PHNG PHP PHN TCH COD TRONG NC

Khi nim v ngha COD l lng oxy cn thit oxy ha hon ton cht hu c bng cht oxy ha mnh. COD tnh bng mg/l. Th nghim o COD c s dng rng ri trong lnh vc kim sot nhim mi trng do nhng u im sau: S liu COD thng c dng chuyn i sang BOD khi vic th nghim tin hnh nhiu rt ra h s tng quan c tin cy ln. Kt hp 2 s liu COD v BOD cho php nh gi lng cht hu c tr i vi s phn hy sinh hc. Phng php ly mu v bo qun Ly mu v bo qun theo TCVN 4556 88 phng php ly mu, vn chuyn, bo qun mu. Phng php o Nguyn tc Hu ht cc hp cht hu c u b phn hy khi un si trong hn hp cromic v acid sulfuric CnHaOb + cCr2O72- + 8cH+ nCO2 + (a/2 + 4c)H2O + 2cCr23+ Vi c = 2n/3 + a/6 b/3 Lng Cr2O72- bit trc s gim tng ng vi lng cht hu c c trong mu. Lng Cr2O72- d s c nh phn bng dung dch FAS (Ferrous Ammonium Sulfate Fe(NH4)2(SO4)2) v lng cht hu c b oxy ha s tnh ra bng lng oxy tng ng qua Cr2O72- b kh. Lng oxy tng ng ny chnh l COD. Cc yu t nh hng Cc hp cht bo mch thng, hydrocacbon nhn thm v pyridine khng b oxy ha, mc d phng php ny hu nh oxy ha hon ton hn so vi phng php dng KMnO4. Cc hp cht bo mch thng b oxy ha d dng hn khi thm Ag2SO4 vo lm

cht xc tc, nhng bc d phn ng vi cc ion h halogen to kt ta v cht ny cng c th b oxy ha mt phn. Khi c kt ta halogen, c th dng HgSO4 to phc tan vi halogen trc khi un hon lu. Mc d, 1 g HgSO4 cn cho 50 ml mu, nhng c th dng t hn khi hm lng chloride < 2.000 mg/l (min l duy tr t l HgSO4 : Cl- = 10 : 1). Nitrite cng gy nh hng n vic xc nh COD, nhng khng ng k c th b qua. Dng c v thit b: ng pipet 25 ml ng ong 100 ml Buret 25 ml ng nghim c nt vn Bnh cu 250 ml c nt nhm H thng chng ct hon lu Bnh tam gic 125 ml, 50 ml T sy c iu chnh nhit (1500C)

 Ha cht: Dung dch chun K2Cr2O7 0,0167M: Ha tan 4,913 g K2Cr2O7 ( sy 1050C trong 2 gi) trong 500 ml nc ct, thm vo 167 ml H2SO4 m c v 33,3 g HgSO4 khuy tan, ngui n nhit phng, nh mc thnh 1000 ml. Dung dch chun K2Cr2O7 0,0417M: Ha tan 12,259 g K2Cr2O7 ( sy kh 1050C trong 2 gi) trong nc ct v nh mc thnh 1000 ml. Acid sunfuric reagent: Cn 5,5 g Ag2SO4 trong 1 kg H2SO4 m c (d = 1,84), 1 2 ngy ha tan hon ton. Ch th mu Ferroin: Ha tan 1,485 g 1,10 phenanthroline monohydrate v 0,695 g FeSO4.7H2O trong nc ct nh mc thnh 100 ml (khi hai cht ny trn ln vi nhau th dung dch ch th s tan hon ton v c mu ). Dung dch FAS (Fe[SO4].[NH4]2[SO4].6H2O) 0,1M: Ha tan 39,2 g Fe(NH4)2(SO4)2. 6H2O trong 500 ml nc ct, cn thn cho thm 20 ml H2SO4 m c, ngui, nh mc thnh 1.000 ml. Chun li nng FAS mi ngy vi K2Cr2O7 0,0167M nh sau: Chn th tch mu (dng nc ct thay cho mu) v ha cht s dng theo bng sau: Bng 2.3: T l chn th tch mu v ha cht C ng 16 x 100 mm 20 x 150 mm 25 x 150 mm ng chun 10 ml V mu (ml) 2,5 5,0 10,0 2,5 DD K2Cr2O7 0,0167M (ml) 1,5 3,0 6,0 1,5 H2SO4 reagent (ml) 3,5 7,0 14,0 3,5 Tng V (ml) 7,5 15,0 30,0 7,5

ngui ng n nhit phng v thm 0,05 0,10 ml (1 2 git) ch th ferroin v chun vi FAS. im kt thc phn ng chun , dung dch chuyn t mu xanh l cy sang mu nu . M (FAS) = (VK2Cr2O7 0,0167M, ml / VFAS dng chun , ml) x 0,1

