blackening Reddish violet ring formation at junction |
Alcohols are absent Aldehydes\Ketones absent Amides, thioamides and ammonium salt of
carboxylic acids are absent Ester are absent Carboxylic acids are absent Carboxylic acids are absent Carbohydrates are indicated Carbohydrates are indicated |
Confirmatory test :
|
17-
compound +Fehling’s solution 18-
compound + copper acetate in diluted acetic acid 19-compound+3-4
drops of 1% Alk-d-naphthol + conc. H2SO4 |
Reddish
brown ppt Copper
acetate is reduced Reddish
violet ring formation at junction |
Glucose
is indicated Glucose
is confirmed Glucose
is confirmed |
Melting point determination:
|
20- Observed M.P 21- literature M.P |
146 C 146 C |
Glucose is present Glucose is present |
Result:
The given
compound is found to be glucose.
C6H12O6
EXPERIMENT : 2
Identification & confirmation of unknown
Organic compound (Sucrose)
|
Analysis |
Observations |
Inference |
Physical state
|
|
Physical state |
Crystalline Solid |
Carbohydrates, acids phenol & amide present, Carbohydrates and acid may be present |
|
|
Colour |
Colorless |
|
|
|
Odor |
Odorless |
Solubility Determination
|
|
Soluble in the water |
Soluble |
Aliphatic carbohydrates acids may be present |
|
|
Solubility in ethyl acetate |
Insoluble |
May be aliphatic compounds |
Ignition test
|
|
Heat the compound |
Charring & non Smoky flame |
Carbohydrates or hydroxyl compound present |
Test for Saturation/ Un-saturation
|
|
Compound + Al. KMnO4(s) |
No decolorization of pink colour |
Saturated compound are present |
|
|
Compound + bromine water(s) |
No Decolorization |
Saturated compound present |
Test for Acidity & Basicity
|
|
pH Test |
pH paper show neutral pH = 7 |
Neutral compound may be present |
Functional group Detection
|
01 |
Compound +glacial acetic acid+Conc.H2SO4+heat |
No fruity smell of ester formation |
Alcohols are absent |
|
02 |
Compound+alcohols+2,4DNPH(s)HEAT |
May be yellow crystals on cooling |
Aldehydes/ ketones may be present |
|
03 |
Compound+C2H5OH+Conc.H2SO4
and heat |
No fruity smell of ester formation |
Carboxylic acid are not present |
|
04 |
Compound + NaOH(s)+Heat |
No smell of ammonia |
Amides, ammonium salt of carboxylic acid
are present |
|
05 |
Compound + few drops of NaOH + few drops of
phenophthalen |
Pink colour is not discharge |
Esters are absent |
|
06 |
Compound+NaHCO3(s) |
NO efference |
Carboxylic acids are not present |
|
07 |
Compound+Conc.H2SO4+heat |
Charing & blackening |
Carbohydrates are indicated |
|
08 |
Compound+C2H5OH+Conc.H2SO4+heat |
No fruity smell of ester formation |
Carboxylic acids are present |
Confirmatory test
|
01 |
Compound +
feling’s (s) |
NO colourization |
Sucrose is indicated |
|
02 |
Compound +CuSO4+NaOH |
Blue colour |
Sucrose is confirmed |
Melting point Determination
|
01 |
Observe Melting Point |
160oc |
Sucrose is confirmed |
|
02 |
Litrature value |
160oc |
Sucrose is confirmed |
Result
The Given Sample was formed to be Sucrose.
