Determination of Phosphorous in water 2010

DETERMINATION OF PHOSPHOROUS IN WATER

1. Tiu chun p dng:

Tiu chun AOAC 973.55

2. Nguyn tc: Ammonium molybdate v Potassium antimonyl phn ng vi nhau trong dung dch acid cha dung dch long PO43- to thnh phc antimonyl phosphomolybdate m mu xanh ca n s b gim bi acid Ascrobic. Phng php ny ch dnh cho orthophosphate v cc hp cht c th chuyn thnh orthophosphate. Nhn chung th cc dng Phosphorous phn tch ch yu ph thuc v{o giai on tin x l mu phn tch 3. i tng p dng: Phng ph|p n{y ng dng ph}n tch cho nc mt, nc mui, nc thi sinh hot v{ nc thi cng nghip. Thng thng th ngi ta phn tch tng s P, P ha tan, orthophosphate, v orthophosphate ha tan. Nng ca Cu, Fe, Silicate, Arsenate trong nc bin hu nh khng g}y nhiu n qu trnh phn tch. HgCl2 gy nhiu n qu| trnh ph}n tch, khc phc iu ny cn thm 50 (mg)NaCl/L mu. 4. Dng c-ha cht: 4.1. Dng c: Tt c cc dng c thy tinh phi c ra trong dung dch nng HCl(1:1) v ra sch li bng nc. Thit b o quang ph. Beaker. Bnh nh mc. Bnh tam gic. Cn phn tch. T sy. T lnh. Bp in. Thit b lc 4.2. Ha cht: H2SO4. Potassium antimonyl tartrate solution. Ammonium molybdate solution. Ascorbic acid solution. Phosphorous standard solutions. Ammonium persulfate. phenolphthalien
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Determination of Phosphorous in water 2010

5. Quy trnh tin hnh: Mu phi c lu tr trong chai nha hay thy tinh chu nhit. Nu khng phn tch mu ngay ngy thu thp mu th phi cho thm 40(mg/L) HgCl2 bo qun mu. Trong trng hp ny, phi thm 50(mg/L) NaCl trc khi tin hnh phn tch. Chun b dung dch H2SO4 2.5M: ly 70 (mL) H2SO4 m c pha long trong beaker 1000(mL) cha 500(mL) nc tinh khit khng cha Phosphorous. Chun b dung dch Potassum antimonyl tartrate: cn 1.3715(g) K(SbO)C4H4O6.0.5H2O, ha tan trong beaker 500(mL) cha 400(mL) nc tinh khit, ri cho v{o bnh nh mc 500(mL) v{ thm nc n vch. Dung dch sau khi pha phi c cha trong chai ti m{u, y kn v gi 4oC. Chun b dung dch Ammonium molybdate: ha tan 20(g) (NH4)6Mo7O24.4H2O trong 500(mL) nc ct, sau lu tr trong chai nha v 4oC. Chun b dung dch Ascorbic acid 0.1(M): ha tan 1.76(g) trong 100(mL) nc tinh khit. Dung dch ny n nh trong 1 tun 4oC. Chun b dung dch Hydrolyzing acid: cho chm chm 310(mL) H2SO4 m c vo 600(mL) nc ct, l{m m|t, nh mc n 1000(mL). Chun b hn hp tc cht: tin hnh ha trn cc ha cht the cc t l sau: 50(mL) H2SO4 2.5(M), 5(mL) Potassium antimonyl tartrate solution, 15(mL) Ammonium molybdate solution, v 30(mL) Ascrobic acid solution. Nu thy dung dch b c th tin hnh lc v{ sau yn trong vi pht trc khi phn tch. Dung dch ny n nh trong 1 tun 4oC. Phosphoruos standard solutions [dung dch gc cha 50(mg/L) P ]: ha tan v{ nh mc 0.2197(g) KH2PO4 ~ c sy kh 105oC trong bnh nh mc 1000(mL). Sau tin hnh pha dung dch ph cha 0.5(mg/L) P bng cch pha long 10(mL) dung dch gc thnh 1000(mL). Tin hnh chun b dy dung dch xy dng ng chun: S dng dung dch chun 0.5(mg/L) Vdd chun 0 1 3 5 0 0 0 0 0 (mL) V pha long (ml) Cdd sau khi pha long (mg/L) 0 0 0 0 0 0 0 0 0

0.01

0.03

0.05

0.1

0.2

0.3

0.4

0.5

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Determination of Phosphorous in water 2010

- Phn tch Phosphorous: Thm 1(mL) Hydrolyzing acid solution vo Erlenmeyer 150(mL) c cha 50(mL) mu. Thm 0.4(g) Ammonium persulfate, sau un si trn bp in trong khong 30-40 pht hay ti khi dung dch cn khong 10(mL). Khng mu bay hi ti kh. Hoc c th la chn phng ph|p kh|c l{ chng trong ni hp nhit 121oC trong khong 30 pht. Lm mt v thm vi git phenolphthalein, hiu chnh ti khi c mu hng bng NaOH 1(M). Sau chnh v khng mu vi 1 git Hydrolyzing acid. Lm mt v pha long dung dch thnh 50(mL). Nu dung dch c th lc, thm 8(mL) combined agent, v trn u sau yn khong 10-30 pht sau o bng thit b so mu. Thc hin o mu trng tng t. - Hydrolyzable phosphorus: tng t nh quy trnh trn nhng khng thm Ammonium persulfate. - Orthophosphate: thm 1 git phenolphthalein vo 50(mL) mu; nu thy m{u xut hin th thm tng git Hydrolyzing acid n khi mu khng i, thm 8(mL) combined agent, v trn u sau yn khong 10-30 pht. Thc hin o mu trng tng t. - Curve tiu chun v cch tnh ton: 6. Kt qu v nhn xt:

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