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Chng 1. MT S VN C BN
1.1. Phn tch h thng
Hin nay, i vi cc cation, ngi ta tm ra nhiu h thng phn tch, mi h thng c
nhng u im v nhc im ring. Hai h thng thng c dng l h thng axit - baz v h thng
H2S. Vi cc anion th khng c mt h thng phn tch cht ch no m ch c cc phng php phn
tch ring l cho tng anion mt hoc tng nhm nh m thi.
H thng cc cation theo phng php H2S: Vic phn chia cc cation thnh tng nhm theo
phng php H2S c trnh by trong bng sau:
S phn nhm cc cation theo phng php H2S
Nhm
Thuc th nhm
Cc cation thuc
nhm
HCl long
II
H2S trong mi
trng axit
(pH =0,5)
III
(NH4)2S trong mi
trng NH3 +
NH4Cl
IV
(NH4)2CO3
NaH2PO4 trong mi
trng NH3 +
NH4Cl
Mg2+
NH4MgPO4
Khng c thuc th
nhm
Phng php phn tch theo ng li H2S c u im l cch phn chia cc nhm v cch tin hnh phn
tch rt cht ch, ph hp vi vic trnh by cc s s l thuyt, c bit l vic phn chia cc nhm phn
tch c nhiu im ph hp vi vic phn nhm trong bng h thng tun hon Mendelep, do lin h
d dng gia cc phn ng hc trong gio trnh ho hc v c vi phn ng phn tch. Tuy nhin,
phng php ny c nhc im l H 2S c, nn tin hnh phn tch bng phng php ny cn phi c
trang thit b bo him tt.
H thng cc cation theo phng php axit - baz: trnh phi tip xc vi cht c H 2S,
ngi ta a ra phng php khng dng H2S, phng php ny da trn tc dng ca cc cation vi
cc thuc th nhm l cc axit v cc baz nh HCl, H 2SO4, NaOH, NH4OH. Vic phn chia cc cation
thnh tng nhm theo phng php ny c trnh by trong bng sau:
Nhm
axit
Nhm
Thuc th nhm
Cc cation thuc
nhm
HCl long
II
H2SO4 long
NaOHd + H2O2
IV
NaOH
NH4OH c d
VI
Khng c thuc th
nhm
III
Nhm
Baz
Cc phc amoniacat
Me(NH 3 ) 4 2
HCl long lm kt ta t cc dung dch mui ca ion Hg 22+ kt ta bt Hg2Cl2 mu trng, khng
tan trong thuc th d nhng tan trong HNO3 (y l im khc vi kt ta AgCl).
Hg2(NO3)2 + 2HCl
Hg2Cl2 + 2HNO3
NH2HgCl + Hg + NH4Cl
HgI2 + Hg
CO CO - CONa
Ba + 2NaCl
CO CO - CONa
CO CO - CONa
Ion Sr2+ cng to kt ta mu nu cn Ca2+ th khng.
Tuy nhin, Stronti rodisonat tan trong HCl long ngui, cn iu kin ny bari rodisonat chuyn
thnh hirorodisonat mu ti kh tan.
3.3. Mt s phn ng c trng ca ion Ca2+
Cc phn ng c trng ca ion Ca2+ cng tng t nh ca ion Ba2+
Phn ng vi H2SO4 v cc dung dch mui sunfat
Axit sunfuric long v cc dung dch sunfat tc dng vi dung dch c cha ion Ca 2+ to ra kt
ta tinh th CaSO4 mu trng, c tan tng i ln so vi cc sunfat nhm II khc, l 2g/l ( T CaSO4 =
2.10-4 ).
Ca2+ + SO42- CaSO4
Khc vi cc kt ta SrSO4 v BaSO4 , kt ta CaSO4 tan c trong dung dch amoni sunfat do
to thnh phc tan theo phn ng sau:
CaSO4 + 2 (NH4)2SO4 (NH4)2[Ca(SO4)2]
V vy, ta cng c th dng (NH4)2SO4 kt ta Ba2+ v Sr2+, tch ra khi Ca2+.
