TIU CHUN VIT NAM TCVN 6641 : 2000

RAU, QU V SN PHM RAU QU - XC NH HM LNG SUNFUA DIOXIT TNG S Fruit, vegetables and derived products Determination of total sulphur dioxide content Li ni u TCVN 6641 : 2000 hon ton tng ng vi ISO 5522 : 1981; TCVN 6641 : 2000 do Ban k thut TCVN/TC/F10 Rau qu v sn phm rau qu bin son, Tng cc Tiu chun o lng Cht lng ngh, B Khoa hc Cng ngh v Mi trng ban hnh. 1. Phm vi v lnh vc p dng Tiu chun ny qui nh phng php xc nh hm lng sunfua dioxit tng s trong rau qu, sn phm rau qu, bt k loi sunfua dioxit no. 2. Nguyn tc Axit ha v lm nng phn mu th, sau tch cun sunfua dioxit qua lung kh nit c gii phng. Hp th v oxi ha sunfua dioxit bng cch sc n qua dung dch hidro peroxit long trung tnh. S dng dung dch chun natri hidroxit xc nh axit sunfuric c to thnh. Kim tra vic xc nh hm lng sunfua dioxit bng cch cho bari sunfat kt ta t dung dch c to thnh v theo hai cch: - Cn bari sunfat (ph lc A); hoc - Xc nh nephelometric (ph lc B). 3. Thuc th Tt c cc thuc th phi thuc loi phn tch. Nc s dng phi l nc ct hoc nc t nht c tinh khit tng ng, mi un si. 3.1. Nit, khng cha oxi. 3.2. Hidro peroxit, dung dch 9,1 g/l, khng cha ion sunfat. 3.3. Axit clohydric, dung dch 100g/l. Pha long mt th tch axit clohidric m c, 20 = 1,19 g/ml vi ba th tch nc. 3.4. Dung dch ch th Ha tan 100 mg bromophenol xanh(1) trong 100 ml etanola 20% (v/v). 3.5. Natri hidroxit khng cha ion sunfat; hoc dung dch th tch chun c(NaOH) = 0,1 mol/l(2). 3.6. Natri hidroxit khng cha ion sunfat; dung dch th tch chun c(NaOH) = 0,01 mol/l(3). 3.7. Iod, dung dch th tch chun c(1/2 l2) = 0,02 mol/l (4). 3.8. H tinh bt, dung dch 5 g/l cha 200 g natri clorua/lt lm cht bo qun. Duy tr dung dch ny im si 10 pht trong khi chun b.

1 2 3 4

Cht ch th ny c chn v n khng gy nhiu khi xc nh bng phng php o c. Hitherto c biu th theo dung dch th tch chun 0,1 N. Hitherto c biu th theo dung dch th tch chun 0,01 N. Hitherto c biu th theo dung dch th tch chun 0,02 N.

