26 Nirav College Practical Chemi.

mistr Ino
Sodium Cobaltinitrite:
Take NaNO, Solid and add Co (NO,), soln and add little (one or two drono
acetic acid. This is the reagent used for the detection of K'.
ops
(D) Wet p
tests for positive redicals
O
(a) Preparation of the solution
Take a small amount of the mixture in a
porcelin dish and observe its solubilit
distilled water. If it dissolves in water,
[warm if necessary) prepare a solution by taking 10
15 mg. mixture and some distilled water.
If the mixture is insoluble in water & dissolves in dil. HCl (warm if necessary) Prepare
the soln in dil HCI.

If the mixture is insoluble in dil HCI

test whether it is soluble" in Conc. HCI.
If the
mixture becomes soluble in Conc. HCI
naturally it indicates the absence of first group. Then
add conc. HCI in the mixture
and boil to dryness then dilute it with water.
If the first group is
present prepare the soln. in dil. or Conc. HNO,. In this case it
is advisable to
evaporate to dryness after the removal of the first
then extracted with conc. HCI and dilute group and the residue is
further. with distilled water.
Precautions to be taken while Preparing
a solution

(1) If the oxidising agents like

NO,, CrO* are Present, they must be reduced by
boiling with conc. HCl and
evaporating them to dryness. The process is repeated
for 2-3 times. And the residue is extracted
with dil. HCl and filter if
This soln is used for necessary.
analysis.
(2) Aqueous solution of Sb*", Bi*s, Sn** will
HCI is added. The
precipited as the oxychloride when dil
precipitate
may however be dissolved by few drops of
(3) Concentrated soln cí NaCl and
HCl
BaCl, may some time gives precipitate with conc.
HCI. The precipitates are dissolved on
further dilution with water.
(4) If nitrate is present, the solution is heated with conc.
HCI to dryness and is treated
with dil. HCI and distilled water. So
that the nitrate radical is
replaced by chloride.
 Inorganic Qualitative Analysis
27
Seperation of positive radical into groups
Solution + dil. HCI.

ppt. Filtrate: Take 2 ml soln. in test tube pass H,S.If ppts. obtained pass H,Sintotalbulk of
obtained filter and repeat twice or thriceindiluted solution also, till 2nd groups ppted.completely.
Ist Ppt. Filtate: boil off I1,S [Test with Lead acetate paperjif Fe"or Fe3is detected
group obtaind boil the soln.
present IInd +2 gm soid NL,CI +6N NH,OH till it becomes alkaline
white present [test with Litmus paper. )
Ag Ppt. Filtrate :Pass HS-Test with 2 ml soln-if ppt
Pb2 obtained obtained pass in total bulk of solution.
Hg+2 III A group Ppt. Filtrate: Boil. off H,S and concentrate
present obtained it to half bulk Then add NH,CI1+
III B NH,OH (NH,), CO,.
group ppt Filrate: NH, OH'Na,HPO,
present obtained ppt. obtained VA group present
IV Reject the filtrate

group (V-B group)

(Nat, K, NH,)
by water extract.

Analysis of group :I
White ppts. (AgCl, HgCl,, PbCI,) Boil ppts with distilled water and filter it

Residue (ppts) (HgCl, AgCI).

Add NHOH in ppts. filtrate

shake well and filtrate it,

fitrate (Ag) filtrate (Pb:2)
ppts. (Hg2)
ppts. +3:1 conc. HCl fitrate+ filtrate +
K,Cro,> yellow ppts
+Con dil. HCI which is
HNO, + SnCl,
white ppts Insoluble in acetic acid
solution white ppts
Hg is present Agl is present Pb2 is present
 28 Nirav College Practical
Chemiststry
Ag (C.T.) of Ag
(1) Solution + H,S Black ppt of Ags which is soluble in HNO
(ii) Solution + NaOH Brown ppt of AgO which slowly turns in to bla
(ii) Solution +CH, COOH + K{CrO, Red ppt of AgCrO, which solube inHNO

(iv) Solution + KI Black ppt of Agl

(v) Spot - test

(a) I drop of solution +1 drop Black spot

HCI+2 droply Manganeze
sulfate + 1 drop KOH
(6) 1 drop solution + 1 drop Red spot

(NH), CO,+1droply KC.O,.

