TCVN 5070 - 1995

Sot xt ln 1

Cht lng nc - Phng php khi lng xc nh du m v sn phm du m

Water quality - Weight method for determination of oil and oil product
1. Phm vi p dng Tiu chun ny dng xc nh du m v cc sn phm du m (sau y gi tt l "du") trong cc loi nc thin nhin c nng t 0,3 mg/l tr ln. 2. Nguyn tc phng php Dng clorofom tch du v sn phm du ra khi nc, chng ct lo ht dung mi, cn nh lng. Dng hexan ho tan cc sn phm du v cho qua ct sc k cha nhm oxt tch chng ra khi cc cht phn cc v cc cht khng phi l nhng lin kt ca cacbon c trong du, loi ht dung mi, cn nh lng. 3. Dng c v thuc th 3.1. Dng c Bnh cu, dung tch 3000ml Phu tch chit, dung tch 500ml Bnh tam gic, dung tch 500ml Cc cn , dung tch 25ml Bnh cu nh, dung tch 20ml My khuy Cn phn tch c chnh xc 0,1mg Ct sc k thu tinh, ng knh 10mm - 10ml 3.2. Thuc th Clorofom hoc Cacbon tetraclorua, loi TKHH Hexan (C6H14) TKHH axit clohidric (HCl) TKHH Nhm oxit (Al2O3) TKPT 4. Phng php ly mu Dng ng ly mu c ra sch v c trng bng clorofom thu mu nc sao cho nc b mt khng lt vo trong ng. Lng mu dng phn tch mt ln l 3 lt, c nh mu thu c bng clorofom. Sau nn tin hnh tch chit ngay, lu khng c lc mu, phi dng ton b nc c trong bnh tch chit (3 lt), phn chit c c th bo qun n 10 ngy trong bnh kn iu kin mt v tt. 5. Chun b xc nh Trc khi tin hnh phn tch phi thc hin cng vic theo cc mc sau: 5.1. Nhm oxit (Al2O3) c nghin mn, sng qua sng ng knh mt l 0,1mm v nung nhit 600oC trong khong 4 gi. 5.2. Chun b ct sc k nhm oxit Cho 6g nhm oxit c s l theo mc 4.1 vo cc thu tinh dung tch 500ml, thm vo 10ml hexan v trn u. Chuyn chng vo ct sc k thu tinh sau khi lt khong 1cm bng

thu tinh pha di ct. Trong thi k nh nhm oxit, van ca ct phi m, khi chuyn ht nhm oxit vo ct v dung tch hexan t ti lp mt nhm oxit th ng van li. trnh bay hi dung mi, dng mt knh ng h y ct. 6. Tin hnh xc nh 5.1. Tch du v cc sn phm du ra khi nc 5.1.1. Cho mu nc cn phn tch 3 lt vo bnh cu. Dng axit clohidric (HCL) t trng 1,19 axit ho mu nc ti pH nh hn 5. Cho vo 150ml clorofom hoc cacbon tetraclorua. 5.1.2. t cnh my khuy cch ranh gii phn lp khong 5cm v pha lp dung mi hu c, khuy vi pht sau cht phn ln nc sang bnh khc cng dung tch, phn cn li chuyn sang phu chit dung tch 500ml, phn lp 15 pht, chit phn dung mi c du vo bnh tam gic sao cho nc v lp trung gian khng lt vo . Chuyn phn ny cng vi lng nc c cht ra sang bnh cu dng ln u. Thm vo 150ml clorofom v tin hnh tch chit nh ln trc. Chit phn dung mi c du vo bnh tam gic cha sn phm thu c ca ln u. Loi b nc v lp trung gian. Dng 50ml clorofom trang phu chit v chuyn sang bnh tam gic. 5.2. Xc nh du v sn phm du 5.2.1. t bnh tam gic c cha sn phm chit c ln bp cch thu. Ni bnh vi b ngng v un si thu li clorofom. Khi trong bnh cn 10 - 20ml mu th ngng un, ngui. 5.2.2. bnh tam gic vo trong t ht. t qut cch t ht khong 35cm qut. Rt dn dung dch t bnh tam gic sang cc cn c khi lng xc nh, sao cho dung dch chim ti a 3/4 dung tch. Sau khi dung dch c rt ht, dng mt lng nh clorofom trng bnh tam gic 3 ln v tip tc cho bay hi. Khi trong cc cn khong 0,5ml mu th ngng qut v tip tc cho dung dch bay hi trong khng kh ti khi lng khng i. Kim tra bng cch t cc ln cn v cn mi ln t 1 n 2 pht. Lng du v cc sn phm c trong mu (C 1), tnh bng mg, bng khi lng cc c cht cn phn tch tr i khi lng cc. 5.3. Xc nh cc sn phm du 5.3.1. Cho 2ml hexan vo cc cn c cha sn phm thu c theo mc 5.2.2 v chuyn dn chng vo ct sc k c chun b theo mc 4.2. Di ct t mt bnh nh c khi lng xc nh thu dung dch qua ct. Phi iu chnh van ca ct sc k sao cho tc chy khng vt qu 0,3ml/pht. Dng mt lng nh hexan trng cc 3 ln sau mi ln trng cc li tip tc cho qua ct sc k. Dng hexan trng ct 3 ln, mi ln khong 1ml v thu ton b vo bnh cu nh. Phi duy tr dung dch lun trn lp oxit trong qu trnh sc k. 5.3.2. Loi hexan n khi lng bnh cu khng i nh trng hp loi clorofom (mc 5.2.2). Lng sn phm du c trong mu (C2), tnh bng mg, bng khi lng bnh cu c cht cn phn tch tr i khi lng bnh cu. 7 Tnh ton kt qu 7.1. Nng du v sn phm CX, tnh bng mg/l, xc nh theo cng thc

Cx =

C1 1000 V

Trong : C1 - Lng du v sn phm du c trong mu, mg; V - Th tch mu nc, ml.

1.1. Nng sn phm du CY, tnh bng mg/l, xc nh theo cng thc: C 1000 Cy = 2 V
Trong : C2 - Lng sn phm du trong mu, mg; V - Th tch mu nc, ml.