Phn ng vi (NH4)2C2O4
Amoni oxalat tc dng vi dung dch Ca2+ cho kt ta tinh th CaC2O4 mu trng, tan trong cc
axit v c long nhng khng tan trong axit axetc, y l im khc so vi cc oxalat nhm II khc, nn
phn ng ny c dng nhn bit ion Ca2+ :
Ca2+ + C2O42- CaC2O4
3.4. Mt s phn ng c trng ca ion Sr2+
Phn ng vi H2SO4 v (NH4)2SO4
Axit sunfuric long v amoni sunfat tc dng vi dung dch c cha ion Sr 2+ nng to ra kt ta
tinh th SrSO4 mu trng:
Sr2+ + SO42- BaSO4
Sr2+ + (NH4)2SO4 SrSO4 + 2NH4+
Phn ng vi (NH4)2CO3
Khi cho (NH4)2CO3 tc dng vi dung dch trung tnh cha ion Sr2+ ri un nng, ta c kt ta
SrO3 mu trng tan trong axit v c v axit axetic:
Sr2+ + (NH4)2 CO3 SrCO3 + 2NH4+
SrCO3 + 2H+ Sr2+ + H2O + CO2
Phn ng vi (NH4)2C2O4
Amoni oxalat tc dng vi dung dch Sr 2+ cho kt ta SrC2O4 mu trng, tan trong cc axit v c
long v tan c trong axit axetc:
Sr2+ + (NH4)2C2O4 SrC2O4 + 2NH4+
Mu ngn la:
y l phn ng kh c trng nhn bit cc cation nhm II, cc mui d bay hi ca bari
trong ngn la kh khng mu to thnh ngn la mu vng lc; mui canxi c mu gch, mui stronti
coa mu cacmin.
Mun cho kt ta Al(OH)3 tan hon ton to thnh AlO2- thi phi thm d OH- , mi trng pH
= 11, qu trnh chuyn l hon ton, ngc li mun chuyn AlO 2- thnh kt ta Al(OH)3 th phi ly bt
OH- trong dung dch, mun vy ta thm mt axit yu l NH 4+ v un nng dung dch NH3 bay i, cho
cn bng chuyn mnh v pha to kt ta.
Phn ng vi thuc th hu c alizazin S
Trong mi trng NH3, ion Al3+ to vi thuc th hu c alizazin S mt kt ta mu thm gi
l sn nhm, y l phn ng rt c trng v nhy pht hin ion nhm nhng khng phi l phn ng
chn lc v cc ion Sb3+, Sn4+, Zn2+ cng to c vi alizazin cc kt ta mu xm, da cam v vng
nn phn ng phi thc hin rt cn thn nh sau: nh 3- 5 git dung dch alizazin 0,1% pha trong ru
vo dung dch th, sau thm dung dch NH 4OH long n khi c phn ng kim, un si 2-3 pht,
quay li tm kt ta lng xung y ng nghim. Nghing ng nghim v nh tng git axit CH 3COOH
long theo thnh ng nghim axit ha nh phn dung dch cho n khi mt mu tm ca alizazin S d
s chuyn thnh mu vng, nu c Al 3+ ta c kt ta mu son ti rt p, nu t Al 3+ th dung dch
nhum mu .
4.3. Mt s phn ng c trng ca ion Cr3+
Phn ng vi thuc th nhm
Thm t t tng git dung dch kim long vo dung dch cha ion Cr3+, kt ta v nh hnh dng
keo hidroxit Al(OH)3 mu lc xm c hnh thnh:
Cr3+ + 3OH- Cr(OH)3
Cng tng t nhm hidroxyt, tnh axit v tnh baz ca hidroxit crm u yu, Cr(OH) 3
H3CrO3 HCrO2. H2O, trong mi trng axit:
Cr(OH)3 + 3H+ Cr3+ + 3H2O
Cn trong mi trng kim:
Cr(OH)3 +
lu trong khng kh, kt ta dn dn s ha xanh, c bit khi c mt cht oxyhoas n s bin thnh
xanh m rt nhanh v Fe2+ b oxyhoa thnh Fe3+ v to thnh kt ta Fe4[Fe(CN)6]2:
Fe2[Fe(CN)6] + 3O2 + 6H2O 2Fe4[Fe(CN)6]2 + 4Fe(OH)3
Phn ng vi dung dch kali hay amoni thioxianat vi ion Fe3+:
y l phn ng rt c trng ca ion Fe3+ , to thnh nhng phc cht tan mu mu c thnh
phn thay i ( s phi t SCN- thay i t 1 n 6 ) ty thuc vo nng ca ion SCN- trong dung dch.
