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TCVN 5779 : 1994

Sa bt v sa c c ng Phng php xc nh hm lng ch (Pb)

H Ni 1994

tcvn 5779 - 1994

Li ni u
TCVN 5779 - 1994 c bin son da trn tiu chun AOAC 1984 - 25 ... TCVN 5779 - 1994 do B mn Ho phn tch trng i hc Tng hp H ni bin son, Tng cc Tiu chun - o lng - Cht lng ngh v c B Khoa hc, Cng ngh v Mi trng ban hnh.

tcvn 5779 - 1994

T i u c h u n v i t n a m 5779 - 1994

TCVN

Sa bt v sa c c ng - Phng php xc nh hm lng ch (Pb)

Powdered milk and sweetened condensed milk. Method for determination of lead content.

Tiu chun ny qui nh phng php xc nh hm lng ch (Pb) trong sa bt v sa c c ng sau khi c v c ho mu theo TCVN 4622 - 1994.

Xc nh hm lng ch theo phng php von - ampe ho tan

(phng php trng ti)

1.1 Ni dung ca phng php: in phn lm giu Pb ln b mt in cc hot

ng (git Hg c nh hay mng Hg trn nn in cc than) ti mt in th m xc nh, trong nhng iu kin lp li, sau ho tan lng Pb c lm giu bng cch phn cc ant v ghi nh ho tan tng ng. 1.2 Dng c v ho cht. - My cc ph c h in cc git Hg c nh (hoc in cc rn dng a quay bng than thu tinh hoc than mm [paste cacbone]), in cc ph tr bng Pt, in cc so snh calomen hoc Ag/AgCl; - Nc ct hai ln theo TCVN 2117 - 77 hoc nc c tinh khit tng ng; - Bnh kh N2 (hoc CO2) c b lc; - Axit nitric HNO3 TKPT, d = 1,4g/ml; - Thu ngn clorua HgCl2 (hoc thu ngn nitrat Hg(NO3)2 TKPT, dung dch 0,01 M; - Axit clohydric HCL TKPT, dung dch 1M; - Dung dch Pb tiu chun:

tcvn 5779 - 1994

a) Dung dch gc cha 1 mg Pb/1ml; ho tan 1,5980 gam Pb(NO3)2 TKPT (hoc 1,8300 gam Pb (CH3COO)2.3H2O vo cc 100 ml, thm 10 ml dung dch HNO3 m c, thm nc ct n khong 50ml, lc cho tan ht, chuyn vo bnh nh mc 1000 ml, trng cc cn thn bng nc ct, thm nc n vch, lc u; b) Dung dch lm vic cha 10 g Pb/ml; ly 5 ml dung dch (a) vo bnh nh mc 500 ml, thm vi git dung dch HNO3 lc u, thm nc ct n vch, lc u. Dung dch ny dng trong ngy. 1.3 Cch tin hnh. 1.3.1 Phn tch theo ng chun. 1.3.1.1. Chun b cc dung dch. Ly ln lt vo 7 bnh nh mc dung tch 25 ml cc thnh phn dung dch sau y: 0,0; 0,1; 0,25; 0,5; 0,75 v 1 ml dung dch chun (b) (10 g/ml), trong bnh th 7 ly 10 ml dung dch mu phn tch, thm dung dch HCL 1 M n vch mc, lc u [ nu trong trng hp dng in cc mng Hg trn nn than th trc khi thm HCL, cho thm vo mi bnh 0,25 ml dung dch HgCl2 hoc Hg (NO3)2]. Trong trng hp hm lng Pb trong mu phn tch vt qu ng chun th gim bt th tch dung dch mu phn tch tng ng. 1.3.1.2. o von-ampe ho tan dung dch vo bnh in phn (ln lt t nng nh n nng ln), nu dng in cc gt Hg c nh th to git c ng knh 0,5 mm (theo cch hng dn ca mi loi in cc), t gi tr th in phn 0,7 vn (so vi in cc calomen bo ho). Sc kh N2 (hoc CO2) trong 5 pht (tng bt nh lin tc t di y bnh ln) sau ko ng dn kh ln trn b mt dung dch. Khuy dung dch vi mt tc khng i (sao cho khng to xoy nc). Bt chuyn mch sang pha in phn (hoc cc thao tc t ng theo chng trnh th khi ng chng trnh my tnh) in phn trong 120 giy, ngng khuy 30 giy ri phn cc ngc (v pha +) vi tc khong 6 - 20 mV/s (tu theo loi my cc ph qui nh) cho n 0,0 vn. nh gi nh ho tan ti gi tr - 450 mV 50 mV (cng c th lch cht t tu theo tng my). Trng ra bnh in phn, thay dung dch mi, ri lp li qu trnh vi nhng thng s hon ton ging nh trong ln o th nht (kch thc git Hg [ hoc nh bng li b mt in cc ], thi gian in phn ...). T cc gi tr chiu cao nh thu c, lp ng chun gia chiu cao nh ho tan v khi lng

