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Salt Analysis Procedure-1

Salt analysis of various cations nd anions

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0% found this document useful (0 votes)
49 views8 pages

Salt Analysis Procedure-1

Salt analysis of various cations nd anions

Uploaded by

AADHITHYA'S VIEW
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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G_eneral procedure for the systematic analysis of Simple salt (~EW 201SJ ·

Anions: Dil~acid group: col·,s 2·,N(?£ahd sol·


.cone.acid group: N03",CH3C00·, er, a·( and r

Special group: sol·, Pol· a~d C2ol·- , .

Cations:
Zero group: NH4+
Group I: Pb 2+
Group II: Cu 2•
Group Ill: .A1 3•,Fe 3• _.,,
Group IV: Zn 2•, Mn 2•, Ni2+
Group V: Ca2•,ea2•, sr2• · -•~··"
2
Group VI: Mg • · ' · ., -' ·- . _ .
·,
[ PbS04, BaS04, CaS04 and SrSO4 - will not be given f~r board, since they are,jn~el}:Jb!e salt_s J
. \ .;
·.. ,,:, 1
· EXPERIMENT , OBSERVATiON , .,
. 1. INFERENCE 7. I
Colour of the salt is noted White colour 2 3
Pb \Al \ -
i'
I
2
Zn + ,Ca • , Mg2• -,NH4 + sa Its
. 2
I
Bluish or bluish green colour Cui+ or Ni2+ salts
I
I
Light green colour Fe 2•,Ni2+ salts
!
Yellowish colour Fe3• salts
I
i ..
Light pink/ buff colour Mn 2+ salts
Smell of ammonia NH 4 • salt
2. Nature
Deliquescent nature er or No3·
(i) Amorphous . May be carbonate ·
(ii) Crystalline - May be nitrate,sulphate

u
3. and chlorides ·
Smell
On rubbing the salt give May he ammonium
characteristic ammonia carbon~te l
srriell . . J
4. 3. Action of heat
i) Colourless, odourless gas is evolved · .May be salt contains - -I
Pinch of salt is heated in a which turns lime water milky
dry test tube carbonate lon. '-- "'•, .-
..1
·
ii) Colourless Pungent gas turns May be salt contains
'
'{) acidifi~d Potassium dichr~mate sulphite ion.
paper m to green. ·I
I
I
iii) Reddish bro . d
May be sa_lt contains
I
. wn gas Is evolve ,
which turns f .
. errous sulfate solution nitrate iori.
into brown or bla k
C .

1
,
. zn2+
Residue is observed after· O> Yellow when hot, white
when cold. ,
heating Brown when hot, yellow ~
Pb 2+ '
~; ii) '\ I •

wheh cold.
Fe 3+ .
ill) ·
P ale brown changes to
·.. black.
Ni 2+
Iv) Green cha nges to yellow.
·' ,1 Residue is black i.n ~·otour. '.'
May be Cu~+, Fe 3+ Mn 2+,
v) \' Co z+ . · ·

D vi)" , oecrepitat.ing sound Lead nitrate


,' i; .. , or. barium
nitrate;· ·
'

Condensation of y,.,ater May be hydrated salts


vii)
vap<;> urs like copper sulfate,
nitrate etc,;
5. Flame test: i) Brick red ca2+
Crimson red Sr2+
Salt is mixed with cone. HCI ii)
Light gre-en/apple g_reen · Ba 2+
and made in to paste which is
subjected to flame test
iii)
iv} . Bltish green
·cu 2+ .,

v) · No characteristic colour Absence of th~ ·above


. ·. mentioned cations .
' . '
. •..
6 Solubility test: -·
Salt is added to water . i) Soluble May be nitrate, sulfate
and chloride salts
iiY· · Trisoiubre, May 6e carbonate; ..
sulfide and sulfite(except
Salt is treated with dill HCI Soluble i · • amm.carbonate).
May be carbonate or
.sulfite or sulfide
7. Ash test:
The salt mixture is made into a a] Green ash : May be zinc salt
paste with a few drops of dil b] Blue c!Sh · · , May be aluminium salt
HNO~ and· cobalt nitrate c] Pin~ ash ·J· May be magnesium salt
solution . The paste is taken in d] No c~aracteris_
tic change Absence of ,
a filter paper and burnt in the zinc,aluminium and
non-luminous flame.
magnesium salts
8. Charcoal cavity test:
May be zinc salt
A small amount of the mixture a] Green mass
is taken \ vith twice the
May be aluminium salt
amount of sodium carbonate b] Blue m~;s
in a charcoal cavity. Few drops
of H20 is added and bunseli May be magnesium salt
c] Pink mass
flame is blown till red hot and '.
few drops of cobalt nitrate
and again blow the Absence of
bunsenflame. zinc,aluminium and
d] No characte . : ·-'
nst1...::c..::c~ha~n~g~e:___ _ _....l....'..m.'...::::!ag~n.:.:e::s.:.:iu::..:..m:..:_:..sa_lt_s_ _ __

