TIU CHUN NH NC Nhm I

TCVN 2322-78
THUC TH
PHNG PHP XC NH HM LNG TP CHT PHT PHT
( TRONG DUNG DCH KHNG MU)
Reagents
Methods for the determination of photsphates
Khuyn khch
p dng
Tiu chun ny quy nh phng php xc nh hm lng tp cht pht pht trong cc
dung dch thuc th khng mu.
Phng php da trn mu xah molipden to ra ca hp cht phc phot pho molipden
b metola kh n mu xanh.
Nu phng php da trn mu vng th mu l ca hp cht phc phot pho
vanadat molipdic.
Trong phng php so mu bng mt, cng mu ca dung dch th c so snh
vi mu ca dung dch chun c mt lng ion pht pht xc nh.
Trong phng php so mu bng my, ( theo mu xanh molipden) tin hnh o mt
quang ca dung dch th v dung dch chun trn my so mu n sc di sng 810-820
hm hoc trn my so mu n sc di sng tng ng vi vng hp th nh sng cc
i.
Phng php da vo mu xanh ca molipden dng xc nh pht pht khi hm
lng pht pht trong lng cn ca thuc th em th nm trong khong :
0,01-0,05 mg-phng php so mu bng mt;
0,01-0,15mg-phng php so mu trn my,
Phng php so mu da vo phc cht phtpho vanadat molipdic mu vng dng
xc nh pht pht khi hm lng trng lng cn ca thuc th trong khong 0,01-0,03 mg.
1 CH DN CHUNG
1.1Lng cn ca thuc th em th, cch tin hnh s l s b, cng nh lng PO
4

tnh bng mg cn phi c trong dung dch chun u c ch ra trong tiu chun p dng
ring cho tng thuc th.
1.2.Cn lng cn ca thuc th vi chnh xc n 0,01 g.
1.3 Phi tun th nghim ngt th t thm thuc th vo dung dch th v dung dch
chun v lc u dung dch sau mi ln thm thuc th.
1.4 Tin hnh so snh cng mu ca dung dch th v dung dch chun.
1.5 lc dung dch, phi dng giy lc ra sch ion pht pht bng nc ct.
1.6 Dng amoni hidroxit trung ho dung dch hoc dng axit sunfuric, axit
clohidric trung ho theo ch th giy qu.
2.PHNG PHP XC NH PHT PHT THEO MU XANH MOLIPDEN
2.1 Thuc th v cc dung dch
Amoni molipdat
Nc ct
Metola(p-metylaminofenol sunfat)
Kali pirosunfat
Thuc th A chun b nh sau:
Ho tan 5,0 g amoni molipdat vo 100 ml dung dch axit sunfuric 1 N, lc u. Thuc
th dng tt trong 4 ngy m.
Thuc th B chun b nh sau:
Ho tan 0,2 g metola vo 80 ml nc. Sau khi ho tan, thm 20 g kali pirosunfat, thm
nc n 100 ml, lc u. Thuc th dng tt trong 4 ngy m.
Dung dch cha ion PO
4
chun b theo TCVN 1056-71. Dng nc pha long thu
c dung dch c 0,01 mg PO
4
trong 1 ml.
Axit sunfuric, dung dch 1N.
2.2 Tin hnh th
2.2.1 Phng php so mu bng mt
Cho 15 ml dung dch cn th( hoc lng cn ca thuc th cho c ho tan vo
15 ml nc) vo bnh nn dung tch 100 ml, thm 6 ml dung dch axit sunfuric, sau thm 5
ml thuc th A v 5 ml thuc th B vthm nc cho th tch t 25 ml.
t dung dch 20 pht trn bnh cchthu c nhit 6062
0
C, sau , lm ngui n
nhit phng.
ng thi cng chun b dung dch chun c trong cng th tch lng pht pht nh
ch ra trong tiu chun p dng ring cho tng thuc th v cng lng cc thuc th.
Mu xanh quan st c ca dung dch th phi khng c m hn mu ca dung
dch chun.
2.2.2 Tin hnh so mu
2.2.2.1 Xy dng ng cong chun
Chun b cc dung dch chun
Cho vo cc bnh nh mc dung tch 25 ml mi bnh 15 ml dung dch c lng PO
4

tng ng vi 0,01; 0,02; 0,05; 0,10 v 0,14 mg. Cng ng thi chun b dung dch kim tra
khng c ion PO
4
.Thm vo mi bnh 6 ml dung dch axit sunfuric v 1 ml thuc th A, 1 ml
thuc th B. Thm nc vo cc bnh cho n vch mc v gi 20 pht trn bnh cch thu
c nhit 6062
0
C .Lm lnh n nhit phng.
Cho cc dung dch thu c vo cuvet c chiu dy lm vic l 10 mm v em so
mu ngay trn my so mu n sc di sng 810-820 mm hoc so mu trn my thng
( di sng 650-700 nm) v so snh vi dung dch kim tra.
Da vo s liu thu c, xy dng ng cong chun v t trn trc honh lng
ion PO
4
tnh bng mg.
2.2.2.2 Tin hnh th
Cho lng cn ca thuc th vo bnh nh mc loi dung tch 25 ml, ho tan trong
nc v s l tip nh ni trong iu 3.1.
em so mu dung dch thu c trong cng nhng iu kin nh ch dn trong
iu 3.2.1.
Da vo kt qu xc nh, dng th tm ra hm lng ion PO
4
trong lng cn
ca thuc th.
Ch thch: Trong trng hp phn tch trng ti, dng phng php so mu trn
my so mu n sc.
3.PHNG PHP XC NH PHT PHT THEO MU VNG CA HP CHT
PHC PHTPHO VANADI MOLIPDAT ( PHNG PHP SO MU BNG MT)
3.1 Thuc th v dung dch
Chun b thuc th xc nh pht pht theo TCVN 1056-71. Dung dch cha pht
pht theo TCVN 1056-71. Dng nc pha long dung dch thu c dung dch c 0,01
mg PO
4
trong 1 ml
3.2 Tin hnh th
Cho 15 ml dung dch th c trung ho ( hoc lng cn ca thuc th em th
ho tan vo 15 ml nc) vo bnh nn dung tch 50 ml, thm 10 ml thuc th xc nh
pht pht v lc u.
Cng ng thi chun b dung dch chun c lng pht pht nh ch ra trong tiu
chun p dng ring cho tng thuc th v cng lng thuc th ion pht pht.
Sau 10 pht, mu vng ca dung dch th quan st c phI khng c m hn
mu ca dung dch chun.
Ch thch. 1. C th tin hnh so mu qua s bin i mt quang ca cc dung
dch trn my so mu di sng tng ng vi cc i hp th nh sng.
2. trung ho dung dch th c th dng 1-2 git dung dch p-nitrofenola 0,2% v
dung dch axit nitric hoc amoni hidroxit.