tcvn

tIu chun vIt nam

TCVN 6760 : 2000 iso 9832 : 1992

du m ng vt v thc vt xc nh d lng hexan k thut

Animal and vegetable fats and oids Determination of residual technical hexane content

H ni -2000

Li ni u
TCVN 6760 : 2000 hon ton tng ng vi ISO 9832 : 1992. TCVN 6760 : 2000 do Ban k thut tiu chun TCVN/TC/F2 Du m ng vt v thc vt bin son, Tng cc Tiu chun o lng Cht lng ngh, B Khoa hc, Cng ngh v Mi trng ban hnh.

TCVN 6760 : 2000

TIu chun vIt nam

tcvn 6760 : 2000

Du m ng vt v thc vt Xc nh d lng henxan k thut

Animal and vegetable fats and oils Determination of residual technical hexane content

Phm vi p dng

Tiu chun ny qui nh phng php xc nh d lng henxan k thut ca du m ng vt v thc vt (gi l cht bo). Phng php ny thch hp cho vic xc nh hm lng hexan trong khong t 10 mg n 1500 mg trn kilogam cht bo. Phng php ny khng p dng cho cc loi du c bin.

2 Tiu chun trch dn

TCVN 6128 :1996 (ISO 661 : 1989), Du m ng vt v thc vt - Chun b mu th

nh ngha

Trong tiu chun p dng nh ngha sau y : 3.1 D lng henxan k thut : hm lng cc hidrocacbon bay hi b gi li trong cht bo khi ch bin c dng n cc dung mi hidrocacbon, xc nh bng phng php qui nh trong tiu chun ny. D lng hexan k thut c biu th bng miligam henxan trn kilogam mu.

Nguyn tc

Kh hp th hidrocacbon bay hi bngc cch un nng nhit 800C trong bnh y kn sau khi cho thm cht chun ni. Xc nh hm lng hidrocacbon bay hi c th trong khong trng pha trn bng sc k kh khi s dng ct nhi hoc ct mao dn.

TCVN 6760 : 2000

5 Thuc th

Ch s dng cc thuc th phn tch nu khng c qui nh khc. 5.1 Henxan k thut, c thnh phn ging thnh phn ca henxan c s dng trong sn xut cng nghip, hoc, nu khng sn c s dng n-henxan. Ch thch 1 - Khuyn co rng nn s dng henxan k thut hiu chun. Thuc th ny thng c hm
lng n - hexan 50 % (m/m) v cha phn ln hidrocacbon C5 v C7. cc cht ng phn C6 nhng cng c th cha c

5.2 Cht ni chun, n-heptan. Nu khng sn c n-heptan th c th s dng xyclohexan, vi iu kin l dung mi (5.1) s dng trit hoc hiu chun c hm lng khng ng k ca xyclohexan v / hoc n-heptan hoc cc thnh phn khc c thi gian lu tng t. 5.3 Kh mang, th d : hidro, nit hoc heli... kh k v c hm lng oxi nh hn 10 mg/kg.

5.4 Kh ph tr, hidro (99,9 % tinh khit, khng cha cc tp cht hu c) v khng kh ( khng cha cc tp cht hu c). 5.5 Cht bo hiu chun, m thc vt kh mi v mi tinh ch, cha mt lng hexan k thut

khng ng k. Ch thch 2 - Cht bo hiu chun ny khng nn cha peroxit hoc cc thnh phn khc lm phn hu
to thnh cht bay hi m c th gy nhm ln vi hidrocacbon trong qu trnh th nghim.

