TIU CHUN NGNH

10 TCN 514:2002
NG CC - XC NH HM LNG NG TNG S V TINH BT BNG PHNG
PHP LANE-EYNON
1. Phm vi p dng
Tiu chun ny p dng cho cc loi ht ng cc nh go, m, ng... cng nh cc sn phm
ca ng cc v quy nh php th xc nh hm lng ng tng s v tinh bt bng phng
php Lane-Eynon.
2. Nguyn tc
ng kh trong dch thu phn ng tan v thu phn tinh bt c kh nng kh Cu +2 trong
hn hp pheling v Cu+ (Cu2O) khng tan, mu . Th tch dung dch ng kh cn thit
kh hon ton mt th tch nht nh hn hp pheling c xc nh bng phng php chun
vi cht ch th xanh metylen.
Hm lng tinh bt c tnh bng hm lng glucoza trong dch thu phn tinh bt nhn vi h
s chuyn i 0,9.
3. Dng c v thit b
- My nghin phng th nghim
- Ry c ng knh l sng 0,5 mm
- Ni cch thu c b iu chnh nhit t ng
- Nhit k
- Bp in
- My lc
- Cn phn tch c chnh xc n 0,0001g
- Bnh nh mc dung tch 100, 250 v 500 ml
- Buret u cong dung tch 50 ml
- Pipet 5, 10, 25 v 50 ml
- Bnh tam gic dung tch 150, 250 ml
- Cc thu tinh
- Phu lc ng knh 7 cm
- Giy lc nh lng.
4. Thuc th
Tt c thuc th phi c sch phn tch. S dng nc ct hoc nc c tinh khit tng
ng.
4.1. Hn hp thuc th pheling: Trn hai th tch tng ng ca dung dch pheling A ( 4.2) v
pheling B (4.3) ngay trc khi s dng.
4.2. Dung dch ng sunfat (pheling A): Ho tan 34,639 gam CuSO 4.5H2O trong nc ct v nh
mc n 500 ml. Nu thy dung dch c th c th lc qua giy lc.
4.3. Dung dch kali-natri tactrat (pheling B): Ho tan 173 gam KNaC 4H4O6.4H2O (mui Secnhet)
v 50 gam NaOH trong nc ct v nh mc n 500 ml. yn 2 ngy v lc qua giy lc.
4.4. Dung dch ch th

4.4.1. Dung dch xanh metylen 1%: Ho tan 1 gam xanh methylen bng nc ct v nh mc
n 100 ml.
4.4.2. Dung dch phenolphtalein 1%: Ho tan 1 gam phenolphtalein trong 70 ml ethanol 98%, sau
nh mc n 100 ml bng nc ct.
4.5. Dung dch ch axetat 45%: Ho tan 225 gam Pb(CH 3COO)2.3H2O trong nc ct nng,
ngui v nh mc n 500 ml.
4.6. Dung dch kali oxalat 22%: Ha tan 110 gam K 2C2O4.H2O trong nc ct v nh mc n
500 ml.
4.7. Axit clohydric c (d=1,19 g/ml)
Dung dch axit clohydric 5% v 10%.
4.8. Natri hydroxit : Dung dch 20% v dung dch 1N.
4.9. Dung dch ng chun
4.9.1. Chun b dung dch ng chun 1%: Cn chnh xc 9,5 gam ng Saccarose tinh khit
cho vo bnh nh mc dung tch 1 lt (1000 ml), thm vo khong 100 ml nc ct v 5 ml axit
clohydric m c. yn dung dch 3 ngy nhit 20-25 oC hoc 7 ngy nhit 12-15 oC.
Sau thm nc ct n vch nh mc. Dung dch axit ho ny c th s dng trong vi
thng.
4.9.2. Trung ho v pha long dung dch ng chun ti nng thch hp trc khi dng
c tin hnh nh sau: Dng pipet ht 50 ml dung dch ng chun 1% (4.9.1) cho vo bnh
nh mc dung tch 200 ml, thm tip khong 100 ml nc ct. Dng phenolphtalein lm cht ch
th, trung ho dung dch ng chun bng dung dch NaOH 1N n khi xut hin mu hng.
Sau , thm tng git dung dch HCl 1N n khi mt mu hng. Thm nc ct n vch mc
v trn u. 1ml dung dch ng chun ny ng vi 2,5 mg ng kh.
5. Chun ho, xc nh h s pheling
Ly 2 bnh tam gic dung tch 150 ml, dng pipet cho vo mi bnh 10 ml hn hp pheling ( 3.1),
thm tip 10-20 ml nc ct, lc u.
5.1. nh phn s b: Thm vo bnh th nht 2-3 git ch th xanh metylen, lc u v t ln
bp in c li aming, iu chnh nhit sao cho sau 1-2 pht th dung dch si. Tip tc un
v t buret nhanh chng nh dung dch ng chun (4.9.2) vo bnh cho ti khi mt mu xanh
ca ch th. Tng thi gian nh phn khng qu 3 pht.
5.2. nh phn chnh: Da vo s ml dch ng tiu hao bit trong qu trnh nh phn s b
ta tin hnh nh phn chnh nh sau: T buret cha dung dch ng chun (4.9.2) nh xung
bnh th hai gn ht lng ng chun cn tiu tn c bit th nghim s b (5.1), ch bt
li 0,5-1 ml. un si nh trong 2 pht, vn mu si , thm tip 2-3 git ch th xanh metylen
(ch trnh nh vo thnh bnh). Tip tc nh t t dung dch ng chun vo hn hp ang
si cho n khi mt mu xanh ca ch th v dung dch ch cn mu ca Cu 2O c t trc khi
thm ch th. Ghi th tch ca dung dch ng chun tiu tn trong qu trnh nh phn.
Thng thng th tch ny l 20,37 0,05 ml (i vi 10 ml hn hp pheling). Nu sai khc mc
th cn phi kim tra li thuc th pheling.
Ta c h s F ca dung dch pheling nh sau:
F= a x 2,5
Trong : a l s ml ca dung dch ng chun tiu tn khi chun 10ml hn hp dung
dch pheling.
6. Ly mu v chun b mu
6.1. Tin hnh ly mu theo TCVN 5451-91 (ISO 950-1979).

