Chat Lam Bong

7/27/2019 Chat Lam Bong

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V PH GIA THC PHM - CHT LM BNG

National technical regulation on Food Additive Glazing agent

I. QUY NH CHUNG

1. Phm vi iu chnh

Quy chun k thut quc gia (sau y gi tt l Quy chun) ny quy nh cc yu cuk thut v qun l v cht lng, v sinh an ton i vi cc cht lm bng c s dngvi mc ch lm ph gia thc phm.

2. i tng p dngQuy chun ny p dng i vi:

2.1. T chc, c nhn nhp khu, xut khu, sn xut, bun bn v s dng cccht lm bng lm ph gia thc phm (sau y gi tt l t chc, c nhn).

2.2. C quan qun l nh nc c lin quan.

3. Gii thch t ng v ch vit tt:

3.1. Cht lm bng: l ph gia thc phm c cho thm vo b mt pha

ngoi ca thc phm nhm to bng hoc to lp bo v.3.2. JECFA monograph 1 - Vol. 4 (JECFA monographs 1 - Combined

compendium of food additive specifications; Joint FAO/WHO expert committee onfood additives; Volume 4 - Analytical methods, test procedures and laboratorysolutions used by and referenced in the food additive specifications; FAO, 2006): Ccyu cu k thut i vi ph gia thc phm, Tp 4 Cc phng php phn tch, quytrnh th nghim, dung dch th nghim c s dng (hoc tham chiu) trong yucu k thut i vi ph gia thc phm; JECFA bin son; FAO ban hnh nm 2006.

3.3. M s C.A.S (Chemical Abstracts Service): M s ng k ha cht ca

Hip hi Ha cht Hoa K.

3.4. TS (test solution): Dung dch thuc th.

3.5. ADI (Acceptable daily intake): Lng n vo hng ngy chp nhn c.

3.6. INS (International numbering system): H thng m s quc t v ph giathc phm.


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II. YU CU K THUT, PHNG PHP TH V LY MU

1. Yu cu k thut v phng php th i vi cc cht lm bng c quynh ti cc ph lc ban hnh km theo Quy chun ny nh sau:

1.

1.

Ph lc

1:

Yu cu k thut v phng php th i vi spong1.

2.Ph lc2:

Yu cu k thut v phng php th i vi spCandelila

1.3.

Ph lc3:

Yu cuk thut v phng php th i vi Shellac1.4.

Ph lc4:

Yu cu k thut v phng php th i vi dukhong

1.5.

Ph lc5:

Yu cu k thut v phng php th i vi spvi tinh th

2. Cc yu cu k thut quy nh trong Quy chun ny c th theo JECFA

monograph 1 - Vol. 4, ngoi tr mt s php th ring c m t trong cc ph lc.Cc phng php th c hng dn trong Quy chun ny khng bt buc phip dng, c th s dng cc phng php th khc tng ng.

3. Ly mu theo hng dn ti Thng t 16/2009/TT-BKHCN ngy 02 thng 6nm 2009 ca B Khoa hc v Cng ngh v hng dn kim tra nh nc v cht

lng hng ha lu thng trn th trng v cc quy nh khc ca php lut c linquan.

III. YU CU QUN L

1. Cng b hp quy

1.1. Cc cht lm bng phi c cng b ph hp vi cc quy nh ti Quychun ny.

1.2. Phng thc, trnh t, th tc cng b hp quy c thc hin theo Quynh v chng nhn hp chun, chng nhn hp quy v cng b hp chun,cng b hp quy ban hnh km theo Quyt nh s 24/2007/Q-BKHCN ngy 28thng 9 nm 2007 ca B trng B Khoa hc v Cng ngh v cc quy nhca php lut.

2. Kim tra i vi cht lm bng

Vic kim tra cht lng, v sinh an ton i vi cc cht lm bng phi thc

hin theo cc quy nh ca php lut.

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IV. TRCH NHIM CA T CHC, C NHN

1. T chc, c nhn phi cng b hp quy ph hp vi cc quy nh k thutti Quy chun ny, ng k bn cng b hp quy ti Cc An ton v sinh thcphm v bo m cht lng, v sinh an ton theo ng ni dung cng b.

2. T chc, c nhn ch c nhp khu, xut khu, sn xut, bun bn v s dngcc cht lm bng sau khi hon tt ng k bn cng b hp quy v bo m chtlng, v sinh an ton, ghi nhn ph hp vi cc quy nh ca php lut.

V. T CHC THC HIN

1. Giao Cc An ton v sinh thc phm ch tr, phi hp vi cc c quan chcnng c lin quan hng dn trin khai v t chc vic thc hin Quy chun ny.

2. Cn c vo yu cu qun l, Cc An ton v sinh thc phm c trch nhimkin ngh B Y t sa i, b sung Quy chun ny.

3. Trng hp hng dn ca quc t v phng php th v cc quy nhca php lut vin dn trong Quy chun ny c sa i, b sung hoc thay th thp dng theo vn bn mi.

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Ph lc 1

YU CU K THUT V PHNG PHP TH

I VI SP ONG

1. Tn khc, ch s Beeswax

INS 901

2. nh ngha Sp ong c ly t t ong mt (h Apidae, v d Apismellifera L) sau khi rt ht hoc ly tm ht mt ong. Tong c lm chy vi nc nng, hi nc hoc phidi nh mt tri, sau sn phm tan chy c lc vng thnh bnh sp ong vng. Sp ong trng thu cbng cch ty trng sp ong vng dng cc cht oxy hanh hydro peroxyd, acid sulfuric, hay nh sng mt tri. Spong l mt hn hp cc ester ca cc acid bo v cn bo,cc hydrocarbon v acid bo t do, v c mt phn nh cccn bo t do.

M s C.A.S. 8006-40-4 (sp ong vng)

8012-89-3 (sp ong trng)

3. Cm quan Sp ong vng: cht rn mu vng hoc nu sng, khi lnhth d v, khi v to thnh ming m c, dng ht, khngc dng tinh th, nhit khong 35C tr nn mm do.C mi c trng ca mt ong.

Sp ong trng: cht rn mu trng hay mu trng ng (lpmng thng trong m), c mi nh c trng ca mt ong.