Phn ng ny kh nhy, tuy nhin rt d b nh hng bi cc cht to phc bn vi ion Fe 3+ hay
cc cht c kh nng to kt ta hay hp cht km phn li vi ion SCN- .
Phn ng vi dung dch axit salixilic C6H4(OH)COOH vi ion Fe3+:
Axit salixilic vit tt l H2Sal, trong mi trng axit mnh pH ~ 1 to vi ion Fe 3+ mt ion phc c
mu tm nht, thnh phn ca phc l 1:1, [Fe(Sal)] +; khi tng pH ca dung dch, thnh phn v mu ca
phc s thay i: trong mi trng axit yu pH ~ 4 l phc [Fe(Sal) 2]- c mu da cam, trong mi trng
kim yu pH ~ 9 l phc [Fe(Sal)3]3- c mu vng.
Khi thay axit salixilic bng mt dn xut d tan hn ca n l axit sunfosalixilic th phn ng
cng xy ra tng t nhng nhy hn rt nhiu. Phn ng c s dng xc nh st bng phng
php o quang, thng c thc hin mi trng kim pH trong khong 9 11 cho hp cht phc c
mu vng.
5.3. Cc phn ng ca ion Mn2+
Mangan c th tn ti trong cc hp cht vi nhiu ha tr khc nhau nh 2, 3, 4, 6, 7, trong
ion Mn2+ tng i bn, dung dch nc ca ion Mn2+ c mu hng nht, c phn ng axit yu.
Phn ng vi thuc th nhm:
Khi kim ha dung dch Mn2+ th c kt ta trng tch ra pH > 8,8 ( dung dch Mn 2+ 0,01M), kt
ta ny d tan trong axit long v mui amoni, tan mt t trong kim d do to thnh phc hidroxo:
Mn(OH)2 + 2NH4+ Mn2+ + 2NH3 + 2H2O
Mn(OH)2 + OH- Mn(OH)3Kt ta Mn(OH)2 d b oxyha trong khng kh lm cho mu bin i dn gch v cui cng
l nu en ca oxit mangan, hoc nu c mt cht oxyha th Mn(OH) 2 s b oxyha nhanh hn.
Phn ng vi dung dch amoni pesunfat ( NH4)2S2O8 trong mi trng axit
y l phn ng rt c trng tm Mn 2+ , phn ng xy ra trong mi trng axit v c xc
tc bi ion Ag+, to ra ion MnO4- c mu tm rt c trng:
kt ta mu trng
Khi thm t t dung dch KCN vo dung dch ion Cd 2+, trc tin thy xut hin kt ta Cd(CN)2
nhng sau kt ta tan ngay trong thuc th d to thnh ion phc:
Cd2+ + 2CN- Cd(CN)2
Cd(CN)2 + 2CN- [Cd(CN)4]2Phc xyanua ca cadimi l km bn nht trong cc phc xyanua ca cc ion kim loi nhm V, v
vy c th dng H2S pht hin ion Cd2+ trong iu kin c cc cation nhm ny nu dng KCN
cn:
[Cd(CN)4]2- + 2H2S CdS + 2HCN + 2CN6.4. Cc phn ng ca ion Ni2+
Phn ng vi thuc th nhm:
Cng ging nh ng v cadimi, lng nh amniac kt ta c Ni 2+ to thnh hidroxit cadimi
dng keo, c mu xanh lc nht, rt d tan trong thuc th d do to thnh ion phc [Ni(NH 3)4]2+:
Ni(OH)2 + 4NH3 [Ni(NH3)4]2+ + 2OHPhn ng vi dimetylglyoxim- thuc th Sugaeep:
Trong dung dch amniac, dimetylglyoxim to vi Ni2+ mui ni phc mu hng ti
dimetylglyoximat niken, rt t tan trong nc:
y l phn ng rt c trng nhn bit niken. Cc cation to hidroxit khng tan trong
nc cn tr phn ng.