6.2. T mu th c ly theo 6.1, tin hnh nghin khong 100 gam mu n kch thc lt
hon ton qua mt sng 0,5 mm.
7. Xc nh ng tng s
7.1. Chun b dung dch chit ng tan
T mu phn tch c nghin nh theo mc 6.2, cn chnh xc n 0,1mg khong 2-3 gam
mu cho vo cc thu tinh hoc bnh cu dung tch 150 ml, thm khong 50-60 ml nc ct nng
40oC v lc trn my lc tc 200 vng/pht trong thi gian 15-20 pht, cn y nt mu
khi bn ra ngoi. Sau lc cn thn qua giy lc nh lng v cho ton b nc lc vo bnh
nh mc 100 ml. Ra phn khng tan trn giy lc 2-3 ln bng nc ct nng, lm ngui dung
dch v thm nc ct n vch nh mc, trn u. Dung dch nhn c l phn dch chit
ng tan trong mu th.
7.2. Thu phn dung dch chit
Dng pipet ht chnh xc 50 ml dch chit ng tan (7.1) cho vo bnh tam gic dung tch 150
ml, thm tip 5 ml dung dch HCl 10%, lc u v thu phn trong ni cch thu nhit 7080oC trong 30 pht, thnh thong lc u mu. Lm lnh n nhit phng. Sau trung ho
bng dung dch NaOH 20% vi ch th phenolphtalein nh tin hnh i vi dung dch ng
chun (Xem 4.9..2).
Dch mu th sau khi thu phn v trung ho c chuyn hon ton vo bnh nh mc dung
tch 200 ml. Kh tp cht c trong dch mu bng cch thm 2ml ch axetat 45%, yn 5 pht.
Nu thy xut hin lp cht lng trong sut trn lp cn th vic kh tp cht xong. Loi ion
Pb2+ d bng cch thm 2,5 ml dung dch kali oxalat 22%. Lc u, lng kt ta trong 10 pht.
Kim tra vic loi ion Pb2+ bng cch cho ht sc cn thn mt vi git kali oxalat vo thnh bnh,
nu khng thy vn c khi cc lp cht lng tip xc vi nhau c ngha l loi ht ion Pb 2+
trong mu. Thm nc ct n vch nh mc, lc u v lc qua giy lc nh lng. Dch lc
thu c l dung dch ng kh sau khi thu phn. Dung dch ny c np vo buret c
u cong nh phn. Vic chun tip theo c tin hnh theo phng php chun.
7.3. Tin hnh chun
Khi cha bit nng ca ng kh trong dung dch mu th (7.1), trc tin cn chun s
b bit c s pha long thch hp.
7.3.1 nh phn s b
Ht chnh xc 10ml hn hp pheling (4.1) cho vo bnh tam gic dung tch 150 ml. Nh t buret
15 ml dung dch ng kh ca mu th (7.2), lc u v un n si trn bp in c li
aming. si nh 15 giy. Nu hn hp mt mu xanh chng t lng ng d, cn pha
long dung dch ng kh (7.2) n nng thch hp. Nu vn cn mu xanh, cho thy thuc
th pheling cha b kh hon ton, cn tip tc nh dung dch ng kh ca mu th vo hn
hp ang si cho n khi cn mu xanh nht. Thm 3 - 4 git dung dch xanh metylen v tip tc
chun cho n khi mt mu xanh ca cht ch th. Ghi th tch dung dch ng kh ( 7.2)
tiu tn trong qu trnh chun . Tng thi gian nh phn tt nht l khng qu 3 pht.
7.3.2 nh phn chnh
Da vo s ml dch ng tiu hao bit trong qu trnh nh phn s b ta tin hnh nh
phn chnh nh sau: Dng pipet ht chnh xc 10 ml hn hp thuc th pheling ( 4.1) cho vo
bnh tam gic dung tch 150 ml, thm tip 20 ml nc ct, lc u. T buret nh xung bnh tam
gic gn ht lng th tch cn thit dung dch ng kh ca mu th (7.2) bit trong nh
phn s b, ch bt li 0,5 - 1 ml. un n si trn bp in c li aming. si nh 15 giy
v nhanh chng thm dung dch ng ca mu th cho n khi ch cn mu xanh rt nht. Sau
thm 3 - 4 git xanh metylen v hon thnh vic chun bng cch nh tip dung ch
ng n khi mt mu xanh ca cht ch th. Ghi tng th tch dung dch ng kh ca mu
th tiu tn trong qu trnh chun .
7.3.3. Tnh ton kt qu

