_:__ __p~~~

--
Inorganic Che1111st
•·' • . -.--.__. ~-=--=---- -=--k"ry Expcrriments
'\
-.sJ:ll'•/' !ICRO OUALITATIVI;
_ ANALYS IS .«::c C W CW

--
_ ___

111atiVO analysis of Inorganic salt I - -- -- - -- - -

()11-' P d two b a sic radicals of sa- m xture containing two acidic radical • ol different
0 11
\
~• . ··- groups
111 "'"c ro an alys is amount of
8 1
111 ., h ,i, O on I tu o OJ g r amp e Lak~n for nnalysis i• 0 .1 t.ol.O g. while in
01 ll'n' · ·
fr ,111 n f11 tn o I g
· o so rnp) 15
e
·
used. In semi - nucro unnlvsis amounts
\
r•i:- "' '1.• . · an, u~ed for the Analysis nnd tbt volu mr of iiquid used is
• • • 111 11,., ·" 1va nt age of semi .
~ •.'t.·' · p•• IIu I wn uncj Iab our. The S· m :.o
icro
•
t e<:hniquu • is to save the •che micnls, time,
• •
,!'' ih· lr,,m macro analysis s em,• -m,. cro t ech 1114ue of analvs1 · s d Ot!s not va.ry
,,~~ · · em1 -n11cro quulitntive annlys1ij combine,; the
•d,.11 11 r:1~,·~ of bot h macro a nd micro annlvsis
F '" 1111 pnrtn nt glass nppar tl tlas d d
• •

r · ·
' · an proce ureH used ,or scmumcr o ana lyslS nrc
Jf:.riI11,d n ~ he low
1. Tesl Tube. ce n trifuge tube and sem i-micro boiling tube : Test Tube:
Smnll l'yn; x (or corning) glass tes t tubes (Fig I. I) nre used for renctions. Centrifugt'
ruhe ( Fit! I ,:!l. :\ me t hod of separating n p r ecipitultl Crom o sma ll volu me of a liquid is
r,1lkd .,., .-,• 111 niugntion .
Fo1, th is " 11•n1.nfuge tube is rtJqu ired. ,\ t est tube with tapered bot tom 1s k,nown
•••,, , ,•ut ri ll'i,:e u,he. tn this tuhc con te n1 s ca nnot be boiled which n vmds bumping
'ccntr 1.1:!•· '11lies o f va rious sizes are being u sed but :I ml centnfug1: lS most
communl.v used.
•
·li•
•I t .t ,

'.
..
'

flt J.1 : Tcsl Tube fig 1.l: <<IIlrifIll' Iu"'

I t'lc Ll: Stlr-r\ni rod •

Sem1-.v!icro llo 1. l1ng t ube: Semi-micro boiling tube (60-25 mm. Pyrex. 20 ml) IS

11.,1,d foi bc,d in I,! pu rpuse.

 A Te)(t Book of Elements of Cnen,"trv
216 -~.,,
. . • . , oppo~ite posit ions iI1 t he centriru
t.h b . in chnnu:tn ctt11) kt:.
(o) ln u-oducu • e tu On . d ,v ,t hlv uud brin g tn t hu mr,ximurn
,,. o •-lowlv• un sm-
(I) Storl lbe centrm1g · 11 l•t
•••
with n few turns of the hun dlc. , ed of lhc ce ntTifuge. otherw·
retard t.he spe ••e ,.,.
(g) Do not attempt to stop or . . - •~
. . • · te may be dis persed.
mJurc hands or precrpita . . and observe wlwther it nius .
~ , t\\'O m111u 1et,
(h) Run the ompty centr Itlll!e
1t ,•t:'1
- '
nnd wi thout vibrntion. . It 111
siirnng up 1h,· mixture one.I rnay c.1 ,
. . · . , 11,c~(' ma\' ~ ,11 !'I • 1111~ ,,
(i ) Try hJ a vorJ v1hrn11o n) ••~ ·· · t-

lhc uppnrams. . . , . Ii) is olso einployed. Principle of ,

dr . ·•entrifuve (1 ,g 1. tr,c
ElectricallY ive n c " th 1· b:lllci driven machine . Th ·
.
electricaTI,· dri,•en machine 1s · c • th . same at at o e Otii•
,
difference. i~ that it is rotat ed electTically. . . . .
. I 1 . , . cent r iful!e with s peed mdicator 1s teqllu-,,d
A variable •per.d f'k•ct n .:al Y 'rl\ c n d · h h
fi · · • . . '"'
. . l\'s is \-,. 11c n s ue u ·h m 11c hi1w is e m ploye . sw1tc on t e curr.,n1
or semi mic ro ann , • . h . . . nun s p<,ed. lncronse it slowly by stageA Lu thE,
and k eep t he 111d1c11tor a l t ' minui •
. h ·hi11e has bee n opcra tCcl at the max.mum speed lor
maximu m speed. When t e m ac · h ff h
about one minute. decrease t h e spee d t o minimum and then switc o t e curre111.
(
.
G. Remova I o f su perna ..
tnnt liquid : The r entriiuge .
can accommodate both
. . t • ,. . and cen trifu t'I"P tubes. but the centrifuge tubes are prefer,.d
sem1· 011CT0 t c~~ i.U U Oi.- 0

because t h1•\· hnve th~ following advanta ges.

(o) S ·
• upernatan 1 1·JQ ui cl c·a n be ea s il •v removed fro m lh ti prc.-c1p1tntc withuu••
= ·p 1·tate . If this• is not pos sible. the supernata nt s hould be drawn
. b. .mg t h <' pr~~,
distur
off with a capillary dropper.
(b) SmaJJ cr amount of precipitate is more clearly visible.
F'o r removing supernata nt liquid capillary droppe rs Hr e u sed b ecause they can
reach to the bottom of th e centrifuge t ube.
7. Wash bottle and was hing of precipitates : 30 or 60 ml glass stoppered
bottle or polythene bottle (Figl.7) is used for wstilled water. Wash liquid is usually
distilled water. but some time it may be water containing a dilute solution of an
electrolyte. A s mall amou.nt of disti lled or wash solution is added to the precipitate
and the precipitate is agitated thoroughly until it is suspended. Th e precipitate is
centrifuged and the water is poured off and added to the supernatant liquid. The
process should be repeated and the water discarded. It is more efficient to wash
precipitate several times with s mall portions. Washing is generally done with 5-10
drops of wash liquid each time.
 1.c•I•
•'•·'' •.
'fr n11.src rr in tt ur
• ' .. pt t.' l'l p1 LO lt!
'8u r,• I 1.•.-~1. ·1,.,l,
(\': -I•
t!.o' .,,"',,,e:•1'1\.'I
,... • IL ly nl
t 1~,.
'lu t•\ · I1' .1 H.t •,..
•1.•,1 (I tt,•u U n g of s oh u •·, , ~ ••1,, t,, lu , ,, ,, , : f In ,,.1111111
. . . . l • t h, , I ' Ill 1or r,,,, I JI I
,.. .1
01 1 • I-' " 1•' I ,., ••.,,,t hJ Uk I
~
• 11 '" 11 11 pn rlu na ' "" ' '"'
1" '" "· • "' 1.,. .. ... . ' "" 1,,,1 " "''1"'' "" ' '"
• \ '• •1' tlu lll
t' ..r llH,.• H, "'" ''" ' 11"" •1111, ' " .,.., '" •••
I . II'
1 • .,.. , •u lit ,< ll nl d .... ... . I I ( ' ht ., ,, I
U 11111 111 n . 11 11•
lh ,• ' 111 ~" 'K l k)
1111
•u n. ,,r •h ... ,.,
. ,,.-
1
1' •••Ion'",.,"' ' "' "
11 -h•" '"I I"' PIne t• on " lu h, , I , ,,11 •r ubu , nN (l' t1C lll
I ,,, .,, rroan u x
,1 " " l•• "" "' '' I l
l"H I t I"'" •· ,1 h .
111'
1'
,.
"
no .-,,.,1 , ... "" '' I r '""' ,,r 11111l.&Jr1hl
"_ 1111
~'"W ti Y6 ,,,.I 1,11 1.,
1•'
1 ·l' '.. • n11 tl n I
t 1,r h,,
,11 •'"... -- 1 ut m v "" °lu
tto n. u, '
1' 11 I ut •r ' "" ' ti, ,.
ll' nt ,n .: \II ••·k• ttu• hl t· ' . ... ... ... n, ly 11 w t,•
I II-',.1u th 111' lh,. luI "
.: t H11 nr,, Ufiii'-<I 'I .h uu-\d Ii,·
••
,, r ht •a lHl\-~

► ,~1 ,l' : " 2.~h bo tll n

~,.1.1, s, .,
• ., ... ..
s. .,•ap o ra uo n : Fo r ev
apo ra
--',,.,.-11,'"" · E
" 5111 al l ev ap o ra ttn g a sol 11c1 ..,s ... ..i a... ... .. n.
..
tio n di.qh IS used. Se m · .
;1,1Jl'1rn11t1n. Lo w ev ap Ullon IO a defin'1t.e vo um<' or
or at io n mny be ca rr ie d I even IO
• i,.,ak•·r on a w at er ba o1•m1cro boiling iube rn
th. U in th ay a_lso U6c for
,.,,.-?rl11ra> ,:bould be co nd e e,• np ~l b) ' he al
I'· uc te d in th . f
or au on -in g in a ~ t tu be· cr uo bl
. . co rroS1Ve fu m es are ev e
9. D1ss o lv 1n e um i, cu pb oard ol ve d th e
hoUt ·•? n.xt ur e 1s w ar g of P re ci pi t at es : T h '
·- m ed if ne ce ss ar " on th e re ·.16
1110. P re ci pi ta , · ag en t added tn th e precipitate
8lfll e
-d ti on w it h hy dr o enw at er ba.th un ·1 an d
g u ·
s ul ph id e : In sc m1 pr L~ tp1tate haros ch ss oh·e .
._ Jr •l!"n ,-u p h • e ga -m1c an al ·
1 . 1 s 1s no t pa Ss l!d th ro ug h SO 1Ul lO I\ fo r pr ec 1p 1t atl 0D plJY1
ur,,· tlr...\ "a sh b Ol li , • . )0Sc
e or a ny ot her bo co nt a1 m ng w ys s
··:.u· h, •U 10 H_:-; ge ne ra ttl e • ot er sh ou ld a\wavi; be
to r. Pr ecip ita tio n is ca
rr ie d ou t m a ce nt nf ug
,,nu- mi,-r,1 u?sl cu be . e tu lle o~ in e
I I. C le an in g o f ap p
ar at us : The semi-mic
red -,::th J hr u, :h an d cl ea ro ap pa ra tu s ar e ge ne ra \\y
ni ng po w de r. T he ap pa ra de an ed
llr :ap w at er an d re pe .1t tu s is th en ri ns ed se \'e
ed ly wit h di1:til1Prl ra l runes w ith
u irlllable fu r ,;! 'm i- m ic ro w nt Pr . Sr ec ia l br us he s (F ig l.1
te st tu be s an d ce nt ri \) ar e
b1 ur,:t re movin g th e fu ge lu be s. D ro pp er s ar e be st de
ru bb er bu lbs or te at s an ed
throu gh 1he cu be s. T he re an d al lo w in g di.,rilled
ag en t bo tt le s ar e cl ea w ater to ru.n
ne d by re pe at ed ly f1\\i
ng tb em Wlth
:.;tilled w at er an d em pt yi
12. G as ad so rp ti on ng th em .
p ipet te : D ur in g th e
n;any gases ar e evolve idenufication of acid
d. T hese gases ar e t.e st ed ra dica ls m
by pa ss in g th.rough an ot
her re ag en L
~ ,,,.,,,.,,s --
. ,,,v I LIA: F eSO . ' Al CJ
( , fl.
J

