Li ni u TCVN 8134 : 2009 hon ton tng ng vi ISO 937 : 1978; TCVN B134 : 2009 do Ban k thut tiu

chun quc gia TCVNRRC/F8 Tht V Sn phm tht bin son, Tng cc Tiu chun o lng Cht lng ngh, B Khoa hc v Cng ngh cng b.

TIU CHUN QUC GIA

TCVN 8134 : 2009

Tht v sn phm tht - Xc nh hm lng nit (phng php chun)

Meat and meat products - Determination ofnitrogen content (Reference method)

1 Phm vi p dng Tiu chun ny qui nh phng php chun xc nh hm lng nit trong tht v sn phm ti 2). 2 Ti liu vin dn Cc ti liu vin dn sau rt cn thit cho vic p dng tiu chun ny. i vi cc ti liu vin dn ghi nm cng b th p dng phin bn c nu. i vi cc ti liu vin dn khng ghi nm cng b th p dng phin bn mi nht, bao gm c cc sa i, b sung (nu c). ISO 3100 (2) Tht v sn phm tht Ly mu. TCVN 7149 : 2007 ((ISO 385 : 2005), Dng c th nghim bng thu tinh - Buret. 3 Thut ng, nh ngha Trong tiu chun ny s dng cc thut ng v nh ngha sau y: Hm lng nit trong tht v sn phm tht (nitrogen content of meat and meat products):
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(Xem thm ISO 1871, Agricultural food products- Gnral directions for the detemination of nitorgen by the Kjeldahl method (sn phm lng thc, thc phm Hng dn chung xc nh nit bng phng php Kjeldah)l 2) ISO 3100 c thay th bng hai tiu chun ISO 3100-1: 1991 ( c bin son thnh TCVN 4833-1: 2002) v ISO 3100-2: 1991 ( c bin son thnh TCVN 4833-2: 2002). Hin nay, ISO 3100-1: 1991 b hu v c thay th bng ISO 17604: 2003 (c bin son thnh TCVN 7925: 2008 Vi sinh vt trong thc phm v thc n chn nui Phng php ly mu thn tht ti phn tch vi sinh vt)

Lng nit tng ng vi amoniac c sinh ra v xc nh c di cc iu kin quy nh trong tiu chun ny. 4 Nguyn tc Phn hu phn mu th bng axit sulfuric m c, dng ng (ll) sulfat lm cht xc tc, chuyn ha nit hu c thnh cc ion amoni; kim ho, chng ct amoniac gii phng vo trong dung dch axit boric d, chun bng axit clohydric xc nh amoniac lin kt vi axit boric v tnh hm lng nit ca mu t lng amoniac to thnh. 5 Thuc th Ch s dng cc thuc th loi tinh khit phn tch. Nc c s dng phi l nc c t hoc t nht l nc c tinh khit tng ng. 5.1 ng (ll) sulfat ngm nm phn t nc (CuSO4.5H2O). 5.2 Kall sulfat (K2SO4) khan. 5.3 Axlt sulfurlc, 20 = 1 ,84 g/ml. 5.4 Dung dch natrl hydroxit, khng cha cacbonat, cha khong 33 g natri hydroxit (NaOH) trong 100 g dung dch. Ho tan 500 g natri hydroxit trong 1000 ml nc. 5.5 Dung dch axlt boric Ho tan 40 g axit boric (H3BO3) trong nc v pha long bng nc n 1000 ml. 5.6 Axit clohydric, dung dch chun 0,1 N, bit nng ng lng n bn ch s thp phn. 5.7 Dung dch ch th: Ch th hn hp ( metyl-xanh metylen 3), c chun b bng cch ho tan 2 g metyl v 1 g xanh metylen trong 1000 ml etanol 95 % (th tch). S thay i mu ca dung dch ch th ny xut hin pH 5,4. Bo qun dung dch ch th trong l mu nu ni ti v mt. 5.8 Cht iu chnh si 5.8 Dng phn hu Bi thu tinh, silic cacbua hoc mnh s cng. 5.8.2 Dng chng ct Silic cacbua hoc cc vin bt va mi c nung. 6 Thit b, dng c S dng cc thit b, dng c ca phng th nghim thng thng, tr khi c qui nh khc v c th nh sau: 6.1 My xay tht bng c, c phng th nghim, c gn tm c l, ng knh l khng qu 4 mm. 6.2 Giy khng thm m, c kch thc khong 9 cm x 6 cm. 6.3 Buret. 50 ml ph hp vi loi A ca TCVN 7149 : 2007 (ISO 385 : 2005).
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I khi ch th bit l Tashiro