2
I'

Preparation of sodium carbonate extract: Tak~ _0.S g of the given salt a~d add Sg sodium carbonate
followed by 20 ml of distilled water and boil this content for about 10 m,_nutes and then filter. The
t
filtrate is used for the anion analysis and also for.the conffrmatorv teS '.
· . C)iroup -I anions.. · · ,: . , .
Anions idel)tified by uslng.dilute·HJO.,( cot, sot, No2· a,,d s2·J ·,

OBSERVATION INFERENCE
EXPERIM ~NT . . 2
i)Colourless, odourless gas is May be C03 ·,
9. Little salt is treated with dilute H2S04
and observed . released

Umewater turns milky. cot is confirmei.


.. ·..
( ·:
The liberated gas is passed thorough
:
limewater.
,

1~,
;May be SO/
The liberated gas is checked witH ii) ~olour~ mi,wW\'4
acidified pot dichromate and pot ga~s evo ve . .
Pink colour of pot. '
I. permanganate paper. '
Permanganate disappears sot is confirmed.
and dichromate paper turns
to green . ..
I
I I
I
iii) Reddish brown gas is IMay be No 2•

evolved

Ferrous sulphate solution N02is confirmed.


Gas is passed tho·ugh ferrous
turns to dark brown or black. ·-
sulphate solution. ·
·.,6 smell gas is May be s2·

Iv) Rott!'!:-
. '
- ~-_v1ved.
•''
:!
I

Lead acetate paper turns to s~·is confirmed.


, - ;_,..,c:r dl~u gas is ~hecked with lead silvery black. ·
acetate paper

7.,3.~e.r t~e· neutralisation of Sodium


s2·is confirmed.
Purple or violet colour
·carbonate ext"ractby using dil.HCI add formation. '
sodium nitroprusside solution.
Absence of CO/, SO/,
No characteristic change N02·and s2·..

3
· Group II anforis; ,'•,
\, '
,, 1

Identified by using cone, HaS04 (er, Br", r,.No,;, cH,coo·)


OBSERVATION INFERENCE

10.
EXPERIMENT
Little _salt is heated with c~nc. H2S04,
i)Colourless ga~ with May be er
pungent smell ·is evolved.
observed in cold and also after warming.
;

Add Mn0 2 and heat it


G.reenish yellow coloured May be er
gas is evol~ed. ·

Confirmatory test
Sodium carbonate extract is neutralize~ White curdy ppt, soluble er is confirmed.
byadding dill.HN03 till effervescence in excess of ammonium
ceases then AgN03 solution is added. hydroxide solution . .
I
'
ii)Violet vapours appear. May be r.
''

..
Violet vapourintensifies. · Maybe r. '
Add Mn0 2 and heat it. . Turns to blue-black May be·r.
... . •. '
Check the gas with starch paper. :·,

Confirmatory test Yellow precipitate is


Sodium carbonate extract is neutr_alized. -_,; __ - formed which is insoluble r is confirmed.
,.
by adding dill.HN0 3 till effervescence in excess of
ceases then AgN0 3 solution is added. amm.hydroxide
.

iii) Reddish brown gas is May be N0 3·, Br"


eVolved.
Reddish brown gas May be ·No3: ··
Add piece of copper turning .
intensifies. · ,

Reddish brown gas does May be Br-.


not intensify.
Confj_rmatory test for Br-
Sodium carbonate extract is neutralized Yellow precipitate is Br - is confirmed. · ··
by adding dill.HN0 3 till effervescence formed which dissolves in
ceases then AgN0 3 solution is added.
'
excess of amm.hydroxide
solution. '
((
, -~--:-·· _ ·_;..- A·~' .i,
r--confirmatorv test for Nos· · . ...
v Sodium carbonate extract is neutralized Brown ring is formed at NO3. is confirmed. (·

by adding dil H2S0 4 till all effervescence the junction of two


..
ceases then add freshly prepared F-eS0 4 .. liquids .
solut•on, then add con H2S04 through the
sides of the test tube.