Structure C12.H22.O11
EXPERIMENT: 3
Identification &
Confirmation of Unknown Organic Compound (Starch)
|
Analysis |
Observations |
Inference |
Physical state & Odor
|
1. Physical state & colour |
Colorless & Crystalline solid |
Carbohydrates & phenols & amides |
|
2. Odor |
Odor less |
May be present. Carbohydrates & acid may be present. |
Solubility determination
|
1. Solubility in distilled water |
Insoluble |
Aliphatic carbohydrates may be present |
|
2. Solubility in Ethyl acetate |
Insoluble |
May be Aliphatic compounds |
Ignition test
|
1. Heat the compound on curable lid |
Charring & neon smoky flame |
Carbohydrates of hydroxyl acid may be
present |
Test for
Saturation/Unsaturation
|
1. Compound + Alc KMnO4 |
No decolorization of pink colour |
Saturated compounds are present |
|
2. Compound + Br water solution |
No decolorization of pink colour |
Saturated compounds are present |
Test for acidity basicity
|
1. pH test |
pH paper show neutral pH |
May be aliphatic may be neutral compound
present |
Functional group Detection
|
1. Compound + glacial acetic acid + conc.H2SO4 + heat |
No fruity smell of ester formation |
Alcohols are absent |
|
2. Compound + alc + 2,4-DNPH + heat for few minutes |
No yellow crystals on heating |
Aldehyde , Ketones absent |
|
3. Compound + NaOH + heat |
No smell of ammonia |
Amides, Tridamides , salts of Carboxylic
acid are absent |
|
4. Compound + few drops of NaOH + few drops of phenolphthalein |
Pink colour is not discharged |
Esters are absent |
|
5. Compound + NaHCO3 |
No effevercense |
Carboxylic acids are absent |
|
6. Compound + C2H5OH + Conc. H2SO4 & heat |
Ni fruity smell of esters formation |
Carboxylic acids are absent |
|
7. Compound + 3-4 drops of 1% alkaline α-naphtol +Conc. H2SO4 |
Reddish violet ring formation at the junction |
Carbohydrates are indicated |
Confirmatory Test
|
1. Compound + Iodine |
Iodine solution turns blue |
Starch is confirmed |
|
2. Compound +HCL + Heat |
Soluble |
Starch is confirmed |
Result
The given compound is found to be
starch.
Structure
- (C 6H 10O 5) n-
Experiment # 4
Identifications
and confirmation of unknown organic compound ( Alcohol )
|
Analysis |
Observations |
Inference |
Physical
state &odor
|
Physical state |
Colorless liquid |
Phenol , Amides & Alcohol |
|
odor |
Strong
smell |
Alcohol
may be present |
Solubility
Determination
|
Solubility in distilled water |
Soluble in water |
Due to polar nature |
|
Solubility in ethyl acetate |
Insoluble
|
Due
to absence of h-bonding |
Ignition
test :
|
Heat the compound on curable acid |
No Charming |
Alcohol may be present |
Test for
saturation / unsaturation
|
Compound + Br water solution |
No decolorization of pink color |
Saturated compounds may be present |
Test for
acidity and basicity
|
Ph test |
Litmus paper show both acidic and basic ph |
Aliphatic compounds may be present |
Functional
group detection
|
|
|
|
|
1.compound +
alc+2,4-DNPH+heat for few minutes |
No
yellow crystals on heating |
Aldehydes,
Ketones absent |
|
2.Compound + NaOH+heat |
No
smell of ammonia |
Amides
, Triamides,salts of Carboxyl acid are absent |
|
3.compound + few drops of
NaOH +few drops of phenolphthalein |
Pink
color is not discharged |
Esters
are absent |
|
4.Compound + NaHCO3 |
No
effervescence |
Carboxyl
acids are absent |
|
5.Compound + C2H5OH |
No
fruity smell of esters |
Carboxyl
acids are absent |
|
6.Compound + glacial
acetic acid |
Fruity
smell of ester formation |
Alcohol
are present |
Lucas Test
Primary, secondary and tertiary alcohols
are identified by reacting them with conc.HCL in anhydrous ZNCL2.An oily layer
of alkyl halides is formed.
1) Tertiary
alcohols will form layer immediately
2) Secondary alcohols will for layer in 5
to 10 minutes
3) primary will form layer only on heating.