. ,up IIJB:N iCb , Ba So

( 1f'l.l
1
219

dic ntd kaf a o f G

11011 aci . •o~ p_1
1"'
(II r.,k e II pin ch of 111i xt ui- .in
e ·1 l
bo il). No tu I h . b' Ost t Hhc, " lttI ndd 2

p- _i-·
, <f)u no t .
. I · . 1·1cu tec1 b,'-' o "Cn 'll ltur ,, u . . . ntl <lt1 11 tu • ul h . •u:u
••·,r•' ·itl rntl tc n " 111,- - - ) <.: onl'i1·rn ~ ~•w n, in th . ,, unc
Con
l and
li
M>J J l '-' foll ow, n ~ tabl 1,
nti ons UJo ry test.i; . h . irm
Ql,s erv
l nre ,•. - gi ve n in th1.: ht ,e.
- - -
w,t h - ~ .!:..___ --- _
,;ri- " ••lh-.n \.:'.;!-l."( • n r P ~ ~ Alo ry-::T:-e-"_•_ __
s. OI lh p-
, \ 1,lut wn of colo·.1rlc 8 th --J ~
t1 ll'I odo urle ss gas l 11
l\.•J,.••111 rhha r• 1,tas 1h1ou~h ?;;;,·le
.,,_ Ir tho 1, - t t um~ wat er
--•-
- - ''11 ' of he-m luho. The bm, • w n h •r
Colc •11t·ll•:,;:, l.ta~ vfl'ith t h(', So,,, -,. ..," --. - - -turn -. ttulk\·• · ro ,, eonr,'1ma .
--
_111 dl ,,I' hur111n g s uJi) hu r d ~hnss Liu, \i:IIJI t hrv"'~h , m - ,.-,-u-m_ __J
- -:-,-J><l-.,,
J)rc, .,l'r\ t
ol 1'1
1c: rnu111h: • utu1 n, w i:>lu llon
KM.l\:n.. SO,: f'On lirrn.L
. l umi ,
I
Col our less i:os wit h tho
j _.
S> --:- -
ts Pl'l!ser,1
Or hol,1

II I
.
a J>iecc of fi11ter p11µ.•r th. ppt!d .m
JlOlllJismm du:h rom ai., 110lution nt the
_ JI
of l t&t t ubo 1'h• P• 1wr ,urn s ~r.,on.
-
mou th

- " d n piece of filt er 1,. 1,c, d,pped u, l• •d

.nw U ()f t'ull ~n e ~~s ( N,S I •ce tate llOlu tinn nt th• mou th of tho
.,,., tube .
gn s )
~- --i The l•l\pur turns b row- nish hloc k. s1 con [mn s.
~.m - lo-ure d pun ge
,~-,- : :n;- ;::,'·:-7
17"~N0 1H·e•cn1 H Id - - __ __ ____,
B O II piec e of filte r pupc r dipp ed m rt
sn,r,ll ing g 11a mu l ure of st.arch and pol &M<t um iodj
de \
ube . Tho \
solu tiu n ut t ho mout h of th• u,st t
. NO, - c:on llrD U,
_ _ __ _ _....,:P:.:•:.:P:.:"::.r..:.tum s blue

11
0e1eclion of aci dic radical o f Group
lric a cid
e and add 1 ml con cen tra ted sul phl
TakP a pin ch of mi xtu re in a tes t tub le. Co1lfl.rm the aci d
s as giv e n in th e foll ow ing tab
nnd ,, arn t. No t e t he ob ser v at ion
the tab le.
rad u:al by confir ma tor y te::. ts given in - -ConOrmatory Te =
Oh s erv a t ion s Inf er enc e
11wen mix ~ll.n! \
Cl is Silver nitr utc test : OU!oolve n . pi_nch ~{
l'olourless pun gen t ft nd add silver
indica ted in tlist1tled wut cr or 2ml dtl. mln c acid
w\11l~ \
nitra te solution . formation of 11 curdy
JlON
h~dro~i de
precipiu1te wl11ch d.issolve in nmmoni11m
n1tnc acid
nnd re1111pct1rs on oddit1o n of dilu te
t-onf1rm s Cl .
-- -- -- -
ve. For ~ation I
Pe rform silver nitrntc tes t n N l(ive n abo
Br is m I
lfodd ish bro wn gn8 of O pnl c yellow precipilllle par tly soluble
indica ted nm mo mu m hydroxide indicotes Br
w11h 11u nge nt s me ll
mixture 0 ~
Lny~r ~) ii; so lw · 11 pin ch of give n
._ ____ -
'I
r 21B AText Book of Elements of Chemistry.111 s..,,

Ta semi-micro analvsis the gas evolved is nol sufficient to be passed with the ho,I
. · F' 12) I> or
a delivery tube. For such cases gas absorption pipettes ( igl. are use d.
0'

R,;I.U ; Srmi ulicro buSh fl&l , ll: ti,25 atl.Mfrpdou pipe~

flc.l•.l U: Hunn: Hl«:k

Important Note:
1. Somi micro a.noJytils j~ :iimiln.r lo m:14:ro analysis techniqu e. e xcept fi)t-~ti_o n. The fil~nlion --;-
replaced by cont rifugacior... rr ccn uifuco mncb..we nn d nppri.rnt us fo r l't~rnl mi':1'o onalyslS ta.tt: not \
n,•ail.abli! in la horutorv cht.m ••ou mnv Lnm· out t he tHl.W t! t e.'it.S by u.sw" a,•llilo.ble a.ppo.tatu.i. hv
t.nklng small nmoun t ~~ !=10luh ~n/ rcn~«mts ~d by routine tihrotion technique.
As p er syllnbus. mirturo 10 be provided to the st udent• fo~ _quulitativ• "'."'lym
of ino rgW1ic salt
m.ixt un.o shuuld. contain two bas ic nullcals of same crou.p. I h Prefore for conve.ruencc of Mt\ldcnts.,
I
· 1

nnnly.sis of nU the bnsic grouptt given be.re irs started with original solution inst~ud of u1U]g
filtrure of previous groups.

Detection of Acidic Radicals

Any two of the following acidic radica ls may be present in a given tn.ixl'llle
These are divided in lb:ree groups.
Group I: This group consists of acidic: radicals which evolve gases un lreatment
with dilute sulphuric acid. These a re car bonate (C0 , 2 ·).sulpb.1te (SQ3> ) . S ulphide (S')
and nitrite (NO,·).
Group II: This group consists of acidic r adicals which evolve gases on treatment
with concerned sulphuric acid. TI1ese are chloride (Cl ), bromide (Br ). iodide (l-) and
nitrate (N03).
Group ill: This group consists of acidic 1·adica.ls which does aol evolve gases
with clilu te or concentrated s ulphuric acid. This is sulphate (S0 42-)

Suggested Inorganic Mixtures:

Group II A: CuSO,. BiNQ3

Group lIB: As20a. SnC'2. Na2C03
Group IHA: FeSO,, CrC0:1
Gro up 11.I B: CoC!a, MnSO,
Group N: CaCh, BaSO,
f 222 A Text Oook of Elements of Cheml<try.

Jf the tnbctu:re is wb.itt•, the n <.:u' ·. Cr •·, Fe"·, Ni' ·. Co' · may be absent.
2. Flame test: The chlorides of some basic radicals are \'olatile and .
---.:;_
111
•-
. .,.Ill

11 anie of Bunsen lmrncr thc,;c chlocides .,omzes

. . respec t·1ve cutions i.n llitsc
to g,ve ll\ th,,

form. Tb~se 1onti give 11 chr.trncturistic colo ur to Bunsen flame. Therefore the Colo 0\15
. IlOSU:
t h o fl-a.mt!' cnn shuws tht• prc:;onct! of correspoo d tng . rn d 1'c n Is 1n
. n ffllXt:\Jrc
. .
Urar

Test: Moist a little of the ~ivc n mixture' hy few drop g of cone. HCI nnd Lnkc it
cleon p loti.num win , ur· char red mt1tch s ti<'k r..- glo ss rod nnd s lowly burn illon
colourle.ss Ouus.,n Dame. rl oh.J the wu·e horizonrnlly II litlle a l~ove the ~urner in lb:
outer edge of a flame. Observe th~ colour of the flame ns gwcn rn following tnbt.,
r CoJvur Ra
-J._ _ __ d_i c_o_ls_ _ _]
Rric.k rod or dull red C a:i• 7
Ccimti-On n:d S tz.

Aps,lt.t ~'l'l'-l'n
Olw.-.i;;r ct:n

'rbe colour of Lhr• Onmc c:nn he seen of the flame 1s ubs..,rv11bll! for n V<ll'y s mall
Jur11Lion. Therefore a consta nt obscr" atio n is requir<'<I.
Borax bead test: Certain coloured salts leave colou.re<I residue on dry heating
They can also form colou:red low melting borates in the form of coloured beads on
heating with borax .. The colour of these beads is characteristic of the metal present
The refore it can be used for detection of basic radica ls. This test is to b,; p or fOl'Dled
only when t he compound is coloured.
Test.: Hi,nL n plnrinum wire or glass rod s tron gly ti ll it. becomes r.,,1 hot and
diJJ the hot loop in borax powde r. The borax adllen,~ to the wire or glnss rod . Heat it
again. Tbe borax first s wells up and on furthe r hea ti ng n colourless trans parent
bead is obtained. Touch the head with the powder u.nder analysis and heaL it again
io an oxidizing Ila me (outer blue zone) till the bead melts. Observe the colour of the
bead. Note the presence of basic radicals from Lhc foll ow; ng table .

