TIU CHUN VIT NAM TCVN 5496:1991 (ISO 2447 - 1974)

SN PHM RAU QU XC NH HM LNG THIC BNG PHNG PHP SO MU Li ni u TCVN 5496-1991 ph hp vi ISO 2447-1974. TCVN 5496-1991 do Trung tm Tiu chun - o lng - Cht lng ngh v c y ban Khoa hc Nh nc ban hnh theo quyt nh s 488/Q ngy 8 thng 8 nm 1991.

SN PHM RAU QU
XC NH HM LNG THIC BNG PHNG PHP SO MU Fruit and vegetable products-Determination-of tin by spectropho tometric method. Tiu chun ny quy nh phng php so mu xc nh hm lng thic trong cc sn phm rau qu m trong 1 kg c cha nhiu nht ti: - 1,25 g ng - 0,6 g ch - 0,6g km - 40g pht pho Tiu chun ny ph hp vi ISO 2447-1974. 1. Nguyn tc: Sau khi phn hy cc cht hu c bng axt sunfuric v axt nitric v chuyn ha thic v dng stanic, to thnh mt phc cht trong dung dch m c pH = 1,0 - 1,2 (nu cn th cho st (III) bng cch kh vi axt ascobic). Phc cht ny c nhum mu da cam vi phenylfluoron v mu ny c so snh vi cc mu thu c trong cng iu kin nhng t cc dung dch chun ca thit nguyn cht. 2. Thuc th: Cc thuc th em dng phi l loi tinh khit phn tch v nc phi l nc ct hoc loi nc t nht c tinh khit tng ng. Ngoi cc thuc th dng phn hy cc cht hu c cn cn dng cc thuc th di y: 2.1. Axit sunfuric 20 = 1,84g/ml. 2.2. Axit sunpuric, dung dch 2,5N. 2.3. Axit ascobic, dung dch 50g/l. 2.4. Ru polyvinyl dung dch 16g/l: Ha tan 1,6g ru polyvinyl trong mt t nc, c lm nng nh v khuy. Pha long thnh 100ml sau khi ngui. 2.5. Dung dch m cha 450g natri axetat (NaCH3COO) v 240ml axit axetic (CH3COOH) trong 1 lt nc. 2.6. Thic, dung dch chun cha 500 g/ml trong mi trng axit sunfuric c nng chng 6N.

Ha tan bng cch un nng 0,5g thic tinh khit trong hn hp 50ml axit sunfuric (2.1), 5ml axit nitric (20 = 1,42 g/ml v 25ml nc. Sau khi ha tan hon ton, oxy ha thic n dng stanic bng cch un si cho n khi bc khi trng. ngui, chuyn dung dch vo bnh nh mc 1000ml c sn 116ml axit sunfuric (2.1) v 100ml nc. ngui v pha long ti 1000 ml bng nc. 2.7. Thic, dung dch chun cha 10 g/ml trong mi trng axit sunfuric, nng chng 0,5N. Ly 20ml dung dch thic chun (2.6) cho vo bnh nh mc 1000 ml. Thm 10ml axit sunfuric (2.1) v pha long ti 1000ml bng nc. 2.8. Thuc th phnylfluoron (2, 6, 7 tri hydroxy 9-phenyl-3- izo-xanton). Ha tan 0,1g phenylfluoron trong x 10ml metanol v 1ml axit clohyric m c 20 = 1,19g/ml trong 1 bnh nh mc 500ml, Pha long bng etanol 95% (V/V) n vch mc. Thuc th phi ng trong l nu, ch ti v c bo qun khng qu 1 tun l. 3. Thit b v dng c: Cc thit b v dng c thng thng, nu khng c quy nh no khc, cng vi cc thit b, dng c phn hy cc cht hu c v c bit l: 3.1. Bnh nh mc mt vch, dung tch 50 v 200ml theo quy nh hin hnh. 3.2. Pipet, dung tch 1, 2, 3, 4, 5, 10 v 20ml theo quy nh hin hnh. 3.3. Ph quang k hay my so mu o di sng 500-530 mm vi knh lc mu xanh v t bo c ca s sng 10mm. 3.4. Cn phn tch: 4. Trnh t th: 4.1. Chun b lng mu cn: tt nht l cn mt khi lng mu chng 10g, chnh xc ti 0,01g. 4.2. Phn hy cht hu c: Sau khi phn hy mu xong thm vo dung dch thu c 5ml axit sunfuric (2.1). ngui ri chuyn vo bnh nh mc 200ml (3.1) v pha long bng nc ti vch mc (dung dch A). 4.3. So mu: 4.3.1. Dng pipet (3.2.) cho vo mt bnh nh mc 50ml(3.1) mt th tch thch hp dung dch A nh sau: - 20ml nu hm lng thic trong mu di 50 mg/kg. - 10ml nu hm lng thic trong mu t 50 ti 125mg/kg, pha long ti 20ml bng dung dch axit sunfuric (2.2). - 5ml nu hm lng thic trong mu trn 125mg/kg, pha long ti 20ml bng dung dch axit sunfuric (2.2). 4.3.2. Sau cho thm theo th t: - 10ml dung dch m (2.5); - 1ml dung dch axit ascobic (2.3);(1) - 5ml dung dch ru polyvinyl (2.4); - 3ml thuc th phenylfluoron (2.8). lc bnh trnh s hnh thnh bt ca ru polyvinyl. yn 5 pht.
(1)

Nu hm lng st (III) bng hoc nh hn 25mg/kg th khng cn thm axit ascobic.

Pha long bng nc ti vch mc v yn 30 pht na ri so mu bc sng 505mm trn ph quang k hay my so mu q quang in. 4.3.3. Tin hnh xc nh 2 ln trn cng mt mu ly phn hy cht hu c (xem 4.1) 4.4. Xy dng th chun: 4.4.1. Cho vo mt dy 6 bnh nh mc 50ml(3.1) mi bnh c sn 20ml dung dch axit sunfuric (2.2) nhng th tch dung dch thic chun(2.7) sau: - 0,ml tng ng vi 0 g thic - 1ml tng ng vi 10 g thic - 2ml tng ng vi 20 g thic - 3ml tng ng vi 30 g thic - 4ml tng ng vi 40 g thic - 5ml tng ng vi 50 g thic 4.4.2. Ri tin hnh nh quy nh mc 4.3.2 4.4.3. V th chun biu din s khc nhau ca mt quang l hm s microgam thic 5. Cch tnh: 5.1. Phng php tnh v cng thc: Bng th chun chuyn s liu c c (4.3.2) thnh micrgam thic. Hm lng thic (x) tnh bng miligam trong 1 kg sn phm c tnh theo cng thc:

X =
Trong :

m1 200 103 m1 x 200 x x = , 1000 V mo Vxmo

- mo: khi lng lng mu cn, tnh bng gam - m1: khi lng thic tm c trn th, tnh bng microgam - V: th tch dung dch A ly so mu, tnh bng mililit, (4.3.1) Ly trung bnh cng ca nhng ln xc nh lm kt qu, nu yu cu v lp li c tha mn (5.2). 5.2. lp li: Chnh lch kt qu gia hai ln xc nh song song hoc lin tip nhanh do cng mt ngi phn tch khng vt qu 5% gi tr trung bnh. 6. Bin bn th: Trong bin bn th phi ghi phng php th dng v kt qu t c. Cng phi cp n nhng iu kin thc nghim m tiu chun ny khng quy nh hay coi nh khng bt buc cng nh bt k nhng iu kin no c th nh hng ti kt qu. Bin bn th phi bao gm tt c nhng chi tit nhn bit y v mu th.