Tiu chun Vit Nam Nc thi Phng php xc nh oxy ha

Nhm I TCVN 4565 88

Waste water C hiu lc t 01/7/1989 Method for the derter mination of chemical oxygen demand (COD) Tiu chun ny c quy nh phng php kali pecmanganat xc nh oxy ha khi thnh phn cc cht hu c trong nc n gin v phng php dng cht oxy ha mnh l kali bicromat xc nh oxy ha khi thnh phn nc thi cha nhiu loi cht hu c. 1. Phng php ly mu 1.1. Ly mu theo TCVN 4556-88 1.2. Mu ly xc nh oxy ha khng nh hn 100ml v cn c nh bng axit sunfuric H2SO4 c (d = 1,84), vi t l 1ml trong 1000 ml mu. 2. Phng php dng kali bicromat (Phng php trng ti) Kali bicromat c kh nng oxy ha hon ton cc cht hu c nn ngi ta gi oxy ha theo bicromat l nhu cu ha hc oxy (chemical oxygen demand. Vit tt l COD). 2.1. Nguyn tc Dng kali bicromt l cht oxy ha mnh oxy ha cc cht hu c c bit l cc cht hu c phc tp (c lin kt i lin kt ba), sau chun lng kali bicromat bng dung dch mui Mo (mt amoni sunfat). 2.2. nh hng cn tr oxy ha hon ton khi trong nc c mt nhiu cht hu c mch thng, cc hydrocacbua thm cc pyridin, pyrimidin kh b oxy ha, cn phi c cht xc tc tham gia. Nu cho bc sunfat AgSO4 lm xc tc 85 90% cc cht trn c oxy ha. Nu nc c nhiu ion Cl- cn phi dng thu ngn sunfat (HgSO4) trnh oxy ha clorua. 2.3. Dng c v thuc th 2.3.1. Dng c Burt, pipt Bnh nn, bnh cu, ng sinh hn hi lu. 2.3.2. Thuc th

Dng c kali bicromt 0,25 N chun b nh sau: sy kh kali bicromat K2Cr2O7 105oC trong 2 gi lin. Cn chnh xc 12,259 g K2Cr2O7 p.a ho tan trong nc ct 2 ln ri cho vo bnh nh mc dung tch 1000 ml, thm nc ct n vch mc. Dung dch st amoni sunfat 0,25 N (mui Mo): ho tan 98 st amoni sunfat Fe (NH4)2.6H2O p.a c lm kh trong bnh ht m mt ngy trong 20ml axit sunfuric H2SO4 c (d = 1,84) cho vo bnh nh mc dung tch 1000 ml thm nc ct n vch mc. iu chnh li dung dch ny da theo dung dch kali bicromat vi ch th mu feroin hay dyphenylamin nh sau: Dng pipet ly chnh xc 10ml dung dch st amonisunfat 0,25 N vo bnh nn, dung tch 250 ml. Thm 20 ml axit sunfuric c. Lc u ri thm 3 5 git ch th feroin hoc diphenylamin. T buret nh dung dch kali bicromat 0,25 N xung n khi chuyn mu t xanh tm sang xanh l. Ch th feroin: Ho tan 1,458 g 1,10 octophenan-throlin monohydrat vi 0,695 st sunfat FeSO4.7H2O trong nc vt v cho nc ct n va 100ml. Ch th definylamin 1% trong axut sunfuric c; Bc sunfat; Thy ngn sunfat. 2.4. Cch tin hnh Cho mt lng mu vo bnh cu 500 ml sao cho hm lng cht hu c t 100 500 mg trong mt lt. Nu qu cao (khong 100 mg/l tr ln) ly khong 10 ml nc th ri pha long bng nc ct n 100 ml. Thm 0,4 g thu ngn sunfat HgSO4. Thm 20ml dung dch kali bicromat 0,25 N. Thm vo mt lng axit sunfuric c (gp 3 ln s ml kali bicromat) cho t t tng lng nh axit sunfuric c va lc bnh va lm lnh di vi nc. Ri cho vo chng 2g bc sunfat AgSO4, cho my vin bi thu tinh hoc t bt vo bnh. Lp bnh cu vo ng sinh hn hi lu un si nh v gi bnh nhit si trong hai gi sau ngui bnh, dng 25ml nc ct ra thnh ng sinh hn. Chuyn dung dch t bnh cu sang bnh nn. Trng bnh cu bng nc ct, chuyn tt c nc trng ra vo bnh nn, pha long hn hp n 200ml ri dng dung dch chun st amoni sunfat vi 3 4 git ch th mu feroin hoc diphenilamin chun lng kali bicromat cho n khi mu ca dung dch t xanh lam sang mu xanh l cy nht. Lm song song mt mu trng vi nc ct hai ln nh lm vi nc thi. 2.5. Cch tnh kt qu Nhu cu ha hc v oxy (x), tnh bng mg/l theo:
x= (a b) x N x S x 1000 V