3.9. Dung dch kali metabisunphit/EDTA. Ha tan 1,20g kali metabisunphit (K2S2O5) v 0,20 g mui dinatri ca axit etylendinitrilotetraaxetic (5) trong mt lt nc. Chuyn cn thn ton b lng dung dch ny sang bnh nh mc mt vch dung tch 1 000 ml. Thm nc cho n vch v lc. 3.10. Sacaroza, dung dch 100g/l. 4. Thit b, dng c S dng thit b th nghim thng thng v thit b c bit nh: 4.1. ng ong. 4.2. Pipet. 4.3. Buret bn vi lng, c dung tch 10 ml. 4.4. Buret, c dung tch 25 ml. 4.5. My trn. 4.6. Thit b tch cun, nh trong hnh v, hoc thit b tng t m bo c vic y v tch cun sunfua dioxit v s hp th ca n trong dung dch hidro peroxit. 4.6.1. Cu to ca thit b A: Bnh cu y trn, c dung tch ln hn hoc bng 250ml. B: B phn ngng t hi lu ngc chiu c hiu qu cao, c th lp kht vi bnh cu (A). C: Phu nh git, c th lp c vo bnh cu (A). D: ng np nit. E v E: 2 b sc kh c lp kht vi b phn ngng t hi lu (B). F: a, bng li st hoc bng amiang, ng knh 150 mm, c 1 l ng knh 40mm tm. a ny dng chng hin tng pht la, c bit, nhng cht chit c c trong sn phm. Ch thch Gia cc ln th, nu vic chng chit vn m bo chm v cn thn th ch cn ra bnh cu (A). 4.6.2. Th nghim kim tra Thit b phi tha mn c ba th nghim kim tra sau y: 4.6.2.1. Cho 100ml nc v 5ml dung dch axit clohidric (3.3) vo bnh cu (A). un nng bnh cu cng lc cho dng nit i qua, khong 1h, nh cc b sc kh (E v E) mi b cha 5ml nc v 0,1 ml dung dch ch th (3.4). Cc cht cha trong mi b sc kh phi trung tnh. 4.6.2.2. Cho 20ml dung dch sacaroza (3.10) vo bnh cu (A). un nng bnh cu cng lc cho dng nit i qua, khong 1 gi. Dung dch sacaroza phi khng mu, v khng c c kt ta nu sm ng trn thnh bnh (th ny kim tra cng un nng). 4.6.2.3. Tin hnh hai thao tc sau y: a) Dng pipet (4.2) cho 20 ml dung dch kali metabisunphit/EDTA (3.9) v 5 ml dung dch axit clohidric (3.3) vo bnh cu (A). Tin hnh chit v xc nh sunfua dioxit trong nhng iu kin ging nh khi xc nh chnh thc, nhng khng cho thm dung dch axit clohidric (ngha l nh qui nh trong 5.2.1, 5.3.2 v 5.3.3).
5

Sn phm ny bo v ion sunfit khi s oxi ha ca khng kh bi to phc cc vt ion ng.

b) Cho 20 ml dung dch kali metabisunphit/EDTA (3.9), v thm 5 ml dung dch axit clohidric (3.3) v 1 ml dung dch h tinh bt (3.8) vo bnh nn dung tch 100ml. Dng buret (4.4) cha dung dch iot (3.7) chun cho n khi bt u xut hin mu xanh da tri. Hm lng sunfua dioxit xc nh c trong mc a) phi nm trong khong 1% ca hm lng xc nh c trong mc b). Khng c tin hnh theo b) chm qu 15 min sau khi hon thnh a) trnh kh nng hm lng sunfua dioxit trong dung dch metabisunphit b thay i. 4.7. Cn phn tch 5. Cch tin hnh 5.1. Chun b mu th Loi b ht ht v khoang cha ht cng nu cn, v nghin k mu. nhng sn phm ng lnh hoc ng lnh su tan gi trong bnh kn, v cho ht nhng cht lng c to ra trong qu trnh tan gi vo mu trc khi nghin. 5.2. Phn mu th Cn 10 n 100 g mu th (5.1), chnh xc n 0,01 g, ty theo hm lng sunfua dioxit d on c trong mu, sao cho phn mu th cha khng qu 10 mg sunfua dioxit; chuyn phn mu th vo bnh (A) ca thit b tch cun (4.6). 5.3. Tin hnh tch cun 5.3.1. Cho vo mi b sc kh (E v E) 3 ml 2) dung dch hidro peroxit (3.2) v 0,1 ml dung dch ch th (3.4), v trung ha dung dch hidro peroxit bng dung dch natri hidroxit 0,01 mol/l (3.6). 5.3.2. Ni phu nh git (C), phn ngng t hi lu (B) v cc b sc kh (E v E) vi bnh (A); m cho lung kh nit thi ht khng kh ra khi bnh (A) v ton b dng c. 5.3.3. Cho 100 ml nc v 5 ml dung dch axit clohidric (3.3) vo phu nh git (C). 5.3.4. cho dung dch axit clohidric pha long cha trong phu nh git (C) chy vo bnh (A) (nu cn tm thi ng lung kh nit li). 5.3.5. un si t t cc cht cha trong bnh, v duy tr im si, cho lung kh nit lu thng u lin tc c mt n hai bt kh/s trong khong 30 pht. 5.4. Chun Chuyn cc cht t b sc kh th hai (E) vo b th nht v chun axit sunfuaric c to ra bng dung dch natri hidroxit 0,01 mol/l (3.6) hoc 0,1 mol/l (3.5) ty theo hm lng sunfua dioxit d on. 5.5. Kim tra 5.5.1. Nu th tch V ca dung dch natri hidroxit 0,01 mol/l vt qu 10ml (hoc 1 ml trong trng hp dung dch natri hidroxit 0,1 mol/l) th tin hnh xc nh khi lng li nh qui nh trong ph lc A. 5.5.2. Nu th tch V nh hn 10 ml th tin hnh xc nh c nh qui nh trong ph lc B. Nu th tch V nh hn 5 ml th ch c dng phng php o c. i vi phn mu th 100g, gii hn 5 ml ny tng ng vi hm lng sunfua dioxit 16mg/kg. Cao hn gii hn ny th ch cn phng php xc nh chun axit.