I - -- --
Coln ur
Gr.•en whe n hnr: him· when cold
Hudicals

Yellow when hClt und cold

Dnrk yellow when hor. green when cold Cr'·
ViolH when hot and cold Mn•·
Blue when hot nnd cold C-0•·
Reddis h brown when cold Ni2·

Detection ot ammonium radical:

The ammonium (NH4+) radical should test at the beginning as follow s.
 220 A Text Book of Elements a l Cherni,
1ry.1II S
-- - - - ~
,l11•t1lltJtl w 11tr r us• 1l1lut .. mtnr ,u: 1J , n.1,111 0 ._.ir- l ~ -.
"C:1~4 t
,iol ut1011 1t1 Mtu l h1..1r h H,1. tuli'l.' if e.um1J pnr1 r1f .. .,...,., 1
.._1 ore,
it1 io.60lublu. ' ro ultw.r tM>lutiun odd t ml nf d1lorofnr.n 1
o r efl r00n le lrm~hlondc Adrl I m l or ,:hlorinc """' " r
(tt:ee tlu, l ll"m t!IIJ< 81rongly of r h lo dut, l,!lka) o r a rt w
drops of ooac, n1111c uc.id . Sbtlku the. h •f>t t ubt,:
v1gnrm1."'lY nr, d wnrrn cnrf>fulty ,r 0('Cl.!AAl11':y. Allo\l. tl1~
luyun- ! (J sep urale Ub:ic.rv•· th~ i::r.1otlr u! the l•>w'-'r
lnye.r. YoUow or brown layer confir m Ur . ,
Violet coloure d l is 1. Silver nitra te tost-: perform the test as g 1,·e.n o.hnv~
pu.ng~nt gitii inWcated Fonn.utio n of a ycllow vre-c:iµltut~ insmluble i.n ·
am mon1um byclroridc ind.icatttE l .
2. Layer LP..'il. Perform t hi" lnycr test ns s)ven abovt'!.
Obsef'\"t.l the colour of the lower layer. \'iolH lnyer
c-.on fi rmA I .
Colourlt.•u or li..:bt l\Oia • is lling l N U: 1'nkc u pjnch of i;iv~n 1ni.xtUtt inn test.
brown gas ind.Jc.ntcd tube und boil w ith 2 ud d1,5:L1lled wnlt)r. llt.-t·nut. off 1.hf!
dear upp-cr s olul inn in nnothcr olunn 1<!.st lube, 1.:o0l
nnd ndd 1 nll of frc~hly prl!plLrf.!d r \.' rTOU S sulph..iu
8olut1on . SI1ukc well nnd a,ld a f1,w dro ps o! cone.
li:u1µhur1c ,wul cun•fully hy the ~irlc of 1c!lt tuU-,:,
l·'ormnt1on o f t h<' hmwn rin~ u l tlu , junc t ion of l'.m1c .
111u lrhunc: t1ci d ontl t he :;ol ution which disuppcnrll on
tihUlunJi: CUI illrw, NO, (NO, o[fiuL ~ro up al11u b~V<.a
tbis tesl.)

Detection of acidic radicals of Group Ill

Test of SO, -: Ta ke a pinch of given mixture in a test tube and dissolve il in 2
ml dilute hydrochJoric acid by boilin g if necessary. Add 2 ml barium chloride
sol ution. Formation of a white precipitate insoluble in cone. hydrochloric or nitric
acid confirms SO.-.
Detection of basic radicals

Any two of the following basic radicals from the same group wil I he 1>resent in a
given mixture. These basic radicals are divided in fol.lowing different g-roups.
Group I : This group consists of basic radicals which ca n form insoluble
precipitates with dilute hydrochloric acid. Thes1i are lead (Pbi•). silver (A1f•) or
mercurous (Hgi -)
Group Il: This group consists of basic radicals which can from insoluble
precipitates with hydrogen sulphide (H2S) in acidic conditions. These are rurther
divided in two groups depending upon the solubility of these sulphides in sodium
hydroxide solution.
 V
224 A ·r...,,-,1 Booll. of Elements of Cheml',try. c
111
:-_:-_-_
- _-_-_-_-_---~-c-
-~~~~========~==========-
CC1lnur
=---......:.=-~~
Radlco.ln - I ..,..,
~
Bluo tiOlutlun Cu 1 ' - 1
nr,-.•n l.'ll)lu tu,n Cul •. Crl' . Fu.:•, N i• •
Vwt.. 1 11o l11Uon C r-1•
lfodJu,b brown us• r~ll,,w i-o lut mn
Pink o r "mk bn.,~11 ao l ul 1(m

Syatem■llc ■naly■la ol oolullon 10 detect baolc redlcnla

4 \1 1 '
,..,.1~•
ur 1\11111 •
J
Thu 8\ttil c rnatic 11 ouJv~it:1 consi:H.S of J) recipilution or basic t'l-tdicah; in tl:"t'nr -
~ - •
1
" '" Ont
grnups and a11w,vs is of the prccipit.nt e s obtnin ed to ronfirn, the arnrticulnr radical
For t his proceed a s follows.

Detectlon ol basic radicals of group I:

To the original Bulut..ion add a little dil. H Cl anrl shake. The forniati<Jn of a wh;i,,
precip itate indicates th~ p resence of g.rouµ 1. lf nu w hite predpit~te is formed ; gl'C,ll)l
r is absen t. Then u se this so lut ion for a n a lysis u[ the group 11. li w hite precipitate is
formed: add more cliJ. HCI ti ll t ho prec ipitotioD is complete . Analsze t h e precipitat•
as given in tbe Table I
Tobie 1: An olysis of group I '
The w f:dt.(' prec1r11 t ntf' mny r n nr1m1 r•M 'I::. AKl"I (JI ll1itJf ' l1. Tn kP I h•· pr••n 111t,nt1• m n t,-s t tub~. Boil .,...~
5 ml w n tc•r fo r !, minu t.t~ und ftlll•r.
/ p-n,
-,-of:p--it-n-, -e l-\'-••--
h-t_h_e_r_r_e_
n _11_11_n_1,-,-,.- ,,-t-, -, ,-.,-t w at••r wtwu 1L 11'1 111 tlw F'1ltn1h• 10t• tto\ut.ion may
I
furuli,•. i. H1.•J(-Cl the wn ~hin~ Xo"' lukv tlw pn•c11n 1n t1• i n n t••nt 1ul>.._• \:ont.u in PhC'h . ll1,'ld1.,, thi-
/ a nd d wk,· 1t w11 h !, ml ~lliUlt 11nJ filh.•r , __j sulu lion in three, JHU1-l:i,
I
r I
If,i';;..,jpitutt-•, Tiit• hJnc.k ppl . m ny
h~ o( (J·IJ,t...·H..:NH:iCU Dli;t>Uh-c
t h e ppt. in U.5 ml .r111uiu ·t:Kltt (:I
Fih r1H,• Tlv· ,!~nlul1o n n'IH)'
cunlllln ..-\g(' I in t hrr fnrm of
11olublt.• cumplcx IA~ (N~h)1l C l
Tu the li.r • t pnrt nrld 11hou1 0.5
ml 111::i:tac add nnd o.rl lnl

I purt.i; orR CJ + J p.nn of HN0 .1) Ot\' IJi• t h~ solutl!ln rn lWf • plln.i ;.
pc11 1't e-.sium chromato (K~CrO,)
Aolution. For-mnLiou of Yellow I
und e, uporn10 the solution to
1

almu:1'1 dryness. C(H)I oo d

dissolv E- the residue in 2 mJ
I To the fir.st udd J ml dil. HNOJ.
Furm..it iu11 uf \\'hilt• JJPL
i:onfumti Ag•.
l'm>t. confirms Pb'.h.
Tn the second i,a.rt add nbout 0.5
ml potassium iodide (KJJ
1
I
1''ater. Divid., the solution in two
pan s.
To the first port add ahout I ml
of s tannous chlorid'.e solution.
Formation of c!Jrty while ppt.
I To the second pan add fl.6 ml of
potassium chromate (K,CrO,)
ond I ml acetic acid. Brick red
flp t. confirms Ag•.
solution. Formation of golde,
yt,llow ppt. confirms Pb: •.
Cool the third part thoroughly
under tap water. Appearance of
\

shiny wbit.e crystals eunlirms \

coufirm, Hg, 2•
To the second part add a piece of I
copper foil. F'orm oticm of Rllvcr I
white conting confi rm&1-11122' .
 , 1 r;'•,1,n•l..s:..------ -- -
1'ukc o. little I> -, - - - - --
J.
,,dt• ~o Iuuon ond bOWtlr•r
. 111 u - ~ __
,, , 1
If'''
,.,,,of NL rl , ·, , 0 11· •Stnc,Jl t J1 l est I\J l.,,. -- - - 22'
. ~i'J . 0 g 8 8. fllh'I , --- .,
0
( ' ',, ll o lcl ll nio,st l'l1d
- b ) ·r1
r ll1uu.s Pa1,o .
" "olv.,d /\ Udu "l>out -
. • rn " II o( urn l) tw . ml. uf SOWUl)l
. ··"
I IL'" ' ' LU e .
II
r
I<! l'ed
I Ul th
r (11l'
l•' ·;.
llrnu
Ho , a gluss i·o I 1· s t 11rnij bl e lllo u t h f
inonm indicaw ti
s '"
' ,, ti<•ll (' {' <i c n s o whi t , t f t lp p ..,,J in , Ut: t or111rrns r n lhe le
lh • t luho. <Do .
f,,,.11• · ,e \lfllus at l cone. l'I C t e tlrescnce f N _not touch ti.
f I I I. i ll tn 11 ""' t h u II ,
arntJon o or 9 nal •olut10 OUtb co111i . e mot1th of th.
preP I , n: H tn• N H , • test tub~.
~,-k r t t 1e s uitnble sol ••
~ . •· Vent f0 •
,1,,1,t.1' 1e.st s 111 the orde ,· . . • llt" Par .
,,I' ' I,a k e u p111ch. o f th l,'lvon
. I•c, Iuw. nt10 11 of •ulu tiun b . , .
1 . e lllL"tt ) per,orinmg fol\owi \
.,,,,. clc11r so Iu t1on. If' ti . tire i11 11 t • ng
,,, f• . I<: n11xt . 4'St tuhe Ad
. ,,; nc,I d ,_s solve, throw t he •ol . Ure IA n ot dio, 1· cl nhout 2 ml water und ~hnk .
•1
~-
'f' k
II
·
( 111,.. . d OP>' 1101 disso lve t, .
u U L10 11 " '" Vt, bo'I . f
·e n Plll_c h of lllixtul'e i o nd Pl'l>cced f,u-~h,,; ll or 2 miuute s. If still it.
1
11 11
test lube Ad 11 2 ·
'
\
r.• 't1iio11 n11tl p r oce e d rurt he ~• it. for 2 minutes · 1·,. . '.u.l dil. II CI uud Shnke . U' the
_.,, 1
,;
. .
Bo1I a pmch of ti
I,
. ' · > Hti 11 11 doc ·
· ., nut<I'tRsolve t hn, w the \
i e nuxturo ~ ,-
.• , 1t, ,s ,,,lve nl t u p re pru· . . ' it 11 2 ml cone H C I
""' d fu rthe r e ori1,: 1nul solutio n If 'L ... . lf ll clcu,· solu tion is for mml,
pr,1f 1!C . . .. . l is m r-oluhle . throw t h e $0 \ u 1.i0 1\ nn rl
.J. Hod a pinch of the mi.xt .
In mos t o f t h e cases the tn·e wiLb 2 ml dil. HNO, •111d ~ce ifit · .. 1 L I
. . L[ mixture will f · '. · •~ ~o uu e.
10 11~'{1H1mve. 1· ow ever. if the mixt
01
.?nl . J C " ubll' m a n y on, of th!.? Holvent 8
111
,h., ;olve 1t 111 cone. 1-INO:, o r finally. ure IS tnsoluule eve n ill d'il. HNOa then lt· y tu
HCl with l pu n of cone. HNQ ). Ill aquare gia (prepnre<l by m.i..UJ1g 3 part s of cone.
3
Thus, after selecting a s uitahl 1 .
t•ompl,•te ly pre pa re a n original solut' e ;ove n~ wl11ch can dissolve the 111i.xtuxe
t,oihng test t ube a nd dissolve it ill ~~ - or th i s, take ah~ul I g of given mixture in
1
. . ,. . . cl . ,- ml of solvtenl. Bml 1f n ecessary. ltll " cle a r
;oluuon 1s oo ta 1ne and cool. This 1s an original solution.
Notes :
I. If _co~c. HN_09 or _a~uaregia is used as a solvent th en firoceed us foliows:
Tnke I g ol. rruxt ure 1n a boiling test tube or c h in a dish and add 3 -6 ml cone. HNOa or
aqua regia and h eal the solu t ion to a lmost dryness. Cool the residue a nd add 10 m\
water a nd boil. Filter if necessary. Use the filtrate as original so\ution.
2. From t he observations of the solubility of a n1ixtu.re we can 11.:;sume about
rhe absence of certain basic radicals. E.g lf the given mixture is soluble in cold dil.
HCL the first grou p radicals are definitely absent.
;3. The colour of t he original solution may also indicate the presence of certain
basic radicals. Observe the colour and note the presence of basic radicals as given in
the following table.
 ,,c.t'
226 A T~xl Book of Elem ,ant .. o f Chcl'ni~\r\' •III t.. 1'l
...,..,.,.
f 11•,•c11,lt.111,. T hr. hludc
,, f l l liln nm~• C(llll-Oin l lw 111t ru t on .., J,lh •· . lh 1',
1-lJt rnl~ · 1 IU IIU I ;, I d r w.
&P.i ._
• '·
O"'o
1111
l. f\ l troLu umJ n•l • n l1 • Y.' r r 111111J d1l H i!.;( J
ppt. 1111, y t~ of lhtS, 'J'u k e n 1mrn ll 11u1·t.u,n u ' · • ttittJ
ti I
little• ulhy l r1l1•t1ht1I (rt-Cl.I ' lt 'I 1>JI
irlt) F',1ru m 1u , 11 11( w l 111t, 1•ri..-c--1p1tm ..-
I
\.
1 11 t 1ltai..,.,
D itidvh•l! th o ppt. ln I
m l aqucarcgin ond
. r,
f I J i•11l 1•tl h )' t b t■ h UIL t lll.tll l.(J l 1c c o rn 11li1l n
cm:o of J-th'.I ' I otu 1a m c . .
o, •
''• 1
Jlrl!JI .. Id I 1; •SU 11 n,I boil c.hu noluuon uJI Lhtt wluu: f. u n1c111 urc r1.,r-l'll..., ~
,w11porAh• t h.- so lution 11dd n m I • :.1.. ' .- · . ._..,.