|
Primary alcohol |
oxidation |
It gives Aldehydes |
|
Secondary alcohol |
oxidation |
It
gives ketone |
|
Tertiary alcohol |
No
oxidation |
It
gives alkenes |
CONFIRMATORY TEST:
|
Iodoform test: Used to distinguish
between ethanol and methanol. |
ethanol |
It will form yellow ppt |
|
|
Methanol |
It
will not form yellow ppt |
RESULT
The given compound is alcohol
(ethanol/methanol)
STRUCTURES:
ETHANOL METHANOL
C2H6O CH3OH
EXPERIMENT
# 5
Identification and conformation of unknown organic compound
Urea
|
Analysis |
Observation |
Inference |
Physical State and Odour
|
Physical state and odour |
Colourless
and Crystaline Solid |
Carbohydrates
amides acids and phenol may be present |
|
Odour |
odourless |
Carbohydrates
acid and phenol may be present |
|
|
|
|
Solubility Determination
|
Solubility
in D-water |
Soluble
|
May
be aliphatic compound |
|
Solubility
i Ethyl acetate |
insoluble |
May
be aliphatic compound |
Ignition Test
|
Heat
compound crucible lid |
Non
smoky flame |
Aliphatic
compound may be present |
Test for saturation/unsaturation
|
Compound
+ alcohol sol |
No decolouration of pink colour |
Saturated
Compounds are present |
|
Compound+Br2
water soloution |
Decolouration
|
Saturated
compounds are present |
Tests For acidity/basicity
|
PH
test |
PH
remains unaffected PH 8 |
Aliphatic
compounds |
Functional group
detection
|
Compound
glacial acetic acid+concH2S04 and heat |
No
fruity smell ester formation |
Alcohols
are absent |
|
Compound
+ alcohol=2,4DNPH sol+heat for few minutes |
No
red yellow or orange crystals o cooling |
Aldehydes
and ketones are present |
|
Compound
+ FeCl3 sol |
No
violet colur appears |
Phenols
are absent |
|
Compound
few drops of NaOH+ few drops of phenolphthalein sol |
Pink
colour isn’t discharged |
Esters
are absent |
|
Compound+NaHCo3
sol |
No
effervesces |
Carboxylic
acid are absent |
|
Compound+C2H5OH+conc
H2S04 + Heat |
No
charring No blacking |
Carbohydrate
are absent |
|
Cmpound+Naoh sol heat |
Amonia evolved on heating |
Amides Thio amides ammonium salts of carboxylic
acids are present |
Confirmatory Test
|
|
|
|
|
|
|
|
Result
The
given compound is urea
Structure
Experiment# 06
“Identification and Confirnmation of
Unknown Organic compound ( Thiourea)
|
Analysis |
Observation |
Inference |
Physical State and odour
|
|
Physical
state |
Colorless
& crystalline solid |
Carbohydrate,acids,phenol,amides
may be present |
|
|
Odor |
Odorless |
Carbohydrate,acids,phenol,amides
may be present |
Solubility
determination
|
|
Solubility
in D- water |
Soluble |
May
be Aliphatic Compound |
|
|
Solubility
in ethyl-acetate |
Insoluble |
May
be Aliphatic Compound |
IGNITION TEST
|
|
Heat compound on crucible lid |
Non-Smoky flame |
Aliphatic compound may be present |
Test for
saturation/unsaturation
|
|
Compound+ Alkaline Kmno4 |
No de-colorization of pink color |
Saturated Compound Present |
|
|
Compound+ Br.H2O Solution |
No de-colorization |
Saturated Compound Present |
Test for acidity/ Basicity
|
|
PH test with compound |
PH remains Neutral |
Aliphatic neutral compound |
FUNCTIONAL GROUP DETECTION
|
|
Compound+ Glacial acetic acid+ conc.
