Giao an phn tch silicat

1
CHUONG 1
PHN TICH THANH PHN HOA HOC
CAC NGUYN NHIN LIU VA SA N PHM SILICAT

1. Muc dich - qui djnh
1.1 Muc dich.
Xac nh ham lng cac xit SiO
2
, Al
2
O
3
, Fe
2
O
3
, CaO, MgO, CKT, MKN, SO
3
. . . t
san phm va cac nguyn liu nganh silicat
1.2 Mt s qui djnh chung.
Khi tin hanh phn tch hoa hoc yu cu du ng:
- Hoa cht co tinh khit loai 1 hay loai 2
- Nc ct lam dung mi phm. Nc ct tiu chun khng c co cac ion Cl
-
,
Ca
2+
, Fe
3+
- Cn phn tch ( c hoc in t ) cn co chnh xac n 0,0002 gam
Tt ca cac phep xac nh phai tin hanh song song v i 3 mu ly gia tr trung bnh
cng.
1.2.Cac khai nim v phn tich.
1.2.1.Phn tch nh tnh: la toan b cac phng phap nghin cu hoa hoc, vt ly va hoa
ly, cac phng o cho phep xac nh ban cht v c hay hu c cua cht phn tch, thanh
phn nguyn t va nguyn t cua no, cung nh phat hin thanh phn chu yu va cac tap
cht co trong mu nghin cu.
1.2.2 Phn tch nh lng: la xac nh thanh phn nh lng cua cac cu t co trong
i tng phn tch (thng la anh gia lng tng i theo %). Cac cu t y co th
la cac nguyn t, ion, cac hp cht, cac pha, cac gc hoc cac nhom chc (trong phn
tch hu c).
1.3 Khai nim chung v pha mu.
Mun phn tch nh lng mt mu cht nao o bng phng phap hoa ho c th cung
ging nh phn tch nh tnh, ta phai chuyen t th b t rn sang dang dung dch, qua
trnh o c goi la pha mu. Hin nay co th chuyn sang th kh phn tch.
Tuy theo ban cht cua mu phn tch ma ta hoa tan no nhit thong hay nhit
cao trong nc, trong axt, trong kim hoc trong dung dch mui. Vi nhng tac nhn
trn khng hoa tan c mu th phai nung chay mu vi cht long( phu gia) thch hp
chuyn v dang h p cht hoa tan trong nc, trong axt. Do o ta co hai phbg
phap pha mu sau:
1.3.1 Pha mu bng phng phap t.
Tac nhn hay dung la nc, HCl, H
2
SO
4
, HNO
3
, HF, HClO
4
, hoc hn hp cac dung
dch axt, cac dung dch hirxt kim. Qua trnh tin hanh trong cc thuy tinh co y
np . Ban u nhit thng, kt thuc qua trnh phn giai mu thng tin hanh
nhit cao hn( bp cach thuy, cach cat, hoc lo nung).
Sau y la cac tac nhn hay s du ng
Giao an phn tch silicat
2
Dung tac nhn axit
Dung HCl
y la axt thng dung nht. No co u im la no d bay hi khi sy hoc nung va
cac mui clorua ph n ln d hoa tan trong nc. Phan ng ion xay ra:
- HCl hoa tan kim loai
Me + 2H
+
= Me
2+
+ H
2

- HCl hoa tan h p kim kim loai vi mt lng nho As, Sb, P
- M
3
X
2
+ 6H
+
= 2XH
3
+3M
2+
( y X = As, Sb, P). Nhng hp kim cua Fe
vi Cr, Ni, Ti, cac khoang cacbnat va qung nh: a vi, lomt. . . khng dung
HCl hoa tan c ma phai nung chay.
Dung HF
HF la axt Flohiric vi s co mt cua cac axt H
2
SO
4
, HNO
3
, HClO
4
se phn huy tt
ca cac silicat va giai phong SiF
4

SiO
2
+ 4 HF = SiF
4
+ 2H
2
O

Dung tac nhn kim
Dung NaOH, KOH dung djch 35%
Thng dung phn giai cac hp kim nhe ( Al, Zn, Si va Mg). Muc ch chuyn kim
loai sang hp cht d tan.
V du i vi nhm va kem:
2Al + 2OH
-
+ 2H
2
O = 2AlO
2
-
+ 3H
2

2Zn + 2OH
-
+ H
2
O = 2ZnO
2
2-
+ 2H
2

1.3.2.Pha mu bng phuong phap kh.
y la phng phap nung chay mu vi cht chay th rn.
Co 2 loai cht chay: cht chay axt va cht chay kim.
- Cht chay K
2
S
2
O
7

Ngc lai vi cht chay kim. S dung trong trng hp cac thanh phn co tnh kim
( cac oxt kim loai).
- Cht chay kim ( cacbnat kim hay cac hydrxyt kim hay cac hn hop kim )
S dung khi chuyn cac thanh phn co tnh axt vao dung dch (cac sunphat, silicat)
thng dung nht la:
+ Na
2
CO
3
(nhit nong chay la 849
o
C)
+ K
2
CO
3
(nhit nong chay 909
o
C)
+ NaOH (nhit nong chay318
o
C)
+ KOH (nhit nong chay360
o
C)
+ Na
2
O
2
, Na
2
CO
3
+ S
V du:
- Cac cht chay cacbnat
Na
2
CO
3
, K
2
CO
3
, dung pha cac mu slicat, sunfat, thach anh, thuy tinh, gm s,
men s . . . ).
Giao an phn tch silicat
3
Khi phn giai cac silicat se xut hin cac silicat va aluminat kim, con cac xt khac
thanh cacbonat, v du:
M
e
SiO
2
+ Na
2
CO
3
= M
e
CO
3
+ Na
2
SiO
3

Sau khi hn h p no ng chay trn ngui, se dung nc hoc HCl chuyn v dung dch,
luc nay tach c vi cac thnh phn tan khac.
- Nung chay vi hirxit kim.
Thng dung nht la KOH va NaOH. Cac hydrxit nay tac dung manh hn cacbnat
thng nhit t 500
o
C- 800
o
C thng dung phn giai cac qung Sb, Sn, Pt i
khi phn giai cac silicat
Cac phuong trinh phan ung hoa hoc xay ra khi pha mu
phan ng nung chay mu va sa nhit 800- 900
o
C
+ t set:
Al
2
O
3
.2SiO
2
.2H
2
O +3Na
2
CO
3
=

2Na
2
SiO
3
+ 2NaAlO
2
+ 3CO
2
+2H
2
O
+ Cac loai trng thach
K
2
O.Al
2
O
3.
.6SiO
2
+ 6Na
2
CO
3
= 6Na
2
SiO
3
+ 2KAlO
2
+ 6CO
2.
Na
2
O.Al
2
O
3
.6SiO
2
+ 6Na
2
CO
3
= 6Na
2
SiO
3
+ 2NaAlO
2
+ 6CO
2

Cac nguyn liu khac :
CaO.SiO
2
+ Na
2
CO
3
= Na
2
SiO
3
+ CaCO
3

MgO.SiO
2
+ Na
2
CO
3
= Na
2
SiO
3
+ MgCO
3

Fe
2
SiO
5
+ Na
2
CO
3
= Na
2
SiO
3
+ Fe
2
O
3
+ CO
2

Chuyn cac silicat v dang dung dch bng HCl
Na
2
SiO
3
+ HCl = H
2
SiO
3
+ NaCl
NaAlO
2
+ 4HCl = AlCl
3
+ NaCl + H
2
O
KAlO
2
+ 4HCl = AlCl
3
+ KCl + 2 H
2
O
Fe
2
O
3
+ 6 HCl = 2 FeCl
3
+ 2 H
2
O
CaCO
3
+

2HCl = CaCl
2
+ H
2
O + CO
2

MgCO
3
+ 2 HCl = MgCl
2
+ CO
2
+H
2
O
Con H
2
SiO
3
em nung:


H
2
SiO
3
= SiO
2
+ H
2
O
SiO
2
+ 6 HF = H
2
SiF
6
+ 2H
2
O
H
2
SiF
6
-> SiF
4
+ HF
1.4.Tng quat v cac phuong phap phn tich silicat.
Mun phn tch mt mu silicat, trc ht xac nh m va lng mt khi nung
(MKN ) cua mu th. Sau o tip tuc xac nh ham lng cua cac xt sau: SiO
2
,
Fe
2
O
3
, Al
2
O
3
,CaO, MgO ,TiO
2
, MnO
2
...
xac nh ha m l ng cua cac xt co hai phng phap
1. 4.1 Phng phap chun .
Giao an phn tch silicat
4
Du ng komplexon III ( EDTA) xac nh nhanh Fe
2
O
3
, Al
2
O
3
, MgO trong phn tch
hang loat ( phng phap nay khng c du ng khi phn tch trong tai v mc chnh
xac co han )
1. 4.2 Phng phap nung cn.
Thng dung khi phn tch trong tai v mc chnh xac am bao hn phng phap
komplexon III


































Giao an phn tch silicat
5
CHNG 2
THUC NGHM PHN TICH THANH PHN HOA

2.1 Xac djnh thanh phn hoa hoc cua ximng.
2.1.1 Xac djnh d m.
a) Dung cu:
- Hp thuy tinh co np cn hoc chen s dung tich 50 ml.
- Bnh hut m, tu sy.
b) Cach lam: Cn mt mu ximng cho vao chen s.
Cho chen s co cha mu vao tu sy va sy trong khoang nhit = 105- 110
o
C
khoang 2-3 gi ly ra cho vao bnh hut m, ngui n nhit pho ng sau o em cn.
Lam lai vi iu kin trn trong 30 phut va cn nh vy cho n khi at trong lng
khng i
m (%) cua ximng tnh bng cng thc :


g
G G
W
100 ). ' (
=
Trong o :
G - la khi lng cua mu va chen s trc khi sy (g)
G

- khi lng cua mu va chen s sau khi sy (g)

g - khi lng mu(g)
2.1.2 Xac djnh luong mt khi nung ( MKN )
a)Dung cu:
- Hp thuy tinh co np cn hoc chen s dung tich 50 ml.
- Bnh hut m, tu sy.
-Lo nung.
b) Cach lam :
Cn 1 gam mu ximng, cho vao chen s nung trong lo nung 950
O
C -1000
o
C
khoang 1 gi . Ly ra cho vao bnh hut m, lam ngui nhit phong va em cn.
Nung lai vi nhit trn trong 15 phut va cn lai nh vy n khi lng khng i.
Ham lng % mt khi nung (MKN) tnh theo cng thc:


g
C C G G
MKN
100 ). ' ( " '
'

=

Trong o: G - khi lng mu va chen s sau khi sy( g)
G - khi lng mu va chen s sau khi nung (g)
C - khi lng chen s sau khi sy (g)
C - khi lng chen sau khi nung (g)
g - khi lng mu (g).
hoc MKN co th tnh theo cng thc sau:
Giao an phn tch silicat
6


W
W
g
G G
MKN

=
100
100 100 ). ' (


Trong o : G - khi lng mu va chen trc trc khi nung (g)
G

- khi lng mu va chen sau khi nung (g)

g: khi lng mu( g)
W m tnh bng %
2.1.3 Xac djnh ham luong SiO
2
va cn khng tan
a) Nguyn tc cua phng phap
Hoa tan ximng trong HCl c co thm NH
4
Cl pha keo, loc, nung va cn axt
silc va cn khng tan.
b) Hoa cht :
- axt HCl dung dch d = 1,19
- NH
4
Cl tinh th
- Nc ra : axt HCl dung dch 5%
- axt HF 40%
- axt H
2
SO
4
dung dch d =1,84
- KHSO
4
tinh th
c) Cach lam :
Cn 1 gam ximng va cho vao cc dung tch 100ml. Tm t bng nc ct va dm
tan ht cuc. y cc bng mt knh ng h , cho t t 5ml HCl (d=1,19) qua ming
cc, dung ua thuy tinh dm tan ht nhng hat en. Cho vao 0,5gam NH
4
Cl khuy
cho tht u. trn bp cach thuy khoang 30 phut. Trong thi gian o khuy nhiu
ln, chu y dm tan nhng cuc b van. Nu dung bp cat phai gi nhit khng qua
100
o
C. Sau o ly ra cho 50ml nc si, trn u, lng, loc qua giy loc khng tan
chay va. Dung HCl 5% un si ra ht kt tua va loc gan 3 ln. Sau o tip tuc ra
kt tua bng nc ct un si n ht ion Cl
-
(th bng dung dch AgNO
3
1%) nc
loc va nc ra gp va o cc 500ml va gi lai xac nh cac thanh phn khac
Kt tua va giy loc sy kh cho vao chen s a nung va cn n khi lng khng
i. t t t cho chay ht giy loc ri nung n nhit 1000- 1100
o
C trong
khoang 1gi. Ly ra ngui n nhit phong trong bnh hut m, cn. Nung lai
nhit o trong 15phut va cn n khi lng khng i.
Cng thc tnh :

g
G G
CKT SiO
100 ). ' (
2

= + .
W 100
100
(%)
Vi G : khi lng kt tua va chen (gam)
G

: khi lng chen khng (gam)

g. khi lng mu (gam)
W: m cua ximng %
Giao an phn tch silicat
7
Trong tr ng h p mun xac nh chnh xac SiO
2
phai nh lng cn khng tan.
Chuyn kt tua a nung sang chen bach kim a nung va cn n khi lng khng
i. Tm t bng nc ct cho vao 15ml HF 40%, 2 giot H
2
SO
4
d = 1,84. Bc hi
trn bp co lot aming n kh. Nung chen nhit 900 - 1000
0
C trong khoang
na gi. ngui trong bnh hut m n nhit trong phong, cn n khi khi
lng khng i. Phn ba nung chay bng KHSO
4
ri hoa tan khi nong chay bng
nc si, nu con vn uc cho vao vai gioi H
2
SO
4
d =1,84 n tan trong. Gp vao
phn nc loc trn, cho vao bnh nh mc 500ml, thm nc n vach.
Cng thc tnh:

g
a a
SiO
100 ). ' (
2

=
W 100
100 .
(%)
Vi a: khi lng kt tua (gm SiO
2
va cn khng tan ) ( g )
a: kh i lng cn khng tan (hay ba) ( g )
a = G - G vi : G la khi lng chen bach kim va ba ( g)
G la khi lng chen bach kim ( g)
2.1.4 Xac djnh ham luong Fe
2
0
3

a) Nguyn tc cua phng phap:
Phng phap xac nh Fe
2
O
3
, Al
2
O
3
, CaO, MgO bng Komplexon III
Dung komplexon xac nh nhanh Fe
2
O
3
, Al
2
O
3
, CaO, MgO trong phn tch hang
loat. Nhng khi phn tich trong tai (cn chnh xac ) phai dung phng phap nung cn
(nh a noi trn).
Chun st bng EDTA pH = 1,8 - 2. Kt thuc chun la s mt mau tm
o cua hp cht st axt sunfosalixilic
( Ethylen Diamino Ttra Axetic -> vit tt EDTA )
HOOC - CH
2
CH
2
- COOH
N - CH
2
- CH
2
N
HOOC - CH
2
CH
2
- COOH


b) Hoa cht:
- Amonihyrx yt NH
4
OH 10%
- HCl 0,004N va 2N
- HNO
3
10%
- Axt sufosalixilic 15%
- EDTA, dung dch 0,01M
c) Cach lam:
Ly 50ml dung dch muc 3 cho vao 1ml HNO
3
10% un si nhe khoang 3 phut,
ngui trung hoa bng NH
4
OH 10% n khi dung dch vn uc. Nu dung dch kt
tua nhiu phai thm vai giot HCl 2N lc n khi tan ht kt tua, ri lai iu chnh nh
trn . Sau o cho 25 - 30ml HCl 0,04N va nho dung dch axt sunfosalixilic n co
Giao an phn tch silicat
8
mau tm o m, un dung dch n khoang 60 -70
0
C; chun bng EDTA 0,01M
n mt mau tm o, dung dch gi lai chun Al
+3