6.4 Bnh Kjeldahl, dung tch khng ln hn 800 ml, c bu thu tinh hnh qu l y knh, nu cn. 6.5 Thit b chng ct bng hi, hoc thit b chng ct thng thng. 6.6 Thit b gia nhit, lm nng bnh Kjeldahl t th nghing sao cho ngun nhit ch tip xc vi thnh bnh thp hn mc cht lng. Khi s dng kh t, th nn dng tm aming thch hp c l trn sao cho ch phn di ca bnh tip xc vi ngn la. 6.7 bung ht khi hiu qu, dng ht khi axit thot ra trong qu trnh phn hu. 6.8 Cn phn tch 7 Ly mu 7.1 ly t nht 200 g mu i din. Xem ISO 3100. 7.2 Bo qun mu sao cho mu khng b gim cht lng v khng b thay i thnh phn. Nu s dng cht bo qun th cc cht ny khng c cha cc hp cht nit vi lng c th o c. 8. Cch tin hnh 8.1 Chun b mu th Dng my xay tht (6.1) xay mu t nht hai ln v trn u thu c mu ng nht. Bo qun mu ng nht trong vt cha kn kh, y np vt cha v bo qun sao cho khng lm gim cht lng v thay i thnh phn ca mu. Phn tch mu cng sm cng tt, ch trong vng 24 h sau khi ng ho. 8.2 Phn mu th Cho mt t cht iu chnh si (5.8) vo bnh Kjeldahl (6.4) sau thm khong 15 g ka li sulfat khan (5.2) v 0,5 g ng (ll) sulfat (5.1). Cn khong 2 g mu th (8.1) (hoc 1,5 g i vi mu giu cht bo), chnh xc n 0,001 g, cho ln giy khng thm m (6.2). Chuyn giy khng thm m v phn mu th vo bnh Kjeldahl. 8.3 Xc nh Thm 25 ml axit sulfuric (5.3) vo bnh Kjeldahl. Trn nh bng cch xoay bnh cha cht lng. C th chn bu thu tinh hnh qu l vo c bnh bng cch cho u nhn xung di, nu cn. t bnh t th nghing (nghing khong 40o so vi chiu thng ng) ln thit b gia nhit (6.6). u tin, un nh bnh cho n khi ngng si bt v mu hon ton ho lng. Sau phn hu bng cch cho si mnh, thnh thong xoay bnh, cho n khi dch lng tr nn trong sut v c mu xanh lam nht. Gi dung dch lng si thm 90 min. Tng thi gian phn hu khng t hn 2 h. Tin hnh cn thn khng cht lng ngng t chy trn ra ngoi bnh. Trnh lm tht thot qu nhiu axit sulfuric do b qu nhit trong qu trnh phn hu, iu ny c th dn n hao ht nit.

