CHNG 2: KHO ST PH HP THU V CC YU T NH HNG N QU TRNH XC NH NG BNG PHNG PHP TRC QUANG VI THUC TH DIETYL DITHIOCACBAMAT 2.

1 Kho st ph hp thu gia ng v thuc th dietyl dithiocacbamat xc nh hm lng ng bng phng php trc quang, trc tin ta phi kho st bc sng ti u nht (max) ca phc ng vi dithizone. Pha dung dch chun ng t 1000ppm xung 100ppm ri tip tc pha long xung nng lm vic Chun b 2 bnh nh mc 50ml, ln lt ht 5ml dung dch ng chun, 5ml thuc th dithizone, nh mc n vch.Chit dung dch t pha nc sang pha hu c yn 5 pht v em o quang. Kho st v qut bc sng t 300 900 nm

2.2 Kho st hm lng thuc th dietyl dithiocacbamat

Xc nh hm lng ng bng phng php trc quang, ta phi tin hnh kho st lng thuc th dietyl dithiocacbamat, bit lng thuc th thm phi m bo cho qu trnh to phc gia ng v dietyl dithiocacbamat. - chun b 7 bnh nh mc - c nh dung dch ng chun 5ml - ln lt thay i th tch lng thuc th thm vo t 1ml, 3ml, 5ml, 7ml, 10ml, 12ml, 15ml. - nh mc bng nc ct
2.3 Kho st nh hng ca pH n phc mu

PH ca dung dch nh hng n cc dng tn ti ca cc hp cht tham gia phn ng. Nu pH ca dung dch thay i c th s lm thay i tc ca phn ng. V vy, vic kho st pH ti u trong h phn ng l cn thit. Ta chun b mu nh bng v sau o quang bc sng thch hp. - chun b 7 bnh nh mc

- ht 5ml dung dch ng tiu chun - ht 5ml thuc th NaDDC - cho ln lt cc th tch khc nhau (2, 4, 6, 8, 10, 12, 15ml) ca dung dch axit NH3 - nh mc bng cloroform. yn 5 pht ri em o quang
2.4 Kho st nh hng ca thi gian n vic to phc

kho st hm lng ng bng phng php trc quang, ta phi tin hnh kho st s nh hng ca thi gian n kh nng bn mu ca phc mu gia ng vi thuc th dietyl dithiocacbamat. Ta thc hin cc bc sau: - chun b 5 bnh nh mc - ht 5ml dung dch ng tiu chun - thm vo 5ml dung dch thuc th - nh mc bng cloroform, sau em o quang cc khong thi gian khc nhau (5, 10, 15, 20, 25, 30 pht)
2.5 Kho st cc ion l Trong mi trng c cha amoniac, xitrat v complexon, a s cc kim loai khc khng gy cn cho vic xc nh ng bng phng php ny, ch c bitmut, bc v thy ngn vn phn ng vi DDC v c th b chit cng vi phc ng.Tuy nhin trong 3 phc ch c phc ca bitmut c mu vng l nh hng, cn cc phc ca bc v thy ngn khng mu hp th nh sng trong vng t ngoi, nn thc t khng nh hng n vic xc nh ng.

kho st nh hng ca ion nu trn, ta tin hnh ly 6 bnh nh mc 50ml to phc mu vi 5ml dd Cutiu
chun,

5ml thuc th dietyl dithiocacbamat,

thm ion cn kho st vo cc bnh tr bnh th nht (nng tng dn). nh mc n vch. i 10 pht em o quang bc sng thch hp
2.6 Kho st khong tuyn tnh LOL

kho st khong tuyn tnh ca ng ta tin hnh thay i th tch ca dung dch ng chun sau ta thc hin cc bc sau: - chun b 7 bnh nh mc - ht cc th tch khc nhau ca dung dch ng chun lm vic (0.1ml, 0.5ml, 1ml, 5ml, 10ml, 20ml, 30ml. - thm 5ml thuc th dietyl dithiocacbamat - nh mc bng cloroform v yn 5 pht sau em o quang.
2.7 Kho st LOD v LOQ LOD: gii hn nh nht ca phng php m my c th pht hin c.
LOD = 3 Cmin N = 3Cmin T S (10 > T = S 3) N

Gii hn nh lng ca phng php:l gi tr nh nht m s nh lng tin cy c, c gi tr bng 10 ln S/N.

Cmin N =10Cmin T S S 3) N

LOQ =10

(10 > T =

Trong : Cmin: nng ti thi im xt S v N. S: mt quang ca mu c nng Cmin. N: mt quang trung bnh ca mu trng. kho st LOD v LOQ, tin hnh mt quang A vi mu trng lp li sau mi ln o mu.

2.8 Kho st hiu sut thu hi ca phng php phn tch mu

 kho st hiu sut thu hi ca phng php chng ti tin hnh thm mt lng ng ng vi nng ca ng 50ppm, 100ppm, 200ppm, vo cc mu xc nh. Tin hnh phn tch mu thm chun v khng thm chun theo phng php kho st.