Add about 1ml of ethyl alcohol. iv) .smell of vinegar. May be CH 3COO -

4
J' .

Pleasant odour.
CH3COO - ,s confirmed.
Confirmatory test
Sodium carbonate extract is neutralized Blood red colour solution
by adding dilHOtill all carbonates are. Is formed.
removed then add neutral FeC'3 solution. Red- br~wn precipitate Is CH3COO - ,s confirmed,
-- Heat the red colour solution. formed.
. No characteristic change. Abse'nce of er, r, N03-,
B(and CH3Coo-

Group Ill Anions ( S042·, PO/" and (COO)z2· or C2042· ions.

EXPERIMENT OBSERVATION
11 . 1.Sodium carbonate extract is INFERENCE -
A white ppt is obtained May be oxalate
neutralized with dilHCI then add 2 ml of
calcium chloride solution.

Add dil H2S0• to the above ppt then add
a drop of KMn0 4 solution and warm it.
The white ppt rema ins, the c20.2• is confirmed
pink colour of pot.
;
Permanganate gets
2. sodium carbonate extract is '
discharged. '
neutralized by adding dilHCl,-then White precipitate is 2
SO4 • is confirmed
barium chloride solution is·added ·f<>rmed, which remain
I insol11~le while adding dll.
I HCI .and dil. HN0 3
3. After the acidification or
neutralization of sodium carbonate Yellow precipitate is
extract using dil.HN0 3then add cone. formed
PO4 3- is confirmed
HN0 3 and add ammonium
molybdate.( heat gently if needed)
I

CATION ANALYSIS

Preparation of original solution for cation analysis: original solution is prepared by dissolving the salt in
any one of the following solvent. 1. Water 2.dil. HCl3. dil. HN0 3 4.conc. HCI. This is called 0 .5.
[prefer to use dil. HN0 3 if the substance is water insoluble]

EXPERIMENT OBSERVATION
0 INFERENCE
To the Salt addNa0H solution is Gas evolved turns moist red litmus Group O present.
added and heated. ·,
blue and gives dense white fumes lJH4+ may be present.
with glass rod dipped in conc.HCI .

Confirmatory test
Salt+· Na0H and heat, pass the Reddish brown precipitate. NH4+ is confirmed.
evolved gasthrough Nessler's
reagent.

5
original salt solution
IAdd dil.HCI vu)

White ppt [Presence of I group ]


r===7 Centnfuga_t,e
pass ga·S;. . . I
.I
Black ppt[ Presence of II group ]
Centrifugate
Boiled off excess H2S.Add two dr ps of conc.HN03.
Add NH 4CI solid, exces NH40H

Centrifugate
Gelatinous white ppt(Al 3+)[Presence of Ill group]
3
Brown ppt( Fe +) Pass H2S gas I.
2
White ppt (Zn +)
C~ntrifugate . •
Flesh colouredppt( Mn 2+) ( Presence of IV group ]
2
Black ppt( Nf+ or Co +) . :.
Boiled off excess H2S. Add NH4CI solid, excess NH40H and {NH 4 }2C03

Whiie ppt[ Ca 2+or Ba 2+ or sr2+]


Centrifugate·
[ Presence of V group )

2
Analysedfor ( Mg +)
[ Presence of VI group ]

EXPERIMENT .. • OBSERVATION · INFERENCE


2
I Confirmatory test for Pb + Pb 2+ may be present
Boil the pr·ec~p/ta~tt'i the distilled Precipitate dissolves
water and divide · two parts
l)Part I of the hot filtrate add Kl Pb2+ is confirmed.
solution. Yellow pre~ipitate is formed .
2)Part II of th~ hot filtrate add ·pb2+ is·c~'~firrried,
potassium chromate solution.
Yellow Precipitate

\
.6
,
.J
"

c·' II Confirmatory test for Cu 2•


Boil the precipitate with 5 ml of 50% Blue colored solution Is formed 2
Cu • may be present
nitric acid. ..
I
Divide the sol~tion in to two parts.
1) Part I add NH40H soln. little and then Pale blue ppt, dissolves in 2
Cu + Is confirmed.
in excess. excess of ammonium hydroxide
solution.
2)Part .LI add potassium ferrocyanide . Chocolate brown ppt. .,
Cu
2
• is confirmed
solution. i

Ill Confirmatory test for Al"~


Dissolve the pt with minimum quantity
of dill HCI and then and divide.in to two
parts. A white ppt formed whi~ti · Al 3+is confirm~d . .
1)To the first part aqd NaOH drop wise dissolves on adding excess of
NaOH.
2) To the second part add blue litmus A blue lake floating in clear AJ 3+ is confirmed.
solution then add NH40H solution. liquid is seen.