Hg C. T. of Hg'*
() Solution+ HS gas Black ppts dull to HgS
(ii) Solution + NaOH Black ppt of HgO
Cii) Solution + KI Green ppt Hg, L, gives black colour with
addition of KI(excess)
(iv) Solution +SnCL HgC1, (with ppt of Hg,Cl, Quikly turns black.
(v) Spot test: 1 drop solution Black spot
+1 drop KNO, solution
Pb C.T. of Pb2
(i) Solution HS Black ppt of PbS, soluble in HNO,
(ii) Solution + NaOH white ppt of Pb(OH),
(ii) Solution +
K,CrC yellow ppt of Lead chromate
(iv) Solution +
HSO, white ppt of lead sultat solube in hot
solution of amonium acetate
Spot test
(a) 1 drop solution + KCN Crystal Red Colour
+1 drop di-thiozone
(b) 1 drop solution + 1 drop Blue colour
sodium Rohzidante
Inorganic Qualitative Analysis 29
Analysis of Second group
Take the ppts. into evaporating dish, add NaOH, Boil and filter.

Residue Filtrate
I1-A group is present Filtrate HCI > A coloureved
HgS (Black) ppts is Obtained
PbS- (Black or Brown) II-B group is present

BiS, (Brown) White ppt is obtained Il-B group is absent

CuS (Black) Sb,S, (orange), As,S, (yellow).

-

Cas (yellow) SnS (brown), SnS, (yellow)

Analysis of II - A group

Take ppts in beaker add dil HNO, boil the mixture and filter it
Filtrate
Residue (Hg*) Filtrate (Pb*2, Cu*?, Cd-2, Bi*3 may be present.)
and filter.
Black ppts, dissolve it in dil. H,SO. ppts obtained, Boil
still
(3:1)conc. HCl+conc.HNO,| whiteFiltrate (Cu, Cd*2, Bi*) add NH,OH
in

fitrate turns in Basic medium

and heat it + SnCl PPts.

white Filtrate (Cu, Cd)

solution white ppts Pb is

present Pppts. Filtrate Filtrate + dil. H,SO

Hg is present
is is blue FeSO, Boil it
Bi +

present then Reject the ppts, take

Cu is the solution. add

present HS > yellow ppts

obtained Cd* present.

|Hg2 C.T. for Hg2 white ppts which turn in gray colour|
i ) Solution+ SnCl, of more reagent
ppts with addition
soluble in Kl
dark Red which is
(ii) Solution + KI

Solution+ NH, SCN Crystal+

cobalt aceetate | Sky- blue
(1i)
(iv) Spot test: Sky-blue -
Violet colour
Solution + 1 drop Di -

phenyl
1 drop
Carbazide alcoholic Solution.
 30 Nirav College Practical Chemistr
Pbt2 C.T. for Pb:2
(i) Solution + H,S Black ppt of lead sulfide soluble in
(ii) Solution + NaOH
HNO.
White ppt of lead
Hydroxide soluble in
Reagent (excess)
(i) Solution + K,CrO Yelllow ppt of lead cromate
(iv) Solution+ H,SO white ppt of lead sulfide
(v) Spot test: Soluble in Ammonium acetate
(a) 1 droup solution + KCN
red spot
crystal + l drop di-thiozone

(b) I droup solution + a drop Blue spot

Sodium - Rohdizonate

Bi C.T. of Bi*3
(i) Solution + H,O White ppts Insoluble in tartaric acid
soluble in HCI.
(ii) Solution + KI Dark-gray ppts which gives organe
ppts in addtion of more reagent.
(ii) Solution + NaOH White ppts which is insoluble in
reagent additon of black ppts.
Civ) Solution + SnCl, + NaOH

(v) Spot test:

1. drop Solution prepared in dark yellow colour

HNO,+1 drop 5% Solution Thio-urea.

Cu C.T. of Cu
(i) Solution + Ammonium mercury thiocynate Violt ppts
Solution KI White Brown ppts
i) +

(ii) Solution + K, Fe(CN), park-red or chocolate colour ppts|

Civ) Solution + NH,OH Sky Blue ppts.

green colour flamne
(v) Flame test
(vi) Spot test :
(a) 1 drop Solution + 1 drop NH,OH greeish yellow ppts

1 drop acetic acid + drop selildoxime.