4. Chc nng Cht lm bng, cht gii phng, cht n nh, cht to ktcu cho ko cao su, cht mang cho ph gia thc phm (baogm mang hng v mang mu), cht lm c.

5. Yu cu k thut

5.1. nh tnh

tan Khng tan trong nc, t tan trong cn, rt d tan trongether.

5.2. tinh khitKhong nng chy 62 65C

Ch s acid 17 24

Ch s peroxyd Khng c qu 5,0. (xem m t trong phn Phng phpth)

Ch s x phng ha 87 104

Sp carnauba t yu cu (xem m t trong phn phng php th)

Ceresin, parafin v mts sp khc

t yu cu (xem m t trong phn phng php th).

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Cht bo, sp Nhtbn, colophan v xphng

t yu cu (xem m t trong phn phng php th).

Glycerin v cc polyol

khc

Khng c qu 0,5% (tnh theo glycerin)

(xem m t trong phn phng php th).Ch Khng c qu 2,0 mg/kg.

6. Phng php th

6.1. tinh khit

Ch s peroxyd Cn chnh xc 5 g mu vo bnh nn 200 mL. Thm 30 mLdung dch cloroform v acid acetic (TT) 2:3 v y nt bnhnn. Lm nng mu trong nc m v xoy trn ha tanmu. ngui n nhit phng v thm 0,5 mL dung dchkali iodid bo ha. y bnh nn bng nt v lc mnh trong

60 5 giy. Thm 30 mL nc lc u v chun ngaybng dung dch natri thiosulfat dng ch th h tinh bt (TT).Tin hnh thm trn mt mu trng.

Ch s peroxyd =m

1000N)ba(

Trong :

a = s mL natri thiosulfat dng cho mu thb = s mL natri thiosulfat dng cho mu trng

N = nng ng lng ca natri thiosulfat

m = khi lng mu (g)

Sp carnauba Cn khong 100 mg mu th vo mt ng nghim, thm 20mL n-butanol. Nhng ng nghim vo chu nc ang si,lc hn hp nh nhng n khi mu th ha tan hon ton.Chuyn mu trong ng nghim vo mt cc c m cha nc 60C, v yn cho nc ngui xung nhit phng. Mt

khi xp cc tinh th mn ging hnh kim to thnh, tch khilp dung dch m trong sut. Di knh hin vi, cc tinh thxp hnh kim hoc cc bi hnh sao, khng c khi v nhhnh, chng t khng c sp carnauba.

Ceresin, parafin v mts loi sp khc

Cn 3,0 g mu vo mt bnh cu y trn 100 mL, thm 30mL dung dch kali hydroxyd 4% (kl/tt) trong ethanol khngcha aldehyd v un nh di ng sinh hn hi lu trong 2gi. Tho b ng sinh hn, nhng ngay vo mt nhit k.Ngm bnh vo chu nc 80C v cho ngui, lin tc lcxoy trn bnh. Khng c c kt ta trc khi nhit tn 65C, mc d dung dch c th trng c.

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Cht bo, sp Nhtbn, colophan v xphng

un 1 g mu vi 35 mL dung dch natri hydroxyd 1:7 trong 30pht, gi nguyn th tch bng cch thnh thong thm nc,ri ngui hn hp. Sp s tch ra, v dung dch vn trongsut. Lc hn hp lnh v acid ha dch lc bng acidhydrocloric. Khng c kt ta to thnh.

Glycerin v cc polyolkhc

Cho 0,20 g mu vo mt bnh cu y trn, thm 10 mL dungdch kali hydroxyd trong ethanol (TT), ni sinh hn hi lu vun trong mt bnh cch thy trong 30 pht. Thm 50 mL acidsulfuric long (TT), ngui v lc. Ra bnh v phu lcbng acid sulfuric long (TT). Gp dch chit v dch ra, phalong thnh 100,0 mL acid sulfuric long (TT). Ly 1,0 mLdung dch vo mt ng nghim, thm 0,5 mL dung dch natriperiodat 1,07% (kl/tt) trong nc, lc u v yn trong 5pht. Thm 1,0 mL dung dch fuchsin lm mt mu (xem di), lc u. Kt ta phi tan ht. t ng vo mt cc cm cha nc 40C. ngui, quan st trong khong 10

15 pht. Nu dung dch chuyn thnh mu tm xanh, muphi khng c m hn mu dung dch chun pha ngthi theo cch tng t nhng dng 1,0 mL dung dchglycerin 0,001% (kl/tt) trong acid sulfuric long (TT).

Dung dch fuchsin c kh mu

Ha tan 0,1 g fuchsin dng base trong 60 mL nc. Thmdung dch gm 1 g natri sulfit khan (tinh khit thuc th) trong10 mL nc. Thm t t 2 mL acid hydrocloric, va thm valc lin tc. Thm nc n 100 mL. yn, trnh nhsng trong vng t nht 12 gi, loi mu bng than hot tnhv lc. Nu dung dch tr nn c, lc trc khi dng. Nusau khi yn, dung dch chuyn sang mu tm, loi mu lnna bng than hot tnh. Bo qun trnh nh sng.

Ch - Th theo JECFA monograph 1 - Vol.4.

- Xc nh bng k thut quang ph hp th nguyn t thchhp cho hm lng quy nh. La chn c mu th vphng php chun b mu da trn nguyn tc ca phngphp m t trong JECFA monograph 1 - Vol.4 phn ccphng php phn tch cng c.

Ph lc 2

YU CU K THUT V PHNG PHP TH I VI SP CANDELILLA

1. Tn khc, ch s INS 902

2. nh ngha Sp candelilla th thu c bng cch un si cc nhnhkh ca cy candelilla (Euphorbia antisyphilitica) trong nc c acid ha bng acid sulfuric gii phng ra sp.Sp tan chy ny sau c loi bo v cho ng c

li, tip theo c tinh ch bng cch x l vi acid sulfuricv qua cc cng on p - lc.

Sp candelilla v c bn cha n-alkanes mch l (C29 n

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C33) vi cc ester ca cc acid v cc ru c mch carbonchn (C28 n C34). Cc acid t do, ru t do, sterol, keotrung tnh v cc cht khong cng c mt.

