TIU CHUN VIT NAM TCVN 5245:1990

(ISO 6632-1981) RAU QU V SN PHM CH BIN Phng php xc nh hm lng axit d bay hi Fruite, vegetables and deriveo products. Determination of volatine acidity Tiu chun ny quy nh phng php xc nh hm lng axit d bay hi trong rau, qu v cc sn phm ch bin t rau, qu; c th p dng cho tt c cc sn phm ti v ng hp khng cha ha cht bo qun v cc sn phm cho thm kh sunfur vo, c hoc khng c mt trong cc cht bo qun sau y: axit socbic, axit benzoic, axit focmic. Tiu chun ny ph hp vi ISO 6632-1981. 1. nh ngha 1.1. Axit d bay hi: tt c cc axit bo c khi lng phn t thp nh axit axetic v axit propionic dng t do hay dng hn hp, khng k axit foocrmic. Axit d bay hi c xc nh bng phng php ghi trong tiu chun ny, biu th bng mili ng lng trn 100 ml hoc trn 100g sn phm hay tnh theo s gam axit axetic trn 100ml hoc trn 100g sn phm. 2. Nguyn tc Axit ha phn t vi axit tctaric, ct li cun axit d bay hi qua chng ct bng hi nc v chun dch ct vi mt th tch dung dch chun natri hydroxit, dng phenol phtalein lm ch th. kt qu ph hp phi loi tr lng axit d bay hi to ra do thm cc hp cht st trng (bo qun) ra khi lng axit d bay hi xc nh nh trn). 3. Ha cht Tt c cc ha cht u phi c tinh khit phn tch (TKPT) c chp nhn. Nc dng phi l nc ct hoc nc c tinh khit tng ng, loi tr kh ccbonic. 3.1. Natri hydroxyt, dung dch chun th tch, nng (NaOH) = 0,1 mol/l (1). Pha ch ngay trc khi dng v kim tra nng bng cch chun trc tip trc khi dng. 3.2. Phenolphtalein, dung dch 10g/l pha trong cn 95% (th tch). 3.3. Axit tactaric, tinh th. 3.4. Nc vi trong pha t l 1 + 4. Ha mt th tch dung dch canxi hydroxit bo ha (3.5) vi bn th tch nc. yn hn hp cho n khi canxi cacbonat kt ta, gn dung dch trong v th tnh kim ca n bng dung dch phenolphtalein (3.2). Dung dch ny dng s dng trong ni hi. 3.5. Canxi hydroxit, dung dch nc vi trong bo ha. 4. Dng c Cc dng c th nghim thng dng v cc dng c c trng ring: 4.1. My nghin 4.2. Thit b ct li cun bng chng ct hi nc (xem hnh v) gm cc chi tit sau:

() Cho n nay c biu th l dung dch chun th tch 0,1N.