Confirmatory test for Fe .,.


Dissolve the brown ppt with dilHCI.

Then divide into three parts.
· 1) To the first part add potassium Blood red colouration Fe 3+ is confirmed.
thiocyana~ {KCNS)solution.
2 )To the second part addNaOH. ' '
Reddish brown ppt Fe 3+ is· confirmed. . ,.,
Solution. i

3) To the third part add Blue ppt Fe 3


+ is confirmed.
potassiumFerrocyanide solution. · I I

IV Conf!..rmato[}! test tor zn1 •


Dissolve the ppt with djlHCI, boil the
content to remove H2S. Cool and divide '
the solution in to two parts.
st
1) To the 1 part add NaOH drnp wise ~hite ppt forms which Zn 2• is confirmed.
and then in excess dissolves in excess of NaOH.
2)To the second part add 2
Bluish white ppt is formed. zn • is confirmed.
potassiumferro cyanide solution. ,
Conf!..rmatoQ!. test tor Ni2+
,.
Dissolve the ppt in minimum quantity
of aquaregia ana evaporate to dry
mass. Extract the residue with water.
Add 1-2 ml of Dimethylglyoxime (DMG) .
solution. Then add NH40H solution. A cherry red colouration. Ni2+ is confirmed.
Confi.rmato[}! test tor Mn2 •
Divide the buff ppt into two parts
1) Dissolve the 1st part in least quantity White ppt is formed, which
of dilHCI. Boil to expel H2S. Add NaOH slowly turns to brown on Mn 2• is confirmed.
solution drop wise. standing.
nd 2
2) Dissolve the 2 part in con HNOJ- Pink colour developed in Mn • is confirmed.
,:. Add 1 gm lead dioxide boil the content. solution.
Di1ute it with water.

7
Confirmatory test for Co 2• ·

Dissolve the ppt in minimum quantity Blue colour residue.


of aqua regia, and evaporate to dry Pink solution.
mass.extract the residue with water
and divide into 3 parts
l)To the first part add acetic acid till Yellow PPt is formed. Co
2
• is confirmed.
·become acidic then add KNO 2 solid and '
warm. , r .

nd
2)To the 2 part add 1ml amyl alcohol Formation of blue cpiour in the Co
2
+ is confirmed.
and 0.Sg of ammonium thiocyanate. · organic layer.

V Confirmatory test for Ca 2•,-sa 2•and Sr~ ·


Dissolve the ppt with hot acetic acid
and divide in to four parts.( you need to
check the cations in order till any one
cation gives positive test)
st
l)To the 1 part add pot.chromate.

nd
Yellow ppt•of barium chromate • Ba 2+ is confi tme\ t .
To the 2 part add dil HiSO4. is formed.
rd
White ppt is formed . Insoluble Ba 2• is., confirmed.
, 2)To the 3 _part add 1ml of in aff acid.
)

: . ~i~eral
.
' concentrated ammonium sulphate
solution and warm.
. Form~tion white ppt of Sr2• confirmed. is
th
strontium sulfate.
3)To the 4 part add 1ml of ammonium

.j
I oxalate solutiqn .. -.. . White pp~ is fo·rr.ed .
Ca
2
+ is confirmed.
PRvJ~;~~~9~y~di~~
J, .•
.
The whit~ dil~,£1~~~-t ::;:~-c.'J.i.,·::: · ·. . ! J • • - • ' }.\/<;!".: i
then add few drops of KMnO4 solution. - Pmk colour of KMnO 4 1s ea + is confirmed:
2
I
I 4)Perform flame test with the ppt. dist harged.
I :· A brick red flame. 2
ca • is cqnfirmed.
A crimson red flame Sr2+ is cohfirmed'.
I .A light green/apple green flame Ba2• is confirm~d.
! VI Confirmatory test for Mg2• : --;-----,------"--1
I Group VI p'resent.
To the above soluiton ofgroup V
l)To one part add ammonium
I phosphate or di sodium hydrogen White ppt is formed
phosphate solution+ 2ml of ethyl
alcohol. Scratch the inner wall of the
test tube with glass rod.
2) To the second part few drops of . Blue PPt is obtained Mg2+ is confirmed.
Magneson reagent followed'by drops
of NaOH.

R~sult:
The given salt contain the acid radical ------ and b •
The sa It ·1s --------.
a
• as,c radical -------.

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