TIU CHUN VIT NAM TCVN 4713:1989

HP RAU QU 1. Ni dung phng php Ct axit sobic t mu bng hi nc, oxy ha bng axit crom sunfuric ti andehytmalonic, dng axit 2-tiobacbituric to phc cht mu hng, o cng mu ca phc bng my so mu bc sng 532 nm hoc vi knh lc xanh. 2. Ly mu theo TCVN 4409-87. Chun b mu theo TCVN 4413-87. 3. Dng c, ha cht Cn phn tch chnh xc n 0,0001 g, My so mu quang in, B ct li cun hi nc, Bnh nh mc, dung tch 25 v 100 ml, Kali bicromat, dung dch 0,49 g/l, Axit sunfuric c v dung dch 1/2. Dung dch cht oxy ha: trn dung dch kali bicromat v dung dch axit sunfuric ngay trc khi dng, theo t l 1/1 Natri hydroxyt 0,1 N, Axit clohydric 1N, Axit 2-tiobacbituric: cn 0,5 g axit 2-tiobacbituric chuyn ton b vo bnh mc 100 ml, thm 50 ml nc ct c sn 10 ml NaOH 0,1N, sau thm 11 ml dung dch axit clohydric 1N, thm nc n vch mc. Dung dch ny khng bn ch s dng trong 5 gi k t khi pha. Axit sobic tinh khit: CH3 (CH=CH)2COOH, Nc ct 2 ln. 4. Tin hnh th 4.1 Xy dng ng chun Pha dung dch tiu chun: ho tan 0,1 g axit sobic vo 10-12 ml dung dch NaOH 0,1N. Chuyn ton b vo bnh mc dung tch 1000ml, thm nc n vch mc. Ly 10 ml dung dch tiu chun chuyn vo bnh mc dung tch 50 ml, thm nc n vch. Dng pipet cho vo 6 bnh mc dung tch 25 ml tun t: 0, 2, 4, 6, 8, 10 ml dung dch pha trn. Thm nc n vch mc, nh vy trong cc bnh c 0-0,4-0,8-1,6-2,0 mg axit sobic trong 1 lt. Ht t mi bnh 10 ml, cho vo bnh mc 25 ml, thm 4 ml dung dch oxy ha, bnh vo bp cch thu un si 10 pht, sau thm 4 ml dung dch axit 2-tiobacbituric v tip tc un cch thy trong 20 pht, lm ngui bnh thm nc n vch mc. Sau 30 pht o mu dung dch trn my so mu quang in bc sng 532 nm hoc vi knh lc xanh. Dng cuvt dy 1-2 cm. Xy dng th chun vi trc tung l mt quang v trc honh l nng tng ng. Dung dch so snh l dung dch tng ng khng c axit sobic. 4.2. Tin hnh o mu Lp b ct li cun hi nc. Cn 5-10 g mu, chuyn vo bnh cu ca b ct, thm 10 ml H2SO4 1N v 10 g MgSO4 thm dung dch NaCl 25% n 3/4 th tch bnh cu, un si bnh sinh

hi v un nh bnh cu. Qu trnh chng ct kt thc khi thu c khong 100 ml dung dch ct. Ly bnh hng ra chuyn vo bnh mc 250 ml, thm nc n vch. Dng pipet ht 10 ml dch ct, chuyn vo bnh nh mc dung tch 25 ml, thm 4 ml dung dch oxy ha, un cch thu 10 pht, thm 4 ml dung dch axit 2-tiobacbituric, un cch thy 20 pht, lm ngui bnh v tip tc tin hnh nh iu 4.1. 5. Tnh kt qu Hm lng axit sobic (X) tnh bng %, theo cng thc:

Trong : n - Nng ca axit sobic trong mu theo ng chun mg/l; V1 - th tch bnh mc dch ct pha long (250 ml theo phng php hng dn), V2 - Th tch dch ct ly xc nh, ml, V3 - Th tch bnh nh mc pha long dung dch so mu, ml, m - khi lng mu cn, g.