Trong :

a- dung lng st amonisunfat tiu tn lc chun mu trng, ml b- Lng dung dch sc amonisunfat dng cho nc thi, ml N - Nng tng g ca dung dch st amoni sunfat (mui Mo); V - Th tch mu nc kim nghim, ml. S ng lng gam ca oxy. 3. Phng php dng kali pemangat 3.1. Nguyn tc Da tn vic oxy ha cc cht hu c c mt trong nc bng dung dch kali pemanganat 0,1 N trong mi trng axit nhit si. Lng d kali pemanganat c chun bng axit oxalic 0,1 N. Kt qu tnh ra mg oxy trong lt. 3.2. Yu t cn tr Clorua, nng ln hn 300 mg trong mt lt loi b bng cch thm vo 0,4 mg thu ngn sunfat. Amoniac c nng cao cng gy cn tr. loi b amoniac un si nc cho cn n 2/3 th tch c. St gy sai s tha phi lc nc loi b st trc khi nh lng cht hu c. 3.3. Dng c v thuc th 3.3.1. Dng c Buret, pipt, bnh nn, bp in. 3.3.2. Thuc th Axit oxalic 0,1 N Cn chnh xc 6,303 g axit oxalic H2C2O4.2H2O tinh khit phn tch (TKPT) ha tan bng nc ct hai ln, sau thm nc ct n vch 1000ml. un soi dung dch trong mt gi. yn trong mt tun v lc qua phu lc thu tinh xp. Dung dch ny hiu chnh nng dung dch KMnO4 cho ng 0,1N. Axit sunfuric m c (d = 1,84). 3.4. Tin hnh xc nh Cho vo bnh nn dung tch 500 ml mt lng mu sao cho nng cht hu c trong khng qu 100 mg trong mt lt, c th ly mt th tch nh ri thm nc ct n 100ml. Thm vo 2ml axit sunfuric H2SO4 c, 10ml kali pemanganat 0,1 N. un si dung dch v si thm 10 pht. Ly bnh ra khi bp in. ngui bt ri thm vo chnh xc 10 ml axit oxalic 0,1 N. Lc u, chun ngc lng axit d bng kali pemanganat 0,1 N n khi mu ca dung dch chm c mu hng tm. Ghi th tch kali pemanganat dng (a). Lm song song mt mu trng nh lm vi thuc th. Ghi th tch kali pemanganat dng cho mu trng (b).

3.5. Tnh kt qu Lng oxy cn thit oxy ha cc cht hu c trong 1000 ml nc thi (x) tnh bng mg, theo cng thc:
x= (a b) x N x S x 1000 V

Trong : N - nng ca dung dch kali pemanganat a- lng kali pemanganat dng cho mu nc thi, ml b- Lng kali pemanganat dng cho mu trng, ml S ng lng gam ca oxy. V - Th tch nc thi ly phn tch, ml