6.5. Phn tch h thng cation nhm V: xem gio trnh thc hnh
Cc anion
c tnh ca nhm
thuc th nhm
Mui bari ca cc
anion ny t tan trong
nc nhng tan trong
axit long (tr BaSO4)
BaCl2 trong mi
trng trung tnh
hay kim yu
mui bc ca cc
anion ny it tan trong
nc v trong HNO3
AgNO3 khi c mt
HNO3
Khng c thuc th
nhm
Ion cc bonat CO32Ion phot phat PO42Ion silicat SiO32Ion borat BO2- hay B4O72Ion clorua Cl-
II
III
Phn tch cc anion c nhng c im ring khc vi cc cation, do cc anion thng khng cn
tr nhau. Chnh v vy, i vi nhiu anion, ta c th s dng cc phn ng c trng tm chng
ngay trong cc phn ring ca dung dch nghin cu. Vic s dng phn tch h thng ch thc hin
trong cc trng hp phc tp khi trong dung dch c mt cc anion ca cc cht kh hay ca cc
cht oxi ho.
7.1. Phn tch anion nhm I
Nhm I bao gm cc anion SO42-, CO32-, PO43-, SiO32-, hay B4O72-, SO32-, S2O32- Cc anion nhm
ny c cc c im l to vi Ba2+ cc mui t tan trong nc, nhng d b ha tan trong cc axit v
c long (tr BaSO4), v vy, thuc th nhm bari clorua BaCl 2 ch kt ta cc anion ni trn trong
mi trng trung tnh hoc yu.
Bng 7.1. Mt s phn ng c trng ca cc anion nhm I
Thuc th
BaCl2 trong mi
trng trung tnh hay
kim yu
Tc dng ca HCl
i vi cc mui bari
Hn hp MgCl2 +
NH4OH +NH4Cl
SO42-
SO32-
S2O32-
CO3
PO43-
SiO32-
BO2-
Kt ta
mu trng
BaSO4
Kt
ta
mu
trng
BaSO3
Kt ta
mu
trng
BaS2O3
Kt ta
mu
trng
BaCO3
Kt ta mu
trng BaHPO4
Kt ta
mu trng
BaSiO3
Kt ta
mu trng
Ba(BO2)2
Khng tan
Tan v
c kh
SO2
Tan v
c CO2
Tan v
c CO2
Tan
Tan v c
H2SiO3
tch ra
Tan
Kt ta
MgNH4PO4
Kt ta
mu trng
mu trng
MgSiO3
Kt ta mu
vng
Cc axit
Kh
SO2
C SO2
v S tch
ra
Kh CO2
Cc mui NH4+,
NH4Cl, (NH4)2SO4
Dung
dch
mu
hng
Fucxin
Lam
mt
mu
hng
Mu ngn la
Natrinitropruxua
Na2[Fe(CN)5NO]
Xanh lc
Cl-
Br-
I-
S2-
AgNO3 khi c mt
HNO3
kt ta mu trng
AgCl
Kt ta mu vng
AgBr
Kt ta mu vng
AgI
Kt ta mu en
Ag2S
Tc dng ca cc
mui bc vi dung
dch NH3
Tan, to thnh
[Ag(NH3)2]Cl
Tan r rt, to
thnh
[Ag(NH3)2]Br
Thc t khng b
ha tan
Khng tan
Cc cht oxihoa
mnh (KMnO4,
K2Cr2O7)
Thot ra Cl2
Thot ra Br2
Thot ra I2
Thot ra S
Nc clo (khi c
Mu nu Br2
Mu tm I2
mt ca benzen)
NaNO2 hay KNO2
khi c mt ca
H2SO4
Thot ra I2
H2SO4
Thot ra kh H2S
Pb(CH3COO)2
Tinh th mu
vng PbI2
CbCO3
Kt ta vng CbS
Fluorecxon
Mu hng eosin
Mu eosin
Axit fucxinsunfua
Mu tm
Na2[Fe(CN)5NO]
Mu tm
