GLYCERIN

Glycerinum

Glycerol

CH2OH

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CHOH

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CH2OH

C3H8O3 P.t.l: 92,1

Glycerin la propan 1,2,3-triol, phai cha t 98,0 en 101,0% C3H8O3, tnh theo che pham khan.

Tnh chat

Chat long sanh, trong suot, khong mau, khong mui, v nong va ngot, hut am manh.

Tron lan c vi nc va ethanol 96%, kho tan trong aceton, thc te khong tan trong benzen, cloroform, dau beo, ether, ether dau hoa, tinh dau.

nh tnh

Co the chon mot trong hai nhom nh tnh sau:

Nhom I: A, D.

Nhom II: B, C, D.

A. Lay 5 ml che pham, them vao 1 ml nc, tron can than. Pho hong ngoai (Phu luc 4.2) cua dung dch tren phai phu hp vi pho hong ngoai oi chieu cua glycerin 85%.

B. Tron 1 ml che pham vi 0,5 ml acid nitric (TT) va them 0,5 ml dung dch kali dicromat 10%, mot vong xanh lam xuat hien be mat phan cach gia hai lp. e yen 10 phut, vong xanh khong phan tan vao lp ben di.

C. un nong 1 ml che pham vi 2 g kali hydrosulfat (TT) trong mot a e lam bay hi, hi nay co mui hac, lam chay nc mat va lam en giay tam dung dch kali iodomercurat kiem (TT).

D. Che pham phai ap ng phep th ch so khuc xa.

o trong va mau sac cua dung dch

Dung dch S: Pha loang 100,0 g che pham thanh 200 ml bang nc khong co carbon dioxyd (TT).

Dung dch S phai trong (Phu luc 9.2).

Pha loang 10 ml dung dch S thanh 25 ml bang nc, dung dch thu c phai khong mau (Phu luc 9.3, phng phap 2).

Gii han acid kiem

Lay 50 ml dung dch S, them 0,5 ml dung dch phenolphtalein (TT), dung dch khong mau. Them dung dch natri hydroxyd 0,1 N (TT) cho en khi co mau hong. Lng dung dch natri hydroxyd 0,1 N (C) dung khong c qua 0,2 ml. Gi lai dung dch sau cung nay cho phep th ester.

Ch so khuc xa

1,470 - 1,475 (Phu luc 6.1).

Clorid

Khong c qua 10 phan trieu (Phu luc 9.4.5).

Lay 1,0 ml dung dch S pha loang thanh 15 ml bang nc va tien hanh th. Dung 1 ml dung dch clorid mau 5 phan trieu (TT) pha loang thanh 15 ml bang nc e chuan b mau oi chieu.

Kim loai nang

Khong c qua 5 phan trieu (Phu luc 9.4.8).

Pha loang 6 ml dung dch S thanh 15 ml bang nc. Lay 12 ml dung dch thu c th theo phng phap 1. Dung dung dch ch mau 1 phan trieu (TT) e chuan b mau oi chieu.

Aldehyd

Khong c qua 10 phan trieu.

Lay 7,5 ml dung dch S cho vao bnh nut mai, them 7,5 ml nc va 1,0 ml dung dch pararosanilin a kh mau (TT). ay nap va e yen trong mot gi nhiet o 25 0,1oC. o hap thu (Phu luc 4.1) cua dung dch nay o bc song 552 nm khong c ln hn o hap thu cua mau oi chieu c tien hanh trong cung ieu kien va cung thi gian bang cach dung 7,5 ml dung dch formaldehyd chuan (co cha 5 phan trieu CH2O) thay cho dung dch S. Ket qua ch co gia tr khi mau oi chieu co mau hong.

Ester

Them 10,0 ml dung dch natri hydroxyd 0,1 M (C) vao dung dch sau cung cua phep th gii han acid - kiem. un soi hoi lu trong 5 phut. Lam lanh. Them 0,5 ml dung dch phenolphtalein (TT). Chuan o bang dung dch acid hydrocloric 0,1 N (C). Lng dung dch acid hydrocloric 0,1 N (C) a dung khong di 8,0 ml.

ng

Lay 10 ml dung dch S, them 1 ml dung dch acid sulfuric 1 M (TT), un nong tren cach thuy 5 phut. Them vao 3 ml dung dch natri hydroxyd 2 M (khong co carbonat) (TT). Tron eu va them tng giot 1 ml dung dch ong (II) sulfat 12,5% (TT) mi pha. Dung dch phai co mau xanh lam va trong. Tiep tuc un tren cach thuy trong 5 phut. Mau cua dung dch van phai xanh va khong c co tua tao thanh.