to n )JUosc d.ry n US$. Cool. Cool udd '1ml wot.c.-r nr1J r1 llow ,11u.n1hug --
1ur :l 11unul{•.,. 1d1tl rtlt t:nr,t.
_ 0
add 2 ml water a nd
1--- • Filte r The soIution 1w1y C•.Jn •~
.....u t nu n n cg-""" -
Prt..>cipit.u tt!': Tho wh 1:c 1 1 Cd "
divide the soluaun In 6 Ulp huu-s of 8 1 · , C u• ' uud , •. A 1l d th,, liu
ppl. mnr hll of PIJS0 , . · · . . ,,1J~.1r
two pans. Take whit,, ppt.. in n ummonfo slowly wnh Hhllk.inJL till th,! soh.1 L1,,n -
To thu firs t pa.rt udJ s m c Us or n1nmonin.. F1ltn
te!"t tube OJld o.dtl ubout f-,----:--:---:-
1ml 1ttu.nnn u ~ chlo ridr• 2 ml a mmonium JJrei:.ipi t11tc: The wlutc l· 1ltr.ttt.: ~ l~t.-
($ 11CI:) solution. n ccln «' solution 1;u that ppl nwy I,~ of 81(01-1)•1. m ny t...1J11h111
Formn tion of dirty 1.Jw pr11 d 1ssol\'f•fl. To D1.i~olv1• t h ~ PJJt . i_n I m l (Cu f~ H 1) i)1· 1111,j
whit~ 1,r,-ciJututc rhiJ' AOlurion udd 1ml , f,nc . HCJ. U1v1dc Lh•• {C,lf!'H I •hP' H th ..
confirm• Hir>• ucvu c ac1c·I nrul U,fl ml &0lu twn m two pnrta. u.uluw-,n Ht t::olourlt;.,_
To tl10 Rcrond pnrt ndd pot.o~ium chromntc T IJ tlw fi r~t pnrt udd !.J.L:· 1. t1b tJt•1H P"-'
a piet,'1.t of oop~r foil snluuon. Formod on of t•xct•.!4:f (I( wurc,-. Thf• H"'c; J:rt, I hw,u"h lb,.
F'ormll u on of a s Lh·er yellow 1,p1. ,:onf1rmR wntor l.tC!Com,•s n11 lky solution F'nrn:uu u')-n r.it
1~
white ooot ing confirms Pb''• which confirm • Ri'· , y ollow ppt . conlirn,,
H,:'·. T n t h.-. S-L-eo 11 d part ndd (;rli • . lf t he solu1.1un I.I
U.5 ml stannous b lu e 10 colour Cui • ano I
chloride (SnCJ,J Cd>- both may I,.
solution and Jml preseot. \
so dium hyd.rolCJdo.
Formutioo of black ppl.
Solu u on + 1 ml dit
areuc acid and l n,J I I
confirnu; U1-t· pouis.-.m m !r cr0<.1·anJd,.,
fK.I F, 1t::s: 1, JI
Formnuon <)f hnck ,..i
L__ _ __ _ _ _ _ _, _ ppt cu11f1rms Cu ..
Table 3: Analysis of group 1113
Take the prec.ipitate of group IIB and add about 5 ml of cone. HCL boil for 5
minutes and filter.
Precipitate: The yellow precipitate may be of Filtrnle: Boil the solution for 5 minuics to rell10\-.
AS.S,. Dissolve ii in 1ml cone. HNO,. Add 1-2 ml H2S gas. o;~; de tbe solution in two pam.
of ammonium moly bdate solution end beat.
I. To the first pnrt a dd ammonium hydronde
Formation of yellow ppt. confirms As' '· solution till it s mells of ommonn,, aml a bout lg o(
solid oxu.lic ncid . Boil a nd 11ass H~S gos for one
minute Forma tion or ornn ge ppl. confirm• :C:b1•
2. To tho second pnrt ndd n ptPCe of zi nr metal ,nd
little cone. HCI. H unt 11nd ftlter Add \ ml oi
mercuric ch loride solution to t he f1lt:rnte
Formation of dirty wbne ppt. co1\f1rms Sn•·
 00 100 110n of Ba •lc rad lca l• or Gro up II: 225
'I'" llw or11n nnl snl ut1 on udd l 't
. 1 L1c wu
i 111111 I on o f II col our ·d rm wn te r und P '" - s H •" ,
'' • . • r
c 1 , rec
.1,, µrs• .:1p 1tn lc 1,; ,a rm e d e ven aft
1p1lule i d
1
0
" i;ns thr ou i; h ,· ,• Th"
•"'
n c11t c11 th t: Jlre sen ce of rnd icn
dil . . ls or group n . If
11 In thi s c -~r uti on und wn rm
. . .
toi ; 1t 1nd1c1Hes the abs enc e of
.:r-• "P
ih·~ 1::
·f ,. n se l 1lro w thi s l test s olu tio n
111 o s uus equ ent gTo up and u se the ori gin a l sol uti o n for
ff I he p r c-c1 pll ulc is for me d
. . LI·1 .
t ,111 pl• •Ic ori g 1na I 1'0 Iutr.o n n nd •m pn s s 11, S for 111 lea st for
2 mi11 ut<e11 thr uu~ h
' lilt "_ . . .
Th ,· C"o lou r of I h e prcc ipi tul , e r . n.1111 1y,w Lho prcc 1p1 tutc a s l(iv en m tab l e 2 .
, · d
, ,,,. ,·n ·•· 1lw col o ur u11ci nul c l can 111 1ca ll- lhl ' pre se nce of ccr tum lms ar rnd
11 ,. und e r ic:1 \1<.
~ ( 'olo ur _L Prt.-capitult=
Dla ck I Hg:S.
• Pl ,,..;,
c•
l:h•,S , ,Cu S, SnS
- -
I Y,·llov. <·d:-o.
, AJ11S, . SnS
~ r n ngc I Sb, S,
,
lfo we, e r wh en mo re tho n on e bas
ic roc-ti.c--a-l_a_r_e_ p_r_e_sen t the colour
,•.irefu lly exa mi ned as bla ck col sho uld be
ou r ma sks oth er colou rs.
~om l'ti mc s wh e n the ori gin al sol
uti on is prc pn red in HN Oa or mi xtu
, x1dJ11ng ag en ts. a yellow is h -wh re con tai ns
i te mi lky colloi dul sol uli un of sul
p:1,;.,:1ng H::S . It s ho uld no t be con ph ur ,s for me d on
fus ed for the prccip1la lc of gro up
pn •c1p11 :11c ;, n re for m e d in s uffici TT rad ica ls . Th e
en t qu a nli ty.
l'lw 11lwve pre cip ita te ma y con tai
n rad ica l uf bo th gro up llA an d
Tlrt>,;t• ca n be icie nti fie d by tre a gro up llB.
l me nt wi th sod ium hy dro xid
(ln .,1•·:i d of N aO H s olu tio n. yel e sol uti on as fol low s.
low nm mo niu ru s ulp hide (N H.)
2S sol uti on or KO H
30 /u rw n ca n als o be use d.)
Ta ke li ttle pre cip ita te of gro up TT
in a tes t tub e. Ad d Na OH sol uti on_
and warm for 2 mi nu tes. S ha ke we ll

If precip ita te is insoluble. group fIA is pre sen t an

d proceed as pe r tab \e 2.
If it is so lub le. gr ou p 118 is
pre sen t an d proceed as pe r tab \e 3.
Ta bl e 2: An aly sis of group llA
Tiw coloure d pre ci pit nte ma y con tai n
Hi: S, PbS. Bi1S ,. CuS nnd CdS. Ta ke
and a dd 5m l moder ate ly con e. HN the pre cip ita te in a test tub e
OJ. ( I par t con e. HNOa + l par t wa
ter ). Boil the sol utions for 5
mi nut es, coo l and filter.
 0410
. , 11011 o l basic rad fcala
. .
•('n tt,e onginal s o futio
- --
Uadd I
-----
o1 group Ill •
A.
---
- - _ __ __
IIIIL

-
227
~n• to convert Fe' (]~ 111) or cou . 1-L
, cl · e rrous · e. NO 1 ·
1· ,t1oniunl chloride (NH CJ) to ns) lo Fe• · "" "· >oil aud cool. (Acidi - f
.,,11 ll f ' and th , ,. err,c . non o HNO,
. 1,,rioll 6JUe s o ammonia F · 1 . e n liquor am . ions). Add abou1 2 g of 1· I
a" · l ter •\n tnon,u ( , so 1<
'fh" colour of t he pre,:· . · · a]y ze the l>t . . or NR ,OH solution) till Lhe
1Plta t i, c· . . ec1p1tate a · . .
. ,jvtu1 helow. an lUdJca t e th ,; 1(1Ven 10 Tnble ,1.
.1:, t,:
--.._ - e Presence f _·
Ct!r tu._m hns ic radicals °
r11,""' Co-
lo u.r -
• G1::lu ~u - _ _ JJ rC CJJ11li11 '-!
u,,.
11 w 1 1