M s C.A.S. 8006-44-8

3. Cm quan Dng cht rn, cng, rn, bng mu nu hi vng, c mithm khi lm nng.

4. Chc nng Cht lm bng, cht to kt cu cho ko cao su, cht ph bmt, cht mang cho ph gia thc phm (bao gm manghng v mang mu), cht lm c.

5. Yu cu k thut

5.1. nh tnh

tan Khng tan trong nc, tan trong toluen.

hp th hngngoi

Ph hng ngoi ca mu th, c lm tan chy vchun b phn tch trn mt tm kali bromid phi tngng vi ph hng ngoi ca sp candelilla tiu chun (xemPh lc).

5.2. tinh khit

Khong nhit tanchy

68,50 72,50

Ch s acid T 12 n 22

Ch s x phng ha T 43 n 65.Ch Khng c qu 2 mg/kg.

6. Phng php th

tinh khit


- Xc nh bng k thut quang ph hp th nguyn t thchhp cho hm lng quy nh. La chn c mu th vphng php chun b mu da trn nguyn tc ca

phng php m t trong JECFA monograph 1 - Vol.4 phncc phng php phn tch cng c.

Ph lc 3

YU CU K THUT V PHNG PHP TH I VI SHELLAC

1. Tn khc, ch s INS 904

2. nh ngha Senlac l nha polyester thu c t cnh kin , chtnha tit ra t loi cn trng Laccifer (Tachardia) laccaKerr (H Coccidae). Senlac ty mu thu c nh qutrnh ho tan cnh kin trong dung dch Na2CO3 trongnc, sau ty mu bng natri hypochlorit, kt ta cnhkin ty mu bng dung dch H2SO4 long v sykh; senlac ty mu khng cha sp c iu ch

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5. Yu cu k thut

5.1. nh tnh

Phn ng mu Phi c phn ng mu c trng.

tan Khng tan trong nc; tan chm trong ethanol; t tan trong

aceton v ether.

Ch s acid 60 89 (xem m t trong phn Phng php th)

5.2. tinh khit

Gim khi lng khisy kh

Khng c qu 6,0 % (sy 400C trong 4 gi, sau lm ngui n nhit phng trn silicagel trong 15 gi)

Rosin t yu cu (xem m t trong phn Phng php th).

Sp Senlac ty mu : khng c qu 5,5% ; Senlac tymu khng c sp: khng c qu 0,2%

(xem m t trong phn Phng php th)

Ch Khng c qu 2,0 mg/kg.

6. Phng php th

6.1. nh tnh

Phn ng mu Cho vi git dung dch cha 1 g amoni molybdat trong 3ml acid sulfuric vo 50 mg mu. Mu xanh l cy c

hnh thnh chuyn sang mu hoa c khi dung dch muc trung ho bng dung dch amoni hydroxyd 6N.

Ch s acid Cn chnh xc 1 g mu nghin mn v ho trong 50 mlalcol trc c trung ho bng NaOH vi cht chth phenolphthalein, v chun bng dung dch KOH0,1N. Xc nh im kt thc bng cch s dngphenolphthalein TS hoc dng c o in th. Nuphenolphthalein c dng, chun cho n khi muhng nht bn t nht trong 30 giy. Tnh ch s acid bngcng thc:

Ch s acid = 56,1V x N/WTrong :

V: Th tch dung dch NaOH (ml)

N: Nng dung dch NaOH

W: Khi lng mu (g) tnh theo cht kh.

6.2. tinh khit

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Rosin Ho tan 2 g mu trong 10 ml ethanol kh nc, vthm t t 50 ml dung mi hexan va thm va lc.Chuyn hn hp vo mt phu tch, ra 2 ln 50 ml ncv loi b nc ra. Lc lp dung mi, c n kh vthm 2 ml hn hp gm 1 phn th tch phenol lng v 2phn th tch methylen chlorid vo phn cn kh va c

c. Khuy v chuyn mt phn hn hp vo h rngca a phn ng mu. Lm y h rng lin k bng hnhp gm 1 phn th tch brom v 4 phn th tch methylenclorid, y c hai h rng bng mt knh ng h. Khngc mu ta hoc mu xanh indigo m c hnh thnh trong hoc bn trn lp dch lng cha cn mu.

Sp Cn chnh xc 10 g mu nghin mn v 2,5 g Na 2CO3vo cc cao dung tch 200 ml. Thm vo 150 ml ncnng, ngm cc trong cch thy si v khuy cho n khimu c ho tan. y cc bng mt knh ng h, gia

nhit trong 3 gi khng khuy, sau lm ngui trongchu nc lnh. Khi sp ni ln b mt, lc hn hp quagiy lc khng tro tc trung bnh, chuyn sp sang giyv ra phu lc bng nc. Rt 5 -10 ml ethanol vo phulc lm kh nhanh. Gi giy vo mt t giy lc rng,buc bng mt si dy nh v lm kh bng cch gia nhitnh. Chit bng cloroform trong dng c chit xut lin tcthch hp trong 2 gi, s dng bnh lm kh v cnkhi lng trc hng sp trch ly v dung mi. Cdung mi, lm kh sp 1050C cho ti khi lng khngi, tnh % sp.


- Xc nh bng k thut quang ph hp th nguyn tthch hp cho hm lng quy nh. La chn c mu thv phng php chun b mu da trn nguyn tc caphng php m t trong JECFA monograph 1 - Vol.4phn cc phng php phn tch cng c.

Ph lc 4


I VI DU KHONG1. Tn khc, ch s Liquid parafin, liquid petrolatum, food grade mineral oil,

white mineral oil

INS 905a

2. nh ngha Hn hp ca cc hydrocarbon lng naphthalin v parafin tinh ch vi im si trn 3500C; thu c t cc cng ontinh ch du khong th khc nhau (v d: chng ct, trchly v kt tinh) v lm sch tip bng acid v/hoc x lhydrogen ha c xc tc; c th cha cc cht chng oxyho c chp thun dng cho thc phm.