Diethylen glycol va tap chat lien quan

Xac nh bang phng phap sac ky kh (Phu luc 5.2)

Dung dch th: Pha loang 10,0 ml dung dch S thanh 100,0 ml bang nc.

Dung dch oi chieu (1): Hoa tan 1,000 g diethylen glycol (TT) trong nc va pha loang thanh 100,0 ml vi cung dung moi.

Dung dch oi chieu (2): Pha loang 1,0 ml dung dch oi chieu (1) thanh 10,0 ml bang dung dch th. Pha loang 1,0 ml dung dch nay thanh 20,0 ml bang dung dch th.

Dung dch oi chieu (3): Tron 1,0 ml dung dch th va 5,0 ml dung dch oi chieu (1) va pha loang thanh 100,0 ml bang nc. Pha loang 1,0 ml dung dch nay thanh 10,0 ml bang nc.

Dung dch oi chieu (4): Pha loang 5,0 ml dung dch oi chieu (1) thanh 100,0 ml bang nc.

ieu kien sac ky:

Cot: 30 m x 0,53 mm, pha tĩnh la polycyanopropylphenyl siloxan 6% va polydimethylsiloxan 94%.

Kh mang: Heli dung cho sac ky kh vi lu lng 38 cm/giay.

Ty le chia dong: 10/1 .

Nhiet o:

 

Thi gian (phut)

Nhiet o (oC)

Cot

0

100

 

0 - 16

100 220

 

16 - 20

220

Buong tiem mau

 

220

Detector

 

250

Detector ion hoa ngon la

The tch tiem: 0,5 l

Th t ra giai: Diethylen glycol, glycerol

Cach tien hanh:

Tiem dung dch oi chieu (3):

Phep th ch co gia tr khi o phan giai gia diethylen glycol va glycerol t nhat la 7,0

Dien tch pic cua diethylen glycol khong c ln hn 0,5 lan dien tch cua pic tng ng trong sac ky o cua dung dch oi chieu (2) (0,1%).

Dien tch cua cac pic phu co thi gian lu nho hn thi gian lu cua glycerol khong ln hn 0,5 lan dien tch pic tng ng vi diethylen glycol trong sac ky o cua dung dch oi chieu (2) (0,1%).

Tong dien tch cua cac pic co thi gian lu ln hn thi gian lu cua glycerol khong ln hn 2,5 lan dien tch pic tng ng vi diethylen glycol trong sac ky o cua dung dch oi chieu (2) (0,5%).

Bo qua cac pic co dien tch nho hn 0,05 lan dien tch cua pic tng ng vi diethylen glycol trong sac ky o cua dung dch oi chieu (4) (0,05%)

Cac hp chat halogen

Khong c qua 35 phan trieu.

Lay 10 ml dung dch S cho vao coc thuy tinh 50 ml, them 1 ml dung dch natri hydroxyd 2 M (TT), 5 ml nc va 50 mg hp kim nhom nickel khong co halogen (TT). un tren cach thuy trong 10 phut, lam lanh va loc. Ra coc va pheu loc vi nc cho en khi thu c 25 ml dch loc.

Lay 5 ml dch loc, them 4 ml ethanol 96% (TT), 2,5 ml nc, 0,5 ml acid nitric (TT) va 0,05 ml dung dch bac nitrat 1,7% (TT), khuay eu. e yen trong 2 phut. Dung dch khong c uc hn dung dch oi chieu c chuan b trong cung ieu kien va cung thi gian.

Dung dch oi chieu: Lay 7,0 ml dung dch clorid mau 5 phan trieu (TT), them 4 ml ethanol 96% (TT), 0,5 ml nc, 0,5 ml acid nitric (TT) va 0,05 ml dung dch bac nitrat 1,7% (TT).

Nc

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

Dung 1,000 g che pham.

Tro sulfat

Khong c qua 0,01% (Phu luc 9.9, phng phap 2).

Dung 5,0 g che pham.

nh lng

Hoa tan 0,100 g che pham trong 45 ml nc. Them chnh xac 25,0 ml dung dch natri periodat 2,14% (TT). e yen cho toi 15 phut, them 5,0 ml dung dch ethan-1,2-diol 50% trong nc (TT). e yen cho toi 20 phut va chuan o bang dung dch natri hydroxyd 0,1 M (C), dung 0,5 ml dung dch phenolphtalein (TT) lam ch th. Song song tien hanh lam mau trang.

1 ml dung dch natri hydroxyd 0,1 M (C) tng ng vi 9,21 mg C3H8O3.

Bao quan

Trong lo kn, tranh anh sang.

Loại thuốc

Nhuan trang, hut am, dung moi hoa tan, ta dc.

Che pham

Dung dch thut trc trang, vien at hau mon.