J
7
'•I Brown l\l(l.lll h
Iii, ~ Y ktt.!t:nbh l;,1•(0 lth
- _ t:r(Oll1,
°"• ..---:-:;::- Table 4 : Anal .•
,,''•. fake tJ,e pr<>C1p11a1e in u test tube• }'lil~ of gro up IQ -'\
' •dtl.•bout 5 ml of wator l I I\ w-:-::-:;--;:---;:-:--:--:----- -- I
---:- _ • Boil for ?.3 • ' tn oOR And 2rnl or h,·droge-n J)troxidE-
,,
l C!f
. !'tf('lplt.t.lt~: r he ppt. may b e of Fe(Q'Lr. .- nunute5 and fi.J r.e.r. " ·
I I\
lltd
I
I
· ''
t.b1.• ppt. m - m
I d 1' I HCI
-
• . n ),. U1asnlve
• D1",de th ti~ ..i;olutton
t"Wo parts.
• in - F ilt:tJ.l_\ e__;_ Tbe e-Olution mt1y en nt3in No:iGrO•
(yellow) r., r Kn.AlO.t (culuurlt.'65) Ii it is colou.r)ce.s
-~ Obsent If 1.h (' solution Iii yollnw, er>·
t.h..- 11 C.:r't• i~
1• t h•• first ,,art adJ u few drop• r .
. I (I' fl' C
I1,r,-c,<vnnit ~
. o potn1"s1uru
' ' 'el N)o)) Pormntivn of d ••cp IJluc
rn pn•~e11 L. U1v1dl• the sol Ut°;On m ,n thrc,• p1u·t~.
T t> th.~ fir~t 1mn. uJ.J 1ml aeetic ncid nntl little
tl'1u t--:- JHn 1,lut.>I colo ur confinn t1 Fo:i ,
Tu tfw s1~,~onrl p:tr l ndri linlo a,,,m - nmu111,·
lt:nd IH'<'l nt+· Fur m ;1tiu11 1.1fyl'11ow µpt . t.:onfinns
Cr ''
I
th11IC \ ' Hllft f ( •:;o}uticm. Formu.tion or 11Joo d rc rl To the AC•cr,nd part mM f:,5 ml inlver nil.rttte
r-olo ur co nfirm:. f e-3·. solutio n. Formorion ofbl":ck red ppt. confirms
j
Cr1 ' .
To the third part ndrl n pinch of aolid NH,Cl and
heut. FormRtion of gclotinous whil e ppL confirms
Al~'.
Aluminon test for i\l'": Di•solw the ppt. obtained
in test 3 .,bove in l ,nl dil. TICl. Add lml
ammonium acctnte solution nnd 0 .5 ml nlwninon
1;o lu tiou . Add s u ffi cll·nl nmmonium c nrbunutl'
•olulion till alku.line. f ormnuon of ro,i ppt.
confirmis AP·

DelecUon of basic radicals of group Ill B:

Take 1 ml of the original solution, add 1 g solid NH.Cl. boil. cool add excess of
NH,OH a nd pass H2S gas. If a precipitate is formed , then add 2 g of solid NH,Cl to
the whole of t he original solution and boil the solulion. Cool and add excess of
' 230 _ _ _ _ __ _ _ _ _ _ _ __ __A_T_e_•_• Book of Element, of Cheminry.

l'dentifi c ation of Acid Radicals (Test for Co mmon Acidic Rad ic.als)-----
Tes t 0 ~ f ' n.'"R llO ll
lnre.c;;;-
111
S.,,,.

Te.st for CO,>- (Cw-booa1,e ): ------

To.kt.• a .smllll quanrity of It mlXt'UJ"e m U'-S f tl1he. n dd Effervesce.net! CO.s: tllft!i ('
rtboui :?ml dil H CI or dtl H: S0, Obuunc-.1 (Carbonate
Pau the t-roh :ed gns through lime wntrr Lim e water turn milk)· I CO,.t- JlTl!bt,
due t o e,,,-olution of (Cn:r+.x1D.l.\ l
CO. gas .
Tcs t Cor SO,' (Sulphate): \\' hw• pn.'-Clp~t.ulc of SO,7 pr!;!S<-nt
Solut10.ll of mu--iW1(in diL HCh BuCl: ::-i,lu11on nr BaSO, t.n::;olubll! m (Sulph•••>
Ba(NO,), S<,lu11on - L'o nc. HC I.
- -- -- -l)urk
- b nm·n nng nt
NO, Present~
Trst (or :,-JO,·{Nitrate) ('R ing t C">t):
To n ~lunon of mLX'tll~ tn w oter add equul .mwutll 1I tl' JUncrion of two \
o f fres_hl~· prepared FcSO.solunon shake & udd <-one, liquiru;
H::~O, uJong the j"H.l~ of U:~l tube wu.huut ili:;1urbrn2
thl:! solution..

Test for Cl·. Br a.ad 1-:

(i) .Mum.1.re T 2ml ronc. H,SO,, heat s lowly & ndd a YcUow green gas I Cl· (Chlonw,) -
p rnch of ~inO,. Reddish brown g
-.-.-Tj--B
- r <Btomui,)
- - -- --+- -- ,--- - -
V, ~1ct fu m e.,; I 1- (lodide)
Prepar~ a :SOiution of m.utu.re m dil H:N03 and
d.J nde the solution mu; t wo parts.
I Ag NO, le><: 1~ Part+ Ag,"10, so
-lu-□--o-'-n-.------t CurJ'\· white Cl fCWotiw,1 7
prectJ.ulattt completely
soluble w '.'<H ,O H
Pale- y~llow prec1pit are Br- (Brotn1del
Jfartly ~ol!lble NH ,OH.

ILaver Test {or Br & lo 2nd Parr - few drops of

Yellow precipitate
in soluble ill NH..Oli
Yellow1sh brown l')yer
C 1lod,de1

- ---·
nr fBromide1
I
I

I cc~ or CHCb + Cb water. shake. Viol et l ayer.

- --,----- - - -- -
C Oudidel

IDENTIFICATION OF BASIC RADICALS

Pre p ara tion of Original Solution (O.S.): Prepare the solution of a given
mi.'rtllre in diJ. HCl. lf a mi.Kttue is not soluble in cold dil. HCl, heat it. The clear
transparent solution obtained is known as original solution (O.S.). Use a small
fraction of O.S. for testing the presence of each group.
 1t·1• ~y
228 A Text Book of Element , o1 Chemist,
~-111 •• ,,,.
,,11'
-- - ~rfl r
NH,OH (or liquor n mmo11ia) Lill it smells of nmmonfo . Pass H 2S ga.s th.ro1.1 ~ 1e'
116
solution tiJJ the precipiu,tion is complete and filter. Analyze the precipitate as lli,, '
lllv• n
i.n Table 5.
The colour of the precipitate cnn indicate the presence of certain basic tad·
•~..1.
11 s given below .
Colour - - - -+-- - - Pr..:1 p1t ,_
n •_ _ - 1

I
Bluck CoS, JsiS
\Vh1to or w:·rc•y ZnS
L1~hL pink :lfoS J
Toblr 5: A_nalysis g[group U1B _ _ _ _ __
r - - - - -T-o_k_e_t_h_e-,-, .-ec
- ip_i_
tn_<_e -in- 11 teSt tube n.nd add abou t 5m l di.I. HCI. S b.u.ke wi:U u.nd filter --,
Precipi<ato: It moy be block due l-'iltr.1te · 11 may contain MnCI, and ZnCb &ii th,· solution r~ I fl
to presence of NiS nnd CoS . minutes t o remo,·c l'hS ga s Cool nod nd d excess of NoQ}l
Dissolve the residue in 2ml
aquaregin ( I.part cone. H.NOJ nnd
S<>lution. Add a few drops oi hydrogen p er oxide, boil and filter.
PrecipilOtt>: Moy be wlutii;;h nr Filt:ratc: 1t mny coolain 1I
{I pnrts cone. RCJ) nnd cvapornt<> brown. Dissolve the 1,p1 in 5ml Na2(Z.a O,). Di\-ide the solution
the solution to ulmos t dryness
Add 5ml wotor untl divide tht.•
dil. JiNO, 13011 a n<I di,;de t h e
:t0lution 111 two ports-
10 two pa rts.

Tn firRI pn r1 ndd 11 f(•w 4.li·opsof

\
N<Jlution in thruo pnrl s. To finu 1,art ndd J~ of lead C H, C-OOH nnd pngs H ,S ga,. II
To the tirst pnrt ndd I ml NH, CI dioxide ( PbO,J or n,d l~ml Format ion of wl111.u Pllt.
solu tion, litclc NH ,OH solution (Ph ,O.,) nnd 2ml of cone JJNO,. ronfirm.s Z.u>· .
and II few drops of dimethyl Boi l for one mrnu t, ·. f'onuatton Tu Lhc second pun odd 2ml
glyvJUmc (D!\-1( 1) solut;uo.
Formation of red ppt. confirms
.,..
N1 ·
of purple colour confirms M_n:r• .
T o the si,rood part add pinch of
sodium b1smuthate & s hake.
dilute HC l ond J ml potassium
forroeyanide solutions.
F o rmation of white ppt.
I I
To the second part add NH,OH . Form ation of purple colour confirm s Zn2•. I
CHaCOOH in excess and tittle confirms Mn 2• . \
potassium nitrite (}L'J0, 1
solution. Formu tion of yollow ppt.
confirms Co 2 • •
To the third portion nnd NH,CI
und NH,OH solution t ill alkaline \
I
11.nd the11 little potassium
ferricyanidc solution. Formation I
of red solution which turns to
hrown ppt. on warming confirms
I
Cot•.
Borax Bead test for Co2·: Perform
a borax bead test using either the
original mixture or ppt. of tJIB
~roup as given earlier. For mation
of a blue coloured bead confi r ms
Co 2•.
 V

- ~-
232
=-==--._-.,.-_-_-.,--:__-_-, - -_:_:_:_:_:_:_:_:_:_:_:_:_:_:_:_:_=._-
d h;d.- the ialur.io n 11110 two ~ ·· · 0
A Tex1 Book of Elements o t Chen,h;,

I .....:...::__.:::.:..:::: rv-111 s .
-=._-=._-=._-=._-=._-=._-=._-=._~-=._-=._-=._-=._-=._-=.__
..
rr~1J1ilute• F iltmte. ---
po.~ Oi.s.solw.r j1 in ntlnlmum Boil lu rutno\'r lf •S \d
I
"Pun "e.i.:c•••
... ·,. oJ' , utu••
, .. t n
· Ji lllln O I1 t yr,f
,-v nc. l:lCI, boil to . ... , 1'h t! I I u d cIdtl •H.,
,1 .a,, , c 1&d l"I Z·• ·
1
unmomn11u 1111..1 lybdotl'.I aolution rtJIUU\'t~ H:S Add NH.OH Ow1tfo tlLi: filt nu- •nt 1 \t,
& hcnt Yt!llow llroc:ipitn l(' solution till 1t 1-" nc,utrnliud llil f\:! . .--, t-.. 11 \
1
•'nnfi r·nu. AS ' (Ar~r m r ) 1110 11 odd nc~:- o ( w11t.1.• r, W h11•• l •1 11nr1 i · u m .mo ,mu 1n ~h:.lyl
2t"ll pun ·• hu t n muumuum prt.!oi11ltnh• o r hu-ln,ht y 1•u11 fi n n .i- t11..1 lu tluo, D n rlc hhw r,r., ,• 111~111
<• bo
.....n r n ni.• !llllu t aun , J\ cidiJy 'A"llh Sh' ' •Aullmony ). or ,:ulorn11ou l"tmtirn,.t:l flH.,," lu
8 11
di L H t ' I Yi:l lo w J1roo1111tnt,~ 1Tml(S1tnnuoui1) nr Sn••
cuufinm AS ' • (Ar!'il:'llWJ l1otuumc) j
2".a p :irc + H i,:Cl: 50lu.tioi1. W1.
• • •ll lp.
P l'CC Ipltiltr t umtnt: y 1,:~,
coniir,m, Sn-· or S n'•.
Analysis of Group IIIA