H2SO4+heat |
No fruity smell of ester formation |
Alcohols Absent |
|
|
Compound+Alcohol+2,4 DNPH Sol+ Heat for
few minutes |
No yellow/orange or red crystals |
Aldehydes/Ketones are absent |
|
|
Compound+C2H9OH+conc.H2SO4+Heat |
No fruity smell of ester |
Carboxylic acid is absent |
|
|
Compound+Fecl3 sol |
No violet color |
Phenols are absent |
|
|
Compound+ NaOH+ few drops of
Phenolphthalein sol |
Pink color not discharged |
Esters are absent |
|
|
Compound+NaHCO3 sol |
No efferscence |
Carboxylic Acid absent |
|
|
Compound+conc.H2SO4 |
No charring and no Blackening |
Carbohydrate are absent |
|
|
Compound+ NaOH sol+ Heat |
Ammonia evolved on heating |
Amides,thioamides or ammonium salts
R–COOH Present |
Confirmatory test
|
|
Heat the compound to melt and then cool |
Blood red coloration |
Thiourea is Confirmed |
Structure:
Result:
“The given Compound was found to be Thiourea”
Experiment # 7
Identification
and Confirmation of unknown organic compound (Resorcinol)
|
Analysis |
Observation |
Inference |
|
Physical
State and Odor |
||
|
Physical
state and odor. |
Brownish
solid with green fluorescence. Carbolic odour. |
Carbohydrates,
acid, phenol, or amide may be present. |
|
Solubility Determination |
||
|
Solubility
in D water |
Soluble |
Aliphatic
acids and polyhydric phenols may be present. |
|
Solubility
in ethyl acetate |
soluble |
May
be aliphatic compound. |
|
Ignition Test |
||
|
Heat
compound on Crucible lid |
Charring and non-smoky flame |
Carbohydrates or hydroxy acid may be
present. |
|
Test
for Saturation/Unsaturation |
||
|
Comp.
+ Alc.KMnO4 solution |
No
decolorization of pink color |
Saturated
compounds are present |
|
Compound +Bromine water |
No decolourization |
Saturated
compounds are present |
|
Test for Acidity/Basicity |
||
|
pH
test |
litmus paper turns red |
Aliphatic
acid Comp are present |
|
Functional
Group |
||
|
I.
Comp |
No
yellow crystals on cooling |
Aldehydes
/ ketones are absent |
|
II.
Comp + FeCl3 sol |
violet color appears |
Phenol
is present |
|
III.
Comp + Conc H2SO4 +heat |
No
changing and blacking |
Carbohydrates
are absent |
|
IV.
Compound + few drops of H2SO4 + few
drops of phenophthalein |
Pink
color is not discharged |
Esters
are absent |
|
V.
Comp + glacial acetic acid + Conc H2SO4
and heat |
No
fruity smell of ester formation |
Alcohol
is absent |
|
VI.
Compound + NaHco3 solution |
No Efferance |
Carboxylic
acid is absent |
|
VII.
Compound + Conc H2SO4 and Heat |
No
Charring and Blackening |
Carboxylic
acid is absent |
|
Confirmatory
Test |
||
|
·
aq.
Sol. Of compounds + conc. H2SO4 + NaNO3 |
Green,
blue or violet colour |
Resorcinol
is present |
|
·
compound
+ CHCl3+ NaOH+ Heat |
Red
solution with green fluorescent |
Resorcinol
is present |
|
·
compound
+ oxalic acid + H2So4 |
Blue ring at the juction |
Resorcinol
is Present |
Melting Point Determination
|
Observed
melting point Literate Melting point |
118 C |
Resorcinol is confirmed |
Result
The given organic compound was found to be
Resorcinol
Structure
Experiment # 8
Identification and Confirmation of unknown organic
compound (Resorcinol)
|
Analysis |
Observation |
Inference |
|
Physical
State and Odor |
||
|
Physical
state and odor. |
Brownish
solid with green fluorescence. Carbolic odour. |
Carbohydrates,
acid, phenol, or amide may be present. |
|
Solubility Determination |
||
|
Solubility
in D water |
Soluble |
Aliphatic
acids and polyhydric phenols may be present. |
|
Solubility
in ethyl acetate |
soluble |
May
be aliphatic compound. |
|
Ignition Test |
||
|
Heat
compound on Crucible lid |
Charring and non-smoky flame |
Carbohydrates or hydroxy acid may be
present. |
|
Test
for Saturation/Unsaturation |
||
|
Comp.
+ Alc.KMnO4 solution |
No
decolorization of pink color |
Saturated
compounds are present |
|
Compound +Bromine water |
No decolourization |
Saturated
compounds are present |
|
Test for Acidity/Basicity |
||
|
pH
test |
litmus paper turns red |
Aliphatic
acid Comp are present |
|
Functional
Group |
||
|
VIII.
Comp |
No
yellow crystals on cooling |
Aldehydes
/ ketones are absent |
|
|
IX.
Comp + FeCl3 sol |
violet color appears |
Phenol
is present |
|
|
X.
