TIU CHUN QUC GIA

TCVN 6202 : 2008

ISO 6878 : 2004
CHT LNG NC XC NH PHOSPHO PHNG PHP O PH DNG AMONI
MOLIPDAT
Water quality Determination of phosphorus Ammonium molybdate spectrometric method
Li ni u
TCVN 6202 : 2008 Thay th TCVN 6202 : 1996
TCVN 6202 : 2008 hon ton tng ng ISO 6878 : 2004
TCVN 6202 : 2008 do Ban k thut tiu chun TCVN/TC 147 Cht lng nc bin son, Tng
cc Tiu chun o lng Cht lng ngh, B Khoa hc v Cng ngh cng b.
Li gii thiu
Tiu chun ny quy nh vic xc nh cc dng hp cht phospho khc nhau trong nc ngm,
nc mt v nc thi vi cc nng khc nhau, dng ha tan v khng tan.
Ngi s dng tiu chun ny phi nhn thc nhng vn c th v an ton v v sinh, c th
cn quy nh thm mt s iu kin.
CHT LNG NC XC NH PHOSPHO PHNG PHP O PH DNG AMONI
MOLIPDAT
Water quality Determination of phosphorus Ammonium molybdate spectrometric
method
Cnh bo Nhng ngi s dng tiu chun ny phi thng tho vi k thut thng
thng ca phng th nghim. Tiu chun ny khng cp n tt c cc vn an ton
trong khi s dng tiu chun, nu c. Trch nhim ca ngi s dng tiu chun l thit
lp cc iu kin m bo an ton v v sinh thch hp tun th ng quy nh quc
gia. iu rt quan trng l cc th nghim c tin hnh theo tiu chun ny phi do
nhn vin c trnh thc hin. Dung dch thi molybdat v antimon phi c thi b
ng quy nh.
1. Phm vi p dng
Tiu chun ny quy nh cc phng php xc nh
- Octophosphat (xem iu 4)
- Phosphat sau khi chit vi dung mi (xem iu 5)
- Phosphat c th thy phn c v octophosphat (xem iu 6)
- Tng Phosphat sau khi phn hy (xem iu 7 v 8).
Cc phng php ny c th p dng vi tt c cc loi nc k c nc bin v nc thi.
Nng phospho trong khong t 0,005 mg/l n 0,8 mg/l c th xc nh theo phng php
ny khng cn pha long.
Quy trnh chit cho php xc nh phospho nng nh hn so vi gii hn pht hin khong
0,0005 mg/l.
2. Cn tr
Mt vi cht cn tr bit nu ra trong Ph lc A. C th c cc cht cn tr khc v cn phi
kim tra li nu c th phi loi b chng.

3. Nguyn tc
Phn ng gia ion octophosphat v mt dung dch axit cha molipdat v ion antimon to ra phc
cht antimon phosphomolipdat.
Kh phc cht bng axit ascorbic to thnh phc cht molipden mu xanh m. o hp th
ca phc cht xc nh nng octophosphat.
Xc nh polyphosphat v mt s hp cht phospho hu c bng cch thy phn chng vi axit
sulfuric chuyn sang dng octophosphat phn ng vi moliopdat.
Mt s hp cht phospho hu c c chuyn thnh octophosphat bng v c ha vi pesulfat.
Nu cn x l cn thn th v c ha vi axit nitric axit sulfuric.
4. Xc nh octophosphat
4.1. Thuc th
Ch dng cc thuc th loi phn tch v dng nc c hm lng phospho khng ng k so
vi nng phospho nh nht trong mu cn xc nh.
Vi hm lng phosphat thp, cn dng nc ct hai ln vi dng c ct hon ton bng thy
tinh
4.1.1. Dung dch axit sulfuric, c(H2SO4) 9 mol/l
Cho 500 ml 5 ml nc vo cc 2 l. Thm cn thn, va khuy va lm lnh 500 ml 5 ml axit
sulfuric, = 1,84 g/ml. Khuy u v dung dch ngui n nhit phng.
4.1.2. Dung dch axit sulfuric, c(H2SO4) 4,5 mol/l
Cho 500 ml 5 ml nc vo cc 2 l. Thm cn thn, va khuy va lm ngui 500 ml 5 ml axit
sulfuric (4.1.1). Khuy u v dung dch ngui n nhit phng.
4.1.3. Dung dch axit sulfuric, c(H2SO4) 2 mol/l
Cho 300 ml 3 ml nc vo cc 1 l. Thm cn thn 110 ml 2 ml dung dch axit sulfuric (4.1.1)
va khuy u va lm ngui. Pha long vi nc trong bnh nh mc 500 ml 2 ml v trn
u.
4.1.4. Dung dch natri hydroxit, c(NaOH) = 2 mol/l
Ha tan 80 g 1 g natri hydroxyt dng ht trong nc, lm lnh v pha long vi nc ti 1 l.
4.1.5. Dung dch axit ascobic, = 100g/l
Ha tan 10 g 0,5 g axit ascobic (C6H8O6) trong 100 ml 5 ml nc.
CH THCH: Dung dch ny n nh trong hai tun nu gi trong bnh thy tinh mu nu trong t
lnh v c th s dng c lu nu dung dch ny vn l khng mu.
4.1.6. Molipdat trong axit, Dung dch I.
Ha tan 13 g 0,5 g amoni heptamolipdat ngm bn nc [(NH 4)6Mo7O24.4H2O)] trong 100 ml
5 ml nc. Ha tan 0,35 g 0,05 g antimon kali tartrat ngm 1/2 nc [K(SbO)C 4H4O8.1/2 H2O]
trong 100 ml 5 ml nc.
Cho dung dch molipdat vo 300 ml 5 ml dung dch axit sulfuric (4.1.1), khuy lin tc. Thm
dung dch tartrat v trn u.
CH THCH: Thuc th ny n nh t nht trong hai thng nu c gi trong bnh thy tinh
mu nu.
4.1.7. Molipdat trong axit, dung dch II.
Ha cn thn 230 ml 0,5 ml dung dch axit sulfuric (4.1.1) trong 70 ml 5 ml nc, lm ngui.
Ha tan 13 g 0,5 g amoni heptamolipdat ngm bn nc [(NH 4)6Mo7O24.4H2O)] trong 100 ml
5 ml nc. Thm dung dch axit v trn u. Ha tan 0,35 g 0,05 g antimon kali tartrat ngm

