Professional Documents
Culture Documents
CHT LNG NC - PHNG PHP XC NH HM LNG FLORUA TRONG NC THI CNG NGHIP
1. PHM VI P DNG Tiu chun ny quy nh phng php so mu vi phc mu Ziriconi-alizarin sunfonat xc nh florua. 2. PHNG PHP LY MU V BO QUN MU - Ly mu theo TCVN 5999-95. - Lng mu ly xc nh florua khng t hn 250ml. - Bo qun mu theo TCVN 5993-95. 3. PHNG PHP XC NH 3.1 Nguyn tc Ion florua to vi mt phn Ziriconi ca phc mu Ziriconi-alizarin-sunfonat. S gim mu ca phc mu t l thun vi hm lng florua. 3.2 Cc yu t cn tr - Clorua cn tr php xc nh, loi tr bng cch thm bc sunfat vo dung dch mu trc khi chng ct. - Sau khi chng ct, cc ion gy cn tr nh st, nhum, sunfat, photphat c loi tr. 3.3 Dng c v thuc th 3.3.1 Dng c - B chng ct (hnh 1). - My o quang, c th dng cuvet dy 2 5cm, bc sng = 520 550mi trng - Cc dng c thu tinh thng thng: bnh nh mc, pipet, ng ong... 3.3.2 Ho cht Cc ho cht s dng c tinh khit phn tch (TKPT) hoc tinh khit ho hc (TKHH). - Natri hidroxit, dung dch 0,2N hoc 5%. - Ct sch chun b nh sau: ly ct trng ra gn nhiu ln, sau ngm trong HCl (1:2) trong khong 3 n 4 gi, ra gn nhiu ln bng nc my v vi nc ct n ht axit theo giy qu. Sy kh trn bp in v nung 1 gi 6000C. - Bc sunfat. - Axit sunfuric d = 1,84 v dung dch (1:2)
- Dung dch Alizarin sunfonat 90mg/l: Ho tan 0,0900g Alizarin sunfonat trong nc v thm n th tch 1000ml. + Axit monocloraxetic 0,4M: Ho tan 37,3g axit monocloraxetic trong nc v thm n th tch 1000ml. + Trn dung dch axit monocloraxetic vi dung dch Natri hidroxit 0,2N theo t l (1:1). - Dung dch Ziriconi clorua 0,001M: Ho tan 0,32g ZrOCl2.8H2O trong 50ml nc ct. Thm cn thn 33,3ml axit sunfuric d = 1,84. ngui, thm nc n 1000ml. Dung dch ng trong chai mu, sau 1 gi chun b c th s dng c. - Dung dch florua tiu chun 0,1mg/ml: Ho tan 0,221g Natri florua, sy kh 1050C, trong nc ct, chuyn vo bnh nh mc 1000ml, thm nc n vch, lc k. - Dung dch florua tiu chun 0,01mg/ml: Pha long 10 ln dung dch 0,1mgF/ml. 3.4 Xy dng ng chun Cho dung dch florua 0,01mg/ml vi th tch tng dn vo cc bnh nh mc 100ml v ln lt cho thm cc thuc th nh trnh by trong bng di y: Bnh s Dung dch Dung dch florua tiu chun 0,01mg/ml, ml Nc ct, ml Dung dch m, ml Dung dch Alizarin sunfonat 90mg/l, ml Ziriconi clorua 0,001M, ml Florua tng ng, mg/l 1 0 89 5 5 1 0 2 0,5 88,5 5 5 1 0,05 3 1 88 5 5 1 0,10 4 1,5 87,5 5 5 1 0,15 5 2 87 5 5 1 0,2 6 3 86 5 5 1 0,3 7 4 85 5 5 1 0,4 8 5 84 5 5 1 0,5
Lc trn cn thn. Sau 20 pht o mt quang bc sng 530nm vi cuvet 5cm. Dng ng chun ph thuc gia hm lng Florua v mt quang. 3.5 Cch tin hnh 3.5.1 Chng ct Nu hm lng florua trong nc nh hn 0,4mg/l phi lm giu trc nh sau: Ly 200ml nc lc cho vo bt s, thm 2 git phenolphtalein, thm tng git natri hidroxit cho n khi mu ca dung dch chuyn sang hng, thm ba git na. un nh cho bay hi n khi cn khong 50ml, chuyn vo bnh ct B (Hnh 1). Nu hm lng florua ln hn 0,4mg/l, ta ly mt lng mu nc sao cho trong cha khong 0,01 0,1mgF vi th tch khng qu 100ml cho vo bnh ct B. Ln lt cho vo bnh ct B vi vin bt, 0,2g ct v nu mu c cha clorua thm 0,2 0,5g bc sunfat. Cho vo bnh 25ml axit sunfric 1:2. Trong bnh A, cho nc n 2/3 bnh, thm vo vi vin bt. un si bnh A. Hi nc t bnh A bc sang bnh B, un bnh B ct florua theo phng php li cun hi nc. Trong qu trnh ct phi theo di nhit nghim ngt m bo nhit bnh ct 138 1400C, tc ct khong 3-5ml/pht. Khi nc ngng 100ml th ngng ct. 3.5.2 Phng php xc nh
Ht mt lng mu sao cho lng florua nm trong khong 0,005 0,05mg. Thm nc ct n 70 80ml, ln lt thm 5ml dung dch m, 5ml dung dch Alizarin sunfonat v 1ml Ziriconi clorua. nh mc n vch, lc k. Sau 20 pht o mt quang ca dung dch bc sng 530nm, cuvet 5cm. C th tin hnh so mu bng mt vi dy tiu chun c chun b trong ng so mu dung tch 100ml nh mc 3.4. 3.6 Tnh kt qu Hm lng florua (X) biu din bng mg/l tnh theo cng thc: C * 1000 X= V Trong : C : hm lng florua tm c theo ng chun hoc thang mu tiu chun, tnh bng mg. V : th tch mu nc ly phn tch, tnh bng ml. Hnh 1 THIT B TRNG CT FLO BNG LI CUN HI NC