tcvn 5779 - 1994

Pb (g) trong dung dch. T cc gi tr nhn c, suy ra khi lng Pb trong dung dch mu phn tch (g). 1.3.2. Phn tch theo phng php thm tiu chun Ly vo bnh nh mc 10 ml dung dch phn tch ri thc hin o nh phn trn ni khi o vi dung dch phn tch, ngay sau khi o xong chun b li in cc nh mt ln o mi nhng khng thay dung dch m thm vo dung dch phn tch mt lng chnh xc dung dch chun (b) cha khong 2 g Pb (tu theo lng Pb c trong mu) ri thc hin o vn-ampe nh ln o vi dung dch phn tch. T hai chiu cao nh (hoc hai in lng ho tan) tnh khi lng Pb c trong mu phn tch. 1.3.3 Tnh ton v x l kt qu: Hm lng Pb trong mu (X) c tnh theo mg/kg, theo cng thc sau y:

X=

m1 x 2,5 m

trong : m1 - khi lng Pb trong mu phn tch, g m - khi lng sa v c ho; g (v d 25 g). Kt qu phn tch c chp nhn khi thc hin 3 php phn tch song song trong cng iu kin cho sai lch tng i khng vt qu 25%.

Xc nh hm lng ch bng phng php quang ph hp th

nguyn t sau khi chit

2.1 Ni dung phng php Ch trong mu sa sau khi v c ho theo tiu chun TCVN 4662 - 1994 c chit bng amoni 1-pyrrolidinecarbodithiolate (APDC) vi dung mi butylaxetat (BuOAc) hoc metylizobutylxton (MIBX) ri phun dch hu c ny vo ngn la n C2H2 - khng kh, o cng hp th bng n catot rng Pb ti vch ph Pb-217 nm (vch 1) hoc Pb-283,3 nm (vch 2). 2.2 My mc v dng c