21) 2)

Thit b loi Lieb v Zaccherl Lng ny theo l thuyt l oxy ha 51 mg sunfua dioxyt, nhng cn c mt lng d

5.6. S ln xc nh Tin hnh hai ln xc nh trn cng mu th (5.1). 6. Biu th kt qu 6.1. Phng php tnh v cng thc Hm lng sunfua dioxit, biu th bng miligam trn 1 kg sn phm, c tnh theo cng thc sau(6): 0,32 trong m l khi lng ca phn mu th (5.2), tnh bng gam; V l th tch ca dung dch natri hidroxit 0,01 mol/l (3.6) dng chun (5.4), tnh bng mililit; 0,32 l khi lng ca sunfua dioxit tng ng vi 1 ml dung dch natri hidroxit 0,01 mol/l, tnh bng gam; Ly kt qu l trung bnh cng ca hai ln xc nh (5.6) vi iu kin p ng c lp li (6.2). 6.2. lp li Chnh lch kt qu ca hai ln xc nh c tin hnh ng thi hoc k tip nhau do mt ngi phn tch, khng c vt qu 5% gi tr trung bnh. 7. Bo co kt qu Bo co kt qu phi ch ra phng php s dng v kt qu th nghim thu c. Cng phi cp n tt c cc chi tit thao tc khng qui nh trong tiu chun ny, cng vi cc chi tit bt thng no khc c nh hng ti kt qu. Bo co kt qu cng bao gm tt c cc thng tin cn thit v vic nhn bit y mu th. V V 103 = 320 m m

Nu s dng dung dch natri hidroxit 0,1 mol/l (3.5) th thay h s 320 bng 3200

Ch thch: ng knh trong ca bn ng ngng ng tm l 45, 34, 27 v 10mm. l iu thun li cho vic thay th hai bnh hnh nn bng bnh cu. Hnh S h thng thit b tch cun