Comp + Conc H2SO4 +heat |
No
changing and blacking |
Carbohydrates
are absent |
|
|
XI.
Compound + few drops of H2SO4 + few
drops of phenophthalein |
Pink
color is not discharged |
Esters
are absent |
|
|
XII.
Comp + glacial acetic acid + Conc H2SO4
and heat |
No
fruity smell of ester formation |
Alcohol
is absent |
|
|
XIII.
Compound + NaHco3 solution |
No Efferance |
Carboxylic
acid is absent |
|
|
XIV.
Compound + Conc H2SO4 and Heat |
No
Charring and Blackening |
Carboxylic
acid is absent |
|
|
Confirmatory
Test |
|||
|
·
aq. Sol.
Of compounds + conc. H2SO4 + NaNO3 |
Green,
blue or violet colour |
Resorcinol
is present |
|
|
·
compound
+ CHCl3+ NaOH+ Heat |
Red
solution with green fluorescent |
Resorcinol
is present |
|
|
·
compound
+ oxalic acid + H2So4 |
Blue ring at the juction |
Resorcinol
is Present |
|
Melting Point Determination
|
Observed
melting point Literate Melting point |
118 C |
Resorcinol is confirmed |
Result
The given organic compound was found to be
Resorcinol
Structure
ExPeriment
# 9
Determination of Carboxylic acids (Oxalic acid )
|
Analysis |
Observations |
Inference |
Physical test and Odour:
|
Physical state and Adour Odour |
Colourless
solid crystalline Odourless |
Carbohydrate,
acid, Phenol,
amide may be present. Carbohydrate
and acid may be present. |
Solubility Determination:
|
Solubility in distil water Solubility
in ethyl acetate |
Soluble
soluble |
Aliphatic
carbohydrates Acid
and hydrated may be present. May
be diphatic hydrated compound. |
Ignition
Test:
|
Heat
the compound In
spatula |
Non-luminous
flame |
Aliphatic
compound With
low % of carbon. |
Test for
saturation and unsaturation:
|
Compound +alkaline KMnO4 Compound
+ Bromine water |
No
decolourization of pink colour. No decolourization |
Saturated
compound are present. Saturated
compound may be present. |
Test for
basicity and acidity:
|
Ph
test |
Blue
litmus paper turned red |
Aliphatic
acidic compound are present. |
Functional
group testing / detection :
|
Compound + conc. H2SO4+ heat. Compound + alcohol+2,4- DNPH+ heat Compound + FeCl3 Compound + glacial acetic acid + conc.
H2SO4+ heat Compound +few drops of naphthalene solution Compound + NaOH solution + Heat Compound + NaHCO3 Compound + ethanol+ conc. H2SO4+ heat |
No
blackening No
yellow crystals formed on cooling No
violet colour appears No
fruity smell of ester pink
colour is not discharge No
smell of ammonia Evolution
of carbon dioxide Fruity
smell of ester formation |
Carbohydrates
absent. Aldehydes
and ketones are present. Phenols
are absent. Alcohols
are absent. Esters
are absent. Ammonia,
Thioammonia and ammonia salts of carboxylic acid are present. Carboxylic
acids are present. Carboxylic
group are present. |
Confirmatory
tests:
|
Compound + calcium chloride solution Compound
+ conc. H2SO4+ heat Compound + ferric chloride |
White
ppts No
blackening No
reaction |
Citric
acid and oxalic acid are indicated. Tartaric
acid is absent. Oxalic
acid is confirmed. |
Melting
point test:
|
Melting
point |
|
Oxalic
acid is confirmed. |
Experiment# 10
Identification and
confirmation of unknown organic Compound (CITRIC ACID)
|
Analysis |
Observation |
Inference |
Physical
State and odor
|
|
Physical
state |
Colorless
& crystalline solid |
Carbohydrate,acids,phenol,amides
may be present |
|
|
Odour |
Odourless |
Carbohydrate,acids,phenol,amides
may be present |
Solubility determination
|
|
Solubility
in D- water |
Soluble |
May
be Aliphatic Compound,Carbohydrates,acids |
|
|
Solubility
in ethyl-acetate |
Insoluble |
May
be Aliphatic Compound |
Ignition
test
|
|
Heat compound on crucible lid |
Charring, Non-luminous flame |
Aliphatic compound with low % of carbon
may be present |
Test for
saturation and unsaturation
|
|
Compound+ Alkaline Kmno4 |
No de-colorization of pink color |
Saturated Compound Present |
|
|
Compound+ Br.H2O Solution |
No de-colorization |
Saturated Compound Present |
Functional group detection
|
|
Compound + Glacial acetic acid+ conc.