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4.2.1. Ni hi, ph hp cho vic sinh ra hi nc khng cha cacbon dioxit, lm bng thy tinh chu nhit hoc kim loi v c dung tch 1500ml. 4.2.2. Bnh sc kh, gm mt ng thy tinh ng knh 30mm v di 270mm, phn di ng kn v phnh ra theo dng hnh cu ng knh 60mm, trong c cha mu th. Bnh sc kh c t trn mt a kim loi c khe h, ng knh 40mm v phn bnh cu ca bnh sc kh c gn vo . 4.2.3. Ct ct phn on, gm mt ng thy tinh ng knh 20mm, di 500mm, bn trong c mt mng li hnh xon c bng thp khng g, s 100, vi mt l ch 15mm. C th s dng mt vi thit b khc c kh nng ct phn on ging nh vy (xem ch thch mc 4.2.4). 4.2.4. ng ngng t, ng knh 16mm, chiu di 400mm, t thng ng m bo vic ngng t ca hi v lm lnh hon ton khi chng ct. Ch thch. Nhng dng c khc vi kiu miu t trn c th c s dng xong phi tun theo nhng yu cu sau y: a) Di nhng iu kin chng ct thng thng, t nht l 99,5% tng s axit axetic thm vo mu phi c tm thy trong 250ml dch ct. kim tra iu ny, dng 20 ml dung dch axit axetic vi nng CH3COOH = 0,1 mol/l (1). b) Di nhng iu kin chng ct ging nhau, khng qu 5 phn nghn tng s axit lactic thm vo mu s c tm thy trong dch ct. kim tra iu ny, cn dng 200ml dung dch axit lactic vi nng C2H5COOH = 1 mol/l (2). c) Hi do ni hi sinh ra phi c loi b kh cacbonic. Kim tra iu ny bng cch nh 2 git dung dch phenol-phtalein (3.2) v 0,1ml dung dch natri hydroxit (4.1) vo 250ml dch ct v thy chuyn sang mu hng (gi mu t nht l 10 giy). 4.3. Bnh nn, dung tch 500ml. 4.4. Pipet chia , dung tch 20ml. 4.5. Buret, dung tch 25ml chia ti 0,1ml. 4.6. Cn phn tch. 5. Trnh t th (Xem iu khon 7 dnh cho sn phm cha cht bo qun l axit d bay hi). 5.1. Chun b mu th 5.1.1. Sn phm dng lng v nhng sn phm trong cht lng c th phn lp d dng (nc cam, sir, nc mt hoa qu, nc mm, v.v). Trn k mu, nu mu gm nhng ht rn trong huyn ph th tch dung dch lng bng cch lc qua phu c lt giy lc. Nu mu trong qu trnh ln men hoc c cha cacbon dioxit th chuyn bng cch dng pipet ht 50 60 ml dung dch mu cho vo bnh 500ml. Loi b ccbon dioxit bng cch lc di p sut thp trong 2 3 pht. trnh s to bt, c th cho thm mt lng nh cht chng si bt, v d chng 0,2g axit tannic, cao trc tip vo mu cn. 5.1.2. Sn phm dng nho v rn (mt cam, nc qu c, nc p c c ca hoa qu, hoa qu, rau kh, v.v). B ht v v cng ca khoang ht nu cn v nghin mu trong my nghin (4.1). 5.1.3. Sn phm ng lnh Sn phm ng lnh phi nguyn trong bnh kn cho tan v cho thm nc vo trong qu trnh ch bin trc khi trn ln.
1 2

() Cho n nay c biu th l dung dch 0,1N

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() Cho n nay c biu th l dung dch 1N.

5.2. Phn mu th. 5.2.1. Sn phm dng lng Dng pipet (4.1) chuyn 20ml mu th (5.1) cho vo bnh sc kh (4.2.2). Trong trng hp mu c tnh axit d bay hi mnh th c th dng mt lng nh hn v b sung cho 20ml bng cch cho thm lng cn thit. 5.2.2. Sn phm dng nho, dng rn hoc dng ng lnh. Cn khong 10g mu th (5.1.2 hoc 5.1.3), chnh xc ti 0,01g, vo mt cc thy tinh. Chuyn mu th vo bnh sc kh bng lng nc cn thit ti thiu, ct li cun ton b mu th v hi lu hn hp lng ny. 5.3. Ct li cun cc axit d bay hi Cho vo ni hi (4.2.1) 2/3 th tch nc vi trong (3.4). Cho thm 0,5g axit tactaric (3.3) vo mu cha trong bnh sc kh (4.2.2), ni phn cui vo ni hi (4.2.1), vo ct ct phn on (4.2.3) v b ngng t (4.2.4). Dng n kh un ng thi ni hi v bnh sc kh. Nu th tch ban u ca cc cht trong bnh sc kh ln hn 20ml, cn iu chnh ngn la cho n khi th tch gim cn 20ml, trong khi hi nc a a vo chm (1). Gim tc un bnh sc kh gi th tch cc cht cho n nh (khong 20ml) trong thi gian chng ct, trong khi hi nc thot ra ni hi (4.2.1) t mc ti a. Qu trnh chng ct s kt thc sau 10 15 pht. Tp trung dch ct vo mt hnh nn (4.3), tip tc chng ct cho n khi ly li c 250ml dch ct. Th tch dch ct t nht phi gp 12 ln th tch ca phn mu th (5.2). 5.4. Chun axit d bay hi Cho hai git dung dch phenolphtalein (3.2) vo dch ct v chun vi dung dch natri hydroxit (3.1) cho n khi xut hin mu hng nht (gi mu trong t nht 15 giy) 5.5. S ln xc nh Tin hnh hai ln xc nh trn cng mt mu th (5.2). 6. Tnh kt qu (Xem iu 7 dnh cho sn phm c cha cht bo qun l axit d bay hi). 6.1. Phng php tnh ton v cng thc 6.1.1. Sn phm dng lng Hm lng axit d bay hi, biu th bng mili ng lng trn 100ml mu th, hoc bng s gam axit acetic trn 100ml sn phm, c tnh theo hai cng thc tng ng (1) v (2). x1 = 10 v1 v0 0,6 v1 v0 (1) (2)