Cng thc tnh:
(%) Fe
2
O
3
= .
100 . 0007985 , 0 .
g
n
w 100
100

Trong o ;
n - lng dung dch EDTA 0,01M a dung (ml)
g - khi lng mu tng ng vi dung

dch a ly (g)
0,0007985 - khi lng st tng ng vi 1ml EDTA 0,01M (g)
w- m (%)
2.1.5 Xac djnh ham luong Al
2
O
3

a) Nguyn tc cua phng phap:
Ion Al
3+
phan ng vi ng (CuEDTA) tach ra ion Cu
2+

Al
3+
+ CuEDTA = AlEDTA + Cu
2+

Cu
2+
tao ra 4, 2 (pyridyl- azo) resorsirmol (PAR) thanh phc cht mau o. Chun
Cu
2+
bng EDTA 0,01M, cui chun t o sang vang sang
b) Hoa cht:
- Dung dch m pH= 4,5- 4,7 va 77 gam CH
3
COONH
4
+ 51,9 ml CH
3
COOH
98% pha thanh 1000ml
- Ch th PAR d
2
0,1%
- EDTA 0,01M
- Dung dch CuSO
4
0,01M
CuEDTA khoang 0,05M . Chun CuSO
4
trong mi trng amoniac bng EDTA
0,05M theo ch th PAR mau chuyn t o sang vang sang .Theo phep chun nay ta
pha nhng lng tng ng 2 dung dch vi nhau se dc dung dch CuEDTA 0,05M
c)Cach lam : dung dch sau khi xac nh Fe
2
0
3
pha loang bng nc ct n khoang
200-250ml. Cho 2-3 giot PAR, 2-3 giot CuEDTA thm cht m a pH v 3,5- 4 .
Cho n khi dung dch co mau o vng (ht khoang 20-25 ml).un si ky , chun
bng EDTA 0,01M chuyn t mau o sang mau vang sang .Tip tuc lam nh th n khi
nao un si ma mau o khng tai hin la c.
Al
2
O
3
tnh theo cng thc:


g
n
O Al
100 . 000509 , 0 .
3 2
= .
w 100
100

Trong o:
n: s ml dung dch EDTA chun .
g: khi lng mu (g)
w: m
2.1.6 Xac nh ham lng CaO
a) Nguyn tc cua phng phap:
Giao an phn tch silicat
9
Chun Ca
2+
bng EDTA theo ch th murexid pH =12
b) Hoa cht::
- Dung dch NH
4
OH 25%
- Dung dch NaOH 20%
- Ch th mau: 0,1 gam murexid va 20 gam K
2
SO
4
a nghin nho trn u va
nghin ky trong ci s .
c) Cach lam :
Ly 50ml dung dch muc 3 tach Fe
3+
va Al
3+
di dang hirxyt vi s co mt cua
NH
4
Cl va H
2
O
2
loai Mn ri cho nc loc vao bnh nh mc 250ml. Ly 25ml pha
loang n 100ml thm 15ml NaOH 20 %. Thm mt lng EDTA 0,01M d oan gn
vi lng dung chun (15-18ml) ri cho ch th murexid, tip tuc chun bng
EDTA 0,01M mau chuyn t o sang tm. Cn lam mu trng tr Ca
2+
trong n c ct.


g
n
CaO
100 . 00056 , 0 .
= .
W 100
100

Trong o :
n - la lng EDTA 0,01M a dung tnh bng ml
g - lng mu tng ng vi dung dch a ly(g)
0,00056 - lng CaO tng ng vi 1ml EDTA 0,01M (g)
W - m tnh bng %
2.1.7 Xac djnh ham luong MgO
a) Nguyn tc cua phng phap:
Chun tng s ham lng CaO va MgO bng EDTA pH=10 .Tnh bng cach tr CaO
b) Hoa cht:
- NH
4
OH 25%
- NH
4
Cl tinh th
- CuEDTA , dung dch 0,05M ( pha nh mu c 5)
- Ch thi PA R , dung dch 0,1%
- EDTA dung dch 0,01M
- Dung dch m pH=10 .Hoa tan 54 g NH
4
Cl vao 200ml nc ct, thm 350 ml
NH
4
OH 25% pha thanh 1000ml
c) Cach lam:
Ly 50ml dung dch muc 3 , tach Fe
+3
va Al
+3
di dang hyrxyt vi s co
mt cua NH
4
Cl va H
2
O
2
loai Mn . Nc loc vao bnh nh mc dung tch 250ml, trn
nc ct n khoang 150-200ml. Cho 25m dung dch m pH=10 . Thm t buret 1
lng EDTA 0,01M gn bng lng EDTA 0,01M a chun CaO, sau o thm 5 giot
CuEDTA, 5-10giot PAR . Chun bng EDTA 0,01M n khi mau chuyn t o sang
vang sang bn vng. Cn lam th nghim trng tr Ca
+2
va Mg
+2
trong nc ct.


W g
a b
MgO

=
100
100
.
100 . 0004037 , 0 ). (

Giao an phn tch silicat
10
Trong o:
b - lng EDTA 0.01M a chun tnh bng ml
a - lng EDTA 0,01M
g - khi lng mu cht tnh bng gam
W - m tnh bng phn %
2.1.8 PHUONG PHAP NUNG CN D
xac djnh Fe
2
O
3
, Al
2
O
3
, setquioxit, TiO
2
, va mangan xit
2.1.8.1 Xac nh ham lng SETQUIOXT
a) Nguyn tc cua phng phap:
Kt tua Fe
+3
va Al
+3
di dang hirxyt nung va cn dang xit .Nu trong
ximng co TiO
2
va MnO
2
th chung cung kt tua di dang hyrxyt. Do o kt qua se
cao hn tng s Fe
2
O
3
va Al
2
O
3
xac nh bng phng phap complexon.
Cng thc gn ung:
Al
2
O
3
= R
2
O
3
- Fe
2
O
3

Chnh xac:
Al
2
O
3
= R
2
O
3
- ( Fe
2
O
3
+ TiO
2
+ MnO
2
)
b)Hoa cht:
- NH
4
NO
3
tinh th
- NH
4
OH dung dch 10%
- NH
4
NO
3
dung dch 2% lam nc ra
- Brm- cresol xanh la cy dung dch 0,1% trong ru hay metyl o, dung dch
0,1% trong ru.
- Hyrperoxt H
2
O
2
dung dch 30%
c) Cach lam:
Dung dch thu c sau khi loc muc 3 cho vao cc 500ml, un si, thm 5ml
H
2
O
2
30% va 1,5 gam NH
4
NO
3,
tip tuc un si va khuy u cho tan. Thm 8-9 giot
ch th brm- cresol xanh la cy hay metyl o, cho tng giot NH
4
OH 10%, va cho
va khuy n khi chuyn mau ch th, sau o cho u khoang 1ml NH
4
OH ri un
si 2 phut. lng yn ch m (50-70
o
C) trong 15 phut kim tra xem a co kt tua
hoan toan cha bng cach cho vai giot NH
4
OH vao phn nc trong nu khng xut
hin kt tua la c. Loc gan qua giy loc khng tan chay nhanh, ra 3 ln bng
NH
4
NO
3
2% a un si. Sau o chuyn kt tua va giy loc tr lai cc a kt tua luc
u, hoa tan kt tua bng 30ml HCl 10%, un nong va dm cho tht nhuyn giy loc,
thm va 100ml nc nong va un si ky, sau o lai tin hanh kt tua nh trn va loc
qua giy loc khng tan chay nhanh. Ra bng dung dch NH
4
NO
3
2% a un si cho
n ht ion Cl
-
( th bng dung dch AgNO
3
1%). Dung dch loc 2 ln gp lai tin
hanh xac nh CaO va MgO
Cho kt tua va giy loc vao chen s a nung, va cn n khi lng khng i.
Sy va t chay ht giy loc, tip tuc nung t 1000- 1100
o
C trong thi gian 30-45
Giao an phn tch silicat
11
phut. Ly ra ngui trong bnh hut m n nhit trong pho ng va cn. Nung lai
15 phut cung nhit trn va cn n khi lng khng i.
Ham lng (%) R
2
O
3
tnh theo cng thuc:

.
100 ). ' (
3 2
g
G G
O R

=
W 100
100

Trong o:
G - khi lng chen va kt tua tnh bng (g)
G- khi lng chen khng tnh bng (g)
g - khi lng mu tnh bng (g)
W - m tnh bng %
2.1.8.2 Xac djnh ham luong Fe
2
O
3

a) Nguyn tc cua phng phap:
Kh Fe
+3
n Fe
+2
chun Fe
+2
bng Kalibicromat theo ch th cua Bari
iphenylamin sunfonat
b)Hoa cht::
- Axit HCl, dung dch d =1,19
- Dung dch clorua thic II: 2,5 gam SnCl
2
hoa tan vao 20ml HCl d = 1,19 un
nong cho tan ri pha thanh 200ml .Cho thm mt t la thic lng xung di
ay
- HgCl
2
5%
- H n hp axt H
3
PO
4
va H
2
SO
4
(150ml H
3
PO
4
d = 1,7 va 150ml H
2
SO
4
d = 1,84
pha thanh 1000ml)
- Bari iphenylamin sunfonat dung dch 0,2%
- Kali bicromat K
2
Cr
2
O
7
0,1N
c) Cach lam:
Cn mt mu ximng cho vao cc 600ml, thm 40ml nc ct, va khuy va thm
10ml HCl d = 1,19. Dung ua thuy tinh khuy cho nhuyn ximng hay con b von cuc
lai. un cho si vai phut thm vao dung dch ang si tng giot SnCl
2
. Khi mt mau
thm tha mt giot. Lam lanh di nc n nhit phong. Du ng tia nc ra sach
thanh cc. oan thm lun 10ml HgCl
2,
khuy

u, sau mt phut thm 10ml H
3
PO
4
+
H
2
SO
4
va 5 giot bari ifenylamin sunfonat 0,2% thm nc n khoang 150ml. Chun
bng K
2
Cr
2
O
7
gn im tng ng phai chun b tht t t cho n khi chuyn t
mau sang tm xanh.
Ham lng% Fe
2
O
3
tnh theo cng thc:

W g
n
o Fe

=
100
100
.
100 . 007985 , 0 .
3 2

Trong o: n - la lng K
2
Cr
2
O
7
0,1N a chun tnh bng ml
g - khi lng mu tnh bng (g).
Giao an phn tch silicat
12
0,007985 - khi lng Fe
2
O
3
tng ng vi 1ml K
2
Cr
2
O
7
0,1M tnh bng
(g)
W - m tnh %
2.1.8.3 Xac djnh ham luong TiO
2

a) Nguyn tc:
Mi trng axt- axtc, axt sunfosalixilc tao vi Ti
+4
mt phc cht mau vang.
Dung axt thioglyColic che mau Fe
+3
,xac nh Titan bng phng phap o mau.
b) Hoa cht::
- Axt sunfosalixilc dung dch 20% (vi lng ximng co ham lng Al
2
O
3
ln
hn 20% dung dung dch 40%)
- Axt thioglycolc dung dch 30%
- Dung dch NH
4
Cl 10%
- Dung dch HCl 0,1N
- Dung dch NaOH10%
- Phenolphltalein dung dch 0,1%
- Dung dch CH
3
COOH: 143ml CH
3
COOH 98% pha ra 1000ml
- Natriaxtat CH
3
COONa : 205g CH
3
COONa pha thanh 1000ml
- TiO
2
nguyn cht
- Kali hyrsunfat KHSO
4
tinh th
- Dung dch H
2
SO
4
d = 1,84
Cach iu ch dung dch mu:
Nung TiO
2
1000
o
C n khi lng khng i, cn ly 1 gam vao chen bach kim, nung
chay bng KHSO
4
. Hoa tan khi nong chay bng nc si, cho thm vai giot H
2
SO
4
d =
1,84 dung dch trong sut sau o cho vao bnh nh m c 1000ml pha nc n vach lc
k. 1ml dung dch nay tng ng vi 0,001g TiO
2