1

1 Solution + 1 drop cupferon reagent green colour

(b) drop
+1 drop NH,OH.
Inorganic Quali*ative Analysis
Cd2 C.T. of Cd2 31

) Solution +
Na,CO, White ppts
(ii) Solution NaCN
White ppt soluble in excess of
ii) Solution +
NH, reagents
White ppt soluble in excess of
(iv) Spot test reagents
I drop
of Solution + 1
drop Red colour
Di phenyl carbazide

Analysis II -
B group
Add dil. HCI the filtrate from II
to
- A group
Coloured ppt is obtained. Boil the
ppt with conc. HCI and
Filtrate
Residue Filtrate (Sb*3, Sn*2
yellow ppts Filtrate+ HS gas
Ast is Orange coloured ppts yellow or gray
present Sbt3 is present coloured ppts
Sn is present

As C.T. for As*3

G) Solution + conc.
HNO, + yellow ppts
amonium molybdate
(ii) Solution CuSO, NaOH green ppts turns to red on heating
(i) Solution +I, (Soluble in KI) + Na,CO Colour of lodine is removed
(iv) Solution + AgNO, yellow ppts soluble in HNO,

(v) Spot test:

Solution in crucible Brown or Black
Take 1 drop of
6% spot
+2 drop con NH,OH + 2 drop
HO, + 2 drop 10% MgCl,
>

slowly heat and vaporized it.

Sb3 C.T. for Sb3

Orange ppts of Sb,S, solublein
i) Solution+ H,S gas HCI
hot Solution of conc.

White ppts soluble in excess of reagent

(ii) Solution+ NaOH
 32 Nirav College Practical Chemistry
(111) Solution Excess of water Solution becomes milky which is
soluble in tartric acid
(iv) Solution + KI Yellow colour Solution
(v) Spot test
(a) 1 drop solution + l drop phospho- | Blue colour after some time
molyblidic acid
(b) 1 drop solution + I part NaNO, + 1 drop Sky-Blue colour
Rhodamine B (10% water solution)
Snt C.T. for Snt2
(i) Solution + Amonium molybdate Sky-blue colour
+dil. HCI
(ii) Solution +
HgCl, white ppts becomes gray black
after some time.
ii) Solution +
K,Cr,O, + conc. H,SO, Green colour Solution
(iv) Spot test
(a) 1 drop of Solution + 1 Red - violet colour
drop Cacothaline solution
(b) 1 drop Solution + 2 drop Green colour
di-thioal Solution.
Analysis of (III - A) group

Precipitate: Al (OH), Fe(OH), C{OH, and a litle Mn0, XH,O, Transfer the ppt in to
theBeakerAdd2gm Na,O,Solution,Boil and filler [Na,O,(NaOH +H0J
Residue: Fe(OH), and MnO, 2H,O | Filtrate (Cr", Al3)
devided it in two parts devided it in two parts
Solution+
Ppts + dil. HC1+ Ppts +conc. HNO, | Iffiltrate contain HCI (make acidic medium)|
KCNS +PbO, boilit yellow Colour +NH OH (Make basic
blood Red than Cr3is medium) heat >
Colouration violet or light pink present Filtrate + white gelatin
Fet is colour Solution CHCOOH +Lead ppts obtained
present obtained Mn2is Acetate yellow ppts |: A is present
present Cr3 is present
 Note ( ) If isFet, 33
present it must be oxidised
conc. HNO,. to Fet by heating with 2 ml. of
(2) If
PO," is present it should be removed
phosphate scheme. before proceeding Insoluble
Fe"
Fe3
C.T. for Fe
i) Solution + NaCN Red gray ppts soluble in excess
reagent and
Solution turns to yellow colour
(ii) Solution + KCNS
Blood Red colour Solution
(ii) Solution +
K, [Fe(CN),] Sky-blue colour ppts
iv) Solution H,S Black pps soluble in acid
Spot test
1 drop Solution 1
+
drop Farongreen colour
Mn2 C.T. for Mn*
(i) Solution +
K, [Fe(CN),] Light pink ppts soluble in acid
(ii) Solution + PbO, + NH, Boil light violet - ppts
(ii) Solution + NaOH light pink ppts. which slowly turn in gray
colour in air.
(iv) Spot test :
1 drop Solution + 1 drop HNO, Violet colour
+ l drop sodium Bismuthate