x2 = Trong :

v0 Th tch, tnh bng mililit, ca mu th (5.2.1) v1 th tch, tnh bng mililit, ca dung dch natri hydroxyt (3.1) dng chun . 6.1.2. Sn phm dng nho, dng rn hoc ng lnh axit d bay hi, biu th bng mili ng lng trn 100g sn phm hoc bng s gam axit axetic trn 100g sn phm c tnh theo hai cng thc tng ng (3) v (4).
1

Dng 20ml mu th dng lng th tch khng i khi a hi nc vo bnh vi tc cc i ti thi im bt u chng ct.

x3 = x4 = Trong :

10 x v 1 m0 0,6 x v 1 m0

(3) (4)

m0 khi lng, tnh bng gam ca mu th (5.2.2); v1 c ngha ging nh mc 6.1.1 6.1.3. Kt qu Kt qu l trung bnh s hc ca cc gi tr thu c bng hai phng php xc nh (5.5) vi iu kin tha mn chnh xc. (Mc 6.2). 6.2. chnh xc 6.2.1. lp li S khc nhau gia cc kt qu thu c bng hai phng php xc nh (5.5) tin hnh ng thi hoc lin tip nhau do cng mt ngi phn tch m nhim, khng c vt qu 0,2 mili ng lng trn 100ml hoc 100g, hay 12ml axit axetic trn 100ml hoc 100g. 6.2.2. nhc li S khc nhau gia cc kt qu thu c t hai phng th nghim khc nhau tin hnh trn cng mt mu th khng c vt qu 0,5 mili ng lng trn 100ml hoc 100g, hay 30mg axit axetic trn 100ml hoc 100g; 7. Trng hp ring i vi sn phm cha kh sunfur, c mt hoc khng c mt axit coocbic, axt benzoic hoc axit froomic th xc nh tng s cc cht bo qun c trong dch ct v hiu chnh li kt qu chun cho ph hp. 7.1. Xc nh kh sunfur trong dch ct (khng c mt cc cht bo qun khc). 7.1.1. Ha cht 1 7.1.1.1. It, dung dch chun th tch nng ( I2 ) = 0,01 mol/l (1) 2 7.1.1.2. Kali ioua, tinh th 7.1.1.3. Axit chlohydric c. 7.1.1.4. Natri borat, dung dch bo ha (khong 60g natri borat decahydrat/lit) 7.1.1.5. Ch th tinh bt Ha 5g tinh bt tinh khit vo 1 lt nc ct c cha 200g natri clorua lm cht bo qun. Khi pha ch cn un nng dung dch trong 10 pht. 7.1.2. Chun Nh mt git axit clohydric (7.1.1.3); 5ml h tinh bt (7.1.1.5) v khong 0,1 g natri iua (7.1.1.2) vo dch ct sau khi chun axit d bay hi (5.4) v chun kh sunfur t do vi dung dch iua (7.1.1.1). Ghi th tch dung dch it dng cho ln chun u tin. Thm 200ml natri borat (7.1.1.4) iu chnh pH khong 9 n 9,5 v chun kh sunfur hn hp vi dung dch ioua (7.1.1.1) cho n khi dung dch chuyn sang my xanh tm (gi mu t nht trong 30 giy). Ghi th tch dung dch iua dng trong ln chun th hai. 7.1.3. Tnh kt qu
1

() Cho n nay c biu th l dung dch chun th tch 0,01 N.

