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Nguyn tc : Dung dch chun iod 0,1N c pha t ha cht iod v Kali iodid. Xc nh h s hiu chnh K bng dung dch chun Na2S2O3 (k = 1,000): I2 + 2Na2S2O3 2 NaI + Na2S2O4 H s hiu chnh K ca dung dch Iod 0,1N : K = V0K0/V K : h s hiu chnh phi tm. V0 : th tch dung dch Na2S2O3 tiu th K0 : H s hiu chnh ca dung dch Na2S2O3 V : th tch dung dch Iod 0,1N dng. 2. Ha cht : - Dung dch chun Na2S2O3 0,1N - Iod - Kali iodid - Dung dch h tinh bt 1% 3. Dng c : - 1 bnh nh mc 250ml - 3 bnh nn nt mi 100ml - 1 cc c m 250ml - 2 cc c m 100ml - Phu thy tinh - Burette v gi - 1 pipet bu 25ml - 3 pipet vch 5ml, 10ml - a thy tinh - 1 ng ong 50ml 4. Cch tin hnh : Cn 3,25g Iod tinh th, sau cn tip 5,00g Kali Iodid trong mt cc c m 250ml. Thm 30ml nc v khuy trong t ht cho n khi tan hon ton. Thm khong 100ml nc v lc qua phu c bng ht nc vo bnh nh mc 250ml. Trng cc bng 50ml nc ct v lc tip vo bnh nh mc ny. Thm nc n vch, y nt, lc u. Ly ng 25,0ml dung dch Iod va pha, cho vo bnh nn c nt mi, thm 30ml nc v chun bng dung dch Na2S2O3 0,1N cho n khi c mu vng nht, thm 2ml dung dch h tinh bt v chun tip cho n khi mt mu. Nu k > 1,000 ta tnh c lng nc cn thm vo theo cng thc : (k1)V, vi V l th tch ca dung dch chun cn phi hiu chnh c k=1,000. Sau khi thm nc hiu chnh, chun li nh trn xc nh li h s K.
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7. Amoni : Khng c qu 20ppm. Ly 10ml dung dch S, pha long thnh 15ml, ri tin hnh th. - ng th : thm vo ng nghim cha 15ml dung dch trn 0,3ml thuc th Nessler, lc u, yn 5 pht. - ng mu : ly chnh xc 10ml dung dch Amoni mu 1ppm, pha long thnh 15ml, thm 0,3ml thuc th Nessler, lc u, yn 5 pht. So snh mu to thnh trong 2 ng th v ng mu. * Pha dung dch Amoni mu 1ppm : Ht 1ml dung dch Amoni mu 100ppm cho vo bnh nh mc 100ml, thm nc n vch, lc u ta c dung dch Amoni mu 1ppm. 8. Calci : Khng c qu 0,01%. Thm HCl (TT) vo hn dch cha 1g ch phm trong 10ml nc cho n khi trung tnh v pha long vi nc thnh 15ml v tin hnh th. - ng th : thm 1ml amoni oxalat 4% vo 0,2ml dung dch Calci mu 100ppm trong ethanol 96%, sau 1 pht, thm vo hn hp gm 1ml CH 3COOH 2M v 10ml Calci mu 10ppm, thm tip 5ml nc. Lc u, yn 15 pht. * Dung dch Calci mu 100ppm trong ethanol 96% : ly 1ml dung dch Calci mu 100ppm, cho vo 9ml ethanol 96%, nh mc thnh 10ml. * Dung dch Calci mu 10ppm : ly 1ml dung dch Calci mu 1000ppm cho vo bnh nh mc 100ml, thm nc n vch, trn u. 9. St : Khng c qu 20ppm. Ha tan 0,5g ch phm trong 5ml HCl long, pha long thnh 10ml vi nc v tin hnh th. 10. Kim loi nng : Khng c qu 10ppm. Ha tan 2,0g ch phm trong hn hp gm 2ml HCl v 18ml nc. Ly 12ml dung dch ny v tin hnh th. 11. nh lng : Natri hydrocarbonat phi cha t 99,0 n 101,0% NaHCO3 . Ha tan 1,500g ch phm trong 50ml nc khng c CO 2 . Chun bng dung dch acid hydroclorid 1M, dng 0,2ml da cam methyl lm ch th. 1ml HCl 0,1M tng ng vi 84,0mg NaHCO3 . Cch tnh : n(ml)* K * 84,0(mg) * 100 C% = P vi : K l h s hiu chnh P l khi lng bt cn nh lng (mg).
