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Salt Analysis

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0% found this document useful (0 votes)
29 views17 pages

Salt Analysis

Uploaded by

rahulharsh326
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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Bat<

indicated
Srt Cat indicated
indicated
indicated
Indicated indicated
Na indicated
K
Cut
+2
by
surrounde
time
yellow
short
flameflame
golden for blue
flame
colourgreenred flame
green
Crimson
red
Immense
yellow Persistent
VioletApple Brick
(ii) (i) (iv) (v) (vi)
(i)
by in it heating
volatile the
bunsen
HCIwiretouching
observe
form platinum
Conc. andof
andsaltflamneflame.
colour
of
with
salts
Flame
test theHCIgiven and
chlorides the
Certaindipping burner
conc.
within
it
3.
Cut indicated
() Blue or bluish green
(ii) Green
Nit indicated
Fet indicated
(i) Light green
(iv) Dark brown
Fet indicated
Co+2
Cot indicatd
(v) Rose red
(vi) Light pink Mrt2 indicated
P6+2 As+3 Cort2
(vii) White
A+3,Zntcat2
+2
sr2 , Mgt2
Bat2,
() Vinegar CH,C00*
No. S.
1.

dil. Take
HTSO4.
little a

Warm saltH,SO4
Dilute
test
Experiment
in (A)
if
nodry a
Preliminary
reaction test

tube
occurs.
and
add
Tests
(iv) (iii) (ii) (i)
acetate
rownblack.
paper
Colourless
acidified
of Colourless Colourless,
smell milky.
effervescence, for
rotten
gas of
Anions
KCrz0;
eggs gas
ving sulphur gas Observation
odourless
which with turns
. ent paper with (Wet
having which
turns suffOcating lime
green. with
gas
Tests)
mell turns water
leadsmell

Inference
NO2 SO2 So co,
Conc. HzS04 test
Take a little salt in test (i) Colourless pungent smelling gas CI
tube and add conc.H,SOA evolved which gives dense white
and heat. fumes with rod dipped in NHOH.
(iü) Yellowish brown gas having pungent Br
smelland turns starch paper yellow.
(ii) Brown coloured gas evolved which NO3
turns FeSOa solution dark brown.
(iv) Violet vapours turn starch paper blue.
(v) Colourless vapours having smell of CH3C00
vinegar.
(vi) Colourless gas with no smell and Cz04
burns with blue flame.
(vii) No gas evolved. CI, Br, I, NO3, SO4
C,Oa2 absent.
CH,CO0,Cz04
Nootan /SC Chemistry Lab Manual XI|
[43)
S. No. Test
Observation Inference (Presence of)
1. Test for carbonate (CO)
(a) Take a little salt in a test tube, add distilled|Salt insoluble in water. Insoluble CO3 2
water and shake.
(b) Treat the residue with dil. HCI. CO, gas evolved which turnsInsoluble CO3 2 present
lime water milky
(c) To onepart of the aqueous solution, add MgS04| White precipitate. Soluble CO
solution. confirmed

(d) Add phenolphthalein to another part of aqueousPink colour Soluble CO


solution. confirmed

(e) To another part of aqueous solution add dil.CO> gas evolved which turns Soluble CO
lime water milky. confirmed
HzSO4.
(SO,)
ConTimed confirmed irm
Contirmedcontirmed
NO3 yellowCI CI
isC
evolved,|
solution conc.HNO3
but iodide soluble
smell,
which
pungent formed
greenish
starch
moist
turns
FeSO, formed
fumes NHaOH.
in
soluble solution.
is
brown turn is in of
insoluble having ppt.
blue.
paper
pnt Evolution NaOH
which White
|Yellow
IDark black. ofgas in
little extract.
and a of dichromate obtained,
passthrough solution.
the
mixture. in ml quantity
a Cool salt 2 and
to soda gas) acetate
chips solidand tube
CO,.
MnO,
small potassiumissolution
of chloride )
Heat ) quantity of
H,SO4.
copper (CI removeg
test lead(Br
0.2of tube. aTo the
solution. brom
chloride (chromyl of
yellowW
Add g test:solidHeat
small about
to 4 the ml
:testthen Boil AgNO3 about 2
conc. for Heat of HSOA.
chioride If andfor
a Take solution.
turn1ng Test To HNO3. AddH,SO4. g evolved acidTest
:test of : 0.3
salt
and ml testtube. Chromyl addconc. acetic
Copper dil.
AgNO3 gasNaOH
1 MnO, Conc.
addadd test salt,andthe add
|(b) (a) (b) (c)
6.
7
CH,CO0 confirmed
confirmed CHC00
blue.
smell
paper
vinegarcolour fruity
starch
red dropsPleasa
|Smell
of
turns Wine
salt dil. alcohol
solid with few
the
solution.
extract ethyl
) a
add
(C
(CH,C00
paste
of of
soda drops
chloride
salt,
tube. Make
a solution. few oxa
neutralised
of
acetate pinch
ferric a
test and
:test neutral for
in for acidTo a H,SO, gently
and
heat
To est
Test
HSOa
test: test:
acidoxalic
Oxalic
add
conc.
Conc. withFeCl,
HCI,Ester
of
(a) (b) (c)
9.
confimed
confirmed
SO,
in
confirmed
SOA
is dil.
HCI acetate
effervescence
BaSOa soluble
insoluble ammo
in
of
steady ppt.
ppt.
HNO3.satura
or
formed, sol
a White White
with
l acetic
Boil
HCI.solution.
SOIUtion. add
dil. extract,
addBaCl,
4 (SO,
extract,
ml soda
sulphate
1
add To aceta
soda
:
for and test
To
Test Cool acetate
lead
:
test
CO. and
BaCl,Lead
acid
off
(a) (b)
11.
Nootan /SC Chemistn Lab Manual AX |49)
After preparing O.S., it can be proceeded for the group separation as given below
0.S.