M s C.A.S 8012-95-1

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3. Cm quan Dng du lng khng mu, trong sut, pht ra hunh quangdi nh sng ban ngy; khng mi

4. Chc nng Cht lm bng, cht chng dnh, cht bi trn, cht ph bov

5. Yu cu k thut5.1. nh tnh

tan Khng tan trong nc, t tan trong ethanol, tan trong ether

t chy t chy to ra ngn la sng chi v c mi ging miparafin

5.2. tinh khit

nht 1000C Khng nh hn 11 cSt

S carbon imchng ct 5%

Khng nh hn 28im si im chng ct 5% cao hn 4220C

Khi lng phn ttrung bnh

Khng nh hn 500

acid hoc kim t yu cu.

Cc cht d than ho t yu cu.

Hydrocarbon a vng

thm

t yu cu.

Parafin rn t yu cu (xem m t trong phn Phng php th).


6. Phng php th

tinh khit

acid hoc kim Cho 20 ml nc si vo 10 ml mu v lc mnh trong 1pht. Tch lp dung dch nc v lc. Cho 0,1 ml dung dch

phenolphthalein TS vo 10 ml dung dch lc c. Dungdch khng mu. Khng c qu 0,1 ml dung dch NaOH0,1N thm vo thay i thnh mu hng.

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Cc cht d dng thanho

Cho 5 ml mu vo ng th c np thu tinh trc c ra sch bng hn hp dch ra acid chromic. Thm5 ml dung dch H2SO4 TS v gia nhit trong cch thy sitrong 10 pht. Sau khi ng th trong chu trong 30 giy,ly ra nhanh v trong khi y np lc 3 ln tht mnh theophng thng ng vi bin 10 cm. Lp li sau mi t

30 giy. Khng c ng th ngoi cch thy qu 3 giycho mi ln lc. Kt thc sau 10 pht tnh t thi gian btu t ng th vo cch thy cho n khi ly ra khi cchthy. Mu gi nguyn mu v acid khng tr nn sm muhn mu chun c chun b bng cch trn trong mtng th tng t 3 ml st (III) clorid TSC, 1,5 ml cobaltclorid TSC v 0,5 ml CuSO4, hn hp ny c ph bng 5ml du khong bn trn.

Parafin rn Lm kh lng mu thch hp bng cch gia nhit 1000C

trong 2 gi v lm ngui trong bnh ht m trn acid H 2SO4

m c. Cho vo ng thu tinh c ng knh trongkhong 25 mm, y ng v ngm ng vo trong chu nc. Sau 4 gi, cht lng to thnh phi trong c thnhn thy d dng mt vch mu en rng 0,5 mm trn nntrng gi thng ng pha sau ng thy tinh.


- Xc nh bng k thut quang ph hp th nguyn tthch hp cho hm lng quy nh. La chn c mu thv phng php chun b mu da trn nguyn tc caphng php m t trong JECFA monograph 1 - Vol.4

phn cc phng php phn tch cng c.

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Ph lc 5


I VI SP VI TINH TH

1. Tn khc, ch s Petroleum wax;

INS 905c2. nh ngha Sp vi tinh th l hn hp tinh ch ca cc hydrocarbon bo

ho, rn ch yu l parafin nhnh, thu c t du m.

3. Cm quan Dng sp khng mu hoc trng, hi trong m, khng v vkhng mi

4. Chc nng Cht gum cao su, cht ph bo v, cht chng to bt, chtlm bng

5. Yu cu k thut

5.1. nh tnh

tan Khng tan trong nc, tan rt t trong ethanol, t tan trongdiethyl ether v hexan.

Ch s khc x n (100, D): 1,434 1,448

Ph hp th hng ngoi Ph hp th hng ngoi ca mu nng chy v chun btrn mt tm caesi hoc kali bromid tng ng vi phtrong phn Ph lc

5.2. tinh khit

nht 1000C Khng c nh hn 11 mm2/giy

Xem m t trong phn Phng php th


Khng c qu 5% cc phn t c s carbon nh hn 25



Khng nh hn 500


Cn sau khi nung Khng c qu 0,1%

Xem m t trong phn Phng php thMu sc Xem m t trong phn Phng php th

Lu hunh Khng c qu 0,4%



Hydrocarbon a vngthm

Mu th phi p ng cc gii hn hp th tia cc tm khitin hnh phn tch nh c m t trong Phng phpth.

Bc sng (nm) hp th cc i/chiu ding truyn (cm)

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280 - 289 0,15

290 - 299 0,12

300 - 359 0,08

360 - 400 0,02

6. Phng php th

tinh khit

nht 1000C (ASTM D 445 c chp nhn vi s cho php t Schthng nin Tiu chun ASTM bn quyn ca Hip hi Mv Th nghim v Vt liu, 100 Harbor Drive, WestConshohocken, PA 19.428 bn sao ca tiu chun ASTMhon chnh c th c mua trc tip t ASTM, in thoi610-832. - 9.585, fax: 610-832-9555, e-mail:

[email protected],website: http://www.astm.org)

S dng nht k mao qun thu tinh, hiu chnh v ckh nng o nht ng hc vi lp li ch c 1/20trng hp vt qu 0,35%. Ngm nht k trong chu chtlng nng nhit 0,10C thch hp i vi mu th, mbo trong sut qu trnh o, lc no mu th trong nht kcng di b mt cht lng trong chu t nht l 20 mm.Cho mu vo nht k theo cch ch dn thit k thit b. Gimu trong chu khong 30 pht. iu chnh th tch mu

n vch qui nh theo thit k ca nht k. Dng p lciu chnh mc trn cng ca mu n v tr cch pha trnca vch mc th nht khong 5 mm trong nhnh maoqun ca thit b. Cho mu chy t do, o, thi gian cnthit cho mt khum ca cht lng chuyn t vch nh mcth nht n vch nh mc th hai. Thi gian o c tnhbng giy vi sai lch 0,2 giy Nu thi gian nh hn 200giy, chn nht k c mao qun c ng knh nh hn vlp li cch lm. o thi gian chy ln hai. Nu c hai ln oc sai s trong khong 0,2%, nht ng hc c tnhbng gi tr trung bnh. Nu c hai ln o khng tng ng

th lp li cch xc nh sau khi lm sch v lm kh cnthn nht k.

nht 1000C (mm2/giy) = C x t

Trong :

C: H s hiu chnh nht k (mm2/giy)

t: thi gian chy (giy)


S carbon l s nguyn t carbon trong mt phn t. Xcnh s carbon c trong mu bng sc k kh. Di y chra mt s iu kin hot ng in hnh xc nh n s

carbon n 45.