Dung dch FAS 2,25M: Ha tan 98 g FAS trong mt t nc ct, thm vo 20 ml H2SO4 m c, ngui v nh mc thnh 1000 ml. Chun li nng FAS mi ngy vi K2Cr2O7 0,0417M, nh sau: Pha long 10 ml dung dch K2Cr2O7 n khong 100 ml vi nc ct. Thm 30 ml H2SO4 m c v ngui. Chun vi FAS dng 0,1 0,15 ml (2 3 git) ch th ferroin. im kt thc phn ng chun dung dch chuyn t mu sang mu xanh l cy. M (FAS) = (VK2Cr2O7 0,0417M, ml / VFAS dng chun , ml) x 0,25 HgSO4 tinh th hoc dng bt. Tin hnh o Phng php un hon lu kn (khi COD > 50 mg/l) Ra k ng COD v np bng dung dch H2SO4 20% trc khi s dng. Chn th tch mu v lng ha cht theo bng hng dn sau: Bng 2.4: T l chn th tch mu v ha cht C ng 16 x 100 mm 20 x 150 mm 25 x 150 mm ng chun 10 ml V mu (ml) 2,5 5,0 10,0 2,5 Dung dch K2Cr2O7 (ml) 1,5 3,0 6,0 1,5 H2SO4 reagent (ml) 3,5 7,0 14,0 3,5 Tng V (ml) 7,5 15,0 30,0 7,5

Ln lt cho mu v ha cht (theo bng hng dn trn) vo ng nghim, cn thn tc nhn axit H2SO4 (H2SO4 reagent) chy dc thnh ng nghim, lu phn ng ta nhit mnh rt nng. Vn cht np, lc k ng nhiu ln. Lm thm mt mu trng v mt mu th khng bng nc ct. Thc hin tng t nh cc bc lm mu. Xp ng nghim mu v mu trng vo gi inox v t vo t sy nhit 1500C trong 2 gi. Mu th khng nhit phng (khng un 1500C) c dng nh phn li nng dung dch FAS (v dung dch FAS c nng khng n nh theo thi gian).

 mu ngui n nhit phng. Thm 3 git ch th ferroin v nh phn bng dung dch FAS 0,1M n khi dung dch va chuyn t mu lam lc sang mu nu , ghi th tch B dung dch FAS va dng. nh phn mu trng ghi nhn th tch A dung dch FAS dng nh phn. o Phng php un hon lu h (COD < 50 mg/l) ong 50 hoc 100 ml mu cho vo bnh cu COD c th tch 250 ml Ln lt thm 1 g HgSO4 v vi vin bi thy tinh, cn thn thm 5 ml H2SO4 reagent lc u cho tan HgSO4. Tip tc thm 25 ml dung dch K2Cr2O7 0,00417M. Ni vi h thng un hon lu, cn thn thm tht chm 70 ml H2SO4 reagent cn li qua phu t trn ming ng lm lnh. Lc nh trn u hn hp trong bnh. Bt bp un hon lu trong 2 gi. Tt bp, ngui n nhit phng, dng bnh xt nc ct ra sch dung dch cn ng trn thnh ng lm lnh. Tho ri bnh cu COD khi h thng. nh phn bng dung dch FAS 0,025M vi 3 git ch th mu ferroin. Kt thc nh phn khi dung dch va chuyn sang mu nu . Tnh kt qu: Chun li nng dung dch FAS 0,1M CFAS = (VK2Cr2O7 x 0,1) / VFAS COD ca mu c tnh theo cng thc sau: COD (mg/l) = (A B) x CFAS x 8000 / Vm Trong : VK2Cr2O7 : Th tch K2Cr2O7 dng, (ml). VFAS: Th tch FAS dng nh phn mu nc ct (khng un), (ml). A: Th tch FAS dng nh phn mu nc ct (un 1500C), (ml). B: Th tch FAS dng nh phn mu (un 1500C) (ml). CFAS: Nng FAS c nh chun li, (M). Vm: Th tch mu, (ml)