6 Thit b, dng c
S dng cc thit b dng c ca phng th nghim thng thng v c bit nh sau: 6.1 Cc l nh vi lp mng ngn, dung tch 20 ml. 6.2 Mng ngn, tr vi cht bo v dung mi, c lm bng vt liu nh cao su butyl hoc cao su

khng cha cc cn dung mi hidrocacbon v c cht lng thch hp chng khng n ra trong khi s dung, np nhm l thch hp dng vi l (6.1) v kp gp. 6.3 Kp, thch hp gi cc l nh (6.1). 6.4 Xy lanh, c dung tch 10 l ch s dng phn tch d lng hexan k thut. Khng c ra chng bng dung mi hidrocacbon. 6.5 Xy lanh, dung tch 1l ch s dng phn tch d lng hexan k thut. Khng c ra chng

bng dung mi hidrocacbon. 6.6 Xy lanh kh kn, dung tch 1000 l ch s dng phn tch d lng hexan k thut. Khng c ra chng bng dung mi hidrocacbon. 6.7 Sc k kh, c detector ion ho ngn la v b phn tch v / hoc b ghi, c trang b vi hoc l: a) ct thu tinh nhi, di 2 m n 4 m v c ng knh trong khong 3,2 mm, c nhi bng

TCVN 6760 : 2000

diatomit ra bng axit, c c ht t 150 m n 180 m (Chromosorb P NAW 60-80 mesh l thch hp)
1)

, c ph bng 10% squalance hoc bt k pha no khc tch c sc ph theo yu cu,

hoc . b) ct mao dn thu tinh, di khong 30 m v c ng knh trong khong 0,3 mm, c ph bng

mng mng metylpolyxyloxan 0,2 m. Nhit tim v pht hin phi 1000 C v nhit t sy 500 C. Nu s dng ct mao dn [xem b)], th thit b phi c h thng tim tch 1/100. Ch thch 3 - phn tch hng lot, th sc k kh bung khng gian hi vi tim mu t ng l thch hp.
Trong trng hp ny tim tay l khng thch hp.

6.8 Ni un nng, c trang b b kp gi cc l, c iu chnh nhit 800 C 20 C. Ch thch 4 - thc hin lin tc, nn dng glyxerol lm mi trng un nng. 6.9 My lc.

7 Ly mu
iu quan trng l phng th nghim nhn c ng mu i din v khng b h hng hoc thay i trong sut qu trnh vn chuyn v bo qun. Vic ly mu khng quy nh trong tiu chun ny. Nn ly mu theo TCVN 2625 : 1999 (ISO 5555) 2) . Bo v mu trnh hp th thm hoc tht thot dung mi.

8 Chun b mu th
Chun b mu th theo TCVN 6128 : 1996 (ISO 661), ch trnh b hp th thm hoc tht thot dung mi.

9 Cch tin hnh

9.1 Hiu chun 9.1.1 Cn 5 g cht bo hiu chun (5.5) chnh xc n 0,01 g cho vo tng l trong dy by l (6.1). y cc l bng mng ngn v np (6.2). Dng xy lanh (6.4 hoc 6.5) ly lng dung mi (5.1) nh qui nh trong bng 1 cho vo su trong by l (6.1) thu c cc nng qui nh. Khng cho dung mi vo l th by.

1)

Chromosorb P NAW 60 - 80 l v d v sn phm ph hp, d tm thy trong thng mi. Thng tin ny

ch a ra s tin li cho ngi s dng tiu chun ny v khng xc nhn sn phm trong ISO.
2)

ISO 5555 : 1999 - Du m ng vt v thc vt - Ly mu.

TCVN 6760 : 2000

Lc mnh su l thm dung mi bng my lc (6.9) khong 1 h nhit phng. 9.1.2 Cui giai on ny dng xy lanh (6.4) tim 5 l 0,1 l cht ni chun (5.2) vo tt c by l qua mng ngn.
Ch thch - i vi nng hexan t 10 mg/kg, thch hp nht l thm 2 l cht chun ni (5.2)

Bng 1 - Hm lng hexan trong cc mu hiu chun Th tch dung mi (5.1) c cho thm l 0,5 1 2 4 7 10 hexan k thut 67 134 268 536 938 1340 n- hexan 66 132 264 528 924 1320 Hm lng hexan (mg/kg) khi s dng

Trn tht mnh lng cha trong l khong 1 pht bng cch dng tay xoay trn theo mt phng nm ngang sao cho cht bo khng chm n mng ngn. Nu cht bo chm n mng ngn th hu b l ny v bt u lm li vi phn cht bo hiu chun khc.