tcvn 5779 - 1994

- My quang ph hp th nguyn t v ph kin c n catot rng Pb; - Phu chit c nt thu tinh dung tch 100 ml; - My li tm c th cha cuvet 15 ml, vng quay 2000 v/pht. 2.3 Ho cht - Ch dn chung: Cc ho cht phi tho mn yu cu tinh khit quang ph, trong trng hp cn thit phi tinh ch li hoc phn tch mu trng hiu chnh. - Amoni 1 - pyrrolidinecarbodithiolate (APDC) 2%. Ho tan 2,0 gam thuc th trong 100 ml nc ct, tinh ch bng cch chit 1 - 2 ln mi ln 5 ml MIBX hoc BuOAc; - Butylaxetat ct li (BuOAc); - Metylizobutylxeton (MIBX); - m focmiat c pH = 3 : trung ho cn thn dung dch HCOOH 0,1 M bng dung dch NaOH 0,1 M n pH = 3 (in cc ch th thu tinh); - Bromocresol lc, dung dch 0,1%, ho tan 0,100 gam mui Na ca Bromocresol lc trong 100 ml nc ct, thuc th c phm vi chuyn mu t pH 3,8 - 5,4 (vng sang xanh); - Amoni hydroxit NH4OH, dung dch m c v 1:1; - Axit xitric, dung dch 20%; - Magi clorua MgCl2, dung dch 50 g/l; - Dung dch chun Pb: xem mc 1.2 (Phng php 1). 2.4 Chit cc dung dch chun v dung dch mu phn tch. Ly vo 6 phu chit ln lt cc dung dch cc cht sau y: cc phu t s 1 n 5 ln lt 0,0; 0,1; 0,2; 0,4 v 0,6 ml dung dch chun 10 g Pb/ml; phu s 6 ly 10 ml dung dch mu phn tch (nu hm lng Pb ln qu ng chun th th tch dung dch phn tch c th ly t hn), thm vo cc phu 2 ml dung dch MgCl2, thm nc ct cho th tch 25 ml. ri c th chit theo mt trong hai cch sau y: 2.4.1 Chit bng dung mi MIBX: thm vo mi phu chit 5 ml dung dch m

focmiat (ring trong dung dch phn tch trc khi thm dung dch m th trung ho bng tng git dung dch NH3 1:1 theo giy ch th n pH khong xp x 3), 5 ml 6

tcvn 5779 - 1994

dung dch APDC, lc u, sau thm 25 ml MIBX, lc mnh trong 5 pht, yn trong 5 pht cho phn lp, tch ly phn dung mi hu c vo cc bnh c nh s tng ng, y nt kn. 2.4.2 Chit bng butylaxetat (BuOAc) : thm vo mi bnh 5 ml axit xitric, 2 - 3 git

ch th bromocresol lc, iu chnh pH n 5,4 bng dung dch NH4OH 1:1 (n khi dung dch c mu xanh), thm 5 ml dung dch APDC, lc u, thm tip 10ml butylaxetat ri lc mnh khong 2 pht, yn cho tch lp hon ton. Nu lp dung mi hu c vn c th tch ly n vo ng nghim li tm c dung tch khong 15 ml, bt bng giy nhm hoc cht do n hi ri em li tm 2000 v/pht trong khong 1 pht, tch ly cc phn hu c vo cc l tng ng c nt kn. 2.5 o ph hp th. Thit lp cc ch ti u ca my o vch Pb - 217 hoc Pb - 283, 3 nm theo cc ti liu hng dn k thut ca tng hng. V d cc thng s sau y i vi my Philipe Pey Unicame SP9/800: - Vch: Pb - 217 nm; - Khe o: 0,5 nm; - Cng n: 80% gi tr cc i; - Chiu cao ngn la (burner): 4,5 mm; - Tc dn mu: 5 ml/pht; - Kh t: Khng kh: 4,2 lt/ pht; axetylen: 1:1 lt/pht; Cho my chy khng ti 20 - 30 pht t cn bng nhit v n nh. t ng nn (im khng ca tn hiu) bng cch t dung mi BuOAc hoc MIBX bo ho nc. o ph ln lt t nng thp n nng cao, dung dch mu phn tch o sau cng, mi mu o 3 - 5 ln ly gi tr trung bnh, ra h thng dn t sau mi ln o bng nc bo ho dung mi. T kt qu thu c v s ph thuc khi lng Pb trong dch chit - s ch ca my (A hoc D), t suy ra khi lng Pb c trong mu phn tch (g). 7

tcvn 5779 - 1994

2.6 Tnh ton v x l kt qu. Hm lng Pb trong sa (X) c tnh theo mg/kg, theo cng thc:

X=

m1 x 2,5 m

Trong : m1 - khi lng Pb c trong dung dch phn tch, g m - khi lng mu sa ly v c ho, g. Kt qu phn tch c chp nhn khi thc hin 3 php phn tch song song trong cng iu kin cho sai lch tng i khng vt qu 25%.

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