Cach dung duong cong chun ly 2 lng dung dch mu t nho n ln (0,1- 5 mg)
chun b nh muc cach lam, ly nc ct lam dung dch i chiu .So mau bng may
so mau quang in hay may so mau .Pulfrch vi b c song 420 m .Ghi lai tt quy
v day lp dung dch 1cm ng vi mi ham lng TiO
2
a ly.
Trn toa d vung goc truc tung ghi tr s tt, truc hoanh ghi tr s ham lng TiO
2

va ve ong cong chun theo cac tr s a thu c .Sau 1 tun l phai kim tra lai mt
vai im trn ng cong.
c) Cach lam:
Ly phn nc loc muc 3 cha khoang 2mg TiO
2
khoang 50 ml cho vao bnh ng
mc 250ml. Thm 20ml axt sufosalixilc, 2ml dung dch NH
4
Cl 10% trung hoa n
khi chuyn mau phenolphtalein. Sau o thm HCl 0,1N tng giot cho n khi mt mau
hng cua phnolphtalein thm 16,4ml CH
3
COOH va 3,6ml dung dch CH
3
COONa pha
nc ct n vach
o tt day lp dung dch bng 5cm, dung nc ct lam dung dch i chiu
Giao an phn tch silicat
13
tt c quy v day 1cm lp chung dch i chiu vi ng cong chun tm
ham lng TiO
2

Ham lng (%) TiO
2
tnh theo cng thc:


W g
C
TiO

=
100
100
.
100 .
2

Trong o:
C - ham lng TiO
2
tm c theo ng cong chun tnh bng gam
g - khi lng mu tng ng vi dung dch a ly tnh bng gam
W- m tnh bng %
Ghi chu : khi o ham lng TiO
2
phai ly t dung dch sau khi a kim tra tinh khit
SiO
2
gp vi dung dch loc ( SiO
2
+ KT)
2.1.8.4 Xac nh ham lng mangan xyt
a) Nguyn tc cua phng phap:
Oxy hoa Mn
+2
khng mau thanh MnO
4
-
mau tm hng bng amonipe sunfat co AgNO
3

lam xuc tac.Xac dnh mangan bng phng phap o mau
b) Hoa phm:
- Axt HNO
3
dung dch 1: 4
- Bac nitrat AgNO
3
dung dch 3,5g/l
- Amonipesulfat (NH
4
)
4
S
2
O
8
dung dch 15%
- Axt H
3
PO
4
dung dch 1:1
- Thuy ngn II nitrat Hg(NO
3
)
2
dung dch 1%
Cach dung duong cong chun
Cn 3,1446g MnSO
4
a sy trong chn khng hoa tan nc ct pha thanh
1000ml. Ly lai 100ml dung dch nay pha thanh 1000ml. Ly lai1ml dung dch nay
tng ng vi 0,1mg MnO.
Ly nhng lng dung dch tng ng t 1- 5 mg MnO chun b nh muc cach lam
ri so mau vi nc lam dung dch i chiu vi bc song 530 m.Ghi lai tt v
day dung dch la 1cm .Ve ng cong chun theo cach a trnh bay phn 3.
C) Cach lam:
Cn 1g ximng, hoa tan trong 30ml HNO
3
1: 4, loc qua giy loc thng ra 4 -5 ln
bng nc si cho vao bnh nh mc 100ml hay 200ml (tuy theo ham lng MnO co
trong Ximng) Thm 1ml Hg(NO
3
)
2
1% 10ml AgNO
3
8,5g/l, un si ky trn bp cach
thuy 5 phu t. Cho t t 10ml (NH)
4
S
2
O
8
15%. Lc ky, lam ngui n nhit trong
phong. Thm 1ml H
3
PO
4
1:1 va thm nc n vach,so sanh mau vi dung dch nc
cn so sanh.
Ham lng % MnO tnh theo cng thc:


W g
C
MnO

=
100
100
.
100 .

Giao an phn tch silicat
14
Trong o: C- Ham lng MnO bng cach quy tc o c v day dung dch 1 cm
va so vi ng cong chuan tnh (g)
W - m %
2.1.8.5 Xac djnh ham luong Al
2
O
3
Ham lng % Al
2
O
3
tnh theo cng thc:
Al
2
O
3
= R
2
O
3
- ( Fe
2
O
3
+ TiO
2
+ Mn
3
O
4
)
Trong o: R
2
O
3
kt qua xac nh theo muc 5.1.8.1
Fe
2
O
3
muc 5.1.8.2
TiO
2
muc 5.1.8.3
Mn
3
O
4
quy t xac nh MnO theo muc 5.1.8.4
2.1.8.6 Xac nh ham lng CaO
a) Nguyn tc cua phng phap:
Kt tua Ca
+2
trong mi trng amoniac di dang canxi oxalat. Hoa tan canxi oxalat
bng pemanganat kali hoc nung cn di dang canxi xyt
b) Hoa cht::
- Axt oxalic H
2
C
2
O
4
, dung dch 4% hay amoni oxalat (NH
4
)
2
C
2
O
4
dung dch 4%
- Amoni hyrxyt NH
4
OH, dung dch 10% va 25%
- Axt HCl dung dch 20%
- Nc ra amoni oxalate (NH
4
)
2
C
2
O
4
dung dch O,1%
- Axit H
2
SO
4
dung dch 5%
- KMnO
4
dung dch 0,1%
c) Cach lam:
C phn nc loc muc 3.6.1 con khoang 300ml. Cho vai giot HCl 20% n
chuyn mau ch th. un si 2 phut ri cho vao 50ml H
2
C
2
O
4
4% hay ( NH
4
)
2
C
2
O
4

4%, tip tuc un si khuy u. Trong luc ang si trung hoa bng tng giot NH
4
OH
10% ri va khuy u va un si trong 3 phut loc qua giy loc khng tan loai day
bng cach lng gan .Trc khi loc cn nhu ng giy loc vao dung dch ( NH
4
)
2
C
2
O
4

.Ra 5ln bng nc r a (NH
4
)
2
C
2
O
4
0,1% .Nc loc va nc ra gi lai.
Kt tua va giy loc cho tr lai cc a kt tua. Hoa tan kt tua bng 20ml dung dch
HCl 20% pha thanh 200ml. Cho vai giot Brom cresol xanh la cy , un gn si , cho
50ml H
2
C
2
O
4
4% hay (NH
4
)
2
C
2
O
4
4%
un si khuy u ri cho t t NH
4
OH 25%. Cho n khi chuyn mau ch th
lng ch m t 40 -60
0
C trong khoang 2gi. Loc vao giy loc khng tan loai day.
Sau o xac nh lng CaO bng 1 trong 2 phng phap sau :
Chun d bng KMnO
4
: Ra kt tua bng cach gan 3 ln vi nc NH
4
OH 2% a
un m, sau o ra bng nc ngui co thm 1 vai giot NH
4
OH cho sach ion clo (th
bng AgNO
3
1%). Kt tua va giy loc cho tr lai cc va hoa tan bng 150ml H
2
SO
4
5%
bng cach un 60 -70 . Sau o chun bng KMnO
4
0,1N n hin mau hng.
Giao an phn tch silicat
15
Nung cn duoi dang CaO: Ra kt tua bng amoni oxalat 0,1% cho n sach Clo.
Cho kt tua va giy loc vao chen s a nung va cn n khi lng khng i, sy, t
chay ht giy loc, ri nung 1000- 1100
o
C. ngui n nhit phong trong bnh hut
m. Khi cn phai chun b chu ao, ly chen ra la cn ngay tc khc tranh hut m.
Nung lai nhit o 15 phut va cn n khi lng khng i.
Nc loc va ra va phn trn xac nh MgO.
Ham lng( %) CaO tnh theo cng thc:


W g
n
CaO

=
100
100
.
100 . 002804 , 0 .


Trong o: n - la lng KMnO
4
0,1N a chun (ml).
g - khi lng mu(g)
W - m %


W g
G G
CaO

=
100
100
.
' '
100 ). ' (

Trong o: G - khi lng chen va kt tua (g)
G - khi lng chen khng (g)
g - khi lng mu ng vi dung dch con lai (g)
2.1.8.7 Xac djnh ham luong MgO
a) Nguyn tc cua phng phap :
Kt tua Mg
+2
di dang magi amoni fotfat. Sau o nung thanh magie py rofotfat
va tnh ra magie oxt
b) Hoa cht:
- dung dch NH
4
OH 25%
- iamoni- hirfotfat( NH
4
)
2
HPO
4
dung dch 10%
- amonitrat NH
4
NO
3
dung dch 2%
c) Cach lam:
C phn nc loc muc 3.6.6 con khoang 300ml, ngui, thm 10ml dung dch
(NH
4
)
2
HPO
4
10% thm NH
4
OH va mt lng bng 1/3 th tch dung dch.
y cc bng mt knh ng h lng 18 ting, loc qua giy loc khng tan loai day (
hoc chen loc bng s a nung va cn n khi lng khng i ). Ra bng NH
4
NO
3

2% n ht ion Clo ( th bng AgNO
3
1% ).
Cho kt tua va giy loc vao m t chen s a nung n khi lng khng i. Sy kh
va t chay ht giy loc nung nhit 1000-1100
o
C. Ly ra ngui trong bnh hut
m n nhit phong. Cn nung lai 15 phut nhit trn va cn n khi lng
khng i.
Ham lng % MgO tnh theo cng thc:

Giao an phn tch silicat
16

W
G G
MgO

=
100
100
.
100
100 . 3623 , 0 ). ' (

Trong o:
G - khi lng chen va kt tua (g)
G - khi lng chen khng (g)
0,3623 - h s chuyn t Mg
2
P
2
O
7
thanh MgO
G - khi lng mu
W - m (%)
2.1.9 XAC DJNH HA M LUONG CAC HOP CHT CU A LUU HUY NH
2.1.9.1 Xac djnh ham luong sufat bng phuong phap khi luong
a) Nguyn tt cua phng phap:
Kt tua sunfat d i dang BaSO
4
.T lng BaSO
4
thu c tnh c SO
3

b) Hoa cht::
- Dung dch BaCl
2
10% : hoa tan 100g BaCl
2
.2H
2
O 1000 ml nc ct
- Nc ra : axt HCl dung dch khoang 2% (d= 1,008)
c) Cach lam:
Ly dung dch loc c khi pha mu xac nh ham lng cht khng tan muc
3.5.3. un si dung dch nay ng thi cung un si dung dch BaCl
2
cho vao 10ml
dung dch BaCl
2
khuy u tip tuc un si nhe trong 5phut yn dung dch trong
3 gi cho kt tua lng xung. Loc qua giy loc khng tan chay chm ra kt tua va
giy loc bng nc ru a vi nc ct un nong cho n khi ht ion clo ( th bng
AgNO
3
1%).
Cho kt tua va giy loc vao mt chen s a nung va cn n kh i lng khng i.
Sy kh, t cho chay ht giy loc. Nung nhit = 1000- 1100
0
C. Ly ra
ngui trong bnh hut m n nhit phong. Cn, nung lai 15 phut nhit trn va
cn n khi lng khng i.
Ham lng ( %) SO
3
, tnh theo cng thc:

W g
G G
SO

=
100
100
.
100 . 343 , 0 ). (
'
3

Trong o: G - Khi lng chen va kt tua ( g).
G

- Khi lng chen khng ( g).

0,343 - h s chuyn t BaSO
4
thanh SO
3
.
g - khi lng mu (g).
W- m( %).
2.1.9.2 Xac djnh ham luong sunfua bng phuong phap khi luong.
a) Nguyn tc cua phng phap :
Oxi hoa lu huynh dang sunfua thanh sunfat bng nc brm va sau o kt tua
di dang bari sunfat, loc, cn.
b) Hoa cht:
Giao an phn tch silicat
17
- Nc brm, dung dch bao hoa lanh co brm tha lng di ay. Cho khoang
35g brm vao 1000ml nc ct.
- Axt clohidrc ( HCl), dung dch d = 1,19.
- Bariclorua (BaCl
2
) : hoa tan 100g BaCl
2
. 2H
2
O trong 1000ml nc ct.
c) Cach lam:
Cn 2g mu cho vao mt cc 250ml, thm t bng vai ml nc ct. Thm vao 70-
80ml nc brm. Khuy u, yn 2- 3 gi. Sau o thm vao 20ml HCl (d= 1,19),
cho t t va cho va khuy. Sau khi Xi Mng a hoa tan hoan toan, chuyn tt ca
dung dch t cc sang mt bat s, cho bc hi n kh tach silc. Ly lai bng HCl
va nc si. un si, ra sach ion cl ( th bng AgNO
3
1%).
Trong dung dch loc, xac nh lu huynh tng s bng phng phap kt tua di
dang BaSO
4
theo muc 3.7.1.
Ham lng ( %) sunfua, tnh theo cng thc :
S= 0,1373 ( A-B).
W 100
100


Trong o :
A- Khi lng BaSO
4
tng ng vi lu huynh tng s theo muc 3.7.2
B- Khi lng BaSO
4
tng ng vi lu huynh dang sunfat muc 3.7.1.
W- m ( tnh bng %).
2.1.9.3 Xac djnh ham luong clorua.
a) Nguyn tc:
Kt tua clorua bng AgNO
3
. Chun lng NO
3
-
tha bng amoni sunfoxyanua.
b) Hoa cht:
- Axt HNO
3
pha loang, dung dch co d= 1,18 vao khoa ng 29%.
- Dung dch AgNO
3
0,1N : Hoa tan 16,989 AgNO
3
trong 1000ml nc ct.
- Amoni sunfoxyanua NH
4
CNS dung dch 0,1N : hoa tan 7,611g NH
4
CNS trong
1000ml nc ct.
- Amoni- stIII sunfat NH
4
Fe(SO
4
)
2
dung dch bao hoa nhit thng
c) Cach lam:
Cn 2g ximng vao mt bnh non 500ml thm vao 50ml nc ct va 20ml HNO
3

un no ng hoa tan. Lam ngui, pha loang vi 200ml nc ct. Thm chnh xac 5ml
dung dch AgNO
3
0,1N, 2-3ml dung dch NH
4
Fe(SO
4
)
2
va chun lng AgNO
3
tha
bng dung dch NH
4
CNS 0,1N
Ham lng (%) Cl, tnh theo cng thc:


W
b a
Cl

=
100
100
.
100
100 . 003546 , 0 ). (


Trong o: a - lng AgNO
3
0,1N a cho vao (ml)
b - lng NH
4
CNS0,1N a chun (ml)
Giao an phn tch silicat
18
g - khi lng mu (g)
w - m %
2.1.10 XA C DJNH HAM LUONG CHT KIM
2.1.10.1 Xa c djnh ham luong kali xit bng phuong phap khi luong.
a) Nguyn tc cua phng phap:
Dung natritetraphenylborat Na[B(C
6
H
5
)
4
] kt tua kali di dang hp cht kho tan
trong mi trng axt yu pH = 4- 5
b) Hoa cht:
- Dung dch Natri tetraphenylborat : 1,2g Na[B(C
6
H
5
)
4
] trn vi 0.5 g Al
2
O
3
va
100ml nc ct. Khuy manh dung dch trong 10 phut loc dung dch loc phai hoan toan
trong sut .
Nc rua : dung dch nc bao hoa K[(C
6
H
5
)
4
] loc kt tua ra kt tua bng nc. Hoa
tan kt tua trong nc ct 25
0
C
- Axt HCl dung dch d = 1,19
- Dung dch NaOH 10%
- Metyl da cam dung dch 0,1 %
c) Cach lam:
Cn 1 g mu cho vao cc thuy tinh 100ml trn vi 5ml HCl d = 1,19 cho bc hi
n kh. Dung 50ml HCl va 20ml nc ct hoa tan ba con lai va ra bng nc ct
Ly tt ca nc loc cho vao cc 250ml, thm nc vi khoang 60ml. iu chnh
pH dung dch bng HCl loang hay NaOH 10 % cho n khi chuyn mau cua metyl
da cam t da cam sang hng
Va khuy va nho t t 15 ml dung dch Na[(C
6
H
5
)
4
] yn 1 gi. Loc qua chen loc
thuy tinh a sy 110
0
C va cn n khi lng khng i. Ra bng 35ml nc ra
mi ln khoang 5 ml. Sau cung ra bng 10ml nc ct. Nhit cua nc ra khng
c cao qua nhit phong.
Sy chen loc va kt tua 110
o
C trong 2 gi . Ly ra ngui trong bnh hut m, cn,
sy loc 30 phut nhit trn. Va cn n khi lng khng i
Ham lng % tnh theo cng thc:

W M g
M G G
O K

=
100
100
.
1 . . 2
100 . 2 ). ' (
2

Trong o:
G - khi lng chen va kt tua K[B(C
6
H
5
)
4
(g)
G - khi lng chen khng
M
1
- phn t lng K[B(C
6
H
5
)
4
=358,344
M
2
- phn t lng K
2
O bng 94,2
g - khi lng mu tnh bng (g)
W - m %
Ghi chu: NH
4
+
anh hng n s xac nh K
+

2.1.10.2 Xa c djnh luong Na
2
O bng phuong phap khi luong
Giao an phn tch silicat
19
a) Nguyn tc cua phng phap:
Dung kem uramyl axetat kt tua natri di dang hp cht (CH
3
COO)
9

NaZn(UO
2
).6.H
2
O kho tan
b) Hoa phm:
- Dung dch kem uranylaxetat iu ch nh sau:
- Dung dch I: ly 10g (CH
3
COO)
2
Zn.2H
2
O va 0,9ml axt axetc 98% hoa tan trong
53ml nc ct.
- Dung dch II: ly 30g (CH
3
COO)Zn.2H
2
O va 0,9ml axt axetc 98% hoa tan trong
34ml nc ct
Trn ln 2 dung dch I va II vi nhau lc manh 15 phut. yn 24 gi. Loc vao chai
polyetylen va y kn chai lai dung c lu.
- Nc ra: ru etylic 95%, bao hoa natri kem uranylaxetat. Loc, dung ru etylc
95% ra kt tua. Hoa tan kt tua con t bng ru etylc 95% c dung dch
bao hoa, cho vao chai polyetylen co kt tua lng di ay chai.
- Etyl ete khng ngm nc.
c) Cach lam:
Pha mu nh khi xac nh Kali. Ly nc loc thu c, kt tua sunfat, bng BaCl
2

10%, R
2
O
3
va CaO bng NH
4
OH 25% vi (NH
4
)
2
CO
3
.
Loc gan, r a nc nong 4-5 ln. Nc loc nay gi lai. Hoa tan kt tua bng HCl 1:3, un
cho tan cac hyrxt lai dung NH
4
OH va (NH
4
)
2
CO
3
kt tua R
2
O
3
va CaO.
Loc gan va ra 3-4 ln bng n c nong. Nc loc thu c gp vi nc loc trn
xac nh Na
2
O .
Cho tt ca nc loc vao 1 chen bach kim cho bc hi rt cn tht n kh va nung
500
o
C ui ht mui amoni. Dung nc ct hoa tan ba con lai trong chen bach kim,
loc, ra sach bng nc ct nong. Cho nc loc vao 1 cc thuy tinh kiu cao dung tch
50 ml hay 100ml. Cho bc hi n th tch con 1ml. Dung dch phai trong sut. Va
khuy va nho t t 15ml dung dch kem uranylaxetat O nhit phong y kn. yn
cho n khi dung dch trong khoa ng 1-3 gi. Loc qua chen loc thuy tinh(G
4
)
Ra kt tua 5 ln, mi ln 3ml kem uranylaxetat va 5 ln, mi ln 3ml nc ra. Cac
dung dch nay phai cung mt nhit .
Sau cung ra bng 15ml etyl ete ri hong kh ngoai khng kh lam th nao cho khng
kh co th chui qua pha di mt th tinh xp trong chen loc. V etyl ete bc hi lam
lanh nn co nc ng lai trn chen loc, dung giy loc thm cn thn cho tht kh. Sau
20 phut. Tip tuc kh va cn n khi lng khng i.
Ham lng ( %) Na
2
O tnh theo cng thc :
Na
2
O =
W gM
M G G

100
100
.
1 2
100 . 2 ). ' (

Trong o :
Giao an phn tch silicat
20
G - khi lng chen va kt tua (CH
3
COO)
9
NaZn(UO
2
)
3
. 6H
2
O tnh (g)
G - khi lng chen khng (g)
G - khi lng mu (g)
M1 - phn t lng (CH
3
COO)
9
NaZn (UO
2
)
3
. 6 H
2
O = 1538,09
M2 - phn t lng Na
2
O = 61,99
W - m (%)
Ghi chu : - 1: cn lam th ngim trng vi cac thuc th kim tra kt qua ( cho ca
trng h p K
2
O)
-2: (CH
3
COO)
9
NaZn (UO
2
)
3
. 6 H
2
O tan rt nhiu trong nc nn th tch
dung dch kt tua khng c > 1ml
2.1.10.3 Xa c djnh ham luong kim bng phuong phap quang k ngon lua ( phng
phap nay khng c dung khi phn tch trong tai)
a) Nguyn tc:
Da vao tnh cht nhum mau ngon la cua Na va K va da vao cng mau cua
ngon lua nh lng chung
b) Hoa ph m:
- Axt HCl, dung dch d= 1,19
- Dung dch NH
4
OH, d = 0,91
- Amoni cacbonat (NH
4
)
2
CO
3
, dung dch bao hoa
c) Cach lam:
Cn 0,5g mu ximng cho vao mt bnh nh mc 500ml kh thm 20 ml nc ct
va 5ml HCl c. un hoa tan mu, pha loang n khoang 200ml nc ct un si
thm 10 ml NH
4
OH d= 0,91 va 5ml (NH
4
)
2
CO
3
bao hoa. un si nhe vai phut ngui
va pha thm nc cho n vach lc u loc qua giy loc kh . Bo phn nc loc u ly
dung dch loc em o trn may quang k ngo n la.
2.2 . PHN TICH THANH PHN HOA HOC CUA DT SET
2.2.1 D m xac djnh ging nhu phn ximng
2.2.2 Luong mt khi nung xac djnh nhu phn xi mng
2.2.3 Xac djnh ham luong Silic xyt ( SiO
2
).
a) Nguyn tc:
Sau khi hoa tan mu silc co trong t set c chuyn vao dung dch dang kt tua
keo. Sau o chuyn no t dang kt tua keo v dang kt tua H
2
SiO
3
. Nung kt tua nay
1000 - 1100
O
C chuyn v SiO
2
. X l kt tua nay bng HF, sau o tnh ham lng
SiO
2
co trong mu t set.
b) Hoa phm:
- Hn h p nong chay : K
2
CO + Na
2
CO
3
trn theo t l 1: 1
- Axit clohyric (HCl) dung dch 1: 1
- Axit H
2
SO
4

- Axit HF
c) Cach lam:
Giao an phn tch silicat
21
Cn 1g mu t a nghin mn va a sy nhit 105 -110
0
C cho vao chen bach
kim co cha khoang 3 gam hn hp nung chay (K
2
CO
3
+ Na
2
CO
3
) (sau o pha i ly trn
khoang 800g nung chay na). Nung chay mu trn ngon en kh , thnh thoang lc
mu hoa tan hoan toan. Nung n khi khi nong chay trong sut, nung tip khoang 15
phut na. Ly chen ra nghing v 1 pha ngui khi khi nong chay a ng lai, ly no
ra cho vao bat s bng nc ct un si. Trang chen 2 ln mi ln bng 5ml axt HCl
dung dch 1:1
Lng nc si dung ly ra cn phai t hn 100ml. y bat s bng mt knh cho t
t tng giot HCl c trung hoa n tan ht va khng con sui bot, cho thm 5 ml axit
HCl c na ( tt ca 30 ml HCl m c) c mu trn bp cach cat khoang 1 ngay n
kh kit ( trn m t kn ng ch con nc o ng lai c tip 30 phut n a ).
Ly ra ngui thm vao 30ml HCl 1:1. Ra thanh mt bat va knh ng h bng nc
un si khoang 60 -70 ml. un si trn bp in lng 15 phu t .Loc kt tua qua giy
loc khng tro rua bat s va giy loc trc ht 2 -3 ln bng dung dch HCl loang 2%. Sau
o ra bng nc ct un si n ht axit th bng giy pH. Dung dch loc va nc ra
hng vao bnh nh mc 500ml th tch cua no khoang 300 - 400 ml giy loc co kt tua
H
2
SiO
3
gp lai cho vao chen bach kim t chay giy loc trn bp in, cho chen vao lo
nhit nung 1000 - 1100
0
C khoang 1,5 - 2 gi ly chen ra lam ngui trong bnh hut
m n nhit phong. Cn va ghi khi lng. Nung lai nhit trn 30 phut ri cn
n khi lng khng i chen co kt tua SiO
2
thm t bng vai giot nc ct thm vai
ba giot H
2
SO
4
c khoang 10 ml axt HF lam bay hi trn bp in n kh, thm vao
10ml HF na va lam bay hi ln th 2
SiO
2
chuyn thanh SiF
4
bay hi. Ba con lai cha 1 lng nho Fe
2
(SO
4
)
3
va Al
2
(SO
4
)
3
. Lai
nung chung nhit 1000
0
- 1100
0
C. Cn lai khi lng chen co ba. Ly lai ba bng cach
cho vao chen co ba khoang 2 gam K
2
S
2
O
7
( Nu khng xac nh SO
4
2-
). Khi xac nh ion
SO
4
-2
ngi ta ly lai ba bng cach nung chay vi hn hp Na
2
CO
3
va K
2
CO
3
, nung chay trn
ngon la en kh. Ly ch a nung chay ra bng nc ct un si. Dung dch thu c un si
cho tan ht va gp vao phn dung dch va nc ra thu c trn, thm nc ct n vach (
bnh dung tch 500ml) l c u. Dung dch cha trong bnh 500ml va thu c goi la dung
dch Axt xa c nh Al
2
O
3
, Fe
2
O
3
, MgO, CaO, SO
3
.
Cach tinh
% SiO
2
= 100 .
2 1
g
A A

Trong o : A
1
- Trong lng chen co kt tua SiO
2
trc khi x l.
A
2
- Trong lng chen co ba nung sau khi x l.
g- Lng mu t ly phn tch.
2.2.4 Xac djnh ham luong oxyt st ( Fe
2
O
3
).
a) Nguyn tc:
Trong dung dch sau khi loc Silc, st tn tai dang Fe
+3
mi trng pH= 1,5-2 no
tao vi ch th axt sun fosalixilc mt phc cht mau tm o kem bn hn phc cht cua
no vi EDTA. Trc tin EDTA tao phc v i Fe
+3
ngoai dung dch. Sau o, no tao phc
Giao an phn tch silicat
22
vi Fe
+3
nm trong phc cua Fe
+3
vi ch th va giai phong ch th dang t do. Phep ch
th kt thuc khi dung dch mt mau o tm cua phc Fe
+3
va ch th.
b) Hoa cht:
- Dung dch NaOH 10%
- Dung dch chi th mau axt sulfoasalixilic10%
- Dung dch EDTA
c)Cach lam:
Dung ng hut nh mc 50ml ly 50ml trong dung dch A (noi phn bai 4-3) tng
ng vi 0,1 gam mu, cho vao cc 300ml thm vao 2ml ch th mau axt
sulfoasalixilic. Trung hoa dn d n bng NaOH 10% n khi dung dch co mau tm o (
co pH= 1.5-2 ).
un no ng dung dch trn bp in n nhit 60
0
C-70
0
C. chun khi nong bng
EDTA 0,01M n khi dung dch mt mau o tm.
Tnh ham lng Fe
2
O
3
theo th tch dung dch EDTA 0,01M a tiu tn trong phep
chun o.
Cach tnh:
%Fe
2
O
3
= 100 .
. 0007985 . 0
g
V