Ch thch 6 - Nu cht bo dnh vo mng ngn th n s nhim bn kim tim khi ly mu v cht nhim
bn c th truyn sang ct; iu rt quan trng khi s dng ct mao dn l phi trnh s nhim bn ny.

C sau khong 15 pht (tc l thi gian lu ca cht hi chun), t ngay mt l ngp n tn c trong b un nng (6.8) 80o C cht bo v pha kh t c cn bng. 9.1.3 T mi l c lm nng b un nng trong 60 pht 1 pht, dng xi lanh (6.6) c lm m n 60oC ly 1000 l pha kh (vn nguyn trong b un nng). Tim ngay pha kh ly vo sc k kh.

9.1.4

T sc tng ng vi l th by khng cho thm dung mi, tnh hm lng hexan Ac, biu th

bng phn trm ca tng din tch pic. 9.1.5 T sc tng ng vi mi l cho thm dung mi, tnh h s hiu chun F theo cng thc sau:

TCVN 6760 : 2000 F=

trong Ac l hm lng hexan tnh c trong 9.1.4; ais l hm lng cht ni chun c trong cht bo hiu chun (5.5) c thm dung mi, tnh bng phn trm ca tng din tch pic. At l hm lng hidrocacbon tng s, k c cht ni chun c trong cht bo hiu chun (5.5)

wh Ais ( At Ac Ais ) wis

c thm dung mi, tnh bng phn trm ca tng din tch pic. Wh l hm lng dung mi (5.1) c trong cht bo hiu chun (5.5) c thm dung mi, tnh

bng miligam trn kilogam; wis l hm lng cht ni chun c trong cht bo hiu chun (5.5) c thm dung mi, tnh

bng miligam trn kilogam, tc l 680 i vi n-heptan hoc 780 i vi xyclohexan. Ch thch 7 - Nu ch cho thm 2 l trong 9.1.2 th Wis s bng 272 i vi n-heptan hoc 312 i vi xyclohexan. Ly kt qu n ch s th ba sau du phy. Cc h s hiu chun ca su mu hiu chun phi xp x bng nhau. Tnh gi tr trung bnh F, s khong 0,45 i vi heptan. H s F tnh c c th s dng xc nh cc hm lng hexan mc nh hn 60 mg/kg. Nu gi tr F tm c i vi l cha 0,5 l dung mi (5.1) thp hn ng k so vi gi tr trung bnh F, th sai lch ny c th l do kh khn trong vic ly chnh xc 0,5 l v loi b php xc nh ny v lp li php xc nh mi. H s tiu chun trung bnh i vi xyclohexan thng thng khong 0,5 7v i vi n-heptan l khong 0,45. 9.2 Tin hnh xc nh 9.2.1 Cn 5 g phn mu th (iu 8), chnh xc n 0,01 g cho vo l (6.1) cng nhanh cng tt. y

mng ngn v np (6.2). 9.2.2 Dng xy lanh (6.4) tim 5 l cht chun ni (5.2) qua mng ngn. Trn tht mnh lng cha trong l khong 1 pht bng cch dng tay xoay trn theo mt phng nm ngang sao cho cht bo khng chm n mng ngn. Nu cht bo chm n mng ngn th hu b l ny v bt u lm li vi phn cht bo hiu chun khc. (Xem ch thch 6 trong 9.1.2). t l ngp n c trong ni un nng (6.8) nhit 80o C trong 60 pht 1 pht. 9.2.3 Dng xy lanh (6.6) c lm m n 60oC ly 1000 l pha kh trong khi vn nguyn l

trong b un nng. Tim ngay pha kh ly vo sc k kh. 9.2.4 Xc nh hm lng d lng hexan k thut ca mu t sc (xem th d hnh 1), o cc pic

nhn bit c l ca hexan v khng phi ca cc sn phm phn hu. 9.3 S php xc nh

TCVN 6760 : 2000

Tin hnh xc nh lin tc trn hai phn mu th ca cng mt mu th.

10 Biu th kt qu
Hm lng hexan k thut ca mu, w, tnh bng miligam trn kilogam theo cng thc:

w= trong

At t A,is F w ,is A,is

A'is l hm lng cht ni chun, tnh bng phn trm ca tng din tch pic; A't l hm lng hydrocacbon tng s, k c cht ni chun, ca mu th, tnh bng phn trm ca tng din tch pic.