1/2 nc [K(SbO)C4H4O8.1/2 H2O] trong 100 ml 5 ml nc. Thm dung dch axit molipdat v
trn u.
Dng cc thuc th ny khi mu c axit ha bng axit sulfuric (4.1.2). (xem iu 6, 7 v 8).
CH THCH: Thuc th ny n nh t nht trong hai thng nu c bo qun trong bnh thy
tinh mu nu.
4.1.8. Dung dch b chnh c mu
Trn hai phn th tch dung dch axit sulfuric (4.1.2) v mt phn th tch axit ascorbic (4.1.5).
CH THCH: Thuc th ny n nh trong vi tun nu c bo qun trong bnh thy tinh nu
v trong t lnh.
4.1.9. Dung dch natri thiosulphat pentahydrat, = 12,0 g/l.
Ha tan 1,20 g 0,05 g natri thiosulphat ngm nm nc (Na 2S2O3.5H2O) trong 100 ml 5 ml
nc. Thm 0,05 g 0,005 g natri cacbonat (Na2CO3) lm cht bo qun.
CH THCH: Thuc th ny n nh t nht trong bn tun nu bo qun trong bnh thy tinh
mu nu
4.1.10. Dung dch chun gc octophosphat, p = 50 mg/l
Sy kh vi gam kali dihydrogen phosphat ti khi lng khng i 105 oC. Ha tan 0,2197 g
0,0002 g KH2PO4 trong khong 800 ml 10 ml nc trong bnh nh mc 1 000 ml. Thm 10 ml
0,5 ml dung dch axit sulfuric (4.1.2) v thm nc ti vch.
C th s dng sung dch chun gc sn c th trng.
Dung dch ny n nh t nht trong ba thng nu c bo qun trong bnh thy tinh nt kn.
Nn bo qun khong 4oC trong t lnh.
4.1.11. Dung dch chun octophosphat, p = 2 mg/l.
Dng pipet ly 20 ml 0,01 ml dung dch chun gc octophosphat (4.1.10) cho vo bnh nh
mc nc 500 ml. Thm nc ti vch v trn u.
Chun b dung dch trong ngy phn tch.
CH THCH: 1 ml dung dch chun cha 2 g P
4.1.12. Axit clohydric, (HCl) = 1,19 g/ml
4.1.13. Axit clohydric, c (HCl) = 2,5 mol/l
Cn thn thm 200 ml 10 ml axit clohydric (4.1.12) vo 500 ml 10 ml nc. Khuy v lm
ngui n nhit phng, lm y ti 1 000 ml bng nc.
4.2. Thit b, dng c
4.2.1. My o ph, loi lng knh, loi chia vch hoc loi knh lc, loi c kh nng t c
cc cuvet dy t 10 mm n 50 mm.
My o ph c chn cn thch hp o hp th trong vng kh kin v vng hng ngoi
gn ca quang ph. Bc sng nhy nht l 880 nm, nu chp nhn thp hn c th o
700 nm.
CH THCH: Gii hn pht hin ca phng php ny s tt hn nu s dng my o ph vi
cuvet 100 mm.
4.2.2. B phn gn thit b lc, gi b lc mng vi kch thc l 0,45 m.
4.2.3. Dng c thy tinh
Trc khi s dng, tt c dng c thy tinh cn ra vi dung dch axit HCl (4.1.13), khong
nhit t 40oC n 50oC v trng k vi nc. Khng dng cht ty ra cha phosphat.

