DIETHYL PHTALAT

Diethylis phthalas

 

 

 

 

 

C12H14O4 P.t.l: 222,2

Diethyl phtalat la diethyl benzen-1,2-dicarboxylat, phai cha t 99,0 en 101,0% kl/kl C12H14O4.

Tnh chat

Chat long sanh, trong suot, khong mau hoac co mau vang rat nhat. Thc te khong tan trong nc, hoa lan vi ethanol 96% va vi ether.

nh tnh

Co the chon 1 trong 2 nhom nh tnh sau:

Nhom I: B, C.

Nhom II: A, D, E.

A. Ty trong tng oi: t 1,117 en 1,121 (Phụ lục 6.5)

B. Ch so khuc xa: t 1,500 en 1,505 (Phụ lục 6.1).

C. Pho hong ngoai (Phu luc 4.2) cua che pham phai phu hp vi pho hong ngoại cua diethyl phtalat chuan (C), dung ky thuat phim mong.

D. Phng phap sac ky lp mong (Phu luc 5.4)

Ban mong: Silica gel GF 254 (TT)

Dung moi khai trien: Heptan ether (30 : 70)

Dung dch th: Hoa tan 50 mg che pham trong ether (TT) va pha loang thanh 10 ml vi cung dung moi.

Dung dch oi chieu: Hoa tan 50 mg diethylphtalat chuan (C) trong ether (TT) va pha loang thanh 10 ml vi cung dung moi.

Cach tien hanh: Cham rieng biet len ban mong 10 ml moi dung dch tren. Trien khai sac ky en khi dung moi i c 15 cm. Lay ban mong ra e kho ngoai khong kh roi quan sat di anh sang t ngoai bc song 254 nm. Vet chnh thu c t sac ky o cua dung dch th phai giong về vị tr v kch thước vi vet chnh thu c t sac ky o cua dung dch oi chieu.

E. Lay khoang 0,1 ml che pham, them 0,25 ml acid sulfuric (TT) va 50 mg resorcinol (TT). un tren cach thuy trong 5 phut. e nguoi, them 10 ml nc va 1 ml dung dch natri hydroxyd 42% (TT). Dung dch tr nen vang hoac vang nau va co huynh quang xanh luc.

o trong va mau sac cua dung dch

Che pham phai trong (Phu luc 9.2) va khong c co mau am hn mau mau V6 (Phu luc 9.3 phng phap 2).

Gii han acid

Hoa tan 20,0 g che pham trong 50 ml ethanol 96% (TT) a c trung hoa trc vi dung dch phenolphtalein (TT). Nho dung dch natri hydroxyd 0,1 N (C) ti khi xuat hien lai mau hong. Lng dung dch natri hydroxyd 0,1 N (C) tieu thu khong c qua 0,1 ml.

 

Tap chat lien quan

Xac nh bang phng phap sac ky kh (Phu luc 5.2), dung naphtalen (TT) lam chuan noi.

Dung dch chuan noi: Hoa tan 60 mg naphtalen (TT) trong methylen clorid (TT) va pha loang thanh 20, 0 ml vi cung dung moi.

Dung dch th (1): Hoa tan 1,0 g che pham trong methylen clorid (TT) va pha loang thanh 20,0 ml vi cung dung moi.

Dung dch th (2): Hoa tan 1,0 g che pham trong methylen clorid (TT), them 2,0 ml dung dch chuan noi va va pha loang thanh thanh 20, 0 ml bang methylen clorid (TT).

Dung dch oi chieu: Lay 1,0 ml dung dch th (1), them 10,0 ml dung dch chuan noi va va pha loang thanh 100,0 ml bang methylen clorid (TT).

ieu kien sac ky:

Cot thuy tinh co chieu dai 2 m va ng knh trong 2 mm, c nhoi diatomaceous earth a silan hoa dung cho sac ky kh (TT) (150 mm en 180 mm) c tam 3% (kl/kl) polymethyl phenylsiloxan (TT).

Kh mang la nit dung cho sac ky (TT) co lu lng 30 ml/phut.

Detector ion hoa ngon la.

Gi nhiet o cua cot 150 oC, nhiet o cua buong tiem mau va detector 225 oC.

Cach tien hanh: Tiem 1 ml dung dch oi chieu. Cac chat c ra giai theo th t nh sau: naphtalen va diethylphtalat. ieu chnh o nhay cua detector sao cho chieu cao cua pic naphtalen khong c nho hn 50% thang o. Phep th ch co gia tr khi o phan giai gia cac pic naphtalen va diethyl phtalat t nhat la 10.

Tiem 1 ml dung dch th (1). Tren sac ky o thu c khong co pic co thi gian lu bang thi gian lu cua chuan noi.

Tiem rieng biet 1 ml dung dch th (2) va 1 ml dung dch oi chieu. Tien hanh sac ky dung dch th trong thi gian gap 3 lan thi gian lu cua diethylphtalat. T sac ky o cua dung dch oi chieu, tnh ty le (R) gia dien tch pic cua diethyphtalat va dien tch pic cua chuan noi. T sac ky o cua dung dch th (2), tnh ty le gia tong dien tch cua cac pic phu khac vi pic chnh, pic chuan noi va pic dung moi, vi dien tch pic cua chuan noi, ty le nay khong c ln hn R (1,0 %).

Nc

Khong c qua 0,2% (Phu luc 10.3).

Dung 5,0 g che pham.

Tro sulfat

Khong c qua 0,1% (Phu luc 9.9, phng phap 2).

Dung 1,0 g che pham.

nh lng

Can 0,750 g che pham vao bnh thuy tinh dung tch 250 ml. Them 25,0 ml dung dch kali hydroxyd 0,5 N trong ethanol (C) va vai vien a bot. un soi tren cach thuy di sinh han ngc trong 1 gi. Them 1 ml dung dch phenolphtalein (TT) va chuan o ngay bang dung dch acid hydrocloric 0,5 N (C).

Song song lam mau trang.

1 ml dung dch kali hydroxyd 0,5 N trong ethanol (C) tng ng vi 55,56 mg C12H14O4.

Bao quan

ng trong lo kn, e ni kho mat.

Loi thuc

Tr ghe, nga.

Che pham

Thuoc m DEP.