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Chiu di ct (m) 25 30 15

ng knh trong(mm)

0,32 0,53 0,25

Pha tnhDB-1

methylsilicon

RTX-1

methylsilicon

DB-5 5%phenylmethylsilicon

dy lp phim mng(m)

0,25 0,25 0,25Kh mang heli heli heli

Tc dng (ml/pht) 1,56 5,0 2,3

Tc tuyn (cm/giy) 33 35 60

Chng trnh nhit

Nhit ban u 800C 800C 800C

Tc nng nhit(0/pht)

10 8 5

Nhit cui cng 3800C 3400C 3500C

K thut bm ngui trnct

nguitrn ct

nguitrn ct

Detector FID FID FIDNhit 3800C 3400C 3750C

Dung tch mu (l) 1,0 1,0 1,0

Lu : Bng cch ti u ho chiu di ct tch v/hocnhit ct, cc loi sp vi s carbon cao hn 45 cng cth phn tch c.

Cc chun hiu chun v nh tnh:

Cc mu chun ca parrafin thng thng bao ph khongs carbon ca mu c tinh khit ln hn 95%.

Chun tuyn tnh

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Chun b mt hn hp bit khi lng ca cc n parafinc chui carbon C16 C65, ho tan hn hp trong cyclohexan.S dng nhng lng tng ng ca mi loi parafin cn chnh xc n 1%. Cc dung dch c nng 0,01 %(tnh theo khi lng) c th c s dng. Khng nht thitphi bao gm mi n-parafin trong hn hp ny min l n

cha C16, C44, v c C60 nu xc nh s lng carbon caohn lin quan) v t nht mt trong mi n - parafin th t.Cht chun ny phi c y cht ngn nga tht thotdung mi.

Dung dch ni chun:

Chun b dung dch gc cha 0,5% (theo khi lng w/w) n C16 trong n hexan ( tinh khit ti thiu 98%) bng cchcn chnh xc 0,4 g n C 16 cho vo bnh nh mc dung tch100 ml. Thm 100 ml cyclohexan v cn li. Ghi khi lng n C16 ( WISTP ) ti trong khong 0,001 g v khi lng ca

dung dch gc ( WS ) ti trong khong 0,1 g. Chun b dungdch ni chun long bng cch pha mt phn dung dch gcvi 99 phn cyclohexan. Tnh nng dung dch ni chuntheo cng thc sau:

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Trong :

CISTP: Nng ca n C16 trong dung dch ni chun long (%

theo khi lng)WS: Khi lng dung dch gc (g)

Kim tra mu trng:

Bm 1 l dung mi. Khng c pick no c pht hin trongkhong thi gian lu m sp ra gii.

phn gii ct:

Bm 1 l dung dch 0,05% mi n C20 v n C24 trongcyclohexan. phn gii ct R khng c nh hn 30 ctnh ton theo cng thc sau:

Trong :

d: Khong cch gia cc i pic ca n C20 v n C24 (mm)

W1: Pic bng mt na chiu cao ca n C20 (mm)

W2: Pic bng mt na chiu cao ca n C24 (mm)

tuyn tnh:

Phn tch chun tuyn tnh. Cc h s p ng khi lngtnh ton lin quan n hexadecan phi trong khong 0,90 1,10.

lp li thi gian lu:

Phn tch chun tuyn tnh 2 ln. Cc thi gian lu i viphn tch 2 ln phi khng chnh lch hn 0,1 pht.

Hiu chun i vi xc nh n parafin:

Xc nh thi gian lu ca tng n parafin trong chui C 16 C44 ( hoc C60 nu xc nh s carbon cao hn lin quan )bng cch bm lng nh ca mi parafin hoc ring bithoc trong hn hp bit trc.

Ly mu:Gia nhit mu ti nhit cao hn 100C so vi nhit spc nu chy hon ton. Trn u bng cch khuy... sdng ng nh git sch, nh mt vi git ln trn mt tm lnhm sch, ng c v b thnh tng ming. L nhmthng c cha sn mt mng mng bng du. Trc khi sdng, du ny phi c loi b bng cch ra l nhm bngcc dung mi nh hexan hoc cn khong.

Cch tin hnh:

Cn chnh xc 0,01 g mu ( Wmu ) thu c theo m t trongphn ly mu, cho vo mt l thu tinh c dung tch 15 ml.Thm khong 12 ml dung dch ni chun long, y np l vcn chnh xc khi lng ca dung dch ni chun pha longthm vo ( WINSTD ). Lc l cho n khi sp ho tan hon ton,

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Hnh 1: Tng s carbon (sc k vi ng nn nmngang)

Tnh kt qu:

i vi mi s carbon, hm lng tnh theo % khi lngc tnh theo cng thc sau:

Ai WISTDCi = ----------- x RRFi x -------------- x CISTD

AISTD Wmu

Trong :

Ci: Hm lng hydrocarbon c s carbon i (% theo khilng)

Ai: Tng din tch ca cc hydrocarbon vi s carbon i

AISTD: Din tch ca pick ni chun n C16

RRFi: H s p ng lin quan n n C16

WINSTD: Khi lng dung dch ni chun long

Wmu: Khi lng mu sp

CISTD: Nng n C16 trong dung dch ni chun long

Hm lng tng hp ca cc thnh phn c s carbon nhhn 25 khng c qu 5%.


S dng phn b s carbon thu c trong phn th v Scarbon ti im chng ct 5% tnh khi lng phn t trungbnh theo cng thc sau:

Trong :

i: S carbon

Ci: Hm lng cc thnh phn c s carbon i (%)

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Cn sau khi nung Cn chnh xc 2 g mu cho vo a s hoc platin bitkhi lng v gia nhit trn ngn la. Mu bay hi m khngthot ra mi hng. Nung nhit khng qu sc ti chon khi khng cn carbon. Lm ngui trong bnh ht m vcn.