Na2[Fe(CN)5NO]
NO2-
Vng mu nu ca phc
[Fe(NO)SO4]
Vng mu nu ca phc
[Fe(NO)SO4]
iphenylamin
Antipyrin
Mu r ca nitro- antipyrin
Mu xanh lc r ca nitrozo
antipyrin
Cu + H2SO4
Tch kh NO2
Tch kh NO2
KI khi c mt H2SO4
Tch I2
Lm mt mu tm
Thuc th Grigg
To dung dch mu
Tch N2
Thuc th
Ni chung, vic phn tch tm cc anion thng thc hin trong tng phn dung dch ring, khng
nht thit phi theo mt quy trnh nghim ngt. Ngi ta ch s dng cc phn ng tch trong mt s
trng hp phc tp, v d nh khi ng thi c mt cc anion Cl -, Br-, I-, hay S2-, SO32-, S2O32- v SO42-.
Thng tin hnh th trc cc dung dch phn tch xc nh trong dung dch vng mt cc
anion no. Sau , tin hnh tm cc anion ring bit c mt trong dung dch.
BI TP P DNG
1. Gii thch ti sao thuc th nhm ca cc cation nhm I (Ag +,Pb2+ v Hg2+) l dung dch HCl
long, ngui m khng phi l HCl long nng, dung dch NaCl hoc HCl c.
2. Vai tr ca C2H5OH khi c s dng vi H2SO4 long lm thuc th cation nhm II?
3. Vai tr ca H2O2 khi c s dng vi NaOH lm thuc th cation nhm III?
4. Trnh by s tch v nhn bit tng cation trong hn hp sau:
a/ dung dch A: Pb2+,Ba2+;Al3+,Cr3+,Fe3+,Mg2+
b/ dung dch B : Ag+,Ca2+,Pb2+,Zn2+,Fe3+,Cu2+.
c/ Dung dch C: Pb2+,Ba2+,Ca2+,Al3+;Zn2+,Fe3+.
6.Cho 10 ng nghim , trong mi ng ng 1 mL cc dung dch sau:
NaCl; CdSO4; Pb(NO3)2; Ba(OH)2 ; Na2S2O3 ; BaCl2; FeSO4 ; KI ; NaHCO3 ; NH4SCN . Ch dng
cc vi ng nghim, ng nh git, dung dch HNO 3 v dung dch phenolphtalein, hy trnh by
cch nhn bit tng ha cht.
7. Cho 9 ng nghim, mi ng c 0,5 mL dung dch cha mi cht sau:
NaCl AgNO3 KI
HCl
Pb(NO3)2
BaCl2 H2SO4
Na2CO3
NaOH
Ch dng cc vi ng nghim, cc ng nh git v dung dch phenolphtalein c th nhn bit tng
dung dch . Trnh by phng php .
Gi cch trnh by:
- C 9 ng nghim ng dung dch mu, ln lt c nh s t 1 n 9.
- S dng ng nh git trch mi ha cht ra vi ng nghim (khong 5 git) lm mu th, ln lt
nh s th t tng ng. Lu khng chm u ng nh git vo thnh ng nghim.
- Ln lt nh 1-2 git dung dch phenolphtalein vo tng mu th, mu th no chuyn mu
dung dch sang hng l Na2CO3 v NaOH.
8. Cho hn hp cc ion SO42-; SO2-3; S2-;S2O32- v Na+. Trnh by cch nhn bit tng anion trong
hn hp .
9.Cho hn hp cc ion SO42-;CO32-;S2-; PO43-; K+. Trnh by cch nhn bit tng anion trong hn
hp.
10. Cho hn hp cc ion: Cl-,SO42-; NO3-,CO32- , Na+. Trnh by cch nhn bit tng anion trong
hn hp