0 .S. + 1 rnl Cone. l·L'l/O, . 8 oi.l fur n m inutrs. Cool & ndd obou L 2 g sohd NH,CL
The n ndd cxc:~ss of NH ,Ofl soluiion till it s me Us of a mmonia. lf precipitote ia
obtninct.l. !,'l'Ot.lp I [L<\ is 11resunt. Fil tor th e sol ution .
Pr<'<'ipit Ate + <JXccss Kn OM solul io n . filter.
Prt'!ci11ltal e- F'JlLraa.ui-. - -,
Prec1p1talt-t ... (2cnJ NuO H ,._ -lml f.110:1 Hrid 1.hr- 11io luuf111 & fih ~r To I hlO filtmto, ndd • Plni:b

I
Prl!ti,pit.ate• 1-"'ULrate- of aolid r-.H,Cl & boil
01
Oi~!lolve the p re\·ipitntc in dil, HCI & To this fihm h.•, 11JJ ... .xc...ss uf Whil< gclnllnou,
\I'
divide in rv.·o pans. CH.,COOH solution. The n odd procip itat e oon.ti nus _lJ;;. t 5.(
Ci) 1n part + pot11s.siuw foud a r.eutte solution. boil it. \Aluuuruum).
Fcrrocya.nidc.- K, Fe (l ~ Yt•How precipitate confi~!!C~
.solution. Pnu;sian Llu1.• (Chromium ).
pn:cipit.alc confirms
Wernr) '
f11) i 11 d p nr1 n mmum11.1m
i h i,w::,nnntf" flo lutinn. flfood ll\!J
\
proc.1pit.0ru crm(irrn~ Fe 1•
(l~t'i'rJC),

Analysis or Group 1118

I I
O.S. in dil. HCI+ solid NH,CI + excess NH,OH. till it smells of ammonia. Pass
H2S gas. If precipitate is obtained, group UlB is present. Filter. Use this precipitate
for analysis of group 111 B.
Precipi tate + 10ml diL HCI. Shake. Do not heat. Filter it.
Precipitate• Filtrate-
Dis.wlvo I.he f>r<'<:ipitJ1te in nqunregia solution. (I Boil tho fillrttle to r emove H,S grrn. i\d,\ u.-.ss \
part cone. H NO, + 3 1>nrt cone. UCI.) Evnpornle
 .,..,s_ _ _ _ _
,,,. - - -- --
• .,.,s> ;;. , ., chi- H Cl + \'l ute
,. of G ro uP 11
l.
11 •• pr .,s . . r . ho1I & ----- -
·II ' U c nt . F, lt. ,r th l ll
r._, I I••..; ~f•~ S'-' th o flt" ~-Cll) lll
I: ,;o l . 11u so II •"' •
•~n
. ,,,11 n n10 1m t o f pr oc ip
•llc Urllo n. n·I,Ut,-,e !(UthKe. m
Ir
co lo re
'1\. al. e + or nnulybls of l,'l I lruh• d pr...-ci1H tn lc
N ao 1h
'OU p II w ith w Mer
. . b t utob&
uuoi
nu
:nd,
in
11 ,., ,,,·1v1111tu , :i 111s0\ ub \ e. i;r -o u 0
,. TI.H
! so
. lu110 - ,

~··...
..,,,,,,1. \\ ,s
I> />. L'< pr es tn l. B ut if . . su lu bl c, ..-roup II B ·••

,.•~"•' G
rJk <' pr
, oeci pi ta te of,U-A- -gT-OUp in a t .
,.,,,,.: Ll
,,, . , .. ,,~
".- .,_ ..- •2m l- w at er) . Boil &. fi ltees
r t tu be
_: --
, ad d 4 m l m od er nl t,\v Cone H ..'0
•·2
. .. ,. "
1 ,, , ,1u ,1n..·h'ln lk ul th ~ ftl tr nte la w;·
-
PT ec ip ita t.c: - -
. . Fl h. r-
_ _ _ Bdd u.f'b a of
,,, f1.T )ni t:M ,
t1 •tr• -.:on e
:, , , ,,,.,r, r,mc HCI), Du ;so h'1 t th~
.
S l\ u,uluuon & (a.\t.<r .
. · pr tt1 p1 ta i. 1.11 • - o•
·: • M°"' ue ~. ~dd wu te r - - -- - -
,.,_
,
~ t1, qu on Ol )' of d .,_ H CI & d
•
-d - • «• 1r Ut ra UO-
'"c
'
c:, n<lJ Cu -foll- Cu -foil 60_ uu on lD lO •-
- Io pa ns ..
nw um um \ ti th e fil • o\ on r..., ,a t !or \
_.
... .- .. ..,h ~'" .- hire wtucb
~

__ fitlll ~ 1:1~=· \m er
cu ric)
(1)t l np lll 'l + os

tw :n m ilk y ...
ce .s
,_ , • th • Cdl '
on lv, · B Ul . ii 11 t<
dt ,,d e th • oo\ution
tnU
co\ot t<i.
> ~• \
0
(ll1• m ut h) . lu chwcvatnluirmwa te r pa rts
• B1• \ "'
hi l 2"'pBM- + .., d , ,, T 0 th " l"
th p._rt. ad d
(1-\.,COO II <1r<>pw1.c
, uU m• \
co lo re d "'11U1t;on
,,_ , . .,;;:;::u·
y.Ur,ow ..,
~•"
-.. .-(Bismuth) . con irm s
1
\u tio n ..-ill be colou
th en
,..,,,....
•
1<0lut1o n
r! -.
•d d
po1.11a11um \
"''"°'" I
Re<ldt1h br ow n
\ pr<'<'P• 10 1• c:oafiru>' Cu' ' \
\C up ric),
·?.. port • lU ..,1uuon
I
lu l
. ye\\DW \
pr ec ip itn te conf irm
s C u"
(C up nc ).
liil\ ln lo 3" pi ut , pa ss
\i, S ga&. \
ye\lo"' p f(' cip itat<!
_..-1-- - - - - - - --- - - - - ~ \
Cd
1
' (C admiu m),
confirn>S

\
Analysis of Group 118
T ,ke th • pcec ip it ,t• of
UB "°"' inn a " " ' tube - M d ,b
ou t tO m l" '" '· KCI.
boil fo r 5 m in ut es & fi
lte r. ft luat.e-
J>reapitat.e- To tb e filtrate . ad d ?IB
,O\-1 s0\u tion rill it beco
ad d ob ou t 2gms solid mes al're)ino. 1' ,e.n
Prtcipiw te + co ne. \-{)101 oxalic acici. Soi\ & pa,_ss
Boil is obtained. filt.er.
to d1 ssolt:~ th e p~ 1p
it el e &
 - -
3. R h o d h: o 01 1 t e le s1 :

0
0
..J
.,_••
- ns \

1 a... o
0

,~J
°"'~
•o
o I .- 0
0
er' , ) o' """,
Soo...,,
"'°""""'"'"
r,.,.... " d ro o 2lh• "l < ,111 60( 01• n
p o r 0

.h h p r• •p u re d • ,. 8< I in o11 a r.Jie

'".,, 1ir i11~ I 'h •• . , Ul1 on or a1>er ll od or
ROc1 1u ,n •h r _P "" '.' It W ith 3 d: op
od tz on nt e. Fon ~ a t, o n or a bl
o r H ,.. no g.
I s,,or resl lo r H g ,' • 9 ·
Ur

I ~- C o b a lt th:•o l.-y a n a t
te st : Pince a dro
ly P rep a r d e
., ,fr11p o f bfr es h li e te a Cent or Udd P of te st solution on a_ISJ>Ot pl at e. Add
.
r~•l!.J•.-ing y so d
co b al t a a SmalJ. cry5ta1 Hu m thiocyanate
ce ta te. ,\ bl P rodu ce d o fc o ~ o m
\Je COio u r is "' g>·.
.. .. ,"
H g 2~ + C o2 · 4 sC N ·
),I
- - .C o [H g(SCN
SpO I rest fo r A
g ':
-
P o tas s iu m c L
5. u c o rn a te t es t : Place a drop of . Add a
ro m a no n o n a &J )O l p la te.
si u m c h f so lu confirms
,0 ,m l o f p o t- as te . The formation o needle like re d CfJstals
,\g.
.
? A -2 • 2
- + CrO4 - _ __,.
,\ g2 CrQ•
R h o d a n in e te st ; S o -• · h
e fi lt er pa · th a sa tu ra te d aCEtone solution of
6. "" ' t per v .,
. Now 8 1. 2 ...-ed by a drop of
the re ag e n t a n d
n
m a
th
k
e
e
fi
it
lt e
d
r
ry
p ap J 0
s _f te st so
e APP ·V.lod)oro.,tpst m n confirms Ag· .
lu tion follo

:!.\ n it ri c a ci d o r. re
HN - CO

a t - - {',. NI\
I e>t,
SC C'-'2
C>t,
s

>- : ce a
S po t te at fo r e1
p ap er u si n g th e reagent a n d pla
f
h o n in e -K l te st : Mo is te a piece o or a n g e re d sp ot is obtained
7. C in c . A n
y a c id ic le st solution upon it
h tl
drop o f th e sl ig er
confir m s Bi •.
3
er cu ry . b is m u th . lead an d copp
g m
ro p o f te st so lu ti o n con ta in in en t. four zones can be
\V h en a d w it h I.be re ag
u p o n a b so rb e n t p a p e r sonked a n o ra nge ring due to
p la c e d u ry (ii)
rad1cal11 is in g c o n ta in in g th e
m e rc
c e n tr a l r
obse rved . (i) w h it e
 - 7
234 A Text Book of Elements of Chomi s-try. 111 S..n,

1. By bringing LOge ther one drop of test solution and one drop of reagent
fil te r paper or glass .or porcelain. -
2. By placing u drop o f test solution on filte r pape r soak with particul at
reogent .
3. By ploc.ing II drop of reagent on a s mall quant ity of the solid sample or v\ce
versa .
-1. By subjecting n drop of reagent to the gases liberated by a reaction.
Th e s pot t est a,ialysis is better t han Lraditionnl m e thod of an3.lysis bccaUse
these test are easier and quicker LO carry out, inte rpcete::d more rcndily. re quire \ 1::,s
tim e and r eagents.

Spot test on filter paper:

Whatman filter paper No.3 or No. 42 are use to perform the spot t est. The paper
should be cut into strips of 6x6 or 2x2 cm depending upon the requirement. Spot
reactions on paper do not always involve [nteraction between a drop of test solution
and one of the reagents. Sometimes the paper is soaked with the reagent and dry
soaked reagent paper is spotted .,.,jth a drop of the solution. The use of filter paper
has advantages. as it is possible to detect a given ion in presence of interfering ions
without special separation.