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Hiu chnh th tch V, ca dung dch natri hydroxit (3.1) dng chun , axit ha kh sunfur t do v hn hp, biu th bng s ml dung dch kim 0,1 mol/l, bng cng thc (5) sau y: V1 = V1 Trong : V1 Th tch, tnh bng ml, ca dung dch natri hydroxit (3.1) tng ng hiu chnh lng axit d bay hi. V2 th tch, tnh bng ml, ca dung dch ioua (7.1.1.1) dng chun kh sunfur t do; V3 th tch, tnh bng ml, ca dung dch ioua (7.1.1.1) dng chun kh sunfur hn hp. Cng thc nu mc 6.1 c th p dng trc tip bng cch thay V1 bng V1. 7.2. Xc nh axit soocbic trong dch ct (c hoc khng c mt kh sunfur). 7.2.1. Ha cht 7.2.1.1. Axit soocbic, dung dch chun tng ng vi 20mg axit soocbic trn mt lt hoc 26,8mg kali soocbat trn 1 lt. 7.2.1.2. Cht oxy ha Ha tan 0,5g natri hydrogen cacbonat v 0,001g ng (II) sunfat pentahydrat trong 1000ml nc ct. 7.2.1.3. ng (II) sunfat, dung dch 0,1g/l. 7.2.1.4. Dung dch axit cromicsunfuric Ha tan 50mg kali dicromat trong khong 90ml nc vo bnh nh mc c 200ml. Thm 10ml axit sunfuric nng (H2SO4 = 0,3 mol/l) (1) v nh mc n vch bng nc. Ch thch: 1 lt dung dch axit sunfuric nng H2SO4 = 0,3 mol/l (1) cha 14,7 axit sunfuric hoc 8ml axit sunfuric S20 = 1,84 g/ml. 7.2.1.5. Dung dch axit thiobabituric Ha tan 0,5g axit thiobabituric vo 50ml nc v thm 10ml dung dch natri hydroxyt nng NaOH = 1mol/l (2). Chuyn vo bnh nh mc c 100ml, thm 11ml dung dch axit clohydric nng HCl = 1 mol/l (2) vo v pha long vi nc n vch. Dung dch ny khng bn vng, ch c s dng trong vng 5 gi k t lc pha ch. 7.2.2. Dng c 7.2.2.1. a s hoc a thy tinh chu nhit, ng knh 55mm. 7.2.2.2. Bnh nh mc 1 vch, dung tch 10, 20 v 250 ml. 7.2.2.3. Ni cch thy 7.2.2.4. My quang ph, ph hp s dng trong vng nhn thy v vng t ngoi ca quang ph, gn vi cuvet silica c chiu di 1cm. 7.2.3. Nhn bit v xc nh Tp trung, th tch V bit (chng 250ml) ca dch ct trnh by mc 5.3. Xc nhn s c mt ca axit soocbic v xc nh hm lng ca chng trc khi xc nh axit d bay hi. 7.2.3.1. Nhn bit
1 2

V2 v 3 10 20

(5)

() Cho n nay c biu th l dung dch 0,3N

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() Cho n nay c biu th l dung dch 1N.

7.2.3.1.1. Ly 10ml dch ct vo mt ci a (7.2.2.1) Kim ha bng cch cho vo 1ml dung dch nc vi trong (3.4) v 1 git dung dch ng (II) sunfat (7.2.1.3) v (dung dch ny lm xc tc cho qu trnh oxy ha kh sunfur bi oxy ca kh quyn). C cn dch trn ni cch thy (7.2.2.3). Nh vy s oxy ha kh sunfunr, cn v cc loi ru khc d bay hi, andehyt, xeton, cc este thm, v lm cng cc axit thnh mui canxi. Ha tan mu c vi 10ml nc. 7.2.3.1.2. Chuyn 5ml dung dch ny vo mt bnh nh mc c 10ml, cho 2ml dung dch axit cromic-sunfuric (7.2.1.4) vo. t bnh nh mc trong ni cch thy 10 pht. Cho thm 3ml dung dch axit thiobabituric (7.2.1.5) vo v t tip ln ni cch thy 20 pht na. Vic xut hin mu hng c dng nhn bit s c mt ca axit soocbic. 7.2.3.2. Xc nh Tin hnh xc nh axit soocbic trong dch ct bng mt trong cc phng php sau y: 7.2.3.2.1. Phng php so mu Sau 20 pht un trn ni cch thy, lm ngui dung dch mu hng thu c mc 7.2.3.1.2. Trong mt b nc . Pha long bng nc ti 10ml v o hp th ca dung dch bng my quang ph (7.2.2.4) ti bc sng 532nm, s dng cht lng so snh l dung dch mu trng c pha ch theo cng mt th tc mc (7.2.3.1.2), nhng ch s dng 5ml nc cho vo dch ct. So snh hp th vi dung dch axit soocbic chun pha long thch hp (7.2.1.1), x l nh trnh by mc (7.2.3.1.2). 7.2.3.2.2. Phng php hp th tr ngoi (1) Pha long dch ct vi t l 1 + 3, 1 + 9 hoc 1 + 19 vi cht oxi ha (7.2.1.2) trong bnh nh mc c 10ml hoc 20ml (7.2.2.2) (dung dch ny lm xc tc cho qu trnh oxy ha kh sunfur bi oxy ca kh quyn). Trn u v phi ra gi vi pht. dung dch ny vo cuvet silica (xem mc 7.2.2.4). o hp ph ca dung dch bng my quang ph (7.2.2.4) vi di bc sng l 256nm dng cht lng so snh l dung dch mu trng c pha ch ging mu nhng s dng nc ct thay cho dch ct. hp ph o c phi nh hn 0,7. iu ny quyt nh t l pha long s chn. So snh hp ph ny vi hp ph ca dung dch axi soocbic chun (7.2.1.1) pha long 1 + 3 vi cht oxy ha (7.2.1.2). 7.2.4. Tnh kt qu Lng axit soocbic trong dch ct, tnh theo miligam trn mt lt, biu th bng cng thc (6) sau: M = 20 x Trong : Ax hp ph ca dch ct pha long bc sng 532nm (xem mc 7.2.3.2) hoc di sng 256nm (xem mc 7.2.3.2.2). Ar hp ph ca dung dch so snh (7.2.1.1) pha long tng t bc sng 532nm (7.2.3.2.1) hoc bc sng 256nm (7.2.3.2.2). 7.2.5. Xc nh axit ca dch ct. axit ca axit soobic (X5) tnh theo mililit dung dch kim 0,1 mol/l, biu th bng cng thc (7) sau: Ax Ar