Dng c thy tinh ch dng cho xc nh phospho. Sau khi dng cn ra sch nh trn, che y
v gi cho ti khi cn dng.
thy tinh dng cho giai on to mu thnh thong cn trng vi dung dch natri hydroxyt
(4.1.4), tip theo cn trng k bng nc (4.1) loi tr cn cc phc cht c mu c xu
hng bm thnh mng mng trn thnh thy tinh.
4.3. Ly mu v chun b mu
4.3.1. Ly mu
Ly mu phng th nghim vo l polyetylen, polyvinyl clorua hoc tt nht l bnh thy tinh.
Trong trng hp nng phosphat thp, nht thit phi dng bnh thy tinh.
4.3.2. Chun b mu th
Lc mu (4.3.1) trong vng 4 h sau khi ly mu, nu mu c gi lnh, cn a v nhit
trong phng trc khi lc.
Ra sch mng lc c kch thc l 0,45 m bng cch cho 200 ml nc m t 30 oC n 40oC
chy qua loi b cc phosphat. Loi b phn nc ra ny. Lc mu qua mng lc v b
10 ml dch lc u tin. Ly phn dch lc cn li cho vo bnh thy tinh sch, kh xc nh
ngay octophosphat (4.4.4).
Nu dch lc c pH nm ngoi khong t 3 n 10, iu chnh bng dung dch NaOH (4.1.4) hoc
dung dch H2SO4 (4.1.3).
Thi gian lc phi khng qu 10 min. Nu cn thit, dng b lc c ng knh ln hn.
Cn phi kim tra hm lng phospho ca mng lc hoc phi ra nh m t. Cc mng lc
bn sn trn th trng khng cha phospho cng phi ra nh m t trn y.
4.4. Cch tin hnh
4.4.1. Phn mu th
Th tch phn mu th ln nht dng l 40,0 ml. Th tch ny ph hp xc nh nng
octophosphat ti p = 0,8 mg/l khi dng cuvet dy 10 mm. Th tch phn mu th nh hn cn
c dng to thun li khi xc nh nng phosphat cao hn nh trnh by trong Bng 1.
Tng t, nng phosphat thp c th xc nh c bng cch o hp th trong cuvet dy
40 mm hoc 50 mm.
Bng 1 Nng v th tch mu
Nng octophosphat

Th tch phn mu th

Chiu dy cuvet

mg/l

ml

mm

0,0 n 0,8

40,0

10

0,0 n 1,6

20,0

10

0,0 n 3,2

10,0

10

0,0 n 6,4

5,0

10

0,0 n 0,2

40,0

40 hoc 50

4.4.2. Th mu trng
Tin hnh th mu trng song song vi phn tch mu, theo ng quy trnh, cng mt lng
thuc th nhng dng th tch nc tng ng thay cho mu th.
4.4.3. Hiu chun
4.4.3.1. Chun b dy dung dch hiu chun

Dng pipet ly tng ng, v d 1,0 ml; 2,0 ml; 3,0 ml; 4,0 ml; 5,0 ml; 6,0 ml; 7,0 ml; 8,0 ml; 9,0
ml; 10,0 ml dung dch chun octophosphat (4.1.11) cho vo bnh nh mc 50 ml. Pha long vi
nc ti khong 40 ml. Nhng dung dch ny cha cc nng octophosphat p = 0,04 mg/l
n 0,4 mg/l.
4.4.3.2. To mu
Thm vo mi bnh 1 ml dung dch axit ascorbic (4.1.5) tip theo l 2 ml dung dch axit molipdat I
(4.1.6). Thm nc ti vch v lc k.
Qu trnh tin hnh cho cc khong nng phosphat khc c nu Bng 1.
CH THCH: hp th o 700 nm b gim khong 30% nhy so vi o 880 nm.
4.4.3.4. o ph
o hp th ca mi dung dch bng my o ph (4.2.1) sau 10 min v 30 min bc sng
880 nm, hoc 700 nm nu chp nhn nhy thp hn. Dng nc i chng.
4.4.3.4. Dng ng chun
V th hp th (theo trc y) v hm lng phospho (theo trc x), (mg/l), ca dy dung dch
hiu chun. Tng quan gia hp th (trc y) vi hm lng phospho (trc x) l tuyn tnh.
Xc nh dc ca th.
Thng xuyn kim tra li tnh tuyn tnh ca th, c bit l khi dng m ha cht mi.
4.4.4. Php xc nh
4.4.4.1. To mu
4.4.4.1.1. Quy trnh chun
Dng pipet ly lng mu th nh (4.4.1). Vs vo bnh nh mc dung tch 50 ml v pha long
vi nc ti 40 ml 2 ml, nu cn. Tip tc nh m t 4.4.3.2.
Nu mu th cha asenat th phi kh bng thiosulphat trong mi trng axit thnh asenit. Vic
kh c nh lng cho asenat n nng t nht l 2 mg As/lit, c trnh by nh sau:
Dng pipet chuyn nhiu nht l 40 ml mu th vo bnh nh mc 50 ml. Thm 0,4 ml dung dch
axit sulfuric (4.1.2), 1 ml dung dch axit ascobic (4.1.5) v 1 ml dung dch thiosulphat (4.1.9)
khuy v qu trnh kh ko di 10 min 1 min. Thm 2 ml dung dch axit molipdat II (4.1.7).
Thm nc ti vch, khuy u. Lm tip nh 4.4.3.3.
4.4.4.1.2. Tin hnh vi trng hp mu b c
Nu mu th c v/hoc c mu, lm nh sau:
Thm 3 ml thuc th b chnh c mu (4.1.8) vo phn th tch mu th chn. Pha
long thnh 50 ml v o hp th. Gi tr hp thu o c theo quy nh 4.4.3.3 phi tr
i hp th ca dung dch ny.
4.4.4.2. o ph
Xem 4.4.3.3
Nu mu th cha cht gy cn tr asenat c x l bng thiosulphat, phi o trong vng
10 min, nu khng mu s b nht mu.
4.5. Biu th kt qu
4.5.1. Tnh ton
Nng octophosphat, p, biu th bng miligam trn lt c tnh theo cng thc:

( A A 0 )Vmax
f x Vs

Trong ,
A l hp th ca mu th
Ao l hp th ca dung dch mu trng
f l hm s dc th hiu chun (4.4.3.4), tnh theo lt trn miligam (l/mg);
Vmax l th tch mu (50 ml) ca mu th (ml);
Vs l th tch thc ca mu th (ml).
Bo co nng phospho nh sau, khng ly hn ba s c ngha:
p < 0,1 mg/l chnh xc n 0,001 mg/l;
p < 10 mg/l chnh xc n 0,01 mg/l;
p 10 mg/l chnh xc n 0,1 mg/l.
4.5.2. chm
D liu v chm nu Bng B.1, thu c t mt cuc th lin phng th nghim vi 16
phng th nghim tham gia.
CH THCH: V s cn tr xem Ph lc A
4.6. Bo co kt qu
Bo co kt qu cn c cc thng tin sau:
a) Mi thng tin cn thit nhn bit mu.
b) Vin dn tiu chun ny;
c) Vin dn phng php s dng, v iu/mc;
d) Kt qu thu c;
e) Cc thao tc khng c trong iu ny hoc c coi l ty chn, cng vi mi bt thng c
th nh hng n kt qu.
5. Xc nh octophosphat sau khi chit
5.1. Kh nng p dng
Phng php ny dng xc nh phosphat trong mu vi nng nh hn 0,01 mg/l P.
Phng php ny c bit thch hp cho xc nh nc bin.
5.2. Thuc th
S dng thuc th quy nh trong 4.1.5, 4.1.6 v 4.1.10 v thm:
5.2.1. 1-Hexanol (C6H13OH).
5.2.2. Etanol (C2H5OH).
5.2.3. Octophosphat, dung dch chun, p = 0,5 mg/l P.
Dng pipet ly 5,0 ml 0,01 ml dung dch gc chun octophosphat (4.1.10) vo bnh nh mc
dung tch 500 ml. Thm nc n vch v khuy u.
Chun b dung dch trong ngy dng.
5.3. Ly mu v chun b mu

Xem 4.3
5.4. Tin hnh
5.4.1. Phn mu th
Dng ng ong ly 350 ml 5 ml mu th (4.3) chuyn sang phu chit dung tch 500 ml
5.4.2. Th mu trng
Tin hnh th mu trng song song vi phn mu, theo cng mt quy trnh v s dng cng
lng thuc th nh vi phn tch mu, nhng thay mu bng 350 ml nc.
5.4.3. Hiu chun
5.4.3.1. Chun b dung dch hiu chun
Thm 300 ml 10 ml nc vo nm phu chit. Dng microburet ly 1,4 ml; 2,8 ml; 4,2 ml; 5,6
ml v 7,0 ml dung dch chun octophosphat (5.2.3) vo dy nm phu chit 500 ml. Pha long
tng dung dch ti 350 ml 10 ml vi nc, nt li, lc trn k. Nhng dung dch ny cha
octophosphat vi nng p = 0,002 mg/l, 0,004 mg/l, 0,006 mg/l, 0,008 mg/l v 0,01 mg/l,
tng ng.
5.4.3.2. To mu
Va lc va thm vo mi phu chit 7,0 ml 0,1 ml dung dch axit ascorbic (4.1.5) v 14,0 ml
0,1 ml. Dung dch I axit molipdat (4.1.6).
Sau 15 min, thm 40,0 ml 0,1 ml 1-hexanol (5.2.1) vo tng phu chit v y kn. Lc k trong
1 min. cho hin tng tch pha xy ra ri dng pipet ly 30 ml 0,01 ml mi phn trn chit
bng 1-hexexanol cho vo mt lot cc bnh nh mc kh dung tch 50 ml. Thm 1,0 ml 0,2 ml
etanol (5.2.2) vo tng bnh v pha long bng 1-hexanol ti vch.
5.4.3.3. o ph
o hp th ca tng dung dch 1-hexanol 680 nm trong cuvet dy 40 mm hoc 50 mm,
dng 1-hexanol trong cuvet so snh.
5.4.3.4. Dng ng chun
V th lin quan gia hp th (trc y) v hm lng phospho (trc x), mg/l, trong dung dch
hiu chun. Xc nh hm s nghing ca th.
Thng xuyn kim tra tuyn tnh ca th, c bit l khi dng lot ha cht mi.
5.4.4. Php xc nh
5.4.4.1. To mu
X l phn mu th (5.4.1) nh quy nh trong 5.4.3.2 i vi dung dch hiu chun
5.4.4.2. o ph
Xem 5.4.3.3
5.5. Biu th kt qu
Nng octophosphat, p, tnh bng miligam trn lt (mg/l), theo cng thc
p =
Trong :
A l hp th ca mu th;
Ao l hp th ca mu trng;

f l hm s dc th hiu chun (5.4.3.4), tnh theo lt trn miligam (l/mg);