Add dilute HCI

ppt. Group ! Filtrate


(PbCl) Pass HS gas

Black or yellow Filtrate


ppt. Group ll () Boil off H,S gas
(i) Add few drops of conc. HN03.
(PbS, HgS, CuS, CdS, As,S_) Heat and cool.
(ii) Add a pinch of NH,Cl and
NH,OH in excess till it smells NH3.

ppt. Group ll Filtrate


[AI(OH). Fe(OH)3l Pass H,S gas

ppt. Group IV Filtrate


(CoS, NiS, ZnS, MnS) Boil off H,S and then add
NH,OH and (NH¡)2C03
solution in excess.

ppt. Filtrate
Group V Group VI
(BaCO3. SrC0,. CaCO,) (Mg*)

GROUP ZERO (NHZ)


This group contains only ammonium ion (NH). It does not require original solution.The salt in
the solid state is used for its identification.
1. Heat the small amount of salt mixture with some caustic soda (NaOH) solution. The
evolution of colourless gas with ammonical smell indicates the presence of ammonium
ion. This gas gives white dense fumes with moistened rod of conc. HCI.
2. The evolved gas is passed thru nessler's reagent which turns brown. this confirms
presence of ammonium ion in the mixture.
2 1. and formed. |Add
ution. Yellow
K,CrO4addsolution’
Potassium ppt.
Potassium divide
Dissolve dilute

into
chromate iodide the HTS04
solution
Yellow two solution
(Pbt)
white Colourless
parts: and
(KI)
(KCrO4) ppt.
test little
in
ammonium
:
test To ethanol.
the
ppt. :
soluble To first
the acetate A
part, white
second
in
NaOH add solution ppt.
part|
KI is
2. 1. Boil
lution blue
second solution.
Potassium NH,OH Ammonium off
HoS
part
solution and

with
rrocyanide Bluish
olate hydroxide
divide
little in
u green
acetic excess the
brown (NHaOH): solution
alFe(CN)6] solution
acid
ppt. with
and shaking into (Cute)
add To
two
test one
e(CN)6l parts:
part,
Acidify
Deep
add
Nootan ISC Chemistry Lab Manual XI|
(53]
2. K4[Fe(CN)6] test :
[Cu(NH,)4J(NO,), + 4CHCOOH
Cu(NO3)2 + 4CH,COONH4
2Cu(NO3)2 + K4[Fe(CN)6]
Cu,[Fe(CN),J + 4KNO3
Chocolate brown
ppt.

FLOW CHART FOR ANALYSIS OF GROUP-II


Filtrate of Group I
Pass H,S gas

Precipitate No precipitate
Group ll present Group Il absent

Proceed for
Filter analysis of
Group ll to VI
Black precipitate

Heat with 50% HNO3.