Mu sc Lm tan chy khong 10 g mu trong chu hi nc v cho 5ml cht lng vo ng th vi sinh bng thu tinh sch, kchthc 16 x 150 mm: cht lng c lm m, tan chy khngc sm mu hn dung dch c to ra bng cch trnhn hp gm 3,8 ml st (III) clorid TS (FNP 5) v 1,2 ml cobalclorid TS (FNP 5) trong ng th tng t, so snh hai ngbng phn chiu nh sng tng phn vi nn mu trng,cc ng th c gi trc tip tng phn vi nn mt gcm khng c hunh quang.

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Lu hunh (ASTM D 2622 Xem php th i vi nht 1000C v

Bn quyn cho php)

Xc nh bng php o ph tia X s dng cc iu kin sau:

Dng c, thit b:

- My quang ph tia X c trang b pht hin tia mm

trong di 537 .- ng truyn quang ca heli

- Thit b phn tch chiu cao xung hoc cc thit b phn bitnng lng khc

- Detector c thit k pht hin cc tia X bc sng di

Tinh th phn tch ph hp vi tn sc ca tia X K luhunh trong khong gc ca thit b quang ph c sdng. Pentaerythritol v germani l ph bin nht mc dnhng cht t phn chiu hn nh EDDT, ADP v thch anhc th c dng.

ng tia X pht bc x K lu hunh.

ng tia X vi mc tiu vonfram, platin hoc crom.

nhy chun:

Cc cht petroleum lng cha lu hunh cc nng xpx khong gia th hiu chun c s dng cho php th.

Chun hiu chnh:

Chun b chun hiu chnh bng cch pha cn thn lng di-n-butyl sulfid (chun tinh khit cao vi mt phn tch cchng nhn, sn xut c bit nh mt cht hiu chnh chophng php ny, lun c sn ca Cng ty Philips Petroleum,Bartlesville, OK, M) vi du trng (cha nh hn 5 mg/kg).Cc nng chun chnh xc c chun b gm 0,1; 0,25;0,5 v 1,0% (theo trng lng).

ng chun:

o bc x lu hunh pht ra thc t mi chun hiu chnh.V th cng , di dng s m thc trn giy, vinng lu hunh.

duy tr gi tr ng chun vi s thay i nh v nhycc thit b, o nhy chun ti cc khong thi gianthng xuyn trong cc ngy chy. Thit lp t l tnh cachun ny bng cch o nhy ca chng ti cc khongthi gian thng xuyn trong qu trnh chun b ng hiuchun. Tnh h s hiu chnh i vi cc thay i nhy cathit b hng ngy bng cng thc sau:

Trong :

A: S m ca nhy chun c xc nh ti thi im

hiu chnhB: S m ca nhy chun c xc nh ti thi gianphn tch

Cch tin hnh: 20


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- Xc nh bng k thut quang phhp th nguyn t thchhp cho hm lng quy nh. La chn c mu th vphng php chun b mu da trn nguyn tc ca phngphp m t trong JECFA monograph 1 - Vol.4 phn ccphng php phn tch cng c.

Hydrocarbon avng thm

Hng dn chung:

Do nhy ca php th, kh nng sai s pht sinh t nhimbn l kh ln. iu quan trng nht l tt c dng c thutinh phi c c ra sch nghim ngt loi b tt c cccht hu c nh du, m, d lng cht ty ra,... Kim tratt c dng c thy tinh, bao gm c nt v cc van, di nhsng t ngoi pht hin bt k nhim hunh quang cnst li. Nh mt bin php phng, khuyn ngh thc hnhra tt c dng c thy tinh vi isooctane tinh khit ngay

trc khi s dng. Khng s dng bt k m bi trn nohoc khp ni. Ht sc cn thn trnh nhim cc musp trong vic x l v m bo khng c bt k chtkhng lin quan pht sinh t bao b khng thch hp l iucn thit. Bi v mt s cc hydrocarbon a vng tm ctrong th nghim ny rt d b oxy ha bi nh sng, ton bquy trnh phi c thc hin di nh sng du.

Thit b, dng c:

- Phu chit: dung tch 250 ml, 500 ml, 1.000 ml v tt nht lloi c dung tch 2.000 ml, c kho van bng polymertetrafluoroethylen.

- Bnh cha: dung tch 500 ml, c trang b mt khp nithon chun 24/40 ni ti y bnh v mt khp ni cu trnnh bnh ni vi ngun cung cp nitrogen. Khp ni thchhp phi c trang b cc mc thu tinh.

- Ct sc k: di 180 mm, ng knh trong 15,7 0,1 mm,c trang b vi mt a thu tinh xp th, kho van polymer

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tetrafluoroethylen v mt khp ni thon chun 24/40 c l lp v tr cui i din. (chiu di ton b ca ct vi khpni c l lp l 235 mm).

- a: c lm bng polymer tetrafluoroethylen ng knh2 inch, dy 3/16 inch c l gia va kht thn ct sc k.

- o gia nhit: hnh nn, dng cho phu chit dung tch 500ml. (c s dng vi b kim sot bin nhit).

- Bnh ht: Bnh lc dung tch 250 ml hoc 500 ml.

- ng sinh hn: khp ni 24/40, ni vi ng kh, chiu dikhng bt buc

- Bnh c (khng bt buc): Tt c bnh thu tinh dung tch250 ml hoc 500 ml c trang b vi np y thon chun cng dn vo v ra cho php nitrogen qua ngang b mt cacht lng c c.

- Dng c chng ct chn khng: tt c bng thu tinh (

lm sch dimethyl sulfoxid); bnh ct dung tch 2 lt c o gianhit; sinh hn Vigreaux c bao chn khng (hoc tngng) c chiu di khong 45 cm v u chng ct ni ving sinh hn c th chia nhnh lnh. Dng polymertetrafluoroethylen bc ngoi cc khp ni thu tinh ngnng bng. Khng c s dng m cc kho van hoccc khp ni.

