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TRNG I HC KHOA HC HU KHOA HA

PHNG TH NGHIM HA HC NG DNG

QUY TRNH PHN TCH PHOTPHAT V TNG PHOTPHO TRONG NC

HU 7 - 2011

XC NH PHOTPHO TRONG NC BNG PHNG PHP AXIT ASCORBIC


(4500-P E ASCORBIC ACID METHOD) 1. Nguyn tc Amoni molypdat v kali antimonyl tatrat phn ng vi octo photphat trong mi trng axit to thnh axit d a photpho molypdic. Axit d a ny b kh thnh xanh molypden bng axit ascorbic. o mt quang ca dung dch 880 nm c th xc nh c nng P. Ph thuc vo vic x l mu nc cn phn tch m kt qu xc nh P c th c phn thnh: - Photpho phn ng (photpho hot ng): bao gm octo photphat, cc photphat ngng t khc nh pyro -, tripoly -, hecxa, meta photphat, mt s hp cht photphat hu c. - Photpho thy phn trong axit: bao gm cc poly photphat khng c phn ng to sn phm xanh molypden. Cc dng photpho ny s b chuyn thnh photpho phn ng, sau khi un si trong axit mt thi gian. - Photpho tng: gm tt c cc dng hp cht cha photpho trong nc dng tan hay cc ht cht rn. xc nh P tng, cn phn hy mu nc bng mt trong cc phng php sau: Phn hy bng hn hp HNO3 - HClO4 Phn hy bng hn hp H2SO4 - HNO3 Phn hy bng pesunfat 2. Yu t nh hng - Asen (> 0,1 mg/l) nh hng vic xc nh P bng phng php ny, do asen cng to ra sn phm c mu xanh tng t nh P. - Cr(VI) v NO2- nng 1 mg/l gy ra sai s m khong 3%, hoc 10 15% vi nng 10 mg/l. - S2-, SiO32- khng nh hng khong nng 1,0 10 mg/l. 3. Bo qun mu - Xc nh cc dng photpho ha tan: lc mu ngay sau khi ly v bo qun -100C hoc bng 40 mg HgCl2/1 lt mu (vic thm HgCl2 s bo qun mu c lu hn nhng khng khuyn co dng v l do mi trng). - Xc nh cc dng ca photpho: bo qun lnh -100C, khng c axit ha mu hay bo qun mu bng CHCl3. - Xc nh tng photpho: axit ha mu n pH < 2 bng H2SO4 hay HCl v bo qun 40C hoc lm lnh su m khng cn thm bt c ha cht bo qun no. 4 Dng c ha cht 4.1. Dng c Thit b
PTN Ha hc ng dng Khoa Ha Trng HKH Hu 1