Trong o :
0,0007985 la s gam Fe
2
O
3
tng ng vi 1ml EDTA 0,01M.
V - th tch EDTA a tiu tn trong phep chun.
g - lng gam mu trong dung dch ly chun .
2.2.5 Xac nh oxt nhm ( Al
2
O
3
).
a) Nguyn tc:
Trong dung dch sau khi loai st va titan bng dung dch NaOH 30%. Nhm con lai
dang mui aluminat tan mi trng pH=5,7 , nhm phan ng v i 1 lng d EDTA
tao thanh mt phc kem bn v ng hn ph c cua no v i Natriflorua ( NaF ) lng d
EDTA c chun bng dung dch axetat kem vi ch th da cam. Sau o cho NaF
vao ph c bn vi nhn va giai phong EDTA a tac dung vi nhn.
- Chun lng EDTA va c giai phong ( tng ng vi Al ) bng dung dch
axetat kem. T th tch dung dch axetat kem tiu tn ln chun th hai la tnh ra ham
lng Al
2
O
3
co trong mu t.
b) Hoa cht:
- Dung dch NaOH 30%.
- Dung dch HCl 1:1.
- Dung dch m pH=5,4:100ml CH
3
COOH 90%, 100ml NH
4
OH 25% + 8% nc
ct.
- Ch th xylenol da cam 0,1%.
- Ch th fenolphtalein 0,1%.
- Dung dch kem axetat 0,025M [ Zn( CH
3
COO )
2
].
Giao an phn tch silicat
23
- Dung dch Natriflorua 3%.
c) Cach lam:
Dung ng hut nh mc 50ml ly 50ml dung dch A( noi phn bai 4-3 ) tng ng
vi 0,1g mu cho vao cc 300ml thm vao 30ml dung dch NaOH 30%. un si dung
dch sau 15-20 phut. Loc kt tua bng giy loc thng. Ra nc loc trc ht vai ln
bng dung dch NaOH loang 2%. Sau o ra bng nc si. n khi nc loc ht phan
ng kim ( th bng giy pH ). Nc loc va nc ra cho vao cc 500ml ( th tch cua
no khng c ln hn 200ml ) thm vao o 20ml dung dch EDTA 0,025M va 3 giot
ch th fenolphtalein 0,1%.
Trung hoa t t bng dung dch HCl 1:1 n khi mt mau hng. Thm vao 15ml dung
dch m pH = 5,7. un no ng n 50-60
0
C thm 4 giot ch th xylenol da cam 0,1%.
Dung dch co mau vang. Chun lng EDTA d bng dung dch axetat kem 0,025M.
n khi dung dch co mau hng thm vao 15ml dung dch NaF 3%. un si 2 phut
NaF tao phc bn vi nhn va giai phong EDTA. Lng EDTA c giai phong ra
tng ng vi lng nhm co trong dung dch. Dung dch co mau vang ngui n
50-60
0
C. Long EDTA va c giai pho ng bng axetat kem 0,025M n khi dung
dch co mau hng thm vao15ml dung dch NaF 3 %. un si 2 phut NaF tao phc
bn vi nhn va giai phong EDTA . Lng EDTA c giai phong ra tng ng v i
lng mui co trong dung dch. Dung dch co mau vang ngu i n 50- 60
o
C lng
EDTA mi c giai phong bng axtat kem 0,025M n khi dung dch co mau hng.
Cach tnh:
100 .
. 0012745 , 0
3 2
g
V
O Al =
Trong o:
0,0012745 s gam xt nhm tng vi1ml Zn( CH
3
COO)
2
0,025M.
V - th tch dung dch Zn( CH
3
COO)
2
0,025M tiu tn ln chun th 2.
g - s gam mu trong dung dch ly xac nh Al
2
O
3

Chu y: nhit va s nhn mau hai ln chun phai ging nhau.

2.2.6 Xac djnh CaO
a) Nguyn tc:
Trong dung dch sau khi loai ion Fe
3+
va Ti
4+
, Canxi tn tai di dang ion Ca
2+
.
mi trng pH = 12 ion Ca
2+
tao vi ch th fluorexon mt phc cht mau xanh quynh
quang ( vi ch th murext mt phc kem bn mau o nho ) kem bn hn phc cua no
vi EDTA. Chun trc tip ion Ca
2+
bng EDTA vi ch th fluorexon hay murexit,
giai phong ch th dang t do co mau h ng nhat ( hay tm hoa ca khi dung murexit )..
Phep chun kt thuc ham lng CaO trong t tnh theo th tch EDTA 0,01M tiu
tn.
b) Hoa cht:
- Dung dch KOH 25%
Giao an phn tch silicat
24
- dung dch NaOH 30%
- Dung dch NH
4
OH m c
- NH
4
Cl tinh th
- Ch th fluorexon: 1 gam ch th + 100gam KCl trn u va nghin mn
- dung dch KCN 5%
- dung dch EDTA 0,01M
c) Cach lam:
Du ng ng hut nh mc 100ml dung dch A ( noi muc 3 & 4) tng vi 0,2 gam
mu, cho vao cc 300ml thm 2g NH
4
Cl va nho t t tng giot NH
4
OH m c, va
nho va khuy u n khi kt tua ht Fe
3+
, Al
3+
, Ti
4+
( dung dch tr nn sang ). un
si trn bp in loai ht NH
3
d. Loc kt tua qua giy loc thng. Ra bng nc ct
un si n ht phan ng kim th bng giy pH. Dung dch loc va nc ra hng vao
bnh nh mc 250ml thm nc n vach va lc u. Dung dch thu c goi la dung
dch B. xac nh Ca
2+
va Mg
2+
dung ng hut 100ml ly 100ml dung dch B tng
ng vi 0,04 gam mu cho vao cc 250ml ( hay bnh tam giac 250ml) thm vao 15ml
KOH 25% , 5ml KCN 5% , mt hat ng ch th fluorexon ( hay murexit th thay 15ml
KOH25% bng 15ml NaOH30%). Khuy u va chun bng EDTA 0,01M n khi
dung dch mt mau xanh quynh quang ( nu dung murext th dung dch t mau o nho
sang mau tm hoa ca) cua phc cht gia Ca va fluorexon. Ghi th tch EDTA 0,01M a
tiu tn trong phep chun .
Tin hanh mt th nghim trng:
Ly 100ml nc ct cho vao cc 250ml thm vao 15ml KOH 25% ( hay dung
NaOH30% nu du ng murexit ) 5ml KCN 5%, mt hat ng ch th fluorexon ( hay mui
murexit ) khuy u va chun bng EDTA 0,01M. Ghi th tch EDTA a tiu tn khi
chun.
Cach tinh
100 .
) 2 1 ( 00056 , 0
g
V V
CaO

=
Trong o:
0.00056 s gam Cao tng ng vi 1ml EDTA0,01M
V1 s ml EDTA 0,01M a tiu tn chun ion Ca
2+
trong dung dch.
V2 s ml EDTA 0,01M tiu tn chun mu trng.
g - s gam mu trong dung dch ly xac nh CaO
2.2.7 Xac djnh MgO
mi trng pH = 10,6 th Mg
2+
va Ca
2+
cung tao phc vi ch th Eri crm en T ( ki
hiu ETOO) mt phc cht mau o ti, ph c cht nay kem bn hn phc cua chung vi
EDTA. Trn c s o ngi ta chun ng thi Ca
2+
va Mg
2+
t do ngoai dung dch,
sau o no tao phc bn vi ion Ca
2+
, Mg
2+
trong phc khng bn cua chung vi ch th
giai phong ch th dang t do. Dung dch chuyn t mau o ti sang mau xanh.
Tin hanh mt th nghim trng:
Giao an phn tch silicat
25
Ly 100ml nc ct cho vao cc 250ml thm vao 15ml KOH 25% ( hay dung
NaOH30% nu du ng murexit ) 5ml KCN 5%, mt vai giot ETOO khuy u va chun
bng EDTA 0,01M. Ghi th tch EDTA a tiu tn khi chun.
Cach tinh
100 .
) 2 1 ( 00056 , 0
=
g
V V
MgO

0.00056 s gam Cao tng ng v i 1ml EDTA 0,01M
V1 - s ml EDTA 0,01M a tiu tn chun ion Ca
2+
trong dung dch.
V2 - s ml EDTA 0,01M tiu tn chun mu trng.
g - s gam mu trong dung dch ly xac nh CaO.

2.3 PHN TICH THANH PHN HOA CUA DA VI
2.3.1 D m xac djnh ging nhu phn ximng
2.3.2 Luong mt khi nung xac djnh nhu phn xi mng
2.3.3 Xac djnh ham luong SiO
2
:
a) Nguyn tc:
Hoa tan mu bng dung dch HCl, c can tach SiO
2
.nH
2
O. Loc kt tua em
nung ri cn.
b) Hoa cht:
- Dung dch HCl m c.
- Dung dch HCl 1:1.
- Dung dch AgNO
3
1%.
c) Cach tin hanh:
Cn 3 g mu vao cc thuy tinh, tm t mu bng nc ct, y cc bng mt
knh ng h. Nho t t dung dch HCl 1:1 n khi ngng sui bot, thm vao cc
15ml HCl m c, trang thanh cc va mt knh ng h bng nc ct. t cc
ln bp cach cat, c n kh, tan vun kt tua , c thm 30-60 phut nhit trn
(<115
0
C) kt tua hoan toan SiO
2
.
ngui cc, tm t mu bng 10ml HCl m c sau 5 phut thm vao cc
100ml n c ct si, khuy u un nhe (khng un si) hoa tan cac mui. Loc
dung dch qua giy loc bng vang, ra sach cc bng n c ct nong, tip tuc ra kt
tua n ht ion Cl
-
(th bng AgNO
3
1%).
Chuyn kt tua va giy loc vao chen s (a nung va cn bit khi lng) t
chay giy loc ri nung nhit 950
0
C khoang 1-1
h
30 ngui trong bnh hut m
ri cn. Dung dch loc ra nh mc 250ml xac nh thanh phn cac xit khac
(dung dch 1).
Tnh ham lng SiO
2
trong mu.
Ham lng MKN tnh bng cng thc.
SiO
2
(%) = (G
1
- G
0
).100
Giao an phn tch silicat
26
G
Trong o:
G
1
: Khi lng chen va kt tua (g).
G
0
: Khi lng chen khng (g).
G: Khi lng mu em phn tch (g)
2.3.4 Xac djnh ham luong Fe
2
O
3
.
a) Nguyn tc:
Chun lng st bng EDTA tiu chun theo ch th sunfosalisilic pH=1,5-
2.
b)Hoa cht:
- Axit sunfosalisilic.
- Dung dch HCl 1:1.
- Dung dch NaOH 10%
- Dung dch EDTA 0,02M.
c)Cach tin hanh:
Ly 50ml dung dch 1 cho vao cc thuy tinh, thm nc ct khoang 100ml, 2ml
axit sunfosalisilic 10%. Dung NaOH 10% va HCl 1:1 iu chnh dung dch n
pH=1,5-2.
un nong dung dch n 70
0
C chun dung dch khi con nong bng EDTA
0,02M n khi dung dch chuyn t mau tm o sang khng mau (hay vang
nhat). Ghi th tch EDTA 0,02M tiu thu (ml).
Tnh kt qua.
V.0,0015970.100
Fe
2
O
3
(%) =
a
Trong o:
V: Th tch EDTA 0,02M tiu thu.
a: Lng mu em xac nh (g).
0,0015970 la s gam st tng ng vi 1ml dung dch EDTA 0,02M.
2.3.5 Xac djnh ham luong Al
2
O
3
.
a) Nguyn tc:
Tach Al khoi Mg, Ca, Fe bng NH
4
OH va NaOH. Chun thay th Al
t complexonat theo ch th xylenol dacam pH=5,5-5,7.
b)Hoa cht:
- Dung dch EDTA 0,02M.
- Dung dch m pH=5,7.
- Dung dch Zn(CH
3
COO)
2
0,02M.
- Dung dch NaOH 30%.
- Dung dch NaF 3%.
- Dung dch AgNO
3
1%.
- NH
4
Cl.
Giao an phn tch silicat
27
- Dung dch NH
4
OH 1:1.
- Dung dch HCl 1:1.
- Cht ch th xylenol.
- Cht ch th metyl o.
- Cht ch th phenolphtalein.
c) Cach tin hanh:
Hut 100ml dung dch cho vao cc thuy tinh, thm 1g NH
4
Cl un no ng
dung dch. Thm vao cc 1 giot ch th metyl o. Dung NH
4
OH 1:1 nho tng
giot vao cc va khuy u cho n khi ch th chuyn sang mau vang, cho d 1
giot NH
4
OH. un nong ng tu kt tua, loc dung dch qua giy loc bng o,
ra kt tua t 1-2 ln bng nc ct nong.
Hoa tan kt tua trn giy loc cho tr lai cc kt tua Fe(OH)
3
va
Al(OH)
3
bng HCl 1:1 dung nc ct nong r a sach kt tua n ht ion Cl
-
(th
bng AgNO
3
1%). Thm vao cc 30ml NaOH 30% va un dung dch ti si.
ngui dung dch, chuyn vao bnh nh mc 250ml, nh mc ung 250ml bng
cach thm nc ct va lc tht u. Loc dung dch a nh mc qua giy loc
kh, phu kh vao mt bnh non 250ml (dung dch 2). Ly 100ml dung dch 2
cho vao cc 250ml, thm tip vao o 5-7ml EDTA 0,025M khuy u, nho mt
giot phenolphtalein ri dung HCl 1:1 va NaOH 30% iu chnh n mt mau
hng. Thm tip vao cc 20ml dung dch m pH=5,7. un nong dung dch n
70-80
0
C, nho vao o 1 giot xylenol da cam. Chun dung dch con nong nay
bng Zn(CH
3
COO)
2
0,02M n chuyn mau t vang sang hng. Thm tip vao
cc 15ml NaF 3%, un dung dch ti si.
ngui dung dch n 70-80
0
C va chun dung dch nay bng
Zn(CH
3
COO)
2
0,02M n khi chuyn mau t vang sang hng. Ghi th tch tiu
thu.
Tnh kt qua.

