PHU GIA TRONG THIT BO ~ PHUONG PHAP QUANG PHO Preservatives in Beef Spectrophotometric Method
1 Phm vi p dng Tiu chun ny duoc p dung d xc dinh hm luong cc cht phu gia: benzoate, sorbate v sulphit trong thit b. 2 Nguyn tc Chit cc cht phu gia c trong thit bng nuoc ct. 2.1 Phn tch sulphit Sulphit c trong dung dich chit phan ung voi thuc thu p-rosanilin trong HCl v HCHO tao phuc mu hng tm v duoc dinh luong bng phuong php so mu o buoc sng 560 nm. Phan ung xay ra nhu sau: 2 NaCl + HgCl 2 = 2Na + + [HgCl 4 ] 2-
SO 2 + [HgCl 4 ] 2- + H 2 O = [HgCl 2 SO 3 ] 2- + 2H + + 2Cl -
[HgCl 2 SO 3 ] 2- + HCHO + 2H + = HO-CH 2 -SO 3 H + HgCl 2 HO-CH 2 -SO 3 H + C 19 H 18 N 3 Cl
+ HCl = axit Pararosanilin Metylsulfonic (Pararosanilin) (mu do tm) 2.2 Phn tch benzoate, sorbate Chit sorbate, benzoate c trong dung dich chit mu d duoc axt ha bng diethyl ete. Lop dietyl ete sau khi chit duoc do o : - Buoc sng 225 nm d phn tch benzoate - Buoc sng 250 nm d phn tch sorbate 3 Thit b|, dng c, ha cht, dung d|ch a. Thit b, dng c - My quang ph phn tu UV-VIS (190 -1100 nm) - Cn phn tch, d chnh xc 0,1 mg. trang 2/4 - Pipt bu, pipet vach cc loai - Bnh dinh muc dung tch 50mL, 100mL, ... - Dung cu thuy tinh thng dung: erlen, becher, phu loc, ... b. Ha cht Ho cht phai l loai tinh khit duoc su dung d phn tch, gom: - p-rosanilin. - Thuy ngn clorua (HgCl 2 ) - NaCl - Formaldehyde (HCHO) - Axit clohydric dm dc - Dietyl ete c. Cht chun: - Natrisulphit - Kali sorbate - Natri benzoate d. Dung dch th v dung dch chun - Thuc thu p-rosanilin: chuyn 100mg p-rosanilin vo bnh dinh muc 1000 mL, thm vo bnh dinh muc 200 mL nuoc ct v 160 mL HCl (1:1). dinh muc dn vach bng nuoc ct. - Dung dich HCl (1:1): cho tu tu 100 mL HCl dm dc vo 100 mL nuoc ct - Dung dich [HgCl 4 ] 2- : ha tan 4,7 g NaCl v 10,9 g HgCl 2 trong 1900 mL H 2 O, dinh muc 2000 mL bng nuoc ct. - Dung dich chun Natri sulphite 1000mg/L: ha tan 100 mg cht chun Na 2 SO 3
trong 100mL H 2 O. - Dung dich formaldehyde 15 mg/100 mL: pha long 2 ml HCHO thnh 100 mL bng H 2 O. Rt 2 ml dung dich ny pha long thnh 100 mL bng H 2 O. 4 Xy dng dy chun 4.1 Dy chun sulphit - Dung dich chun Natri sulphite 1000mg/L: ha tan 100 mg cht chun Na 2 SO 3
trang 3/4 trong 100mL H 2 O. - Chun bi cc bnh dinh muc c nt dy, dung tch 50 mL. Dnh s thu tu cho mi bnh. Cho ln luot vo mi bnh ln luot cc cht theo bang sau: Dung dich 0 1 2 3 4 5 Dung dich chun 1000 mg/L 0 0.5 1 1.5 2 3 Dinh muc dn vach 50 ml bng H 2 O ct. Lc du Nng d Natri sulphit tuong ung, mg/L 0 10 20 30 40 50 Ly chnh xc 1 mL mi dung dich trn cho vo cc ng nghim ring bit Dung dich [HgCl 4 ] 2- 5 mL Dung dich p-rosanilin 2.5 mL Dung dich HCHO 1 mL D yn 30 pht ri do o buoc sng 560 nm. 4.2 Dy chun sorbate v benzoate Dung dich 0 1 2 3 4 5 Dung dich chun 1000 mg/L 0 0,5 1 1.5 2 3 Nng d chun tuong ung, mg/L 0 5 10 15 20 30 Dinh muc dn vach 50 mL bng H 2 O Rt chnh xc 5 mL mi dung dich trn cho vo cc bnh dinh muc 50 mL khc + 0,5 mL HCl (1:1). Dinh muc dn vach bng dietyl ete, lc manh 1 pht. Rt ly lop dung dich pha trn do.
5. Phn tch mu - Cn khoang 10g mu d duoc dng nht vo ng ly tm 50 mL. Thm khoang 40 mL nuoc vo ng, lc du 2 pht. D yn 10 pht. Ly tm ly phn trong. Dinh muc dung dich thu duoc thnh 50 mL. - Phn tch Natri sulphit: Rt 1 mL dung dich trn cho vo ng nghim 10 mL, thm tip 5 mL dung dich [HgCl 4 ] 2- , 2.5 mL dung dich thuc thu v 1mL dung dich HCHO, d yn 30 pht ri do tai buoc sng 560 nm. trang 4/4 - Phn tch sorbat, benzoat: Rt 5mL dung dich mu thu duoc o trn cho vo bnh dinh muc 50 ml. t hnh tuong tu nhu chun. 6 Tnh kt qua - Dng phn mm Excel dung duong chun biu thi mi quan h giua d hp thu (Abs) v nng d cc chun cua cht phn tch - Tnh ton h s tuong quan hi quy tuyn tnh (R 2 ) - Tnh nng d cht phn tch trong dung dich thng qua duong chun xy dung o buoc trn. - Nu mu c gi tri do duoc cao hon cc tri s cua cc dung dich chun, phai pha long mu bng dung dich Blank. - Hm luong cht phn tch c trong mu duoc tnh theo cng thuc sau: f m V C kg mg X dm
= 0 ) / ( Trong d: - C 0 : nng d cht phn tch tnh tu duong chun, mg/L - V dm : th tch dinh muc mu, mL - m: khi luong mu phn tch, g - f: h s pha long (nu c)