( ( ) i vi cc sn phm cha du v cc hp cht thm d bay hi (nh ausertisceae) ch dng c phng php so mu.

X5 = Trong :

20 A x v' x x 11,2 A r 1000

(7)

V Th tch cn li ca dch ct, tnh bng mililit, t hn V mt cht (V l th tch dch ct c tp trung li xem mc 7.2.3); Ax v Ar c ngha ging nh mc 7.2.4. 11,2- Khi lng, tnh bng miligam, ca ng lng axit soocbic ng vi 1ml dung dch natri hydroxyt 0,1 mol/l. 7.2.6. Phng php tnh v cng thc Hiu chnh th tch V4 ca dung dch natri hydroxyt (3.1) dng chun axit soocbic. 7.2.6.1. Sn phm lng axit d bay hi ca mu, tnh theo mili ng lng trn 100ml hoc tnh theo s gam axit axetic trn 100ml, biu th theo hai cng thc tng ng (8) v (9). 10 20 Ax V' V x x ) ..... (8) V4 ( V0 11,2 Ar 1000 V ' 0,6 20 Ax V' V X7 = x x ) ..... (9) V4 ( V0 11,2 Ar 1000 V ' X6 = Trong : V4 th tch c hiu chnh, tnh bng mililit, ca dung dch natri hydroxit (3.1) dng chun ; Ax v Ar c ngha ging nh mc 7.2.4; V v V c ngha ging nh mc 7.2.5. V0 c ngha ging nh mc 6.1.1. 7.2.6.2. Cc sn phm dng nho, rn hoc ng lnh axit d bay hi ca mu, tnh theo mili ng lng trn 100g hoc s gam axit axetic trn 100g, biu th bng hai cng thc tng ng (10) v (11): 20 x V4 ( 11,2 0,6 20 X9 = x V4 ( m0 11,2 X8 = 10 m0 Trong : V4 c ngha ging nh mc 7.2.6.1; Ax v Ar c ngha ging nh mc 7.2.4; V v V c ngha ging nh mc 7.2.5. m0 c ngha ging nh mc 7.1.2. 7.3. Xc nh axit benzoic trong dch ct (c mt hoc khng c mt kh sunfur). 7.3.1. Thuc th 7.3.1.1. Axit benzoic, dung dch chun cha 20mg axit benzoic hoc 23,6 mg natri benzoat trn mt lt. Ax V' x ) Ar 1000 Ax V' x ) Ar 1000 V ..... (10) V' V ..... (11) V'