V.0,0010196.100
Al
2
O
3
(%) =
a
Trong o:
V: Th tch kem axetat 0,02M tiu thu (ml)
a: Lng mu em xac nh (g).
0,001096 la s gam Al
2
O
3
tng ng vi 1ml dung dch kem axetat
0,02M.
Ghi chu: Th tch EDTA 0,025M cho vao dung dch 2 phu thuc vao ham lng
Al
2
O
3
trong mu, nu mu (a) em phn tch co ham lng Al
2
O
3
nho hn 15%
th dung 10ml la u, co n cac mu co ham lng Al
2
O
3
cao hn 15-20% th dung
15-20 ml EDTA 0,025M.
2.3.6 Xac djnh ham luong CaO.
Giao an phn tch silicat
28
a) Nguyn tc:
Chun Canxi bng dung dch EDTA theo ch th fluorexol pH>12.
b) Hoa cht:
- Dung dch EDTA 0,02M.
- Dung dch HCl 1:1.
- Dung dch KCN 5%.
- Dung dch KOH 25%.
- Ch th fluorexol.
c) Cach tin hanh:
Hoa tan 0,2 g mu trong cc thuy tinh bng 10ml HCl 1:1 va un n tan.
Chuyn dung dch vao bnh nh mc 250ml. nh mc va lc u (dung dch 3).
Ly 25ml dung dch vao cc thuy tinh, thm nc ct n 100ml, thm tip 5
ml dung dch che du KCN 5% va 20ml dung dch KOH 25% va mt t cht ch th
fluorexol.
t cc ln mt nn en, du ng EDTA 0,02M chun n khi mt mau xanh
huynh quang. Ghi lai th tch EDTA tiu thu.

Tnh kt qua.

(V
1
- V
0
).0,0011216.100
CaO (%) =
a
Trong o:
V: Th tch EDTA tiu tn khi chun (ml).
V
0
: Th tch EDTA tiu tn khi chun mu trng (ml).
0,0011216: s gam CaO tng ng vi 1ml EDTA.
a: Lng mu ly em phn tch (g).
2.3.7 Xac djnh ham luong MgO.
a) Nguyn tc:
Xac nh tng s ham lng CaO + MgO trong mu chun bng EDTA 0,02M
theo ch th ETOO en pH =10,5. T kt qua xac nh CaO suy ra ham lng MgO.
b) Hoa cht:
- Dung dch EDTA 0,02M.
- Dung dch m pH=10,5.
- Dung dch KCN 5%.
- Ch th ETOO.
c) Cach tin hanh:
Ly 25ml dung dch 3 cho vao cc thuy tinh, thm nc ct n khoang 100ml,
thm tip vao cc 5ml KCN 5%, 20ml dung dch m pH=10,5 va 1-2 giot ch th
ETOO. Chun dung dch bng EDTA 0,02M n khi chuyn mau t o nho sang
Giao an phn tch silicat
29
xanh nc bin. Ghi lai th tch EDTA tiu thu. Lam song song m t mu th nghim
trng.
Tnh kt qua.

(V
1
- V

).0,00806.100
MgO (%) =
a
Trong o:
V
1
: Th tch EDTA tiu tn khi chun tng s CaO va MgO (ml).
V
0
: Th tch EDTA tiu tn khi chun mu trng (ml).
V

: Th tch EDTA 0,02M tiu tn khi chun CaO.

a: Lng mu ly em phn tch (g).
2.3.8 Xac djnh ham luong SO
3
.
a) Nguyn tc:
Kt tua ion SO
2-
trong mi trng HCl la mui tinh th. Loc ra kt tua va nung
nhit 850
0
C . T BaSO
4
kt tua ta tnh c ham lng SO
3
trong mu.
b) Cach tin hanh:
Ly khoang 20ml dung dch 1 cho vao cc thuy tinh, thm 1-2 giot metyl o ri
un nong n 70
0
C , nho dung dch NH
4
OH n khi dung dch co mau vang. un nong
dung dch trong 1-2 phut loc dung dch khi con nong qua giy loc bng o , ra kt tua
4-5 ln bng nc ct nong. Nc loc va n c ra thu c xac nh SO
3
. C can
dung dch loc ra n khoang 100ml, nho t t tng giot HCl 1:1 n khi dung dch co
mau o, cho d 4-5 ml HCl na.
un dung dch n si, ng thi un mt t BaCl
2
n si, khuy u dung
dch mu va nho t t tng giot (10ml) dung dch BaCl
2
10% vao cc mu. Tip tuc
khuy va un si 5-10 phut na. dung dch ni ch m khoang 6-8 gi (nhit
khoang 40-50
0
C). Loc kt tua bng giy bng xanh, ra kt tua bng nc ct nong n
ht ion Cl
-
. Chuyn kt tua va giy loc vao chen s (chen s a nung va cn n khi
lng khng i) t chay giy loc. Cho chen s co kt tua vao lo nung va tng nhit
n 850
0
C, lu mu nhit nay 1-1
h
30. ngui chen s trong bnh hut m n
nhit phong ri cn.
Tnh kt qua.

(G
1
- G
0
).0,343.100
SiO
3
(%) =
a
Trong o:
G
o
: Khi lng chen khng co mu (g).
G
1
: Khi lng chen co mu sau khi nung (g).
a: Khi lng mu em nung (g).
0,343 : H s chuyn i BaSO
4
v SO
3
.

Giao an phn tch silicat
30
2.4 PHN TICH THANH PHN HOA CUA THUY TINH
2.4.1 D m xac djnh ging nhu phn ximng
2.4.2 Luong mt khi nung xac djnh nhu phn xi mng
2.4.3Xac djnh ham luong Silic.
a)Nguyn tc:
Trong iu kin axit manh, keo ng vt mang in tch dng tac dung v i axit
silic mang in tch m lam cho axit silic trong dung dch b thoat nc, ngng tu va
kt tua hoan toan.
b)Hoa cht:
- Keo ng vt 1% cn 1 gam keo ng vt pha 100ml nc nhit 70
0
C.
Keo ng vt pha xong phai dung ngay. Kt tua silic phai nhit 70
0
C v nhit
nay hoat va hiu sut kt tua silic cua no la cao nht.
- HCl 1:1; HCl c (ty trong 1,19) va nc ct vi ty l th tch la 1:1.
- KSCN 20%: cn 20 gam KSCN hoa tan trong 80ml nc ct.
- AgNO
3
0,1N: cn 1,7 gam AgNO
3
hoa tan trong 100ml nc ct.
c) Cach tin hanh:
- t cc ng dung dch HCl cua cht nung chay ln bp cach thuy, ay cc ngp
di mt nc, chng cho ti trang thai st.
- Ly ra ri cho vao 20ml HCl c (ty trong 1,19) khuy u va yn 10-12 gi,
hoc t nong 10 phut.
- t cc cha dung dch trn va cc ng dung dch keo ng vt 1% mi pha vao
bp cach thuy.
- Khi dung dch keo at ti nhit 70
0
C th cho 10ml keo vao cc cha cht nung
chay (mi ln cho khoang 2ml, khuy u trong 5 phut).
- Ly ra ngui, loc bng giy loc khng tan, ra kt tua bng nc nong cho ti
khi khng con phan ng cua Fe
3+
(dung KSCN 20% kh ). Nu nh t SiO
2
trong
chen bach kim th phai ra cho n ht ion Cl
-
(dung AgNO
3
0,1N th).
- Dung dch loc c nh mc ti 100ml, dung xac nh Fe, Al, Ca, Mg, Ti,
Ba...goi la nc loc A.
- Du ng giy loc goi ky kt tua cua silic lai, cho vao chen bach kim a bit trong
lng (m
1
), tin hanh tro hoa, tng dn nhit ti 900
0
C trong 1 gi ly ra ngui
bt, ri cho vao Excotor 15-20 phut, dung cn phn tch cn trong lng (m
2
), ri lai
cho vao lo nung t 1 ln na, r i lai cn trong lng. Sai s hai ln cn khng vt
qua 0,3mg la c.
Tnh toan kt qua:


(m
2
- m
1
)
%SiO
2
=
Trong lng
mu cn
x 100
Giao an phn tch silicat
31
2.4.4 Xac djnh ham luong Fe
2
O
3
(Bng phuong phap chun d phuc cht-truong
hop Fe
2
O
3
lon)
a) Nguyn tc:
Dung dch sau khi a pha mu va a loai bo keo H
2
SiO
3
co cha Fe
3+
. Trn c s
cua phng phap chun phc cht dung EDTA chun trc tip Fe
3+
trong dung
dch mu.
Phan ng thc hin hoan toan iu kin pH = 2-3, vi ch th Natrisalisilit
(Na
2
SSal)
b) Hoa cht:
- Dung dch EDTA 0,05N-0,1N
- NaOH dung dch 2N
- HCl dung dch 2N
- Natri sulfosalisilat 10%
- HNO
3
c
c) Quy trnh xac nh:
Hut mt th tch dung dch A (a loai H
2
SiO
3
) tuy thuc ham lng st trong mu
ma ly th tch dung dch thch hp, cho vao bnh no n 250ml, thm 5-6 giot HNO
3

c, un si 1-2 phut. ngui dung dch ri thm tng giot NH
4
OH hoc NaOH 2N
n khi va xut hin vn kt tua mau nu, thm HCl 2N pha kt tua nu o, sau
o cho thm 2ml HCl 2N na co pH 2-3 (dung giy pH van nng th). Ri cho 6-7
giot ch th H
2
SSal 10% un nong dung dch n 60-70
0
C. Dung EDTA tiu chun tin
hanh chun n khi mau tm cua dung dch chuyn sang mau vang rm la c
(dung dch sau khi chun Fe
3+
gi lai xac nh Al
3+
).
Tnh kt qua




Nu ham lng Fe
3+
nho th tin hanh xac nh bng phng phap trc quang so mau.
QUY TRINH XAC DJNH HAM LUONG ST TRONG THUY TINH BNG
PHUONG PHAP THIOXI
* GII THIU CHUNG:
Trong mi trng axit ion Fe
3+
tao phc mau o vi Thioxianat. Phng phap trc
quang nh lng st da trn phan ng nay c dung ph bin v rt tin li,
nhay cao, hoa cht re. Tuy nhin co rt nhiu ion khac cung tao phc vi thioxianat
gy can tr phep xac nh st nh:
- Ag
+
, Hg
2
2+
tao mui khng tan.
- Cac ion Ca
2+
, Bi
3+
, Ti
4+
, UO
2+
, Mo
3+
. cho phc mau vang hoc da cam.
- Ion Co
2+
anh h ng manh, co th loai tr do hp thu bc song khac.
- Cac ion Mg
2+
, Cd
2+
, Zn
2+
, Sb
3+
cung tao phc vi thioxianat st.
mDg. Fe
2
O
3

%Fe
2
O
3
=
Trong lng
mu cn
x 100
Giao an phn tch silicat
32
V vy xac nh st cn phai loai tr c cac yu t trn.
Ngoai cac ion kim loai k trn mt vai anion cung can tr n phep xac nh st
nh: F
-
, PO
4
3-
, HPO
4
2-
, C
2
O
4
2-
v chung cung tao phc v i Fe
3+
lam giam ham lng Fe
3+

trong dung dch phn tch.
Trong thuy tinh cac yu t k trn hu nh khng co hoc co vi ham lng rt nho
, khng gy anh hng n kt qua xac inh st. Cho nn chon phng phap thioxianat
nh lng trc quang st trong thuy tinh la thun li.
* Mt vai iu cn lu y:
- Sau khi pha loang n th tch cui cung dung dch phn tch cn cha n 10
phn triu Fe
3+
nu s dung may o quang vi knh loc 1cm. axit cua dung dch co
th trong khoang 0,05-0,1M (HNO
3
hoc HCl).
- Cac dung dch chun Fe
3+
s dung xy dng ng chun cn cha cung loai
axit va lng ging nh dung dch phn tch, ait hoa th dung axit HCl.
- Thm chnh xac lng SCN
-
sao cho nng cui cung khoang 0,3M.
- Nu trong dung dch phn tch co mt axit H
2
SO
4
th cn phai thm lng o
vao dung dch chun.
- Nhit cn khng i.
* Du ng cu va hoa cht:
- May so mau, du ng knh loc xanh luc .
- KCNS hoc NH
4
CNS nng 3M.
- Dung dch chun phen amoni: Hoa tan 0,8634g NH
4
Fe(SO
4
)
2
.12H
2
O trong nc
ct, thm 2ml HCl c nh mc thanh 1l. 1ml dung dch nay cha 0,1mg st (dung
dch 1). T dung dch trn pha thanh dung dch 0,005mg Fe/ml bng cach ly 50ml
dung dch trn pha thanh 1 lt (dung dch 2).
+*Tin hanh:
Ly 1 th tch dung dch phn tch thch hp (tuy thuc ham lng Fe
3+
trong
mu) vao bnh nh mc 50ml, thm nc ct n 40ml, thm 2ml HCl c, lc u,
thm 5ml KCNS 3M, lc u thm nc n vach. em o ngay mt quang.
- Dng ng chun.
Ly 10 bnh nh mc 50ml, ly ln lt vao mi bnh 0; 0,1; 0,5; 1; 2; 3; 4; 5; 6;
7; 8 ml dung dch chun 2. Thm nc ct n 40ml,thm 2ml HCl c, lc u, thm
5ml KCNS 3M, lc u thm nc n vach. o mt quang va xy dng ng
chun s phu thuc mt quang-lng st.
(Chu y: phc thioxianat rt kem bn, cn phai o rt nhanh)
*Tnh kt qua:

V.f
%Fe =
V
1
.G.10
Trong o: V la th tch dung dch mu sau khi pha mu (ml)
V
1
la th tch em phn tch (ml)
Giao an phn tch silicat
33
f la lng st tm c theo ng chun (mg)
G la khi lng mu (g).
2.4.5 Xac djnh ham luong Al
2
O
3
.
a) Nguyn tc: Phng phap chun ng thi Fe
3+
va Al
3+

- Dung dch sau khi chun Fe
3+
tip tuc cho d chnh xac 1 lng EDTA tiu
chun phan ng hoan toan vi Al
3+
phan ng nay cung thc hin pH = 5-6 (dung
dung dch m axetat, iu kin dung dch nong)
Al
3+
+ H
2
Y
2-
pH=5-6

AlY
-
+ 2H
+

Sau o chun phn d cua EDTA bng mt trong nhng h sau:
* Chun EDTA d bng Fe
3+
chun vi ch th H
2
SSal pH=5-6 im tng
ng xut hin mau o nu.
Fe
3+
+ H
2
Y
2-
pH=5-6