- Cc cng o quang ph: cc cng o lm t thch anh nuchy, chiu di ng truyn quang 5,0 0,005 cm; mt loicng o khc ch kim tra hiu sut ca thit b quang ph,

c chiu di ng truyn quang hc 1,000 0,005 cm. Vinc ct trong cc cng o, xc nh xem c chnh lch hp th hay khng.

- Thit b quang ph: Di quang ph 250 400 nm vi chiurng khe ph 2 nm hoc nh hn, theo cc iu kin hotng ca thit b o hp th , thit b quang ph cngphi p ng cc yu cu thc hin sau y:

lp li hp th : 0,01 ti hp th 0,4 chnh xc hp th : 0,05 ti hp th 0,4 lp li bc sng: 0,2 nm chnh xc bc sng: 1,0 nm- Bnh kh nitrogen: nitrogen tinh khit trong bnh kh nnc trang b b iu p v van kim sot dng kh ti 5p.s.i.g.Nguyn vt liu v ho cht:- Dung mi hu c: Tt c dung mi c s dng trong quitrnh phi ph hp vi cc c tnh k thut v php th cm t trong phn cc c tnh k thut ny. Isooctan, benzen,aceton v methyl alcol c ch r trong danh sch di ys phi qua php th sau:Cho lng dung mi xc nh vo trong bnh tam gic dung

tch 250 ml. thm vo 1 ml n hexadecan tinh khit v c trnchu hi nc di dng nitrogen (o l nhm ri bao quanhbnh s lm tng tc c). Ngng c khi cn li khng qu 1ml cn. (Cho mt phn 10 ml isooctan tinh khit vo cn t

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- Hn hp MgO Celite 545 (2 + 1) theo khi lng: Cho 2phn MgO (60 180 mesh) v 1 phn Celite 545 theo khilng ln lt vo bnh thu tinh c np y ln trncho ph hp. Lc mnh trong 10 pht. Chuyn hn hp sangmt mng thu tinh c lt bng l nhm ( loi ht duchng dnh) v tri hn hp trn tm l nhm mt lp dy 1

2 cm. Li gia nhit hn hp 160 10

C trong 2 gi v boqun trong bnh c y cht.- Na2SO4 khan, tinh khit, tt nht dng dng ht: i vimi bnh cha Na2SO4 tinh khit c s dng, thit lp nhsau, ra trc Na2SO4 cn thit cung cp cc b lc nhyu cu trong phng php: Cho khong 35 g Na2SO4 khanvo trong phu thu xp th c dung tch 30 ml hoc phu lcdung tch 65 ml c cht bng thu tinh; ra ln lt cc phn15 ml dung mi ch nh cho n khi phn ra 15 ml c hp th bng 0/cm chiu di ng truyn ti bc sng 280 400 nm khi c o nh m t trong phn Dung mi hu

c. Thng dng 3 phn ca dung mi ra l .Cch tin hnh:Trc khi thc hin phn tch mu, o hp th trong cngo c chiu di ng truyn 5 cm ti di bc sng 250 400 nm i vi mu trng bng cch thc hin cch tinhnh, khng c mu sp, nhit phng, ghi ph sau giaion chit v sau khi hon thnh cch tin hnh nh m t. hp th trn 1 cm chiu di ng truyn sau giai onchit khng c qu 0,04 ti khong bc sng 250 400nm; hp th trn 1 cm chiu di ng truyn sau honthnh cch tin hnh khng c qu 0,07 ti khong bcsng 250 299 nm, v cng khng vt qu 0,045 tikhong bc sng 300 400 nm. Nu trong c hai ph xuthin pic ca benzen c trng trong vng 250 260 nm, loib benzen bng cch tin hnh trong phn Dung mi huc v ghi li hp th.Cho 300 ml dimethyl sulfoxid vo trong phu chit dung tch 1lt v thm vo 75 ml H3PO4. Lc u cc thnh phn trongphu v yn trong 10 pht. (Phn ng gia sulfoxid vacid to nhit. X p sau khi lc, sau ng np phu li).Thm vo 150 ml isooctan v lc u cc dung mi. Ht ra

tng lp ring bit v gi trong cc bnh thu tinh c np y.Cho 1 kg mu i din ca sp, hoc nu lng ny khngc th cho ton b mu vo trong mt cc c dung tch gpkhong ba ln th tch ca mu v gia nhit trn cch thysi, thnh thong khuy cho n khi sp nng chy hon tonv ng nht. Cn bn phn 25 0,2 g sp nng chy chovo cc cc dung tch 100 ml ring bit. D tr ba trong bnphn phn tch lp sau nu cn. mt phn mu bitkhi lng ngay sau khi nng chy li trn cch thy si vophu chit dung tch 500 ml c cha 100 ml hn hp sulfoxidv H3PO4 cn bng trc, gia nhit trong o nhit nhit

va cao lm nng chy sp. (Ch : Trong qu trnhgia nhit trc hn hp sulfoxid v acid, nh k m np yca phu chit gim p sut).

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Nhanh chng hon thnh vic chuyn mu vo phu trong ogia nhit vi cc phn isooctan cn bng trc, lm m ccnu cn thit, v s dng tng th tch 50 ml dung mi. Nusp tch ra khi dung dch trong ton b cch lm ny, phu chit ng np trong o gia nhit cho n khi sp tanli hon ton. (nh k m np y ca phu chit gim p

sut).Khi sp chy tan thnh dung dch, ly phu chit ra khi ogia nhit v lc mnh trong 2 pht. Chun b sn 3 phu chitdung tch 250 ml vi mi phu cha 30 ml dung mi isooctan cn bng trc. Sau khi tch pha lng, ngui cho nkhi phn ch yu ca dung dch sp isooctan bt u hnhthnh kt ta. Lc xoy nh phu chit khi kt ta lc uxut hin thnh trong ca phu chit nhm lm tng nhanhhn qu trnh ny.Ly cn thn lp pha di, lc chm qua lp bng thu tinhmng va t lng trong phu lc vo trong phu chit th