Bo co kt qu chnh xc ti 0,001 mg/l nhng khi nng octophosphat, p < 0,0005 mg/l th
bo co kt qu cc gi tr nh hn 0,0005 mg/l.
CH THCH: V cn tr, xem Ph lc A
5.6. Bo co kt qu
Bo co kt qu cn c cc thng tin sau:
a) Mi thng tin cn thit nhn bit mu;
b) Vin dn tiu chun ny;
c) Vin dn phng php s dng, v iu/mc;
d) Kt qu thu c;
e) Cc thao tc khng c trong iu ny hoc c coi l ty chn, cng vi mi bt thng c
th nh hng n kt qu.
6. Xc nh phosphat v octophosphat thy phn
6.1. Thuc th
Dng cc thuc th trong 4.1.2, 4.1.4, 4.1.5, 4.1.7 v 4.1.11.
6.2. Thit b
Xem 4.2
6.3. Ly mu v chun b mu
6.3.1. Ly mu
Xem 4.3.1.
6.3.2. Chun b mu th
Lc mu (4.3.1) nh m t trong 4.3.2 v phn tch ngay sau khi ly mu cng nhanh cng tt.
Nu mu c bo qun lnh (5oC n 10oC), lm m mu ti nhit phng trc khi lc.
Thm 1 ml dung dch axit sulfuric (4.1.2) cho mi 100 ml mu lc chnh pH ti 1. Gi dch
lc ni mt v tt ti khi phn tch.
6.4. Cch tin hnh
6.4.1. Phn mu th
Ty theo nng phosphat c tnh c trong mu (xem Bng 1) dng pipet ly nhiu nht 40 ml
mu (6.3.2) cho vo bnh nn. Nu cn dng nc pha long ti 40 ml 2 ml. Axit ha mu vi
dung dch axit sulfuric (4.1.2) ti pH < 1 v un si nh trong 30 min. nh k, thm nc gi
th tch khong 25 ml n 35 ml. Lm ngui, iu chnh pH t 3 n 10 bng dung dch NaOH
(4.1.4) v chuyn sang bnh nh mc dung tch 50 ml, pha long vi nc ti khong 40 ml.
Cch khc, khong ha mu qua lc axit ha trong bnh kn trong 30 min trong ni hp nhit
trong khong t 115oC n 120oC.
6.4.2. Th mu trng
Tin hnh th mu trng song song vi mu th nghim theo cng mt quy trnh, s dng cng
mt lng thuc th nhng thay mu bng nc axit ha.
6.4.3. Hiu chun
6.4.3.1. Chun b dung dch hiu chun

Dng pipet ly 1,0 ml; 2,0 ml; 3,0 ml; 4,0 ml; 5,0 ml; 6,0 ml; 7,0 ml; 8,0 ml; 9,0 ml; 10,0 ml dung
dch chun octophosphat (4.1.11) cho cc bnh nn 50 ml. Pha long bng nc n 40 ml 2
ml. Nng dung dch octophosphat ny p = 0,04 mg/l n 0,4 mg/l. Lm tip tc cho cc dy
nng phosphat khc theo nh trong Bng 1. Axit ha bng axit sulfuric (4.1.2) ti pH < 1 v
un nh trong 30 min tip tc nh trong 6.4.1.
6.4.3.2. To mu
Va lc va thm vo mi bnh 1 ml axit ascobic (4.1.5) sau 2 ml dung dch 2 axit molipdat
(4.1.7). Thm nc ti vch.
6.4.3.3. o ph
Xem 4.4.3.3
6.4.3.4. Dng ng chun
Xem 4.4.3.4
6.4.4. Php xc nh
6.4.4.1. To mu
Tin hnh theo 6.4.3.2, dng phn mu th (6.4.1)
6.4.4.2. o ph
Xem 4.4.3.3
6.5. Biu th kt qu
6.5.1. Tnh ton
Nng octophosphat cng vi phosphat thy phn, p, tnh bng miligam trn lt, theo cng
thc:

( A A 0 )Vmax
f x Vs

Trong :
A l hp th ca phn mu th
Ao l hp th ca mu trng
f l hm s dc th hiu chun (4.4.3.4), tnh theo lt trn miligam (l/mg);
Vmax l th tch mu (50 ml) ca mu th, tnh bng mililit (ml);
Vs l th tch thc ca phn mu th, tnh bng mililit (ml).
C tnh n mi bc pha long v cng nh nhng bc pha long do thm axit sulfuric.
Bo co nng phospho nh sau nhng khng ly hn ba s c ngha:
- p < 0,1 mg/l chnh xc n 0,001 mg/l;
- p < 10 mg/l chnh xc n 0,01 mg/l;
- p 10 mg/l chnh xc n 0,1 mg/l.
6.5.2. chm

D liu v chm trong Bng B.2 thu c t mt th nghim lin phng th nghim vi 15
phng th nghim tham gia (xem c Bng B.1).
CH THCH: V s cn tr, xem ph lc A
6.6. Bo co th nghim
Bo co th nghim cn c cc thng tin sau:
a) Mi thng tin cn thit nhn bit mu;
b) Vin dn tiu chun ny;
c) Vin dn phng php s dng, v iu/mc;
d) Kt qu thu c;
e) Cc thao tc khng c trong iu ny hoc c coi l ty , cng vi mi bt thng c th
nh hng n kt qu.
7. Xc nh phospho tng s sau khi oxy ha peroxodisulfat
7.1. Thuc th
S dng cc thuc th ghi trong 4.1.2, 4.1.3, 4.1.4, 4.1.5, 4.1.7, 4.1.8, 4.1.9 v 4.1.11, v:
7.1.1. Dung dch kali peroxodisulfat
Thm 5 g 0,1 g kali peroxodisulfat (K2S2O8) vo 100 ml 5ml nc, khuy cho tan.
CH THCH: Dung dch ny n nh t nht trong hai tun, nu dung dch qu bo ha th gi
trong bnh thy tinh bosilicat mu nu, trnh nh nng trc tip.
7.2. Thit b
Xem 4.2, v thm:
7.2.1. Bnh bosilicat, 100 ml vi nt thy tinh, ng cht bng kp kim loi (i vi xc nh
phospho tng s dng phng php pesulfat trong ni hp); chai polypropylen hoc bnh nn (c
np xoy) cng dng c.
Trc khi dng, cn lm sch bnh, l bng cch thm khong 50ml nc v 2 ml axit sulfuric
(8.1.1). t vo ni hp trong 30 min nhit 115 oC n 120oC, lm ngui v trng bng nc.
Lp li qu trnh ny vi ln v y kn.
7.3. Ly mu v chun b mu
7.3.1. Ly mu
Xem 4.3.1
7.3.2. Chun b mu th
Thm 1 ml dung dch axit sulfuric (4.1.2) cho mi 100 ml mu th. axit ca dung dch cn phi
khong pH 1; nu cha t cn iu chnh bng dung dch kali hydroxyt (4.1.4) hoc axit sulfuric
(4.1.3)
Gi trong ch ti v mt ti khi phn tch.
Nu xc nh tng phospho ha tan, cn lc mu nh qui nh trong 6.3.2
7.4. Cch tin hnh
7.4.1. Phn mu th
Qu trnh oxy ha dng peroxodisulfat s khng c hiu qu khi c khi lng ln cht hu c
trong mu; trong trng hp ny cn oxy ha bng cch s dng hn hp axit nitric v axit
sulfuric (xem iu 8).