FeY
-
+ 2H
+

Tai im tng ng
Fe
3+
+ H
2
SSal
Khng mau
=
Fe
2
(SSal)
3

o nu
* Chun bng Zn(CH
3
COO)
2
pH=5-6 dung dch ngui vi nhng h ch th sau:
- Hn h p ch th Pheri - pero-Bezidin (t khng mau sang xanh luc)
Zn
2+
+ H
2
Y
2-
pH=5-6

ZnY
2-
+ 2H
+

- Co th du ng ch th xylenol da cam nhn im tng ng mau cua dung
dch chuyn t vang sang hng nhat
b) Hoa cht:
- EDTA 0,1N
- NH
4
OH 10%
- m axetat pH = 5-6 (pha hn hp 58ml CH
3
COOH 1N + 50ml NaOH 1N. Sau
o nh m c bng nc ct n 500ml)
- Metyl da cam 0,1%: Cn 0,1g Metyl da cam nh mc bng nc ct n
100ml.
- Xylenol da cam 0,5%. Hoa tan 0,25g trong 50ml etanol
- Zn(CH
3
COO)
2
0,1N.
c) Qui trnh xac nh:
Dung dch sau khi xac nh Fe
3+
, cho ch xac 1 lng d 25ml EDTA 0,1N, cho
mt giot metyl da cam 0,1%. Dung NH
4
OH 10% trung hoa ti mau vang nhat: thm
20ml dung dch m axetat, un si 5 phut. Sau o ngui n nhit phong ri
cho 1 lng nho xylenol da cam. Dung Zn(CH
3
COO)
2
0,1N chun ti khi dung dch
xut hin mau h ng.
Tnh kt qua:
Giao an phn tch silicat
34
100 .
.
.
) . ( ) . /(
%
2 3
3 2
) (
3 2
Xd
dm
hayZn Fe
EDTA O Al
V
V
V N V N mDg
O Al
+ +

=
mDg(Al
2
O
3
) = 102/4.10
-3
= 0,0255 (tnh theo N
EDTA
)
2.4.6 Xac djnh ham luong CaO.
(Ap dung cho loai mu co cha 0,1-1% CaO)
a) Nguyn tc:
Dung dch A, sau khi a loai bo RCO
3
bng kt tua hydroxit hoc che du RCl
3
-
c goi la dung dch B cha Ca, Mg,...em chun trc tip dung dch nay bng
EDTA tiu chun pH = 12, tai im tng ng c xac nh bng murexit (dung
dch i mau t o nho sang tm hoa ca) hoc ch th xanh huynh quang phluorexin
(mau cua dung dch chuyn t xanh quy nh quang sang hng).
Cac phan ng xat ra trong dung dch se la: H

- Trc khi chun :

Ca
2+
+ H
2
Ind
3-

Murexit
=
pH=12
CaH
2
Ind
-
o nho
- Trong qua trnh chun :
Ca
2+
+H
2
Y
2-

=

CaY
2-
+ 2H
+


- Tai im tng ng:

H
2
Y
2-
(lng d)
+ CaH
2
Ind
-
(o nho)

= CaY
2-
+ H
2
Ind
3-
(tm hoa ca)

K
CaH2Ind
- = 3,9.10
-6

K
CaY
2- = 2,7.10
-11
T o suy ra h lng CaO theo cng thc sau:
100 .
.
.
) . (
%
) (
Xd
dm
EDTA CaO
V
V
G
V N mDg
CaO =

Trong o:
mDg
CaO
= 56,08/2.10
-3
= 0,02804 (tnh theo N
EDTA
)
N
EDTA
: nng ng lng gam cua EDTA (CN)
V
EDTA
: s ml EDTA tiu tn (ml)
Vm

: S ml dung dch mu nh mc ban u (ml)
Vx : s ml dung dch mu ly phn tch (ml)
G: s gam mu phn tch a s dung (g)
b) Hoa cht:
- Dung dch EDTA 0,05M
- Murexit 4% - cn 1g murexit trn u vi 100g KCl trn u nghin mn.
- KOH 20%
Giao an phn tch silicat
35
- Hn hp che : 2ml trietanolamin + 15g NaF + 5g KCN + nc ct n vach
1000ml.
c) Quy trnh xac nh:
Ly c 25ml dung dch N (a loai bo H
2
SiO
3
va R(OH)
3
) chuyn mu vao bnh
non 250ml, pha loang bng nc ct ti vach 100ml, cho vao 10ml KOH 20%. Dung
dch khng uc, cho mt lng nho murexit 1% trn vi KCl dung dch co mau o
nho. Tin hanh chun bng EDTA 0,05M. Tai im tng ng dung dch chuyn
t mau o nho sang tm hoa ca.
Co th che du ri xac nh Ca
2+
. T dung dch u (A) ly 25ml dung dch A
(sau khi a loai H
2
SO
3
) cho vao bnh nh mc 250ml. Thm 10ml KOH h n hp che
u, cho 10ml KOH 20%, cho mt lng nho murexit 1%. Dung EDTA 0,05N chun
Ca
2+
.
2.4.6 Xac djnh ham luong MgO.
a) Nguyn tc:
Dung dch sau khi a loai bo H
2
SiO
3
va RCl
3
- dung dch B c em i chun
tng l ng Ca va Mg bng EDTA pH = 8-10 vi ch th ETOO.
Cac phan ng xay ra la:
- Trc khi chun

Mg
2+
+ HInd
2-

ETOO(xanh luc)
=
pH=8-10
MgInd
-
+ H
+
o nho

K
MgInd
- = 10
-17

- Trong qua trnh chun :
Ca
2+
+H
2
Y
2-

=

CaY
2-
+ 2H
+



Mg
2+
+H
2
Y
2-

=

MgY
2-
+ 2H
+


- Tai im tng ng:

H
2
Y
2-
(lng d)
+ MgInd
-
(o nho)

= MgY
2-
+ HInd
2-
(xanh luc)
+ H
+

Phng trnh tng quat la:

(Ca
2+
, Mg
2+
) + H
2
Y
2-

(o nho)


=
pH = 8-10
MgY
2-
+ CaY
2-
+ H
+
(xanh luc)
b) Hoa cht:
- EDTA: dung dch 0,05-0,1N
Giao an phn tch silicat
36
- m amoni co pH = 8-10 (50g NH
4
Cl + 250 ml NH
4
OH c 25% + nc ct
nh mc n 1000ml.
- KSCN 5% (hoa tan 5g KSCN trong 100ml nc ct).
c) Quy trnh phn tch:
Ly 25ml dung dch B (th tch tuy thuc ham lng Ca, Mg) cho vao bnh non
250ml, pha loang n th tch V=100ml cho thm 20ml m Amoni, cho tip 5-6 giot
KSCN 5% ( che cac kim loai hoa tr 2 nh Cu
2+
, Ni
2+
, Zn
2+
) thm mt lng nho
ETOO, chun trc tip bng EDTA 0,05-0,1N.
Tnh kt qua:
Ham lng MgO c tnh theo cng thc sau:
100 .
.
.
) . ( ) . /(
%
O ) (
Xd
dm
murexit ETO MgO
V
V
G
V N V N mDg
MgO

=
Trong o:
mDg
MgO
= 40,40/2.10
-3
= 0,02020 (tnh theo N
EDTA
)
(NV)
Murexit
: lng EDTA tiu tn khi chun Ca
2+
bng murexit
(NV)
ETOO
: lng EDTA tiu tn khi chun tng Ca, Mg theo ch
th ETOO.
Vm

: S ml dung dch mu nh mc ban u (ml)
Vx : s ml dung dch mu ly phn tch (ml)
G : lng mu cn ban u (g)
XAC NH HAM LNG Pb BNG PHNG PHAP TRC QUANG DITHIZON
Dithizon la thuc th hu c co kha nng tao phc cang cua vi hang loat ion kim loai
trong o co Pb. Phc ch Dithizonat kho tan trong nc nhng d tan trong cac dung
mi hu c nh: CHCl
3
, CCl
4
. Do o ngi ta dung phng phap chit trc quang
xac inh Pb.
Ch Dithizonat c chit chon loc va nh lng t cac dung dch nc co pH =
8-9 cha ham lng d xianua la cht dung che nhiu ion kim loai khac co th cung
b chit vi Pb. Trong mi trng k trn cung b chit vi Pb co Tali, Bimut va Sn(II).
Tali khng can tr vic xac nh Pb nhng Bimut va Sn ngn can. V vy i vi cac
i tng mu co cha nhiu Sn, Bi chung ta cn tach Bi va Sn trc khi xac nh Pb
bng cach nh sau:
Trong mi trng axit Ph khng b chit va con lai trong lng nc, Sn va Bi
c tach ra nh sau: Thm hydrazin vao dung dch mu ang nong kh
Sn(III)Sn(II), ng thi kh mt s kim loai khac, ngui ri thm 10ml c
dung dch Natritactrat va iu chnh pH dung dch n 2-3 bng axit tactric ri tin
hanh chit mi ln 5ml dung dch dithzon 0,05% trong CCl
4
, va tin hanh cho n khi
pha hu c gi nguyn mau xanh cua Dithizon, cui cung lc lng nc vai ln vi
CCl
4
cho n khi pha hu c khng con mau xanh na ri tin hanh xac nh Pb.
i vi cac loai mu ham lng Sn va Bi khng ang k so vi ham lng Pb
tin hanh xac nh Pb t dung dch nc sau khi phn huy mu. Ly dung dch mu
Giao an phn tch silicat
37
thm vao vai giot dung dch phenolphthalein, cho t t dung dch amoniac cho n khi
xut hin mau hng, sau o thm vao 10ml dung dch hydrazin axetat va un no ng h n
hp 90-95
0
C trong 10 phut sau o chuyn ho toan dung dch vao phu chit thm 10
phut dung dch natritactrat, 5 giot thimon xanh va thm NH
4
OH n khi xut hin mau
xanh cua cht ch th, thm 10ml dung dch KCN va tng giot dung dch axittactric cho
n khi dung dch chuyn t mau xanh n c bin sang xanh la cy. Thm vao 10ml
dung dch Dithizon/CCl
4
va chit Pb. Khi chit tht cn thn chuyn h u c vao phu
chit khac (khng nhng giot nc sang phu chit nay. phu chit a chit phai
con lai mt t lng h u c, ri tip tuc chit mi ln 5ml dung dch Dithizon cho n
khi khng i mau thuc th, cui cung 5ml CCl
4
va lc. Tt ca phn chit thu v phu
chit th 2. Va ra lng h u c bng 20ml dung dch ra loai ht Dithizon t do
trong lng hu c.
Chuyn dung dch ch Dithizonat vao bnh nh mc 25mlp nc trong phu
chit c lc vai ln mi ln 1ml CCl
4
ly phn o cho vao bnh nh mc va nh
mc ti vach bng CCl
4
. Do mt quang cua dung dch =520mm. ng thi th
nghim khng vi nc ct va cung th tch Dithizon nh vy lam dung dch so
sanh.
Lp ng chun:
Thm vao 1 loat cc vi th tch 0 ; 2,5 ; 5 ; 10 ; 20 ; 30ml dung dch chun Pb
co cha 2g Pb/ml va thm nc ct vao mi cc n th tch 50ml, dung dch chun
c tin hanh cung iu kin nh dung dch phn tch nhng co th bo qua giai oan
kh. Khi chit ttat ca dung dch chun u s du ng lng nh nhau dung dch
Dithizon.
Ham lng Pb c tnh theo cng thc nh sau:
1. X = C.100/V (g/ml)
C: nng ch tm theo ng chun.
V: Th tch dung dch mu ly phn tch. 100 th tch mu c pha loang.
2. Hoc d ng ng chun bng phng phap bnh phng ti thiu (da ng y = ax
+b ) va da vao ng chun xac nh ham lng Pb trong mu.
Hoa cht:
- Dung dch phenolphthalein 0,5%
- Hirazinaxetat dung dch dung kh trn 15ml dung dch hirazinhydrat vi
50ml CH
3
COOH loai bng dung nc ct pha loang n 100ml.
- Natritactrat 10% cn nn ra dung dch nay bng Dithizon/CCl
4
.
- Axittattric 50%
- KCN ho c NaCN 10 %
- Thimol xanh 0,4 % hoa 0,4 g mui natri cua thimol xanh trong vai chuc ml
nc ct va pha loang ln 100ml.
- Dung dch ra NH
3
+ KCN + Na
2
SO
3
.
Giao an phn tch silicat
38
Thm 10ml dung dch KCN loai 10 % vao 175ml NH
4
OH c va cho vao 7,5 ml
Na
2
SO
3
10% pha loang n 1000ml. Dung dch Na
2
SO
3
cn c lam sach ch bng
cach chit trc bng Dithizon.
Ch Axetat dung dch chun:
- Dung dch gc: Hoa tan 200mg ch kim loai loai tkpt trong 4 ml HNO
3
1:1 un
nong ch tan hoan toan ngui chuyn toan b vao bnh nh mc 1 lit bng nc
ct.
- Dung dch lam vic: ly 10 ml dung dch gc (0,2 g/ml) pha loang bng nc
ct thanh 1 lit dung dch, dung dch nay cha 0,002mg/ml.
- Dithizon:
Dung dch gc hoa tan 50mg dithizon trong 100ml CCl
4
trong phu chit co dung
tch 500ml. Thm vao o 200ml nc ct va 5-10 ml NH
4
OH y nut va lc 2 phut.
Dithizon chuyn vao tng nc sau khi hai tng a phn lp laoi bo tng hu c,
thm vao 200ml CCl
4
va HCl loang cho n khi tng nc co phan ng axit ro. y
nut lc hn hp c thn h n h p di chuyn hoan toan Dithizon sang tng hu c,
chuyn sang tng h u c sang phu chit sach va ra no 3 ln mi ln 50ml nc ct,
chuyn dung dch dithizon/CCl
4
vao bnh thuy tinh mau nu va d l dung dch o,
dung dch HCl 0,5 % co cha NH
2
H
2
SO
4
0,5 % dung dch trong ti.
Dung dch lam vic ly 1ml dung dch gc pha loang va nh mc 500ml bng
dung mi CCl
4
.
2.4.7 PHN TCH BORO TRONG THUY TINH
a)Nguyn tc cua phng phap:
Chun lng axit boric giai phong ra bng NaOH vi ch th la
phenolphtalein. tng bc nhay trong qua trnh chun thm vao poliaxit nh la
Menitol hoc glixerol vi Menitol cho kt qua chnh xac hn.
b) Qua trnh tin ha nh:
Cn 0,5 g thuy tinh a c nghin nho trn u vi 3 g Na
2
CO
3
cho vao chen
Platin nung nong chay 600-700
0
C trong khoang 2-3 phut. Hn hp no ng chay c
lam ngui , cho vao 20-30ml nc nong . Dung ua platin nghin mn hn hp. loc va
ra kt tua bng 3-5ml nc nong, cho dung dch loc va nc ra vao cc 250ml thm
va 7ml HCl c va un cho n gn si. Thm CaCO
3
khan vao dung dch (cho n
khi phan ng co kim yu) un si dung dch trong khoang 10 phut (chu y: mu un
trong thit b co ng sinh han hi lu) loc ra kt tua bng n c nong, gi th tch
khoang 100ml, cho dung dch vao bnh 250ml thm vao mt t Na
2
CO
3
, lp ng sinh
han vao u trn cua ng ni vi u hut cua may hut chn khng un si dung dch
khoang 3-4 phut ngng un, nhng dung dch tip tuc si. Sau khi dung dch ngng si
lam lanh t i nhit phong thm vao 4-5 gio t phenolphtalein va t buret cho tng giot
NaOH 0,1N cho n khi dung dch co mau hng. Thm vao 1g Manitol lc tip tuc
chun ti mau h ng, tip tuc nh vy khi mau hng bn thu c.
1ml NaOH tng ng vi 0,00348 B
2
O
3

Giao an phn tch silicat
39
Chu y: Cac dung cu thuy tinh u phai khng cha Bo.