Colourless solution Bluish green


Boil off HS gas solution
cool and divide Boil off HaS and
into two parts divide the solution
into two parts
KI solution KzCr04 NH,OH K4[Fe(CN)6l
solution solution

Yellow precipitate Chrome yellow Deep blue Chocolate


precipitate solution brown
which dissolves in precipitate
NaOH solution

Pb+2 confirmed Cut2 confirmed


l
2. -A Dissolve group.
tormed,
1subsequenttchloride
he and
NH,OH
excesS in
appears
liquid Lake A excess.
drop
till it
solution.
white NaOH gives these (54)
white
test However,
To
test the the grOups firstIf
ppt. To ppt. itnegative
Add ppt. confirms above
isthis
appears : White and
formed.
twosolution, To in ammonium excess if is
the dilute solution, testpresent, thesecond
firmed AI drops ’ gelatinous
Pale which
first the starting
HCl for
add part presence groups
blue of H,S we
blue dissolves and add
a add
floating pinch divide ppt.
solutionshall
litmus few with are
NaOH [AI(OH)3] hydroxide
of
ofdrops
lead begin
GROUP-III
(Fe,
AI) absent,
ppt. in into Group
solution NH,CI heat.
excess
andNaOH of is
solution tw o acetate filtrate,
in of with
a conc. proceed
parts I I
colourless and solution the
drop cations. paper. it
then2. : HNO,, filtrate iswith5
by|1. boiled
Dissolve
and Filter till boil
colouration.red part one
Potassium it
of ml
Potassium divide fo r the
’ smells
the and
of Prussian part corresponding
the some original of
solution, of theReddish precipitate. cool.
sulphocyanide ferrocyanide the ppt. of
solution time
firmed
Fet +3 blue
solution, in ammonia. Now
brown solution Nootan
add coloured minimum to
into add remove
KCNS group. /S
(KalFe(CN)6}) add tw o
ppt.Preserve
(KCNS) pinch
If a directly. Cnemistry
solution KalFe(CN)6]
solution [Fe(OH)3]
quantity
parts the all
test: th e of H2
: precipitate ammonium But Láb
or of filtrate
To ppt. test gas if Manual
another solution dil. any
Blood until
: HCI Xu
To for is of
Nootan ISC Chemistry Lab Manual XIl [55]

2. KCNS test:
FeCl3 + 3KCNS Fe(CNS)3 + 3KCI
(Blood red)

FLOW CHART FOR ANALYSIS OF GROUP-III


Filtrate of Group I|
(i) Boil off H,S gas
(ii) Add conc. HNO3 and boil
(iii) Add a pinch of NH,Cl and NH,OH solution in excess

Precipitate No precipitate
Group l present Group Ill absent

Proceed for
Filter analysis of
Group IV, V
and VI

White gelatinous Reddish brown


precipitate Al(0H)3 precipitate Fe(0H)3
Dissolve in dil. HCl and Dissolve in dil. HCl and
divide into two parts divide into two parts
NaOH Solution dropwise Few drops of blue litmus KCNS
K4fe(CN)6
then in excess solution and excess NH,OH solution solution
White ppt. which Floating blue
Deep blue Blood red
dissolves in excess lake
solution solution
NaOH

Ar3 confirmed Fe+3 confirmed

GROUP-IV (Zn
+2
Mn+2 NIt2,Co*)
The cations of Group IV are precipitated as their sulphides in presence of NH,OH.
Iffirst, second and third groups are absent,we shall begin with 5 ml of original solution and add
a pinch of NH,CI and excess NH,OH. Otherwise take the filtrate of third group containing NH,CI
and NH,OH. Now pass H,S gas. If a precipitate is formed, it indicates the presence of Group IV If
precipitate appears, proceed for Group V and VI analysis from this solution. Filter the solurion
and collect the precipitate. Analyse the precipitate for Group IV cations and retain the filtrate for the
subsequent groups.
[56] Nootan /SC Chemistry Lab Manual X

Dirty white ppt. (ZnS) Flesh coloured ppt. (MnS)


Dissolve the ppt. in dilute HCI and boil off HS gas and Dissolve the ppt. in dil. HCI and boil off H23.
divide it into two parts.
1. NaOH test : Tothe first part of the solution, add NaOH Bromine water test : To the above solution, add NaOH
solution White ppt. soluble in excess NaOHSolution till the formation of white ppt. Now add Br,
solution. water to this white ppt. ’ Brown ppt.
2. Potassium ferrocyanide KalFe(CN)] test : To the
second part, add2 ml of KalFe(CN)el solution
Bluish white ppt.
Znt confirmed Mnt confirmed

Black ppt. (NiS or CoS)