Dng pipet ly lng mu th (7.3.2) ti a l 40 ml vo cc bnh nn 100 ml. Nu cn, pha

long bng 40 ml 2 ml nc. Thm 4 ml dung dch kali peroxodisulfat (7.1.1) v un si nh
trong khong 30 min. Duy tr th tch khong 25 ml n 35 ml bng nc. Lm ngui, chnh pH
t 3 n 10 bng dung dch kali hydroxyt (4.1.4) hoc axit sulfuric (4.1.3) ri chuyn sang bnh
dung tch 50 ml, pha long bng nc ti khong 40 ml.
Cng c th v c ha trong 30 min trong ni hp nhit t 115 oC n 120oC
CH THCH 1: Thng thng 30 min l v c ha cc hp cht phospho, nhng mt vi
axit polyphosphonic cn ti 90 min thy phn.
CH THCH 2: Asenat c mt trong mu s gy cn tr Asenic c sn trong mu s b oxy ha
thnh asenat trong iu kin nh m t trong mc ny, do cng s gy ra cn tr.
Nu bit r hoc nghi ng c asenic trong mu, cn phi loi b. X l vi dung dch natri
thiosulfat (4.1.9) ngay sau bc khong ha. Trong trng hp khong ha nc bin trong ni
hp th cn loi tr clo t do bng cch un si khong 2 min trc khi kh asenat bng
thiosulfat.
7.4.2. Php th trng
Tin hnh mu th trng song song vi vic xc nh, theo cng quy trnh, cng mt lng thuc
th nhng dng nc thay cho mu th.
7.4.3. Hiu chun
7.4.3.1. Chun b dy dung dch hiu chun
Dng pipet, chuyn lng th tch thch hp, nh 1,0 ml; 2,0ml; 3.0 ml; 4,0 ml; 5,0 ml; 6,0 ml; 7,0
ml; 8,0 ml; 9,0 ml; v 10,0 ml dung dch chun octophosphat (4.1.11) vo cc bnh nn dung tch
100 ml, pha long ti khong 40 ml vi nc. Khong nng octophosphat ca dung dch ny
t p = 0,04 mg/l ti 0,4 mg/l. Tip tc nh trnh by 7.4.1 t on Thm 4 ml dung dch kali
peroxodisulfat (7.1.1) v un nh trong 30 min.
7.4.3.2. To mu
Thm vo mi bnh dung tch 50 ml (trong khi khuy), 1 ml axit ascobic (4.1.5) v sau 30 s, 2 ml
dung dch II axit molipdat (4.1.7). Thm nc ti vch v khuy u.
7.4.3.3. o ph
Xem 4.4.3.3
7.4.3.4. Dng ng chun
Xem 4.4.3.4
7.4.4. Xc nh
7.4.4.1. To mu
Chun b phn mu th t 7.4.1 v tin hnh ging nh quy nh trong 7.4.3.2.
Nu mu th nghim b c v/hoc m, nn tin hnh ngay nh sau:
Thm 3 ml dung dch b chnh c mu (4.1.8) vo th tch phn mu c v c ha
bng peroxytdisulphat. Pha long n 50 ml vi nc v o hp th. Gi tr hp th o
c theo 4.4.3.3 cn c tr i gi tr hp th o c ca dung dch ny.
7.4.4.2. o ph
Xem 4.4.3.3
7.5. Biu th kt qu
7.5.1. Tnh ton
Nng ca phospho, p tnh bng miligam trn lt, c tnh theo cng thc:

( A A 0 )Vmax
f x Vs

Trong :
A l hp th ca phn mu th;
Ao l hp th ca mu trng;
f l hm s dc th hiu chun (4.4.3.4), tnh bng lt trn miligam (l/mg);
Vmax l th tch mu (50 ml), tnh bng mililit (ml);
Vs l th tch thc ca phn mu th, tnh bng mililit (ml).
Cn tnh n mi bc pha long cng nh s pha long do thm axit sulfuric
Bo co nng phospho nh sau, nhng khng ly hn ba s c ngha:
- p < 0,1 mg/l chnh xc n 0,001 mg/l;
- p < 10 mg/l chnh xc n 0,01 mg/l;
- p 10 mg/l chnh xc n 0,1 mg/l.
7.5.2. chm
D liu v chm trong Bng B.3 thu c t mt th nghim lin phng th nghim vi 15
phng th nghim tham gia.
CH THCH: V s cn tr, xem Ph lc A
7.6. Bo co th nghim
Bo co th nghim cn c cc thng tin sau:
a) Mi thng tin cn thit nhn bit mu;
b) Vin dn tiu chun ny;
c) Vin dn phng php s dng, v iu/mc;
d) Kt qu thu c;
e) Cc thao tc khng nu trong iu ny hoc c coi l ty chn, cng nh mi bt thng
c th nh hng n kt qu.
8. Xc nh tng phospho sau khi phn hy bng axit nitric-axit sulfuric
8.1. Thuc th
S dng thuc th quy nh 4.1.2; 4.1.5; 4.1.7; 4.1.9, v:
8.1.1. Axit sulfuric, (H2SO4) = 1,84 g/ml
8.1.2. Axit nitric, (HNO3) = 1,40 g/ml
8.1.3. Natri hydroxit, dung dch, c(NaOH) = 8 mol/l.
Ha tan 64 g 1 g natri hydroxyt dng vin trong 150 ml 10 ml nc, lm lnh v pha vi nc
ti 200 ml 10 ml. Gia trong bnh polyetylen.
8.2. Thit b, dng c
Xem 4.2 v thm:

8.2.1. Bnh kjeldahl, 200 ml

8.3. Ly mu v chun b mu
8.3.1. Ly mu
Xem 4.3.1
8.3.2. Chun b mu th
Thm 1 ml dung dch axit sulfuric (4.1.2) cho mi 100 ml mu th cha lc. axit ca dung dch
cn khong pH 1; nu khng, chnh pH bng dung dch natri hydroxyt (4.1.4) hoc axit sulfuric
(4.1.3). Gi ni mt ti khi phn tch.
Nu xc nh tng phospho ha tan, cn lc mu theo 6.3.2.
8.4. Cch tin hnh
8.4.1. Phn mu th
CNH BO Cn thc hin quy trnh sau trong t ht.
Dng pipet ly ti a 40 ml mu th (8.3.2) cho vo bnh kjendahl (8.2.1). Thm 2 ml axit sulfuric
(8.1.1) v xoay trn u. Thm ht chng tro v un nng nh n khi xut hin khi trng.
Sau khi lm ngui, thm 0,5 ml axit nitric (8.1.2) v un nng cho n khi khi nu thot ra. Lm
ngui v tip tc x l vi axit nitric, va xoay va un nng cho n khi thu c mt dung dch
trong, khng mu. Lm ngui v cn thn cho thm 10ml nc, va xoay bnh mu lin tc va
un nng cho n khi xut hin khi trng. Lm ngui, cn thn cho thm 20ml nc trong khi
xoay bnh mu lin tc. Trong khi lm ngui, cn thn cho thm dung dch natri hydroxit (8.1.3) v
xoay bnh mu lin tc iu chnh pH ca dung dch v nm trong khong t 3 n pH 10.
Sau khi lm ngui, chuyn dung dch vo mt bnh dung tch 50 ml. Trng bnh Kjendahl vi mt
t nc v b sung nc trng ny vo bnh mu.
Cn tr ca As, xem 4.4.4 v A.2.
8.4.2. Th mu trng
Tin hnh th mu trng song song vi xc nh mu, theo cng quy trnh, cng mt lng thuc
th nhng dng nc thay cho mu th.
8.4.3. Hiu chun
8.4.3.1. Chun b dung dch hiu chun
Dng pipet, chuyn lng th tch thch hp, v d nh: 1,0 ml; 2,0 ml; 3,0 ml; 4,0 ml; 5,0 ml; 6,0
ml; 7,0 ml; 8,0 ml; 9,0 ml v 10,0 ml dung dch chun octophosphat (4.1.11) vo cc bnh
kjendahl 200 ml.
Nng octophosphat ca cc dung dch ny: p= 0,04 mg/l. Tip tc nh quy nh trong 8.4.1
t on Thm cn thn 2 ml axit sulfuric (8.1.1) v trn u
8.4.3.2. To mu
Thm vo mi bnh dung tch 50 ml (trong khi khuy) 1 ml axit ascorbic (4.1.5) v sau 30 s, thm
2 ml dung dch molipdat trong axit (4.1.7). Thm nc ti vch v trn u.
8.4.3.3. o ph
Xem 4.4.3.3
8.4.3.4. Dng ng chun
Xem 4.4.3.4
8.4.4. Php xc nh
8.4.4.1. To mu

Tin hnh theo 8.4.3.2 dng phn mu th t 8.4.1.