 ngui n khong 40 oC v cn thn thm khong 50 ml nc. Trn u v ngui. Dng ng ong rt 50 ml dung dch axit boric (5.5) vo bnh nn dung tch 500 ml, thm 4 git dung dch ch th (5.7), trn u v t bnh di bnh ngng ca thit b chng ct (6.5) sao cho u ra ca ng ni nhng trong cht lng. X l lng cha trong bnh Kjeldahl bng mt trong nhng cch sau y: a) Trong trng hp chng ct bng hi Chuyn lng cha trong bnh Kjeldahl sang thit bchng ct v trng bnh bng khong 50 ml nc. Dng ng ong cho thm 100 ml dung dch natri hydroxit (5.4), rt cn thn dc theo nghing c bnh sao cho hai lp trong bnh khng b khuy trn. Gn ngay bnh cu vo u phun ca thit b chng ct. un nng dung dch kim bng cch cho hi i qua cho n si v gi si trong 20 min. u tin un nng nh gim thiu s si bt. Th tch thu c ca dch ct phi t nht l 150 ml. b) Trong trng hp chung ct bnh thng Cn thn pha long lng cha trong bnh Kjeldahl bng khong 300 ml nc v xoay bnh. Chuyn vo bnh 1 lt, nu cn. Sau khong 15 min , dng ng ong cho thm 100 ml dung dch natri hydroxit (5.4), rt cn thn dc theo nghing c bnh sao cho hai lp trong bnh khng b khuy trn. Gn ngay bnh vo u phun ca thit b chng ct. Chng ct t nht 150 ml dch lng, ngay c khi hn hp si khng u. Tip tc chng ct cho n khi hn hp bt u si hoc cho n khi thu c 250 ml dch ct. m bo rng dch ct thc s ngui v trnh cho dung dch axit boric m ln. Trong c hai trng hp, h thp bnh nn ngay trc khi kt thc chng ct, sao cho u ra ca ng ni cao hn mc dch lng. Trng u ra ca ng ni trn dch lng (pha trong v pha ngoi) bng mt t nc. Kim tra vic kt thc chng ct amoniac bng giy qu , c lm m bng nc ct; mu khng c nh hng bi dch lng chy nh git t bnh ngng. Ngng gia nhit. Nu cho thy cha hon thnh qu trnh chng ct, th tin hnh php xc nh mi, tun th cc hng dn. Chun lng cha trong bnh nn bng dung dch axit clohydric (5.6). Ghi li th tch ca dung dch axit clohydric dng, tnh chnh xc n 0,02 ml. Tin hnh hai ln xc nh trn cc phn mu th ly t cng mt mu th. 8.4 Php th trng Thng thng, thc hin php th trng (th kp) khi s dng cc m thuc th mi hoc dung dch va mi c chun b. Nn tin hnh php th trng i vi thuc th v dung dch s dng vi ln.

Tin hnh php th trng theo 8.3, ch dng giy khng thm m (6.2). 9 Biu th kt qu 9.1 Phng php tnh v cng thc Hm lng ni t ca mu, biu th theo phn trm khi lng, tnh bng cng thc:
0,0014 x(V1 V0 ) x 100 m

trong Vo l th tch ca dung dch axit clohydnc 0,1 N dng cho php th trng, tnh bng mililit (ml); V1 l th tch ca dung dch axit clohydnc 0,1 N dng cho php xc nh, tnh bng mililit (ml); m l khi lng ca phn mu th, tnh bng gam (g). Ch thch dung dch axit clohydric chun c dng khng ng nh nng nu trong 5.6. th s dng h s hiu chnh thch hp trong tnh kt qu. Kt qu l trung bnh cc kt qu ca hai ln xc nh, nu p ng yu cu v lp li (9.2). Bo co kt qu chnh xc n 0,01 g ni t trn 100 g mu. 9.2 lp li Chnh lch gia cc kt qu ca hai ln xc nh tin hnh ng thi hoc lin tc nhanh khi s dng cng mt phng php phn tch khng c ln hn 0,10 g ni t trn 100 g mu. 10 Ch vi cch tin hnh 10.1 php xc nh phi c tin hnh trong phng khng c hi amoniac. 10.2 Cng c th xc nh ni t trong phn dch lng ca lng cha trong bnh Kjeldahl. Trong cc iu kin ny, cn iu chnh cho ph hp vi thit b v quy trnh (lng v nng ca thuc th s dng, thi gian chng ct, th tch dch ct). Vic iu chnh ny phi nu trong bo co th nghim. 10.3 ni t c ngun gc t cc hp cht phi-protein s khng tnh n trong php xc nh v s cho cc kt qu khng chnh xc v hm lng protein nu protein c tnh t hm lng ni t. Ngoi vic kt qu tnh theo ni t, nu cn biu th kt qu theo protein, th kt qu cn ch ra h s chuyn i dng. 11 Bo co th nghim Bo co th nghim cn ch r phng php s dng v kt qu thu c, tnh theo ni t; cng cn ch r nu kt qu tnh theo protein, h s

c s dng cho. Bo co th nghim cng cn cp n mi chi tit thao tc khng c quy nh trong tiu chun ny, hoc c xem l tu (trong trng hp c th, nu php xc nh c tin hnh trn phn dch lng - xem 10.2), cng vi mi tnh hung bt thng c th nh hng n kt qu. Bo co th nghim cng phi bao gm mi chi tit cn thit nhn bit y v mu.