nht dung tch 250 ml, ra ln lt bng cc phn 30 mlisooctan cha trong cc phu chit dung tch 250 ml cn li.Thi gian lc i vi mi ln ra l 1 pht. Lp li qu trnhchit bng cch thm hai phn hn hp sulfoxid v acid, thayphu trong o gia nhit sau mi ln chit m bo sp tantrong dung dch v ra ln lt mi phn chit thu c bngba phn isooctan ging nhau.Tp trung cc phn chit thu c (tng th tch 300 ml) chovo phu chit (tt nht dng loi phu c dung tch 2 lt) ccha 480 ml nc ct, lc v ngui trong mt vi pht saukhi phn chit thu c cui cng c thm vo. Thm 80ml isooctan vo dung dch v chit bng cch lc mnh phutrong 2 pht. Rt ra lp tan trong nc pha di trongphu chit th hai (tt nht dng loi 2 lt) v lp li qu trnhchit bng 80 ml isooctan. Rt ra v loi b lp tan trongnc. Ra mi phn chit thu c 80 ml ba ln vi ccphn 100 ml nc ct. Thi gian lc cho mi ln ra l 1pht. Loi b cc lp tan trong nc. Lc phn chit th nhtqua Na2SO4 khan c ra trc bng isooctan (xemNa2SO4 trong phn Nguyn vt liu v ho cht i vichun b phu lc) vo trong bnh tam gic (hoc bnh c ty

chn). Ra phu chit th nht bng phn chit 80 mlisooctan th hai v cho qua Na2SO4. Sau ra ln ltphu chit th hai v th nht bng mt phn 20 ml isooctanv cho dung mi qua Na2SO4 vo trong bnh. Thm 1 ml n hexadecan v c isooctan trong cch thy c thi khnitrogen. Ngng c khi cn li khng qu 1 ml cn. Thm 10ml isooctan vo phn cn, c li ti 1 ml hexadecan v lp liqu trnh ny mt ln na.

Chuyn ton lng phn cn trong isooctan vo bnh nhmc dung tch 25 ml, nh mc ti th tch 25 ml v lc u.o hp th ca dung dch trong cc cng o c chiu di

ng truyn 5 cm so vi isooctan l i chng ti di bcsng 280 400 nm (cn thn khng mt dung dch trongqu trnh mu y cng o).

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Hiu chnh cc gi tr hp th i vi bt k hp th noc ngun gc t ho cht c xc nh bi tin hnh cchlm khng c mu sp. Nu hp th khng vt qu giihn c m t ti Cc c tnh k thut, sp p ng ccc tnh k thut v hp th tia cc tm. Nu hp th hiuchnh trn mi cm chiu di ng truyn vt qu gii hn

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quy nh ti Cc c tnh k thut, tin hnh nh sau:Chuyn ton lng dung dch isooctan vo bnh c lpkhp ni 24/40 dung tch 125 ml v c isooctan trong chucch thy di dng nitrogen ti th tch 1 ml hexadecan.Thm 10 ml methyl alcol v khong 0,3 g natri borohydrid(Gim thiu tip xc borohydrid vi bu kh quyn. Mt dng

c nhng o c th c s dng). Ngay lp tc, rp bnh vimt sinh hn lm ngui bng nc c g lp mt khp ni24/40 v ng lm kh dn vo trong bnh, khuy cho n khiborohydrid tan, yn trong 30 pht nhit phng, thnhthong lc xoy. Ti im kt thc ca giai on ny, thobnh v c methyl alcol trong cch thy c thi kh nitrogencho n khi natri borohydrid bt u tch ra khi dung dch.Sau thm 10 ml isooctan v c ti th tch cn li khong2 3 ml. Lp li, cho 10 ml isooctan v c n th tchkhong 5 ml. Lc xoy bnh lp li nhiu ln m bo ra cn natri borohydrid.

Lp a polymer tetrafluoroethylen ln phn trn ca thn ctsc k, sau ct sc k vi a trn bnh ht v ht chnkhng (p sut khong 135 mmHg). Cn 14 g hn hpmagnesi oxyd v Celite 545 (t l 2/1) v hn hp cht hpph vo trong ct sc k vi cc lp dy khong 3 cm. Saukhi thm vo mi lp, san bng phn trn ca cht hp phbng thanh knh phng hoc pittng kim loi bng cch nhnxung tht chc cho n khi cht hp th c nhi vo. Nilng vi ml trn cng ca mi lp hp ph bng thanh kim loitrc khi b sung lp k tip. Tip tc nhi theo cch ny cho

n khi tt c 14 g cht hp ph c cho vo ct. San bngphn u ca cht hp ph bng thanh knh phng hocpittng kim loi bng cch nhn xung tht chc to ra su ca lp cht hp ph khong 12,5 cm. Tt chn khng vkho bnh ht. Ni bnh nhn dung tch 500 ml vo bn trnct sc k v lm m ct trc bng cch cho 100 mlisooctan qua ct. iu chnh p sut kh nitrogen tc hxung ca isooctan ra ngoi ct l 2 3 ml/pht. Ngng plc ngay trc khi isooctan cui cng t n mc ca chthp ph. (Ch : Khng cho php mc cht lng rt dimc hp ph bt c khi no).

Tho bnh cha ra v gn 5 ml dung dch isooctan m cvo ct v li s dng p lc nh y cht lng rt xung chtrn mc cht hp ph. Nhanh chng hon thnh vic chuyntng t vi hai phn 5 ml isooctan, lc xoy bnh nhiu lnmi ln m bo ra cn. Ngay trc khi ra 5 ml cuicng t n nh ca cht hp ph, thm 100 ml isooctanvo bnh nhn v tip tc thm qua vi tc 2 3 ml/pht.Ngay trc khi isooctan cui cng t n mc hp ph,thm 100 ml dung dch benzen 10% trong isooctan vo bnhnhn v tip tc thm qua vi tc cp trn. Ngay

trc khi hn hp dung mi t n mc cht hp ph, thm25 ml dung dch benzen 20% trong isooctan vo bnh nhn vtip tc cho thm qua vi tc 2 - 3 ml/pht cho n khi ttc hn hp dung mi ny c loi b ra khi ct. Loi btt c dung mi ra gii thu c n thi im ny. Thm

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