Cr C.T. for Cr
(i) Solution + NHOH Dark Green ppt soluble in acid

(ii) Solution + H,0, yellow colour solution

green colour ppts

(iii) Solution + Na,HPO,
iv) Solur al CH,coOH
+Pb (CH,COO),
Spot test
Acidic Solution + 1 drop
Red OR Violet color
AgNO, + 1 drop K,S,O,
it 2 to 3 minute
(kept
+I drop Di-phenyl
Carbazide)
 34 Nirav College Practical Chemistry
Al3 C.T. for Al
(i) Solution +
Na,HPO, White ppts
(ii) Solution +
Na,Co White ppts
(iii) Colour + NH,OH White ppts insoluble in NH,OH
iv) Spot test
2 drops of Solution +2 drop HCI +
I drop Aluminon + 3 drops. NH,OH. Red colouration
Analysis of III - B group

Ppts: [CoS, Nis, MnS, ZnS] Add HCI, boil and filtrate.
Black ppts (CO*2, Ni2) Filtrate (Mn*2, Zn*2) Boil to
Dissolve ppt in (3:1) HCI remove HS now add
conc. +
conc.
HNO, Boil evoparate to dryness cool. nore NaOH and filtrate
and add 1'ml water to dissolve residue
Devide the solution in two parts
Part JJ Part II Ppts filtrate
Solution + KNO, | Solution+ Turns pink Filtrare +
CH, COOH NHOH + D.M.G in air
Na,HPO,+
yellow ppts Red ppts Mn2 is iNH OH white ppt
Co is present Ni*2 is present present Znt2 is present
Co2 C.T. for Co2
i) Solution + NaCN light brown ppts which is soluble in
excess of reagent

(ii) Solution +
NaHCO, +
Br, light green colour ppts
(ii) Solution + NaOH sky blue ppts
(iv) Solution +
H,S Black ppts
(v) Spot test:
(a) 1 drop solution + 1 drop NH, SCN Blue colour
solution
(b) 1 drop Solution + 1 drop DMG Dark Green colour
+1 drop NH OH
Inorganic Qualitative Analysis
35
Ni C.T. for Ni2

i) Solution + NaOH +
Br, Water Black ppts
ii) Solution (NH,), S Black ppts
(ii) Solution + NaCN
light green ppts which is soluble in
excess of reagent
(iv) Spot - test
1 drop Solution drop 1% DMG
+ 1 Red colour
(preparedin alcohol) +1 drop NH,OH|
Mn*2 C.T. for Mn2

) Solution +
KFe (CN), light pink ppts soluble in acid

(ii) Solution + PbO, + HNO, Redish Violet ppts

ii) Solution + NaOH light pink ppts turns to gray in air

(iv) Spot - test :

(a) 1 drop Solution + 1 drop HNO, Violet colour

+1 drop sodium Bismuthate

sky-blue colour
(b) 1 drop Solution + 1 drop NaOH
+1 drop Benzidiyn

Znt? C.T. For Zn*2

White ppts soluble in acid
i) Solution + HS
Solution + NaOH white ppts soluble in excess of reagent
(ii)
white ppts soluble in NHOH
(iii) Solution + NH,CI + Na,HPO,
white ppts
(iv) Solution + K, [Fe(CN),]
(v) Spot test
+ 1 drop
() drop of solution
1 drop sky blue ppts
0.02% cobalt sulfate
+

ammonium mercury thiocinate

colour obtained.
slowly blue
b) 1drop of Solution
+1 drop NH,OH
resorcinol (in alcohol)
+1 drop
 Nirav College Practical Chemist
36 Ast y
Analysis of (IV) group
-

White ppts (CaCO,, BaCO,, Sr CO,) Dissolve ppts in dil. CH. COC
COO
Precipitate :

and heat it. Now,

Take few drops ofthis solution and add K,CrO, it yellow ppts obtained than Ba?
(i)
present than add excess of K,CrO, and filter and used this filtrate for Ca2 and S .
ii) If Ba2 is absent than no need to add K,CrO, directly use this solution for
test
of (Sr*2 and Cat).

yellow ppts filtrate : (Ca*, Sr)

which is insoluble filtrate + NH, OH + (NH,), CO, Boil it, take that add
in acetic acid CHCOOH so ppts are diluted and removed CO, gas.