F l h s hiu chun trung bnh xc nh c trong 9.1.5.

w'is l hm lng cht ni chun c trong mu, tnh bng miligam trn kilogam, tc l 680 i vi

n-heptan hoc 780 i vi xyclohexan. Ly kt qu cui cng l trung bnh cng ca hai php xc nh (9.3), vi iu kin tho mn yu cu v lp li (xem 11.2). Nu khng tho mn yu cu v lp li, hu b kt qu v tin hnh hai php xc nh mi trn cc phn mu th ly t cng mt mu th.

TCVN 6760 : 2000

11

chnh xc

11.1 Kt qu th ca lin phng th nghim Mt th nghim ca lin phng th nghim do IUPAC thc hin nm 1985, trong mi phng th nghim tin hnh cc php xc nh kp, cho cc kt qu thng k trong bng 2 (ph hp vi ISO 5725) 3). 11.2 lp li Kt qu ca hai ln th ring r, c lp thu c khi s dng cng mt phng php, tin hnh trn cng vt liu trong phng th nghim, do mt ngi phn tch dng mt loi dng c, tin hnh trong khong thi gian ngn, phi nm trong phm v ca cc gi tr trung bnh trong bng 2, chnh lch tuyt i gia hai kt qu th thu c khng vt qu gii hn lp li c qui v ni suy tuyn tnh t s liu trong bng 2. Ch thch 8 - Nn ch rng, cc gi tr v ti lp R trong bng 2 p dng trong trng hp c bit, khi so snh
cc kt qu xc nh c lp thu c bi hai phng th nghim. Khi thc hin phng php m t v tt nht l so snh cc kt qu cui cng (cc kt qu ny thu c t cc php xc nh kp) thu c bi hai phng th nghim, cc kt qu R nn c i v xc sut 95% cc gi tr ti hn khc nhau, CrD95 c th p dng cho trung bnh ca cc ln xc nh dng cng thc sau:

CrD95 =

( R 2 r 2 / 2)

12 Bo co kt qu
Bo co kt qu phi ch r : - phng php ly mu (nu bit); - phng php s dng; - cc kt qu th nghim thu c v - nu kim tra lp li, nu kt qu cui cng thu c; Bo co kt qu cng phi cp n tt c cc chi tit c cc chi tit thao tc khng qui nh trong tiu chun ny, hoc tu la chn, cng vi cc chi tit bt thng no khc c th nh hng ti kt qu Bo co kt qu cng bao gm tt c cc thng tin cn thit v vic nhn bit y nmu th. _____________________
3)

ISO 5725 : 1986 - chnh xc ca cc phng php th -Xc nh lp li v ti lp ca phng

php th chun bng cc th nghim ca lin phng th nghim.

TCVN 6760 : 2000

Bng 2 - Cc kt qu thng k ca th nghim lin phng th nghim Mu S phng th nghim S phng th nghim cn li sau khi tr ngoi l Gi tr trung bnh ca d lng henxan k (mg/kg) lch chun ca lp li, sr (mg/kg H s bin thin ca lp li (%) lp li, r = 2,83 sr (mg/kg) lch chun ca ti lp,sR (mg/kg) H s bin thin ca ti lp (%) ti lp, R=2,83 sR (mg/kg)
1)

1 16 16 2,95 0,65 22,4 1,8 2,6 89 7,4

2 16 16 13,7 1,70 12,2 4,8 4,1 30 12

3 11 9 104 7,6 7,3 21 28,4 27 80

4 11 10 1048 71,5 6,8 202 293 28 829

Ch thch - Cc s liu i vi mu 1cng c tnh n mc d nm ngoi phmvi p dng ca tiu chun ny. 1) Mu 1:du lc thc phm mi ch bin + 3,3 ppm hexan k thut Mu 2 : du lc mi ch bin bo qun + 13,2 ppm hexan k thut Mu 3 : du ht ci th ( p )+100 ppm hexan k thut Mu 4 : du ht ci th ( p) +1000 ppm hexan k thut

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10