Hm lng ng tng s tnh bng % khi lng (X 1) c tnh theo cng thc:

Trong : F l h s tng ng ca dung dch pheling

V1 l th tch dch chit ng tan , tnh bng ml.
V2 l th tch dch chit ng kh sau khi thu phn, tnh bng ml
V0 l th tch dch chit ng tan em thu phn bng axit, tnh bng ml
T l tng th tch dch ca dung dch ng kh dng chun 10ml hn hp pheling, tnh
bng ml
m l khi lng mu th, tnh bng g
Kt qu ca php th l h s trung bnh ca 2 ln xc nh song song v c tnh n s l
th hai sau du phy. S sai khc gi tr gia hai ln phn tch song song khng c php vt
qu 0,5%.
8. Xc nh tinh bt
8.1. Thu phn tinh bt
Cn chnh xc n 0,1mg t 1-2 g mu th c chun b theo 6.2. Tin hnh chit rt lng
ng tan bng nc ct nng theo 7.1. Kh chc thng giy lc v chuyn hon ton phn
khng tan trn phu vo bnh tam gic hay bnh cu dung tch 150 ml bng 50 ml dung dich HCl
5%. y kn bnh bng nt cao su c lp ng sinh hn hi lu v un cch thu hn hp trong 34 gi. Th s thu phn hon ton bng dung dch iot. Lm ngui, trung ho hn hp bng dung
dch NaOH 20% vi ch th phenolphtalein, sau chuyn hon ton hn hp vo bnh nh mc
250 ml, kt ta tp cht bng dung dch ch axetat 45% v loi b ion Pb 2+ d bng dung dch kali
oxalat 22% ( xem 7.2). nh mc n 250 ml bng nc ct. Lc u v lc qua giy lc nh
lng. Dch lc thu c l dung dch ng kh sau khi thu phn tinh bt.
8.2. Tin hnh chun
Khi cha bit nng ng kh trong dung dch thu phn tinh bt, trc tin cn chun s
b bit c s pha long thch hp. Vic chun tip theo c tin hnh theo phng
php chun.
8.2.1 nh phn s b
Tin hnh tng t 7.3.1.
8.2.2 nh phn chnh
Dng pipet ht chnh xc 10 ml hn hp pheling (4.1) cho vo bnh tam gic dung tch 150 ml,
thm tip 20 ml nc ct, lc u. T buret nh xung bnh tam gic gn ht lng ng kh
cn thit bit khi nh phn s b, ch bt li 0,5-1ml. un nng n si nh trn bp in c
li aming. si 15 giy v nhanh chng thm tip dung dch cho n khi ch cn mu xanh
rt nht. Sau thm 2-3 git xanh metylen v hon thnh vic chun bng cch nh tip
dung dch ng kh cho n mt mu xanh ca ch th. Ghi tng th tch dung dch ng kh
ca mu th tiu tn trong qu trnh chun . Tng thi gian chun tt nht l khng qu
3 pht.
8.3. Tnh kt qu
Hm lng tinh bt tnh bng % khi lng (X 2) c tnh theo cng thc:

Trong :
F l h s pheling
V l tng th tch dung dch sau thu phn, tnh bng ml
T l tng th tch dung dch ng kh ca mu th d dng chun l0 ml hn hp pheling,
tnh bng ml
m l khi lng mu th, tnh bng g
0,9 l h s chuyn i ng glucoza v tinh bt
Kt qu php th l h s trung bnh ca hai ln xc nh song song v c biu th n s l
th nht sau du phy. S sai khc gi tr gia hai ln phn tch song song khng c php
vt qu 0,5%.