Dissolve the ppt. in aqua regia (3 ml of conc. HCI and 1ml of conc. HNO3). Evaporate the solution to dryness. Add
water and divide the solution into three parts :
First Part Second Part Third Part
Dimethyl glyoxime (DMG) Test : Add Potassium nitrite test : Acidify the Ammonium thiocyanate test : Add
NH,OH solution in excessfollowed by solution with acetic acid and add| 1 ml of acetone and solid
DMG solution in excess ’ Scarletsolid sodium or potassium nitrite thiocyanate ammonium
red ppt. (NH,CNS). Shake it
(KNO,) ’ Yellow ppt. Blue colouration in organic layer.
Nit confirmed Co* confirmed Co* confirmed
Chemical Reactions
(58 Nootan SC Chernustry Lah
Manual
FLOW CHART FOR ANALYSIS OF GROUP-IV
Filtrate of Group Il
Pass H,S

Precipitate No precipitate
Group IV present Group IV absent

Filter Proceed for analysis of


Group Vand VI
Precipitate

White ZnS Flesh coloured MnS Black NiS or CoS


Dissolve in dil Dissolve in Dissolve in aqua regia and evaporate to
HCIand boil otf H,S gas dil. HCIand boil dryness. Add water and divide the solution
Divide into two parts offH,S into three parts
Add NaOH ppt. gets Add NH4OH (excess)
Scarlet red
solution dropwise K4lFe(CN)el dissolved followed by DMG ppt.
solution in excesSs
White ppt. Bluish white ppt. NaOH Solution
and then Br, water
Soluble in excess Ni+2 confirmed
NaOH White ppt. which
Acid1fy with CH,C0OH
Yellow ppt.
turns brown or black
and add solid KNO,
on adding Br2 water
Co+2 confirmed
Zn+2 contirmed Mn+2 confirmed
Add 1 ml of acetone
Blue colouration
and solid NH,CNS in organic layer
and shake it well
Co2 confirmed

GROUP-V (Ba +2 Sr, cat2)


Group Vcations are precipitated as carbonates in presence of NH,Cl and NH,OH.
If allthe four groupsare absent, start with 5 ml of original solution. If filrate of Group IV is used
(in case any group is present), boil it for some time to remove H,S and to reduce the volume to
ne-third of its originalvolume and cool. Now add a pinch of NH,CI, NHOH solution and saturated
olution of (NH),CO,. Warm the solution and allow it to stand for sometime. A white precipitate
ndicates the presence of Group V. Retain the filtrate for the cations of Group VI.
Moolan /SC Chemistry Lab Manual XI| (59]
The precipitate is dissolved in hot dilute acetic acid and test for Ba*2, sr* and Ca* strictly in
the givern order.
S. No. Bat2 Srt2 Cat2
11. Potassium chromate (KzCro) Ammonium sulphate (NH¡),so. Ammonium and
oxalate (NH42C;04
Srt2 are absent,
test : Add KgCrO4 solution to test : To second portion of the test : If Bat
the first part A yellow ppt. above solution, add (NHA),SOA add (NHa),CO4 Solution to the
(If yellow ppt. is not obtained, solution Awhite ppt. (If white third part of the solution ’A
perform the test for Srt) ppt. is not obtained perform the white ppt.
test for Cat).
2. Flame test : Perform the flame test| Flame test : The above ppt. gives Flame test:The above ppt. gives
with the ppt. obtained above crimson red flame on performing|brick red flame on performing
Grassy green flame. flame test. flame test.

Bat² confirmed Srtz confirmed Cat confirmed

Chemical Reactions
Test for Ba +2
Nootan /SU LI
Lab Manual y
ANALYSIS OF GROUP-V
FLOW CHART FOR
Filtrate of Group IV
volume
and reduce the
(a) Boil off H,S gas
NH,CI, NH,OH(excess)
(b) Cool and add solid
and (NH ),CO3 solution
inexcess

No precipitate
White Precipitate Group Vabsent

Proceed for analysis


of Group VI
Filter it and
dissolve the ppt. in
hot dilute acetic acid
and divide the solution
into three parts.

First part Second part Third part


If both Ba2 and Sr+2
Add K,CrO4 If Ba+2 absent,
solution add (NH¡)2SO4 absent, add (NH¡)2C204
solution solution

Yellow precipitate White precipitate White precipitate

Ba+ confirmed Srt2 confirmed Ca+2 confirmed

GROUP-VI (Mg
To the fltrate of the previous group (or original solution if all the five groups are absent),
add ammonium hydroxide in excess and disodium hydrogen phosphate (Na,HPO4) solution or
ammonium phosphate (NH4)3PO4 solution. Scratch the sides of the test tube. Formation of white
crystalline precipitate confirms the presence of Mg*+2 in the salt.

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