Ba2 is Devide solution in two parts.

present Part II Part II

Solution + CaSO, Solution + (NH,),SO,
boil it after sometimes+ NH,OH Boil reject the ppts
white ppts. obtained filtrare +
(NH,) C0,
Sr2 is present + NH,OH > White ppts
Ca2 is present.
Ba2 C.T. for Bat?
(i) Solution + K, CrO yellow ppts, addition of acid turns in orange
(ii) Solution +
(NH),C,O, white ppts
(iii) Solution +
HS0, white ppts insoluble in acid
(iv) Solution +
(NH,,SO, white ppts
(v) flame test light green flame
(vi) Spot - test :
I drop solution + 1 drop Reddish gray ppt
0.5% Sodium Rohsidante
SrC.T. for Sr*2
(i) Solution + (NH), CO, White ppts which is
Soluble with effervescence of
CO, by addition of acid
(ii) Solution + dil. H,SO, White ppts insoluble in acid
(iii) Solution +
K,CrO Yellow ppts soluble in acetic acid
Inorganic Qualitative Analysis 37
(iv) flame test
Crimson red flame
(v) Spot test
Idrop solution + I drop sodium Reddish gray colour
Rhodizonate (0.5%)
Ca C.T. for Ca
i) Solution + dil. H,SO, White ppts
(ii) Solution +
(NH,), CO, White ppts soluble in acid

With effervescence of CO,

(ii) Solution +
(NH,, C,O White ppts soluble in acid
(v) flame test No ppts.
(a) 1 drop sodium rhohdizonate Brick read flame
(0.2%) + 1 drop0.5 N NaOH
b) 1 drop of solution + 4.5 drops ppts are White ppts
Ammonium ferrocynide +2 drops alcohol
Analysis of V - A group

White ppts [Mg (NH), PO,J

Add dil HCI to dissolve ppts add 1 ml water +3 drops solution +sodium hypoiodide
(NaOl)
+L + NaOH) Reddish -gray ppts. Mg" is present.
Mg C.T. for Mg*2
Solution NaOH White ppts soluble in NaOH
(i) +

(ii) Solution + NH,OH +(NH), HPO, White ppts soluble in acid

(ii) Solution + (NH,), C.O White ppts soluble in acid

Spot Test
(a) 3 drops solution 3 drop sky blue ppts

HCI+ 1 drop Magnason

+ 2 drops NaOH
(b) 1 drop solution + 1 drop Dark (Red)
orange colour
Titan yellow + 1 drop in NaOH
 Nirav College Practical Chet
38 mist
Analysis of (V
-

B) groupp

this positive 10ns are soluble in ns

In this group contained Nat', K', NH,",
out by Water Extract (W.E.) test.
Analysis of such group is carried
(i) W.E. + NaOH > Smell of ammonia and white fumes obtained with glase
glass
of HCI NH,' is present
(ii) W.E. + Fresh solution of sodium cobaltynitrate + CH, COOH -> vellow n
is present
(iii) W.E. + Zirconyle acetate yellow ppts Na* is present.

NH:C.T. for NH,

i) W.E. +NaOH Smell amonia, which turns,Red litmus to blu
ii) W.E. + sodium cobaltynitrate Yellow ppts
(iii) W.E. + Nessler's reagent Reddish- gray ppts
(iv) Spot test :
I drop W.E. +1 drop conc. NaOH |Red-orange spot
+1 drop Nessler's reagent
K* C.T. for K*
(i) W.E. + sodium cobaltinitrate Yellal ppts insoluble in acetic acid
(ii) W.E. + Picrie acid Yellow ppts
(iii) W.E. + tartaric acid White ppts
(iv) flame test: Violet flame which observed crimson
Red in cobalt glass
() Spot test
(a) 1 drop W.E. + 1 drop White ppts
sodium tetra phenyl borate (2%)
(b) 1 drop W.E. + 1 drop of
icryle amine 0.1N Orange Red ppts.
( i h is prepared in 10% Na,CO,
Na C.T. for Na*
() W.E. + Magnesium Uranyle acetate
Yellow ppts
(ii) W.E. + zinc uranyle ctate
Yellow ppts
(ii) Flame test
continuous golden -

yellow
(iv) Spot test
1 drop W.E. +2-3 drops zinc uranyl
acetateYellow ppts