7.3.2. Nht bit v xc nh Tp trung th tch V bit (khong 250ml) ca dch ct nh nu trn mc (5.3). Kim tra s c mt ca axit benzoic trc khi xc nh axit d bay hi. 7.3.2.1. Nhn bit Cho 2ml dch ct vo cuvet silica (7.2.2.4) v ghi hp ph quang ph gia di sng 220nm v 300nm. Nu hp ph vt qu 0,7 th tin hnh kim tra tng t nh vy trn dch ct pha long 1 + 1; 1 + 3 hoc 1 + 9 vi nc. Trong dung mi ny axit benzonic c c trng bi hai ng cong hp ph cc i, mt gia di sng 225 v 230nm v mt ng cong khc bc sng 268nm. 7.3.2.2. Xc nh 7.3.2.2.1. Khi khng c cc loi du d bay hi, cc hp cht thm v kh sunfur, th o hp ph cc i gia bc sng 225nm v 230nm ca dch ct c pha long thch hp trong cuvet silica (xem 7.2.2.4), dng nc lm cht lng so snh. So snh hp ph vi dung dch axit benzoic chun (7.3.1) pha long 1 + 1 vi nc. 7.3.2.2.2. Nu sn phm cha kh sunfur th pha long dch ct theo t l 1+1, 1 + 3 hoc 1 + 9 vi cht oxy ha (7.2.1.2), lc v hong trong khng kh vi pht. o hp ph cc i gia bc sng 225nm v 230nm, dng cht lng so snh l mt mu trng c chun b bng cch pha long cht oxy ha (7.2.1.2) vi nc thay cho dch ct. 7.3.2.2.3. Nu sn phm c cha du d bay hi hoc cc hp cht thm d bay hi (v d nh ausertisceae), c mt hoc khng c mt kh sunfur, th cho 10ml dch ct vo mt chic a (7.2.2.1), kim ha bng 1ml dung dch nc vi trong (4.4) v nh mt git ng (II) sunfat (7.2.1.3) vo c cn trn ni cch thy (7.2.2.3). Pha long cht c trong 10ml nc ct. o hp ph cc i ca dung dch di sng khong 230nm vi dung dch so snh l mt mu trng c chun b tng t nh nu trn nhng dng 10ml nc thay cho dch ct. So snh hp ph vi dung dch axit benzonic chun (7.3.1.1) c pha long 1 + 1 vi nc. 7.3.3. Tnh kt qu Lng axit benzoic cha trong dch ct, tnh theo mililit trn mt lt, biu th bng cng thc (6) sau: M = 20 x Trong : Ax- hp ph ca dch ct pha long (xem 7.3.2.2); Ar- hp ph ca dung dch so snh (7.3.1.1) pha long ging nh trn (xem mc 7.3.2.2). 7.3.4. Xc nh axit ca dch ct axit ca axit benzoic, tnh bng s mililit dung dch kim 0,1 mol/l, c tnh theo cng thc (12) sau: X10 = Trong : V th tch cn li, tnh bng mililit, ca dch ct, nh t hn V(th tch ca dch ct c tp trung. Xem mc 7.3.2); Ax v Ar c ngha ging nh mc 7.3.3; 20 A x V x x ............ (12) 12,2 A r 1000 Ax (6) Ar

12,2 Khi lng, tnh bng miligam, ca ng lng axit benzoic ng vi 1 ml dung dch natri hydroxit 0,1 mol/l. 7.3.5. Phng php tnh v cng thc Hiu chnh th tch V5 ca dung dch natri hydroxit (3.1) dng chun axit ca axit benzoic nh sau: 7.3.5.1. Sn phm dng lng axit d bay hi ca mu, tnh theo mili ng lng trn 100ml hoc tnh bng s gam axit axetic trn 100ml, c tnh bng hai cng thc tng ng (13) v (14): 10 20 Ax V V x x ) ..... .....(13) V5 ( V0 12,2 Ar 1000 V 0,6 20 Ax V V X 12 = x x ) ..... .....(14) V5 ( V0 12,2 Ar 1000 V X 11 = Trong : V5- th tch c hiu chnh, tnh bng mililit, ca dung dch natri hydroxit (3.1) dng chun ; Ax v Ar c ngha ging nh mc 7.3.3; V v V c ngha ging nh mc 7.3.4; V0 c ngha ging nh mc 6.1.1. 7.3.5.2. Sn phm dng nho, dng rn hoc dng ng axit d bay hi ca mu, tnh theo mili ng lng trn 100g hoc tnh bng s gam axit axetic trn 100g, c tnh theo hai cng thc tng ng (15) v (16) sau: 10 20 x V5 ( m0 12,2 0,6 20 X 14 = x V5 ( m0 12,2 X 13 = Trong : V5- c ngha ging nh mc 7.3.5; Ax v Ar c ngha ging nh mc 7.3.3; V v V c ngha ging nh mc 7.3.4; m0 c ngha ging nh mc 6.1.2. 7.4. Xc nh axit d bay hi khi c axit foocmic c hoc khng c mt kh sunfur). 7.4.1. Ha cht 7.4.1.1. Natri axetat, tinh th 7.4.1.2. Dung dch thy ngn (II) chlorua Ha tan 1,5g thy ngn (II) chlorua trong 100ml nc ct 7.4.1.3 Kali dicronat, dung dch 33,79g/lit. 7.4.1.4. Axit sunfuric, pha long 2 + 1. 7.4.1.5. St (II) sunfat Ax V V x ) ..... .....(15) Ar 1000 V Ax V V x ) ..... .....(16) Ar 1000 V