H2SO4+heat |
No fruity smell of ester formation |
Alcohols Absent |
|
|
Compound+Alcohol+2,4 DNPH Sol+ Heat for
few minutes |
No yellow crystal encoding |
Aldehydes/Ketones are absent |
|
|
Compound+conc.H2SO4+Heat |
No charring and no blackening |
Carbohydrate are absent |
|
|
Compound+NaOH+Heat |
No smell of ammonia |
Amides are absent |
|
|
Compound+ NaHCO3 |
Effervesces(evaluation of CO2) |
Carboxylic Acid are present |
|
|
Compound+ ethanol+conc.H2SO4+Heat |
Fruity smell of ester formation |
Carboxylic Acid are present |
Confirmatory test
|
|
Compound+CaCl2 sol |
White ppt |
Citric acid and oxalic acid are
indicated |
|
|
Compound+conc.H2SO4+Heat |
No blackening occur |
Tartaric Acid are absent |
|
|
Compound+NaOH+Fecl3 |
Buff Coloration |
Citric Acid confirmed |
Melting point determination
|
|
Observed Melting Point |
100C° |
Citric Acid is confirmed |
|
|
Literature value |
100C° |
Citric Acid is confirmed |
Result:
“The given compound was found to be Citric
Acid”
Structure :
Citric acid
Experiment # 11
Identification
and Confirmation of unknown organic compound Tartaric acid.
|
Analysis |
Observation |
Inference |
|
Physical
State and Odor |
||
|
Physical
state and odor. |
Odorless
and crystalline solid. |
Carbohydrates,
acid, phenol, or amide may be present. |
|
Solubility Determination |
||
|
Solubility
in D water |
Soluble |
Aliphatic
carbohydrates acid hydratic compound |
|
Solubility
in ethyl acetate |
Insoluble |
May
be aliphatic dehydrated compound. |
|
Ignition Test |
||
|
Heat
compound on Crucible lid |
No-Luminous
flame |
Aliphatic
compound with 1000% age of 07 carbon |
|
Test
for Saturation/Unsaturation |
||
|
Comp.
+ Alc.KMnO4 solution |
No
decolorization of pink color |
Saturated
compounds are present |
|
Test for Acidity/Basicity |
||
|
pH
test |
Blue
litmus paper turns blue |
Aliphatic
acid Comp are present |
|
Functional
Group |
||
|
XV.
Comp |
No
yellow crystals on cooling |
Aldehydes
/ ketones are absent |
|
XVI.
Comp + FeCl3 sol |
No
violet color appears |
Phenol
is absent |
|
XVII.
Comp + Conc H2SO4 +heat |
No
changing and blacking |
Carbohydrates
are absent |
|
XVIII.
Compound + few drops of H2SO4 + few
drops of phenophthalein |
Pink
color is not discharged |
Esters
are absent |
|
XIX.
Comp + glacial acetic acid + Conc H2SO4
and heat |
No
fruity smell of ester formation |
Alcohol
is absent |
|
XX.
Compound + NaOH solution +heat |
No
smell of ammonia |
Amides,
Triamides, Ammonium Salt of Carboxylic acid is absent |
|
XXI.
Compound + NaOH solution |
Efferance |
Carboxylic
acid is present |
|
XXII.
Compound |
Fruity
smell of ester formation |
Carboxylic
acid is absent |
|
Confirmatory
Test |
||
|
·
Compound + CaCl solution |
No
white ppt. |
Citric
acid is absent |
|
·
Compound + Conc H2SO4 and Heat |
Blackening |
Tartaric
acid is present |
|
·
Compound + FeCl3 solution |
Reaction
occurs |
Oxalic
acid is absent |
Result
The given organic compound was found to be
tartaric acid.
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