Bi 3 : PYRIDOXIN HYDROCLORID
1. Tnh cht : Bt kt tinh trng hay gn nh trng, chy 250C km theo phn hy. D tan trong nc, kh tan trong ethanol 96%, thc t khng tan trong cloroform v ether. 2. nh tnh : a. Ph hp th nh sng t ngoi ca dung dch 0,001% trong acid hydroclorid 0,1M c 1 cc i khong 288-290nm bc sng cc i ny t 420-445. b. Ha tan 0,1g ch phm trong 10ml nc, ha bng 0,5ml acid nitric 2M, thm 0,4ml dung dch bc nitrat 2%, lc u to thnh ta trng ln nhn. 3. trong v mu sc dung dch : Dung dch S : Ha tan 2,50g ch phm trong nc khng c carbon dioxyd c 50ml, dung dch S phi trong v khng c c mu m hn mu mu V7. - Ha tan 46g st III clorid trong acid hydroclorid (25ml HCl + 975ml nc) 1000ml. - Ha tan 60g CoCl2 (Cobalt Clorid) trong dung mi A (25ml HCl + 975ml nc) 1000ml. Ly 24ml mu vng + 6ml mu + 70ml HCl 1% Sau ly 2,5ml hn hp trn + 97,5ml HCl 1% dung dch V7. 4. pH : ca dung dch S t 2,4 n 3,0 5. Kim loi nng : Khng c qu 20ppm Ly 12ml dung dch S th theo phng php 1 Dng dung dch ch mu 1ppm chun b mu i chiu 6. Mt khi lng do lm kh : Khng c qu 0,05% (1g, 100 - 105C) 7. nh lng : Ha tan 0,15g ch phm trong hn hp gm 5ml acid acetic khan (TT) v 6ml dung dch thy ngn II acetat (TT). Chun bng dung dch acid perclorid 0,1M, dng 0,05ml dung dch tm tinh th (CT) lm ch th cho n khi dung dch c mu xanh lc. 1ml dung dch acid perclorid 0,1M tng ng vi 20,56mg C8H11NO3.HCl Pyridoxin hydroclorid phi cha t 99,0- 101,0% C8H11NO3.HCl tnh theo ch phm lm kh.
dung tch 100ml, thm 20ml nc ha tan. Chun bng dung dch Iod 0,1N cho n khi xut hin mu xanh bn vng trong 30 giy ( ch th H tinh bt 1% ) 1ml dung dch Iod 0,1N tng ng vi 8,806mg Vitamin C Tnh kt qu : N(ml)* K* 8,806(mg)*M(mg) C% = P(mg)*500(mg) Vin bao phim Vitamin C phi cha t 95,0 n 110% hm lng ghi trn nhn.
1ml dung dch Kali iodat 0,1N tng ng 8,806mg C6H8O6 Cch tnh kt qu: n(ml) * K * 8,806mg * 100 C% = V(ml) * a V : Th tch ch phm ly nh lng A : Nng ch phm (mg/ml).
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- ng mu : Cho vo ng nghim 10ml dung dch ch mu 1ppm v 2ml dung dch S, thm 2ml dung dch m acetat pH = 3,5, ri 1,2ml thuc th Thioacetamid, lc u, yn 2 pht. * Pha dung dch ch mu 1ppm : - Ly 1ml dung dch ch mu 1000ppm, thm 9ml nc, th tch cui l 10ml. - Ly 1ml dung dch mi pha cho vo bnh nh mc 100ml, thm nc n vch. Ta c dung dch ch mu 1ppm. g. St : Khng c qu 20ppm. - ng th : Ly 5ml dung dch S, thm 5ml nc trong ng Nessler, thm 2ml dung dch acid citric 20% v 0,1ml acid mercaptoacetic, lc u, kim ha bng dung dch amoniac 10M v pha long vi nc n 20ml. - ng chun : Cho vo ng Nessler 10ml dung dch st mu 1ppm, 2ml acid citric 20%, thm tip 0,1ml acid mercaptoacetic (TT), kim ha bng dung dch amoniac 10M v pha long vi nc n 20ml. yn 5 pht ri so snh mu to gia ng chun vi ng th. - Pha dung dch st 1ppm : Ly 0,5ml dung dch st mu 200ppm v pha long trong bnh nh mc 100ml bng nc ct ti vch. h. Mt khi lng do lm kh : T 48,0 n 52,0%. Sy 0,500g nguyn liu 110 120OC trong 1gi, sau 400OC. i. nh lng : Magnesi sulfat phi cha t 99,0 n 100,5% MgSO4 tnh theo ch phm lm kh. Ha tan 0,45g ch phm trong 100ml nc, thm 10ml dung dch m Amoniac (pH = 10) v thm khong 50mg hn hp ch th Ericrom en T. Lc u, un nng dung dch n 40OC v chun nhit bng dung dch Trilon B 0,1M cho n khi mu tm chuyn sang mu xanh lam. 1ml dung dch Trilon B 0,1M tng ng vi 12,04mg MgSO4.
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- Tin hnh : Dung dch th, cn 1 khi lng bt vin tng ng 0,1g Amoxicilin vo bnh nh mc 100ml, thm nc ct khong 60ml v lc cho tan hon ton, thm nc n vch, trn u. Lc, b khong 20ml dch lc u. - Ly chnh xc 2,0ml dch lc cho vo bnh nt mi dung tch 100ml, thm 2,0ml dung dch NaOH 1N, lc u yn 15 pht. Chun Iod tha bng dung dch Natri Thiosulfat 0,01N cho n khi mt mu. Ch th l h tinh bt cho vo lc mi nh lng. Ghi nt ml. Ly 2ml dung dch th cho vo bnh nn dung tch 100ml khc, thm 0,12ml acid hydroclorid 1N v 10ml dung dch Iod 0,01N. Chun ngay bng dung dch Natri Thiosulfat 1N cho n khi mt mu. Ghi Nt ml. Dung dch chun : Cn chnh xc 1 lng bt Amoxicilin chun khong 0,1g trong bnh nh mc 100ml, ha tan vi nc va 100ml. Song song tin hnh ghi dung dch th. Hm lng % Amoxicilin c tnh theo cng thc : Nt - nt Pc m C% = * * C% * * 100 Nc - nc Pt 500mg Trong : Pt l khi lng bt th cn chun Pc l khi lng bt chun cn C% l hm lng bt Amoxicilin chun.
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n(ml) * k * 23,27 * m * 100 C% = 500(mg) * p Trong : m l khi lng trung bnh vin (mg) P l khi lng bt cn nh lng (mg)
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