7.4.2. Dng c 7.4.2.1. Knh hin vi 7.4.2.2. Ni cch thy 7.4.2.3. a chu nhit, dung tch 500ml 7.4.3. Nhn bit axit foocmic v xc nh axit d bay hi. 7.4.3.1. Nhn bit axit foocmic Tp trung mt th tch V bit (chng 250ml) ca dch ct nh m t mc 5.3. Xc nh s c mt ca axit foocmic trc khi xc nh tnh axit d bay hi. Cho 2ml dch ct (1) vo mt ng th. Thm vo 0,25g natri axetat (7.4.1.1) v 1ml dung dch thy ngn (II) chlorua (7.4.1.2). un trn ni cch thy (7.4.2.2) trong 10 pht. Sau khi lm ngui, kim tra tinh th kt ta ca thy ngn (II) chlorua di knh hin vi, thy tinh th c dng lin kt ngang hoc ch X c trng cho axit foocmic. Di nhng iu kin c ch ra trn th s c mt ca axit foocmic c pht hin trong sn phm du (5.2) mc pht hin ti thiu l 0,5 g/l, nh hn nhiu so vi lng st trng c hiu qu. Tuy vy mt lng nh hn ca axit foocmic c th xut hin t nhin trong sn phm rau m khng th pht hin bng cch ny. 7.4.3.2. Tnh oxy ha ca axit foocmic v mt vi kh sunfur Chun axit d bay hi ca dch ct vi dung dch natri hydroxit (3.1), dng phenol phtalein (3.2) lm ch th. Cho 10ml dung dch natri hydroxyt vo dch ct to kim ha mnh v c cn th tch ny trong mt ci a (7.4.2.3) trn ni cch thy (7.4.2.2) cho n khi ch cn li khong 2 5ml cn lng. Ru, aldehyt, axeton, este, du d bay hi v cc hp cht thm u b loi bng cch . Cho cn lng vo bnh sc kh (4.2.2) ca thit b chng ct (4.2), trng a vi 10ml (Kali dicromat (7.4.1.3) v thm 10ml dung dch axit sunfuric (7.4.1.4), tp trung ton b dung dch lng vo bnh sc kh. Lc v yn t nht 15 gi. Di nhng iu kin trn, th axit foocmic v kh sunfur s b oxy ha hon ton trong khi axit axetic v cc hp cht ng ng to nn tnh axit d bay hi vn khng b nh hng (th tc ny khng cho php xc nh ring axit foocmic cha trong dung dch ct). Gim p sut trong bnh sc kh v lc ui kh ccbonic to ra. Gim lng d kali dioromat bng cch cho thm 2-3g st (II) sunfat (7.4.1.5), tp trung dch ct v chun b axit d bay hi theo th tc c m t mc 5.3 v 5.4. 7.4.4. Tnh kt qu Xem mc 6.1. 8. Bin bn th Bin bn th ch r phng php s dng v kt qu thu c, trnh by r phng php tnh ton dng. N cng s cp n tt c nhng chi tit tin hnh m khng c ghi trong tiu chun ny hoc khng c coi l bt buc, cng nh nhng yu t c th nh hng n kt qu. Bin bn th s a ra nhng thng tin cn thit nhn bit mu mt cch ton din.

( ( ) Ly 2ml dch ct nhn bit axit foocmic (8.4.3.1) gy ra sai s khng ng k i vi kt qu xc nh chng (8.4.3.2).

Thit b chng ct hi nc (4.2)