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Tiu
chun
Vit
Na
H Ni 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.
T i u c h u n v i t n a m 5779 - 1994
TCVN
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.
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:
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%.
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
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
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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