Spot test for Pb'·'

1. Diphneyl thiocarbazone (Ditbizone) Test:
/ NI+- NH - CsHs
s- ~
N= N-CsHs

Shake vigorously a drop of the test solution in a small test tube with a drop oi a
dith.iozone solution in CCI~. The green colour of the reagent changes t o red confirms
Pb2+.
2. Benzidine test:

1-½N NI-½

Place a drop of test solution on a filter paper. To this add a drop of 5N NaOH
followed by a drop of bromine water. Add a drop of ammonia. After dryi.og the spot
add two drops of the reagent solution. A blue colouration confirms Pb 2• •
 ~J
PJticC a drop of tl
,JrvJO.d e (2""
f
,.,,) solut · tc, l •• t sot-. -- -
ton Ut10 - ---
- 1} ~
.,, (!rop o the rcag "''d 11 ,._ 11 on a ---
ch e
111 •
,rc•·1p1tate 11 t
anbrin1; r . lll\d 2
u.i;ul>
of l>ota ~ t Pin,., A -- --
sn 237..
f UJ>Jdly t d ro1, •siu,r, . dd one I
.-ADI felit for A.a'·: 0 &"r{;t:niu.h or rotrno1 ~Ynnidt: o o--'o/ ,irop ?f thu s odium
:,y- hlue t'f) t e hyil'-' fi l utuuun. lntroduc
J :J. Betendorrs tc Hfll"ll\11 Cd, , u Ut1o n {•\O'\r11) ,\ \1ro.....·t:
n
St• 'i' ·
JCI uHd two drops f · o u <lr
I o ~utu . op of "-lk .
• ..-,w 1es clurk brown a d r,,tcd ti al,n~ te
,,< n f'itia11 n (IL) ch . st •ulution n
y binck d lorid., sol"t'1 dcl two clrups of cone
211u;a... Ue to ~ on and , ·
• -+- 3Sn2~ Separation of warm. 1 he solution
- - - . '> ,, _ arsenic confirms ,, - >·
spOI test lor Sb,.: --~ + 3Sn 1 .. ''-!)

13. Rhodamine _ .,
" 'res t:
(~f\~ N \
, p ''. 0
~ J.N(CzH,~,

~ COOH

"-./
Place a drop of t he test 1 .
• -- I f . so Ulton on a sp0 t I
0 ,;rna 11 c1y~ta. o sodium ni'-'t
.. , e. S,
tir and add
Pale. Add two drops of con·c, H.CI an d
rhr reagent ch ange8 to blue. confirms $ bl• a drup nf reagent. Th~ bright colour of
15. Molybdenum blue test: Th~ r .
(H, (PM0120◄o)): Place 8 drop f h eagent 18 phosphomolybd\c acid
·011.ked with the phos h ~ bl _e test_ solution upon filter paper which bas been
, P ~mo Y_ die ec1d reagent. Hold the paper in st.eam.
Appearance of blue colouranon within a few minutes confirms Sb,, .
2
SpOI test for Sn •:

16. Moly bdenum blue test: Soak filter paper with a solution of
phosphomlybdic acid and then hold it for a short time over ammonia gas to form the
yellow sparingly soluble ammonium sal t. clry. Place a drop of the test solution on
2
r.his paper, a blue spot appears which confirms Sn • .
J7. Ditbiol test: The reagent is 4-methyl-1,2-dimercaptobenzene.

{(SR
H,C SH
 I'
236 A Text Book ot Elements of Chcmlstrv-111se.,,

bismuth. (iii) yellow ring of lead iO<tide nnd (iv) a brown ring of ioclin o libc r11tecJ 1
. ' );,
Urn reaction with copper .
8. Pyroga.llol Test:

J:.. .,-OH

UloH
Place n drop of tht: test solution on the filter poper. Expose it 1.0 lhe vnpoitrs 1,r
ummonin. 'l'httn add a drop o f dil. nitric acid and " drop of t h e reogcnL Thi' yell<iw
precipitat,; confirms Bi"' .

Spot teat for cu••:

9. Benzoin a -oxi.me (or cupron) test: Pl ace a drop of test solution on the
filter pape.r. Add a drop of the reagent and hold it over ammonia vapour . A green
colouration confirms Cu:i+.
c . H,CHOH C - c . H,
II
NOH
10. Rubeanic acid test: Place a drop of the test solution on the filer paper.
Expose it to the vapours of ammonio and add a drop of t h e r e age nt . A black or
greenish black s pot confirms Cu•·.
f-½N - C- C- Nf-½
II II
s s
Spot tffl for Cd 2':
11. 1, 5 - Diphenyl carbazide test: Place a drop of test solution on the tilter
paper. Add a drop of the reagent and hold it over ammonia vapour. A re d spot
confirms Cd 2•.
O= c( NH- NH - CsHs
N+- ,.,.._CsHs
12. Bis (p-nitrophenyl)carbazide test:

Nt-t- NH- 0 - ' N~

/ -
o= c
" ' NH- NH- o - N~
 , . y ~ .
,.
111
~ ,1c;~---·- --- ---~
-.....
¾, ,,. . d 1"111 bydroxido CNaOHJ6 •• - - - -
a.. ~
''6
..,~1 .
. n i;r-.J. ammorua 8-0lut ·
.L'lf
· " •ltll'lJo ~ : -------...-...__
~ •1,l" ' . Io n ( ·-~ n so t · -- 215
q _. IK .,. · cone. ~,
fl(jj
11" < •,-1..,,•"'··1.11te111 fcrrocyarude
(K,CrO,,)0 .5N
, ..- e(C N)
Ut1u n (dil
,~H ) 15
. . - -
- 1'H 1·N
•IO.S/11 . f " N, •ilve ' ., '. barium chlorid•
118
Of t1.
1•"'
,:,.' wl/N • ' H ) CO
:,! 5N
· n ceti
c Uci d
' e rric h · t IUlrnte
c lorrde CF lAgN0,10. 1N
•
<1a , 1',1111 . (d il •CL)O 5N .
tltt • ,, •· J)ropper Bultlt-s· 1-i"d · C H,COOH) . · P<>laasiu.m
0 •. f.••· . , •Ochlo · 5 N, .
•te i ' ,,,1J (con,;·. M, S0, )36N nc •<-ill (co n a 1n m o nium
a ,,ur1 . • , ulpt,u . • c. MCI) p
illo1- .;I ,I 1J1l . I 11'0,)5N nc ilc111 (d 1'I
8 e .,. 1 • • •
- N. h)·drochl
M,so ,sN . °""• :.cn1
• .
!d,1. l:ic.n SN
• 5 ce ntrifuge : Preci pit . t • . nnnc acid (cnnc .H.1\lO ) 16N.
. .. ·'f . a e,; lll uv ,. • .
. 1,y c·1. nll I uga tion . By r . , u e beAl
. ,1,1, r Olo t111g th . Acpu.rale d fro
• 11H I.•' i" iorced to t he bot t . e llltlClu re ut . 11\ smaU vo\.umcs of
~,,11 0 m ol the , a hi gh spe •d ·
· Ii ,,,1,•,•rl ! 1mes th e force of . t u be by th . c l.ll a centrifuge the
. . . . grav1Ly. e centn fugal force which ma
ll'ld " pnu-rn:rs. Lbe ltqwd cont3 . . · Y be
eJp l " . • · l n.t11 g the
·"' ccnLriluge tube . It is balanced b s us pended pr eci"itat . la .
:~-•· - J · Y pla •· . ,. e is P ced m a semi-
._,i,,g!l1i 11g che :,o uhon , a s econd tube of trhec~ng. d1~met ricaUy opposite lQ ~hi: tube
· ., co cha t of t he solution. S tart the cenlrifuame S\Ze containing 8 vo1urne o£ water
. •·;,u
·: r it deve lops full speed. The pre . . ge and let it run two or three • tes
;;~<' . c 1p1t ate will mm.u
.,., cantrifu gatlon ~ place s filti-a tio n f separate
0 m acro a nal , · Th
out at bottom of the tube.
.... ,..
. r~iidi ly s e pa rateo from th e preci ita b ) sis . e supernal.ant l iquid can
.< · d ·
,•uiJ so obl,11ne JS calle d t h e cen t rif u ge
,, hi h
P te V means of
Th ·
ill
cap a r y dropper . The dear
. e advnntages o[ cent rifugation are·
11• / DuE:.' to g speed
. of centrifua-e ., · t h e suspended pr eci 1'tat · dil
,,'f ra1ed frnm rhe s o lutions . ·P es are rea y
3
ihl The pr tiCipita te is conce nt r ated into
· a s ma ll vo1u me h ence can b e ob served
;,.3d1ly
(L') {'rci.:.ipitl'l te s may be washed several times rapidly and e[f1ciont\y.
(d) Concentrated a cids , a lkalies a n d oth er corrosive liquids can be handled
1J1houc diffi c u lty.
Whe n us ing a hand driven centrifuge, the following precautions must be
rorefu!Jy observed.
(a) The two tubes must be of the same size and of the same weight.
(b) Tubes should not more than three fourths full since liquids which are
spilled may r ust the machine.
(cl An unbalanced centrifuge causes vibrations and thus tubes may break.
(d) Never use centrifuge tubes with broken or cracked tips.
 240
A Tt.'Jd Book o f f lcmcn u o t Chtmlnry.
~
111
> ----
1 lace u1 drop of lh.:utru.l Lot:1I i;olut.i on on o t11>ol µhate . ALld u drop or t'Clill
IH'Clttt o solution nnd 2 Urop uf U111 r uuJ(ont A rut! colourutiun i~ obt.aincd. conn \lnt
Co' ' . ' 111<
25. Ammo,~imu t blocyunule lest : Mix u J.rup or test solution with 5 d,01,. or
soturntcd soluuou of a mmonium thiQCvnrutulc 1.n ucetono. A grc.~ to bl
'
colourntJon "ppenrs which confirms Co' ·.
. ~

co~· + 4SCN - - ,(Co{SCN ).,J2·

Spot lest lor N I'':

26. Dlmc,Chyl 11lyodme l tsl :
CH,. C = :-.JO M
I
Cl-13 - C= N 0 11
Place a dlrop of test solution on II filler papc,r. Add a drop of the reagent und bold
the paper over a m.moms vapour. A red spot or colouration is produced confirms Ni,.,

Spot test for Mn'":

27. Fonnaldoxin1e test:
M,C = NOH
r
Pince two drops of 1es1 solution cm u s pot plnte. Adel 2 dro ps or 2M i;odI u111
hydroxide und :l drops of tho rcngont. ,\ red colour confirms Mn• · . 1
28. Potass ium p e roxodis ulphate test : Place a drop of te.st solurion on a &pot
plate. Add a drop of silver nitrate soluLaon itnd stir. Lntroduce a crystal of potassium
peroxodisulphate and heat. The characteristic colour of permanganate or black PPl
of MnO~ appears confirming Mn 2•.