- My trc quang s dng bc sng 880 nm, cuvet c b dy 1 cm - Cc dng c thy tinh pha ch v bo qun thuc th... 4.2. Ha cht Dung dch H2SO4 5 N: pha long 70 ml H2SO4 c thnh 500 ml bng nc ct. Dung dch kali antimonyl tatrat: ha tan 1,3715 g K(SbO)C4H4O6.H2O vo 400 ml nc ct trong bnh nh mc 500 ml, sau nh mc thnh 500 ml. Bo qun trong bnh c nt thy tinh. Dung dch amoni molypdat: ha tan 20 g (NH4)6Mo7O24.4H2O trong 500 ml nc ct. Bo qun dung dch trong bnh thy tinh c nt. Dung dch axit ascorbic 0,01 M: ha tan 1,76 g axit ascorbic trong 100 ml nc ct. Dung dch bn trong 1 tun khi bo qun 4oC. Dung dch thuc th hn hp: trn cn thn theo th t sau: 50 ml dung dch H2SO4 5 N, 5 ml dung dch kali antimonyl tatrat, 15 ml dung dch amoni molypdat v 30 ml dung dch axit ascorbic. Lc u sau khi thm mi thuc th. Nu trong qu trnh trn hn hp, dung dch b c, th lc v yn vi pht n trong, sau mi thm tip dung dch thuc th mi vo. Thuc th hn hp bn trong 4 gi. Dung dch gc photphat: ha tan 219,5 mg KH2PO4 khan v nh mc n 1000 ml bng nc ct. 1,00 ml dung dch ny cha 50,0 g P-PO43- (nng : 50 mg P-PO43-/l). Dung dch photphat trung gian: pha long 10,0 ml dung dch photphat gc thnh 100 ml bng nc ct. 1,00 ml dung dch ny cha 5,0 g P- PO43 (nng : 5,0 mg P-PO43-/l). Dung dch photphat lm vic: pha long 5,0 ml dung dch photphat trung gian thnh 100 ml bng nc ct. 1,00 ml dung dch ny cha 0,25 g P- PO43- (nng : 0,25 mg P-PO43-/l). 5. Quy trnh phn tch Ly 10,0 ml mu vo ng nghim hay bnh tam gic, thm 1 git ch th phenolphtalein, nu dung dch c mu hng, th thm tng git H2SO4 5 N n lc mt mu. Thm 1,6 ml dung dch thuc th hn hp, lc cn thn. yn 10 pht (nhng khng qu 30 pht), ri em o mt quang 880 nm, vi dung dch mu trng lm dung dch so snh. Xy dng ng chun: Pha dy dung dch chun c nng t 0,01 0,25 mg P-PO43-/l theo bng sau: STT Th tch dd photphat lm vic (ml) Th tch dd thuc th hn hp (ml) Th tch nc ct (ml) Nng photphat (mg P-PO43-/l) 1 0,4 1,6 9,6 0,01 2 2,0 1,6 8,0 0,05 3 4,0 1,6 6,0 0,10 4 6,0 1,6 4,0 0,15 5 8,0 1,6 2,0 0,20 6 10,0 1,6 0 0,25
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Cch tin hnh xc nh photphat trong cc mu chun nh quy trnh trn Mu trng: tng t nh mu chun nhng thay dung dch lm vic bng nc ct Xy dng phng trnh ng chun A = f(CP-PO43-) Nng photphat trong mu c xc nh da vo phng trnh ng chun 6. Ti liu tham kho Clesceri L.S., Greenberg A.E., Eaton A.D. (1998), Standard methods for the examination of water and wastewater (4500-P E Ascorbic Acid Method), 20th Ed., APHA, USA.

PTN Ha hc ng dng Khoa Ha Trng HKH Hu

PHNG PHP PHN HY MU BNG PESUNFAT XC NH TNG PHOT PHO TRONG NC


(4500-P B SAMPLE PREPARATION) 1. Nguyn tc Mu c phn hy bng pesunfat trong mi trng axit chuyn cc dng ca photpho c trong mu thnh octo photphat. Tng photpho c xc nh thng qua vic xc nh octo photphat to thnh trong dung dch phn hy bng phng php axit ascorbic. 2. Bo qun mu Axit ha mu n pH < 2 bng H2SO4 hoc HCl v bo qun 40C hoc lm lnh su m khng cn thm bt c ha cht bo qun no. 2. Thit b, dng c - Autoclave - Chai thy tinh c nt vn chu nhit 3. Ha cht Ch th phenolphtalein: 1% trong etanol Dung dch H2SO4: cn thn thm 300 ml H2SO4 m c vo 600 ml nc ct v pha long n 1000 ml (NH4)2S2O8 hoc K2S2O8 rn Dung dch NaOH 1M: ha tan 40 g NaOH trong nc v pha long n 1000 ml 4. Quy trnh phn hy mu Ly 50,0 ml mu cho vo chai thy tinh c nt vn, thm 1 git ch th phenolphtalein. Nu dung dch c mu hng th thm tng git dung dch H2SO4 n khi mt mu hng. Thm 1 ml dung dch H2SO4 v 0,4 g (NH4)2S2O8 hoc 0,5 g K2S2O8. Cho mu vo autoclave v un nng p sut khong 98 130 kPa (0,098 0,13 MPa) trong khong 30 pht. ngui n nhit phng. Thm 1 git ch th phenolphtalein v trung ha bng NaOH n khi va xut hin mu hng. Chuyn ton b mu sang bnh nh mc v nh mc n 100 ml bng nc ct.
(Lu : - Nu dng dung dch pesunfat th phi pha mi mi khi s dng - Trong trng hp xut hin kt ta khi trung ha bng NaOH th khng c lc b kt ta)

P trong dung dch phn hy ( dng octo photphat) c xc nh bng phng php axit ascorbic (phng php 4500-P E). Xy dng ng chun vi nng photphat trong khong 0,05 1,0 mg P-PO43-/l). 5. Ti liu tham kho Clesceri L.S., Greenberg A.E., Eaton A.D. (1998), Standard methods for the examination of water and wastewater (4500-P B Sample Preparation), 20th Ed., APHA, USA.
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