8.4.4.2. o ph
Xem 4.4.3.3
8.5. Biu th kt qu
8.5.1. Tnh ton
Nng tng phospho, p, tnh bng miligam trn lit c tnh theo cng thc:

( A A 0 )Vmax
f x Vs

Trong :
A l hp th ca phn mu th;
Ao l hp thu ca th mu trng;
f l dc th hiu chun (4.4.3.4), tnh bng lt trn miligam (l/mg);
Vmax l th tch mu th (50 ml) tnh bng mililit (ml);
Vs l th tch thc ca phn mu th, tnh bng mililit (ml).
Bo co nng phospho nh sau, nhng khng ly hn ba s c ngha:
- p < 0,1 mg/l chnh xc n 0,001 mg/l;
- p < 10 mg/l chnh xc n 0,01 mg/l;
- p 10 mg/l chnh xc n 0,1 mg/l.
8.5.2. chm
S liu v chm trong Bng B.3 thu c t mt th nghim lin phng th nghim vi 16
phng th nghim tham gia.
CH THCH: V cn tr, xem ph lc A
8.6. Bo co th nghim
Bo co th nghim cn c cc thng tin sau:
a) Mi thng tin cn thit nhn bit mu;
b) Vin dn tiu chun ny;
c) Vin dn phng php s dng, v iu/mc;
d) Kt qu thu c.
e) Cc thao tc khng nu trong iu ny hoc c coi l ty chn, cng nh mi bt thng
c th nh hng n kt qu.
Ph lc A
(tham kho)
Cc cht gy cn tr

A.1. Silic
Silic (Si) nng ti 5 mg/l khng gy cn tr. Nhng nng cao hn s lm tng hp th
Sau thi gian phn ng 30 min gi tr o c trong Bng A.1.
Bng A.1 - nh hng ca cc ion silic n kt qu phn tch
Nng silic, tnh theo Si

Nng phosphat tng ng, tnh theo P

mg/l

mg/l

10

0,005

25

0,015

50

0,025

A.2. Asenat
Asenat to nn mu tng t nh mu o octophosphat to ra. Cn tr ny c th loi tr bng
cch kh asenat thnh asenic (4.4.4.1.1) vi natri thiosulfat (4.1.9).
A.3. Hydro sulfua
Hydro sulfua vi nng S ti 2 mg/l l khng gy cn tr. Nng cao hn c th lm gim
n mc chp nhn c bng cch cho kh nit i qua mu axit ha (nh trong 6.1.4)
A.4. Flo
Flo vi nng ti 70 mg/l khng gy cn tr. Nng cao hn 200 mg/l km hm hon ton s
to mu.
A.5. Cc kim loi chuyn tip
A.5.1. St c nh hng ti mu, nhng vi nng 10 mg/l Fe th nh hng di 5
Vanadat lm tng mu theo quan h tuyn tnh, khong 5 % vi nng 10 mg/l vanadi
A.5.2. Crom (III) v crom (VI) vi nng ti 10 mg/l khng gy cn tr, nhng nng khong
50 mg/l lm tng hp th ln khong 5 %.
A.5.3. ng vi nng ti 10 mg/l khng gy cn tr.
A.6. Nc bin
mn khc nhau c nh hng khng ng k n cng mu.
A.7. Nitrit
Nu nng nitrit trn 3,29 mg/l c th gy ra s nht mu. Lng nh axit sulfamic d c nh
hng trong phn hy nitrit; 100 mg axit ny s x l vi nitrit nng 32,9 mg/l.
Ph lc B
(tham kho)
D liu v chm
D liu v chm trong Bng B.1 thu c t mt th nghim lin phng do Phn Lan t chc
vi 16 phng th nghim tham gia s dng phng php nu trong iu 4.
Bng B.1 D liu v chm cp trong iu 4
M t mu

S lng
mu
n

Trung bnh
mg/l

lch chun
lp li
Tuyt i

ti lp
Tuyt i

Tng i

mg/l

mg/l

Octophosphat khi c
polyphosphat

70

0,0576

0,0022

0,0108

18,8

Octophosphat

69

0,3127

0,00481

0,0324

10,4

Octophosphat khi c
polyphosphat v asenat

78

0,192

0,00401

0,0348

18,1

Octophosphat khi c
asenat

78

0,1013

0,00577

0,0221

21,8

D liu v chm trong Bng B.2 thu c t mt th nghim lin phng vi 15 phng th
nghim tham gia s dng phng php nu trong iu 6.
Bng B.2 D liu v chm nu trong iu 4
M t mu

S lng
mu

Trung bnh
mg/l

lch chun
lp li

ti lp

Tuyt i

Tuyt i

Tng i

mg/l

mg/l

Polyphosphat

79

0,1792

0,00659

0,0446

24,8

Polyphosphat khi c
phospho lin kt hu
c

65

0,1749

0,00709

0,0259

14,8

D liu v chm trong bng B.3 thu c t mt th nghim lin phng th nghim vi 16
phng th nghim tham gia. C quy trnh oxy ha peroxodisulphat v quy trnh thy phn bng
axit nitric/axit sulfuric u c s dng nhng khng quan st thy cc khc bit c ngha
trong cc mu phn tch.
Bng B.3 D liu v chm nu trong iu 7 v iu 8
M t mu

S lng
mu

Trung bnh
mg/l

lch chun
lp li

ti lp

Tuyt i

Tuyt i

Tng i

mg/l

mg/l

Phospho lin kt hu
c v sulfonat xanh
chm

70

0,0687

0,00383

0,00832

12,0

Phospho lin kt hu
c thm phloroglucin

58

0,4381

0,0128

0,0369

8,4

TH MC TI LIU THAM KHO

[1] Schouwenberg, J.C and Wallings, I.Anal. Chim. Acta, 37, 1967 pp 271-274.
[2] Koroleff, F. Determination of phosphorous. Method on seawater analysis. Weinheirm, Verlag
Chemie GmbH, 1977, and 2nd ed, 1983.