2.5.SAI S TRONG PHN TCH NH LNG HO A HOC
Gia tr cua mt phep phn tch nh lng c anh gia ung va lp cua kt
qua thu c.
2.5.1. ung va lp
ung phan anh s phu h p gia kt qua thc nghim thu c vi gia tr thc
cua ai lng o.
lp phan anh s phu hp gi a kt qua thu c trong cac th nghim lp lai
trong cung iu kin thc nghim qui nh cua phep phn tch. Kt qua phn tch co
th co lp cao (chnh xac) nhng khng u ng.
V du: khi kim tra dung dch HCl co nng chnh xac 0,1000M, hai sinh vin A
va B thu c kt qua trong cac th nghim c lp nh sau:
A: 0,1002 ; 0,0999 ; 0,1004 ; 0,0996 ; 0,1003
B: 0,1014 ; 0,1017 ; 0,1016 ; 0,1015 ; 0,1014
Qua kt qua trn chung ta nhn thy rng kt qua cua sinh vin A ung nhng kem
chnh xac, kt qua cua sinh vin B co lp tt nhng u ng th kem.
ung va lp co lin quan cht che vi sai s phn tch. Ngi ta phn bit sai
s h thng va sai s ngu nhin.
2.5..2. Sai s h thng.
Sai s h thng lam cho kt qua phn tch khng u ng. Nguyn nhn cua sai s h
thng la xac nh va v nguyn tc co th bit c. Mi loai sai s h thng lam cho
kt qua phn tch dch chuyn theo mt chiu nht nh (tng hoc giam). Sai s h
thng co th khng i, cung co th thay i theo iu kin. V du, khi cn CaCl
2
trong
mt chen cn khng y np th kt qua cn se tng dn theo thi gian v CaCl
2
la cht
hut m manh. Sai s nay tng theo thi gian cn va b mt tip xuc cua hoa cht vi
kh quyn.. ..
Tuy vy sai s h thng do vic pha hoa cht trong bnh nh mc c chun hoa sai
la ai lng khng i, khng phu thuc vao cac iu kin phn tch khac.
Trong phn tch hoa hoc co th phn chia thanh cac loai sai s h thng sau y:
a) Sai s do s dung may, hoa cht va thuc th, v du s du ng cn va qua cn
khng u ng, s dung cac dung cu o th tch khng chnh xac. Sai s co th xay ra do
cac cht la t bnh thuy tinh, gm....xm nhp vao dung dch hoc thuc th co ln
tap cht.
b) Sai s thao tac do chu quan ngi phn tch gy ra, khng phu thuc may va
dung cu va khng lin qua vi phng pha p phn tch. Sai s nay co th rt nghim
trong vi ngi phn tch thiu kinh nghim, hoc lam vic thiu suy ngh, khng cn
thn.
Giao an phn tch silicat
40
Ngi mi lam phn tch thng pham sai lm nghim trong do khng bit lam
vic. Tuy vy khi a quen cng vic va nu lam vic cn thn, nghim tuc th sai s
thao tac thng la khng ang k.
c) Sai s ca nhn do kha nng cua ngi phn tch khng th thc hin chnh xac
mt s thao tac phn tch. V du, khng th nhn bit chnh xac s chuyn mau cua
cht ch th tai im cui chun .
Thuc loai nay phai k n sai s tm ly, tc la khuynh hng cua ngi phn tch
khi lp lai th nghim mun chon gia tr phu hp vi gia tr a o trc hoc gn vi
gia tr cua ban. Sai s nay kha ph bi n.
d) Sai s phng phap co lin quan vi tnh cht hoa hoc hoc tnh cht hoa ly cua
h o, t lin quan vi thao tac phn tch. V du, phan ng phn tch xay ra khng hoan
toan hoc phan ng phu xay ra lam sai lch tnh hp th c cua phan ng chnh....
2.5.3. Sai s ngu nhin.
Sai s ngu nhin anh hng n lp cua kt qua o va lam giam chnh xac
phn tch.
Sai s ngu nhin do nhng nguyn nhn ngu nhin, khng nhn thy trc c
va lam cho kt qua phn tch dao ng theo cac chiu khac nhau (luc tng, luc giam).
Sai s ngu nhin lun lun xut hin du phep phn tch c thc hin ht sc cn
thn va i u kin thc nghim c gi c nh nghim ngt. Do c tnh cua no nh
vy ma vic x ly va anh gia sai s ngu nhin cua phep phn tch la rt quan trong.
No cho phep xac nh gia tr cua phng phap phn tch, anh gia cht lng lam vic
cua ngi phn tch, anh gia so sanh cng vic phn tch cua cac phong th nghim
phn tch khac nhau....Do ban cht cua no ma sai s ngu nhin phai c x l bng
toan hoc thng k.
2.6. A NH GIA SAI S
2.6.1.Sai s trong phep do truc tip
Phep o trc tip la so sanh vt o vi vt chun, nh cn, o th tch...Mi phep
o trc tip o trc tip u m c sai s ngu nhin va cac sai s nay cung v i cac sai
s mc phai trong cac giai oan phn tch khac nhau se quyt nh chnh xac cua
phep phn tch.
Thng thng, khi tin hanh th nghim chung ta thng thc hin mt s th
nghim c lp trong cung iu kin ging nhau, va t cac kt qua ring re thu c, ta
tin hanh x ly thng k anh gia chnh xac cua phep o. Cac ai lng c
trung thng k quan trong nht la gia tr trung bnh cng va phng sai.
2.6.2. Gia tr trung bnh cng.
Gia s ta tin hanh n phep o c lp ai lng X vi cac kt qua X
1
, X
2
, ...,X
n

Gia tr trung bnh cng
n
X
X
n
i
i
=
=
1
la gia tr gn vi gia tr thc cua ai lng cn
o vi xac sut cao nht trong s cac gia tr o c.
7.1.2. Phng sai.
Giao an phn tch silicat
41
Phng sai cua phep o phan anh phn tan cua kt qua o, c anh gia bng:

k
X X
S
n
i
i
=

=
1
2
2
) (

k: s bc t do. Nu ch co 1 ai lng cn o X th k = n-1.
Gia tr
2
s s = thng c goi la lch chun cua phep o.

lch chun cua ai lng trung bnh cng
X
s c tnh theo.

) 1 (
) (
2
2

= =

n n
X X
n
s
s
i
X

Trong thc t tin tnh toan cac ai lng
X
s s X , ,
2
, ngi ta thng cho n trong
day n gia tr o c X
1
, ...X
n
mt gia tr C sao cho X C . Sau o tnh X va s
2
theo
cac cng thc sau:

n
y
C X
n
i
i
=
+ =
1

va
1
1
2
2

=

=
n
x
s
n
i
i

y
( )

=
n
y
y x
i
i i
2
2 2
y
i
= X
i
- C
2.6.3. chnh xac cua phep o trc tip.
chnh xac la gia tr tuyt i cua hiu gia gia tr trung bnh cng X va gia
tr thc cua ai lng phai o:
= X
Trong thc t c anh gia ng vi tin cy a cho
c tnh theo
k
X
t s
,
=
t
,k
= h s Student ng vi bc t do k cua phep o va tin cy a cho.
2.7 Sai s trong phep do gian tip.
Trong phn tch, chung ta thng s dung cac kt qua o trc tip anh gia mt
ai lng nao o theo mt cng thc lin h nht nh. Trong trng hp nay ai lng
cn xac nh thuc pham vi cac phep o gian tip. Sai s cua phep o gian tip c
anh gia t phng sai cua ai lng o trc tip, d a vao lin h ham s gia ai
lng o gian tip(y) vi cac ai lng o tr c tip (x
i
). Cac biu thc anh gia phng
sai cua mt s ai lng o gian tip (y).

Ham lin h Phng sai
y = x
1
x
2
y = a
1
x
1
a
2
x
2

2 2 2
2 1
x x y
s s s + =
2 2
2
2 2
1
2
2 1
x x y
s a s a s + =
Giao an phn tch silicat
42

=
=
2
1
2 1
x
x
y
x x y

y = f(x
1
,x
2
,x
3
...)

+ =
2
2
2
2
1
2
2 2 2 1
x
s
x
s
y s
x x
y

.... ) ( ) ( ) (
2 2
3
2 2
2
2 2
1
2
3 2 1
+

=
x x x y
s
x
y
s
x
y
s
x
y
s

2.8. QUY TC TNH VA LAM TRON S
Trong cac phep tnh ch c lam tron kt qua cui cung (nhm tranh vic giam
chnh xac cua kt qua o do vic lam tron cac giai oan tnh trung gian).
2.8.1.C ng va tr.
Khi cng va tr ch gi lai kt qua cui cung mt s ch s thp phn bng ung
ch s thp phn cua s hang co s ch s thp phn t nht.
V du: y = 6,145 + 13,24 + 34,7
y = 54,085
Kt qua lam tron: y = 54,1 (gi lai 1 ch s thp phn)
2.8.2 Nhn va chia.
Khi nhn va chia cn gi lai kt qua cui cung mt s ch s co ngha bng ung
s ch s co ngha cua tha s co s ch s co ngha t nht.
V du: y = (3,084 x 0,275)/41,256 = 0,020557
y c lam tron: y = 0,0206
2.8.3Logarit.
V du tnh logarit cua y = 3,34.10
-5

Lgy = -5 + 0,5237 = -4,476.
i vi cac phep o pH th cac s liu o c trn may c coi la cac s liu o
trc tip va c ap du ng theo phng phap thng th ng v tnh ch s co ngha
V du: pH = -lg[H
+
] = 6,47. Tnh [H
+
]
[H
+
] =10
-6,47
= 3,39.10
-7
Lam tron [H
+
] = 3,4.10
-7
(2 ch s co ngha tng t
gia tr pH co 2 ch s co ngha)
Chu y: Nu pH la gia tr o trc tip trn may oth ch s co ngha la ch s cui
cung cua gia tr o. V du: pH o c bng 2,18 co 2 ch s co ngha!
2.8.4 Trong mt s trng h p khi gi lai cac ch s co ngha cn cn nhc sao cho
bt nh tng i kt qua cui cung phu hp v i bt nh tng i cua cac
s liu c dung tnh toan.
V du: 03 , 1
98 , 0
01 , 1
= ma khng vit 1,0 v bt nh cua ca 2 s u bng 1%
( % 1
98 , 0
01 , 0
01 , 1
01 , 0
)




Giao an phn tch silicat
43
TAI LIU THAM KHAO
[1] Phng phap phn tch hoa hoc TCVN 141 - 1986 - B xy dng
[2] Cac tai liu phn tch c s cua nha may san xut vt liu xy dng: nha may
ximng, gm s, gach chu la, thuy tinh.
[3] Nguyn Th Mui - Giao trnh hoa hoc phn tch nh tnh va nh lng-HSP a
Nng.
[4] Nguyn Tinh Dung - Hoa hoc phn tch - tp3 - NXB GD.
[5] Bui Vn Chen - Ky thut san xut xi mng portlang - HBK Ha Ni 1992
[6] Huy nh c Minh, Pham Xun Yn, Nguyn Thu Thu y - Ky thut san xut gm s
- NXB KH&KT Ha Ni 1995.
[7] B mn silicat HBK Ha Ni - Giao trnh cng ngh san xut thuy tinh.
[8] Nguyn Th Huyn - Cng ngh san xut thuy tinh - HBK a Nng 2005.
MUC LUC
1.Muc ch-qui nh ...................................................................................... 1
2.Cac khai nin chung ................................................................................... 1
3.Cac phng phap pha mu ......................................................................... 1
4.Cac phng phap thng dung trong phn tch Silicat .............................. 1
5.Thc nghim............................................................................................... 4
5.1.Phn tch thanh phn hoa hoc cua Ximng ............................................. 4
5.2. Phn tch thanh phn hoa hoc cua t set ............................................. 21
5.3.Phn tch thanh phn hoa hoc cua a vi .............................................. 26
5.4.Phn tch thanh phn hoa hoc cua thuy tinh.......................................... 31
6.Sai s trong phn tch nh lng hoa hoc ............................................... 41
7.anh gia sai s .......................................................................................... 42
8.Qui tc tnh va lam tron s ....................................................................... 44