2Mn 2+ + 5S1 O/ .. + 8H2 O--->2MnO,1 + 10804 2 • + lGH-

Spol le1I tor Zn 2 ':

\
29. Diphenyl thiocarbazone (Dithizone) Tesl :
I
NH - NH - Ct;Hs
/
s- ~
N= N- Ct;Hs

Acidify the solu tion with acetic acid and add a few drops o! the reagent and ie,.
drops of chloroform , the organic phase turn red in presence of Zn2•.
~::'s ~ --------
tu,Ql

' pJacc n dro p of r eagent

' . UJ>on t h
·e )· t to ammonia vap0 l l t t; " fiil•- - --------
~•;•0" nrs t fo rmed clisappe . nn<J t h~n -..:or .
lo PUJlcr . Add . - _ 2:?
,,,r . d nrs lllltl P g luc j- I •• drop vf '
...J. ·uJc r vr r e s po t cc,n_firrn,:, \j·1 Hiler r._,1... . u ~cr::lic a,·,• I L,,u ,,,.H1l solu t ao11
! , •1 .. .i • • !>:Eiln h ... , l '-'11 · ·
ri" '/. 1\ lu.minon test: · "'"'" cc,l,.u, f·fl><>ur until t he b h ic
...J • o r\!c •1uuu,
. 1·,i.,t.n n. :\

Ot-;

( Y COONa
( r\
C-
-=<., ✓- o
J -
.Na Ooc . li ('
1 cooi-.i,,

OH
pia~e n ell-op of the test solution on .
· a Sl)Ot plate. Acidif · .- ·
,, aJll lllOn.Ulva pours. Add a cet ic a cid d ) with dll. HCI and expose
•t -' an a drop of
· . r<':tge nt changes to pink confirms AJ•• reagent.. The bright colour of
1h< •
3
Al ' + 3NH:i + 3H 20 -->3NH 4 • ... A.I _ .
• (OH)3(S) (whrto, gcluunuu,)
Al(O Hh +CH:iCOOH + Aluminon. reagent •(pink )

SpOfleSI for Cr,.:

23. 1,5-Dipheny lcarbazide test: i\,lix a drop of the acidified test solution with
8
drop of saturated potassium persu.lpbate on a spot plate. To this add a drop of 2.-
3,. silver nitrate solution. Keep for 2-3 minutes. Now add a drop of th e reagent.
Violet or red coloura tion confirms Cr 11 ' .
/NH - NH - C6Hl
O= C
'--..
NH-NB-CJls
2•
Spot test tor Co
:
24. Nitroso-R-Salt Test:
NO
OH

3
 ,. ~
r
,,,
•-'
. r1 •· ,
- -- -
L110ul1, 111tu,• !lo,, •• hu lo,u hu,1 , o11,..,
'""',,.•~•bl.,
Lho m,,.,.
,i,..
--
hh,.i, •••••••Hom I, "
...
. ""'"
'°"'"'"'"''""l1"'' "'"•- l)lft) th•
h
a~. II O f n......., th o f C.hri~ lury .111 !i.""
I \ ltl"
,,,...
•,,,, ..1f• I J, .." 1" h1• or ' ""'•
" " "'• .....llCt
' ••··
I\ WI
n• Mno . ••wl~,
• "'"•••
Ll
''
• llmn~- -~
OUl. r U)CCI"
111 , .
., n
A •••I '""'
"j
-
, ,,w
"'
.....
'"""""'"b"""
I
•. ..•• "'Y•Ull•"' "-•u.k &<= - • L 1I \.
'"" 1"""•"•1<1 Wit!, ..,14 .....o, . n,. 1h < " '
S•CI • ,,
'
~c-..... ,,' ""' .. ~
,:'-I /-'

I
~ c, oJ~:,
J ..
....,..~c.· ,o. .
11,...-1 N,• • ~ ... ,. •
,-. \
H<•111!

1
•,, .,.. , ' (I l l
'~ -1,i"'" " ·,
"!l U 11
nd
- _:,
.....
e lhe ppt with h t1\
, ·u:hl • , .... .. ., ... , .., 1',
•
Wnlfl r im~l
' \ a.nd "'"•lln
ru,t, 11, , 1,. lt.11 md hnc fl'lll\
I
~
4
,,..,., -=::-~11•• , di ll•'" t\•lc lltn~ f)oln1 - ......... "c
.,
{ ', ,,,,
.,.,,,... . t:
Lg ~_!' .EflllllNT-3 1
HouII: I \' tdU -
:

-~·
\fd t&11J r mn1 -
l'
•c
f1cr,i:,1ofl ,
,,,.

-n ·•
•-.ill"all I.ll /'•1111,.e>oc<Jillltlld,,. fn"'" Act wwtlll',1,
0
C CH, ~
C- Ct-1,, Mtt
0
"C C~ ,
I
' I iN Ol !H)s o . _ _
I
J _...\ NO,
lH
')
\
-"20
r EXPERIMEHT•2 - '-'''
- - ---
Oxld• don: />;~p.:lTautm vfB,m: m r ac id(,, ,,,, Brn-:altk.hydt•
a..mtc aJ Aw.do n.;

,l.CiJt,1n1llde c»ilt1Q,ac.eWinldct
1:mr..1 "°'
P.ft/UOiil~ifUint\ide
\90%1
<\Jh fm e K.\111411
c,.11,n m + (0 1 c 11t h ( ' t ')QH p1oeudUfO~
, tJ l'l1l'-'" !! i; n1.-ctttn'11tle in Ii :too ml. cuuud hot.Wm 01t!lk anll u.dd 4. ml. ~\aci•\
, ,1-,1 tc uc,il nnd 4 mL cone•H' SO •co \ \: coo\ t h c l1n1o\L m an ,cc
Bc.n.QJ J,tb }'ik 8av11 K «td bn.th.
Thi,, i~ tbr f ('3,L,rou o t (IUdJCJo n or bcnz;.;aJ dc:h)de, m t\ tel \. tube l\n'1.
!\h.-,n1wh1 le .mix 4 1nL cu.ch or curu.:..HN0 1 kllU Canc.f h SO,
' ,
u~i dTUI"·
fippa:1111» and c - ~ •:
'°'"''
\ht" m.1.nu rr. Ad.d thia n\lTi\t\ ng ffllltu re. to th\: ra\uria
C.
n ot l\d!tAn ili.de
w1,u~ witlt rltrrinu und keep \hij hnnpe. raluri, ~ \ow Uf
t, ,<Ins.~ rnt-1. tnt"lt ing poi nt
Pru t IKJUum (l<.H ) r1mdc. IOCJ m J huu..k.1.•r, funn;, ,111) i\ ft,•r t Ill' ,,drlitinn or 1Li ln.ll1\l l hHll\lr ~. f l"n\0 \'C t \w ('\""""
fTt')ln "" 1C'C b l\\.'\ &nd
ion. ttnhyd.rou~ No,COt n nu~tuf '<• m \ o '!00 UU..
ap1mr a, ~. tnple buJ.:,nn -, J.14,•n.ut.l d«'hy do , ft"a1 k.."1.n<J, Solut :,t14l,\ l •• Mtont.l rur l huur. Then trnn i\for the r••nctm
nccu,iu\,dc..
_. 1 , 1iJ V wnt cr co ntaini.nK a pieC't of crushud i.c-., LO ~et cn.u1u \')•nttrn
Proc. . . .;
. .,. . ' ' tivl Allow iL10 stnml for In minutes ,filler on ~ Buchn
er !unn., \ wit h •urtion ,wa•h
, • k e 4ml benza Jdebyd.- and 4 g anhyd rous
l!a:CO., a nd 30 ml of 5% IOfJ>O, i\id" al.,a fot111e d
(i)
n..,, Add (cw pieces of wilh colrl wu\e r ond dry in on oven Rt IOlfC. o,nittollc"tan
G-O/utio n m o mwid botrom n n~k lin ed wirb pn rur ""nde 1,,~cLl11•r with p-i•omcr hut be\11~ moro •11\ubl u 11, wntur rcmn\
n&in the fi\tr11t e.
Nnl urim1 & hunt. at. for JO
pc1n...-cfoiu to µrc,1en t bump ing u( soJucw u. ShnJrn tfu~ cil , pmt when pale yellow
M lll'<'r)' •U1lli1.r n purtmn nf crude produc t with n.-cufl
nun urt...,_ on a 3llnd bath
, solutrou and hent for IO minut oe, rrysl nit< of 11ura 1>-niirancel.nn\liue oh1.ni11crl .
( i i ) Cool <he flask , agrun add :JO ml, KMnO
(iii ) i \gain cool the Ouk and finally a dd
20ml KM,,O, solution. Bent it till
unrea cted KMnO ,. Pinnl
perm a n en t purple colour i~ oblrlio ed due to som e
hent,ng slroul d bl' done nenrly hulf an hour.
 ,,,, r,cJ--I.S __ _ __ _

;,-- 30. A.1nmon iaun : : - - - -

~erc11
,, ,vrd by a drop of cl.ii _ ry lbiocyD - . 24\
fa" 0 · ~ulph . ~Ille t . ,
~JJp-.!.r s ulphntt solution follc U r ic acid on a s p:;t.: r Ince n. dretp or t.tU;.t 1::1,0\ution .
rc.•riJJitu CC cunfinnH Zn:i,_ "-'t!d by o cl.to plnto. To this add o drop of 0.1%
P P of r ong~nl p ,
f 1ast for sr2· and ea:a,.. , o rmut.rnn of n vio\4;:t.
5po •
;1 1. S odium r-hodizo .
n 11te t e,. 1 :

CO-
CO -F
\- ONu
CO- C
O- c I
p J,.c,· " drop nf, t he neut - ONo
rn 1 lest sulu .
,.,,,,~~" ' . A bro wn o r r eddish b t1on on the til ter paper und add dr ( h
. . deli ... r o wn spot . b . . • a op o t c
'frt'SI I lie 'e ~h brown sp01 w .th ts o tn, ned which confirms S:r>· and B •-
. ' a drop of O - !\, n .
j{ bsrrurn ,., present. u· barium i · b ·" · I HCI, o bright red slain is formed
s a sent the d' .
brownish n·d culoul"ation Ol" p . . · spot tsappea.rs. lf bariulln is absent a
. . r ec1p1tate confirms Sr•· .
If lwnum 1_s pr.,se n t . proceed as. ,ollows:
, ·
.Snuk th<· filter pap~r with .
" satu ru1,•d solut· f .
- J'lm:c ii rlrop o f tes t 8 olutio 11 . h. · mn ° potas sium chro malc nnd dry
I1· o n t. lti pupe r and •11't , · ·
,~, r •1•~••11l vn rhe mo istcnted • 1>01 Al
" .. ·
. ' . e r n minute. J>lace I drup of thl!
,rownu;h spot o r riny is furmod conli:rms ~r'2 •.
,.
resl tor Ga :
::ind iurn d ihyd1·oxu1u~ ·· •·ate osa·
J ---·• w i '
, ..
. zone "-'S l :

C6H5 - NH - N = C - COONn

C0 R;, - NH - N = C - COONa
Pl!tce a drop of the neutral test solution on II black spot plate. and add little
re11gent. The formation of whi_te precipitate confirms Ca 2• • lf c1J lcium is absent, t he
reagent dissolves completely.

Spot test tor Mg 2·:

33. Titan yello w tes t: Place a drop of the test solution o n the spot plate;
introduce a drop of reagent and a drop of 2lvl NaOH. A red colour or precipitate
confil'ms Mgi•.