PH LC A

KIM TRA BNG PHNG PHP KHI LNG XC NH ION SUNFAT TO THNH BNG CHUN AXIT A.1 Thuc th Tt c cc thuc th phi thuc loi phn tch. S dng nc ct hoc nc t nht c tinh khit tng ng, mi un si. A.1.1 Bari clorua, dung dch 100 g/l. A.1.2 Axit clohidric m c, 20 = 1,19 g/ml A.1.3 Dung dch ra bari sunfat kt ta. Ha tan trong nc 26 mg bari clorua ngm hai phn t nc (BaCl2.2H2O) vo bnh nh mc mt vch dung tch 1 000ml, thm 1 ml axit clohidric m c (A.1.2) v pha long bng nc cho n vch. A.2 Thit b, dng c Nu khng c quy nh khc, s dng thit b phng th nghim thng thng v: A.2.1 Bnh nn, c dung tch 50ml. A.2.2 Pipet nh mc, c dung tch thch hp. A.2.3 Giy lc khng tro. A.2.4 L nung, c th duy tr nhit 8000C250C A.2.5 Chn nung. A.2.6 Bnh ht m, cha cht ht m mnh (khng phi l axit sunfuric). A.2.7 Cn phn tch A.3 Cch tin hnh A.3.1 Sau khi chun (xem 5.4), chuyn lng cha trong b sc kh (E) v nc dng ra vo bnh nn (A.2.1); tng th tch s khong 25 ml. Thm 1 ml axit clohidric m c (A.1.2) v un n si. Thm 2 ml dung dch bari clorua tng git mt (A.1.1), khuy, sau ngui v yn 12 h. Thu ly cht kt ta to thnh trn giy lc (A.2.3), trc c thm t bng nc si. Ra cht kt ta mt ln bng 20 ml nc ct m, sau ra tip nm ln, mi ln bng 20 ml dung dch nc ra m (A.1.3). ro nc v cho kh. t giy lc v cht kt ta vo chn nung (A.2.5), c sy kh v cn chnh xc n 1mg v nung trong l (A.2.4) 2 h nhit 8000C250C. Ly ra khi l. Sau khi ngui trong bnh ht m (A.2.6), cn a v tro chnh xc n 1 mg. Xc nh s khc nhau ca khi lng bari sunfat thu c. A.3.2 Tin hnh kim tra bng phng php khi lng ca c hai ln xc nh theo 5.6. A.4 Biu th kt qu A.4.1 Phng php tnh v cng thc Hm lng sunfua dioxit, c biu th bng miligam trn kilogam sn phm, theo cng thc: 0,2745 m1 103 m trong m1 l khi lng bari sunfat thu c (xem A.2.6), tnh bng miligam; m c cng ngha nh trong 6.1;

0,2745 l khi lng sunfua dioxit tng ng vi 1 mg bari sunfat, tnh bng miligam. Ly kt qu l trung bnh cng ca hai ln xc nh, vi iu kin l tha mn c yu cu v lp li (xem A.4.2). A.4.2 lp li Chnh lch kt qu ca hai ln xc nh c tin hnh ng thi hoc k tip nhau, do mt ngi phn tch, khng c vt qu 5% gi tr trung bnh. A.5 Thng nht kt qu Kt qu thu c khng c sai khc qu 5% so vi dng phng php chun axit. Trong trng hp s khc nhau gia cc kt qu thu c bng phng php chun axit v phng php khi lng vt qu 5%, th ch bo co kt qu thu c bng phng php khi lng.

PH LC B
KIM TRA BNG PHNG PHP O C XC NH ION SUNFAT TO THNH BNG CHUN AXIT B.1 Thuc th B.1.1 Axit sunfuric, dung dch chun. Cho 31,2 ml dung dch axit sunfuric tiu chun nng c(1/2H2SO4)=0,1 mol/l(7) vo bnh nh mc dung tch 1 000 ml, thm nc cho n vch. 1 ml dung dch ny tng ng vi 0,1 mg SO2. B.1.2 Polyvinyl pyrolidon, dung dch 50g/l, khng cha ion sunfat (khi lng phn t trung bnh 85 000). B.1.3 Bari clorua v polyvinyl pyrolidon, dung dch hn hp. Trn 80 ml dung dch bari clorua 100 g/l vi 20 ml dung dch polyvinyl pyrolidon (B.1.2). B.1.4 Dung dch axit clohidric (xem 3.3). B.1.5 Dung dch cht ch th (xem 3.4). B.2 Thit b, dng c B.2.1 Bnh nh mc mt vch, c dung tch 50 ml ph hp vi yu cu ca ISO 1042. B.2.2 Pipet hoc buret, phn phi 2-4-8-12-16 ml v 25 ml. B.2.3 Quang ph k, thch hp o bc sng 650 nm. B.3 Cch tin hnh B.3.1 Chun b ng hiu chun Cho vo mt lot su bnh nh mc dung tch 50 ml (B.2.1): 0 2 4 8 12 v 16 ml dung dch axit sunfuric chun (B.1.1), 20 ml nc, 0,1 ml dung dch cht ch th (B.1.5), 1 ml dung dch axit clohidric (B.1.4) v 5 ml dung dch hn hp (B.1.3). Thm nc cho n vch v lc u. Cc dung dch thu c tng ng vi ln lt 0 0,2 0,4 0,8 1,2 v 1,6 mg sunfua dioxit. Sau khi thm dung dch hn hp (B.1.3) khong t 15 pht n 20 pht, dng quang ph k (B.2.3) o hp th ca mi dung dch bc sng 650nm.

Hitherto c biu th theo dung dch th tch chun 0,1N.

Dng ng hiu chun ca hp th nh mt bin thin ca hm lng sunfua dioxit, tnh bng miligam trn lt. B.3.2 Tin hnh xc nh B.3.2.1 Trng hp th tch V ca dung dch natri hidroxit 0,01 mol/l nh hn 5ml Sau khi chun (xem 5.4), chuyn lng cha trong b sc kh (E) v nc dng ra sang bnh nh mc mt vch dung tch 50 ml (B.2.1). Thm 1 ml dung dch axit clohidric (B.1.4) v 5 ml dung dch hn hp (B.1.3). Thm nc cho n vch v trn u. B.3.2.2 Trng hp th tch V ca dung dch natri hidroxit 0,01 mol/l t 5 ml n 10 ml Sau khi chun (xem 5.4), chuyn lng cha trong b sc kh (E) v nc dng ra sang bnh nh mc mt vch dung tch 50ml (B.2.1). Thm nc cho n vch v trn u. Chuyn 25 ml dung dch ny sang mt bnh nh mc mt vch dung tch 50 ml khc (B.2.1). Thm 1 ml dung dch axit clohidric (B.1.4) v 5 ml dung dch hn hp (B.1.3). Thm nc cho n vch v trn u. Sau khi thm dung dch hn hp (B.1.3), khong t 15 pht n 20 pht, s dng quang ph k (B.2.3) o hp th ca mi dung dch bc sng 650nm. B.3.3 S ln xc nh Tin hnh kim tra bng phng php o c ca c hai php xc nh trong 5.6 B.4 Biu th kt qu B.4.1 Nu vic kim tra c tin hnh theo B.3.2.1, th hm lng sunfua dioxit, c biu th bng miligam trn kilogam sn phm, tnh theo cng thc: C trong c l nng ca sunfua dioxit c t ng hiu chun (B.3.1) v tng ng vi hp th o c trong B.3.2.1, tnh bng miligam/lt; m c cng ngha nh trong 6.1 ; B.4.2 Nu vic kim tra c tin hnh theo B.3.2.2, th hm lng sunfua dioxit, c biu th bng miligam trn kilogam sn phm, tnh theo cng thc: C trong c c ngha nh trong B.4.1 v tng ng vi hp th o c trong B.3.2.2, tnh bng miligam/lt; m c cng ngha nh trong 6.1 B.4.3 Ly kt qu l trung bnh cng ca hai ln xc nh, vi iu kin l tha mn c yu cu v lp li xem (xem 6.2). B.5 Thng nht kt qu Kt qu thu c khng c chnh lch qu 5% so vi kt qu khi dng phng php chun axit. Trong trng hp s khc nhau gia cc kt qu thu c bng phng php chun axit v phng php o c vt qu 5%, th ch c bo co kt qu thu c bng phng php o c. 1000 2 m 1000 m