TCVN TIEU CHUAN QUOC GIA TCVN 12512-1:2018 ISO 14362-1:2017 Xuét ban lin 1 VAT LIEU DET - PHUONG PHAP XAC DINH MOT SO AMIN THOM GIAI PHONG TL CHAT MAU AZO - PHAN 1: PHAT HIEN VIEC SU’ DUNG CHAT MAU AZO BANG CACH CHIET VA KHONG CHIET XO’ Textiles — Methods for determination of certain aromatic amines derived from azo colorants — Part 1: Detection of the use of certain azo colorants accessible with and without extracting the fibres HANOI ~ 2018TCVN 12512-1:2018 Léi ndi dau TOWN 12512-1:2018 hoan toan tuong duong véi ISO 14362-1:2017. TCVN 12542-1:2018 do Ban ky thugt Tiéu chudn quéc gia TCVN/TC 38 Vat ligu dét bién soan, Téng ‘eye Tigu chun Bo luéng Chat lugng 48 nghj, B6 Khoa hoc va Céng nghé cdng bé. BO tiéu chun TCVN 7619 (ISO 14362-1), Vt isu ot - Phuong phép xée dinh mét s6 amin thom giai phéng tix cht mau azo gdm céc tisu chuan sau: = TCVN 12512-1:2018 (ISO 14362-1:2017), Phan 1: Phat hign viéc stp dung chét mau azo bang cach chiét va khong chiét xo = TCVN 12512-3:2018 (ISO 14362-3:2017), Phan 3: Phat hién vic sir dung mot sé chét mau azo 06 thé giai phéng 4-aminoazobenzenTIEU CHUAN QUOCGIA TCVN 12612-1:2018 Vat liu dét - Phuong phdp xac dinh mét sé amin thom giai phong tir chat mau azo — Phan 1: Phat hién viéc sir dyng chat mau azo bang cach chiét va khéng chiét xo Textiles — Methods for determination of certain aromatic amines derived from azo colorants ~ Part 1: Detection of the use of certain azo colorants accessible with and without extracting the fibres 1 Pham vi ap dung ‘Tiéu chudn nay mé ta phuong phap phat hign vige sir dung mot sé chat mau azo khong duge sir dung trong san xuét ho&c xit ly céc san phAm lam tir xo dét va cé thé phan ng voi cdc tac nhan khir bing cach chiét va khéng chiét xo. Cc chét mau azo c6 thé phan tng véi téc nhan khir ma khong chiét l& céc chat dug sir dung 48 tao mau bang pigment hoac dé nhugm — Xa xenlulo (vi dy: bang, visco). — Xa protein (vi dy: len, to t&m), va — Xo téng hop (vi dy: polyamit, acrylic). Cac chét mau azo cé thé phan ing voi dich chiét va nhGng chat dug si dung d8 nhudm ec xo nhan tao bang thude nhugm phan tan. Cé thé nhugm céc xo nhan tao sau day bang thude nhugm phan tén: Polyeste, polyamit, axetat, iaxetal, acrylic va xo clo. Phuong phap nay cé lién quan dén tat ¢4 cde vat ligu dét duoc tao mau, vi dy: vat ligu dét dug nhudm, in va trang phi 2 Tailiguvién din Céc tai ligu vign dan sau rét cn thiét cho viée 4p dyng tiéu chudn nay. Déi véi cdc tai ligu vién dan ghi nm cng bé thi 4p dung phién ban duge néu. Déi véti céc tai ligu vién din khéng ghi nam cong bé thl ‘4p dung phién ban mai nhdt bao gdm cd cdc sira di, bd sung (néu 6).TCVN 12512-1:2018 TCVN 4851 (ISO 3696), Music ding a8 phan tich trong phéng thi nghigm - Yeu cdu ky thudt va phurong phép thir 3. Thu&t ngiva dinh nghia Khéng cé thuat ngd, dinh nghia trong tiéu chudn nay. 4 Qui dinh chung Bang cch tach khir (cdc) nhém azo, mét s6 cht mau azo cé thé gidi phéng mot hodic nhiéu amin thom sau:TCVN 12512. Bang 1 - Cc amin thom muc tiéu® 86 [_sécas ‘Sb chi din ‘SéEC chat 1 | 92874 612-072-006 202-17-1_ | biphenyt-4-ylamin 4-aminobiphanyl xenylamin 2 | 9267-5 | 612-042.00.2 202-1984 | Benzidin 3 | 954692 612-196-000 202-441-6 _| 4-clo-o-toluidin 4 | 94-508 612-022-003 202-080-4 | 2-naphtylamin S| 97-563 611-006-003 202-581-2 | o-aminoazotoluen 4-amino-2' 3-dimetylazobenzen 4-orolylazo-o-toluiin @ | 99558 612-210-005 202-766-8 | Smnitvo-o-toluidin 2-amino-4-ritrotoluen 7 | 106-47-8 | 612-137-009 203-401-0 —[4-cloanilin @ | 615054 | 612-200-000 210-406-1__| 4metoxy-m-phenylendiamin 2,4-ciaminoanisol 3 | 10r778 | 612-051-004 202-9744 | 4,4-metylendiamin 4,4'-diaminodiphenyimetan 10 | o19e4 612-068-004 202-109-0 | 3,3°-diclobenzidin 3,3'diclobiphenyl-4.4-ylendiamin a4 | 119-904 | 612-036-00-x 204-355-4 | 3,3-dimetoxybenzidin ovdianisiain 2 | 119937 | 612-041-007 204-358-0 | 3,3-dimetylbenzicin 44-beotoluidin 73 | e3e-880 | 612-085-007 212-658-8 | 4,4’-metylendio-toluidin 14 | izo7Ve | 612-209-00x 204-4181 | 6-metoxy-m-toluicin proresidin 5 | tora |” 612078008 202818-9 | 4.4-metylen-bis-(2-do-enlin) 2.2'-diclo-4.4"-metylen-dianilin 46 | i0re04 | 612-199-007 202-977-0 | 4,4°-oxydianilin a7_| 139-654 [612-198-0041 205-370-9 | 4,4-thiodieniin 18 | 95534 | 612-091-00-X 202-428-0 | otoluidin 2-aminotolven 19 | 9580-7 | 61209003 302-453-1 | 4-metylm-phanylendiamin 2,4-toluylendiamin 2,4-diaminotoluen 20 | 437-47-7_[ 612-197-006 205-282-0 | 2,4,5rimetytaniin 21 | 90-040 | 612-035-004 201-963-1_| canisidin 2-metoxyanilin 2 | 60083 | 611-008-004 200-453-6 | 4-amincazobenzen * $$ CAS 97-56-3 (06 5) va 99-55-8 (66 6) dug Kh Uidp dén 36 CAS 95-53-4 (s6 18) va 95-80-7 (86 19). Due bu kign cia phuomg phép nay, chét may azo cb khd nding hinh thanh 4-aminoazobenzen 88 igo ra ann (86 ‘CAS 62-53-3) vi 4 A-phenylendiamin (sb CAS 106-50-2), Do cdc gi6i han phst hin, chi cb thé phat hign cuuge ann, Néu ‘linn due phat hign ken hon § mg/kg thi phal thi sy ob mat cla of chét mau nay theo TCVN 12512-3 (SO 14362-3). © (he amin thom my itu ofc amin thor b cr theo Quin (EC) 6 1907/2006 os Nghi vgn Chau Au va Hi dng gay 18 thang 12 ndm 2006 06 tién quan &én Bang kj, Banh gid, C4p phép va Han ché Hoa chat (REACH) durge thidt lap bai Co quan Hoa chét Chau Au,TCVN 12512-1:2018 5 Nguyén téc ‘Sau khi la chon mét mau thir duge tgo mau tir hang dét, mdu thir duge thir theo phurong php chiét chét mau 461 v6i thuéc nhudm phan tan valhoac phuong phép Khir truc tiép d6i véi cdc logi cht mau khdc (pigment vafhoae thudc nhugm). ‘Vide 4p dung mét trong hal phurong phdp nay dua trén ban chdt (cdc) xo cla mau thir (gdm chi mot loai xo hoe hén hop xo) va phuong phép tao mau (qué frinh in ho&e nhugen) Khi thyc hign phuong phap chiét chdt mau déi vi thudc nhugm phan tan, dau tién chdt mau duge chiét ra khéi xo’ trong khéng gian phia trén (xem Hinh 1) sir dung xylen lam chét hdi luu. Dich chiét duc 05 déc va chuy&n ‘sang binh phan (eng bang metanol dé tiép tc Khir voi dung dich natri dithionit tan trong nude c6 xitrat lam chét dem (pH = 6) 670°C. Néu mau thi khéng mt mau hod toan sau khi chiét bang xylen, edn chudn bj lai mét mu thir méi va ‘uén hanh tai bang phuong ph4p dé vai logi chat mau khong chiét durgc. Khi thy hign phurong ph4p cto cdc logi chét mau khOng chiét urge, mu thir duoc xt ly bang dung dich natri dithionit tan trong ‘nude 06 xitrat lam chdt dem (pH = 6) & 70°C trong mét binh day kin. ‘Sau khi Khir, c&c amin gidi phéng trong qua tinh ny duge chuyén sang pha Lbutyl mefyl ete bang phuong ph&p chiét long-ng sir dung cOt diatomit. Sau 46 cb dc dich chiét Hbuty! metyl ete, va hoa tan phan cn véi mét dung méi phi hop 68 phat hign va xéic dinh céic amin bang céc phuong phép sic ky (xem Phy lye A). Phuong php sang loc sir dung qua trinh chiét léng-lang ma khdng cd cét diatomit duc mé ta trong Phy luc E. Néu phat hién céc amin bang mét phuong phap sac ky thi sau d6 phai xc nhén igi bang mat hoae nhiéu phuong phap khéc. 6 Canh bao vé an toan CANH BAO — Cac chét [amin] Iiét ké trong Didu 4 dwoc phan foal la chit ¢6 nguy co gay ung thu cho nguéi. Vigc xiv ty va thal bd cdc chét nay phal thie hign nghiém ngat theo cdc qui dinh quéc gia vé an toan va vé sinh, Ngwdi sir dung o6 trach nhiém dp dung céc ky thuat an toan va phil hep khi lam viéc véi vat ligu trong Phuong phép thy nay. Tham khdo y kién cla cdc nha sn xuat d& biét cdc chi tiét cy thé, vi dy: phiéu do ligu an toan vat ligu va cac khuyén nghi khac. 7 Thuéc thir Néu khéng cé qui dinh khac thi phai sir dyng cdc hod chét o6 cdp 6 phan tich. 7.4. Xylen (hén hop cae ding phan) $6 CAS 1330-20-7.TCVN 12512-1:2018 7.2 Axetoniteil 7.3 Metanot 7A — thutyl metyl ete 7.5 Dung dich dém xitrat/natri hydroxyt, pH = 6, c = 0,06 mol/l ” 7.6 Dung dich nude natti dithionit, p = 200 mg/ml, chudn bi méi (duge sit dyng trong vong 1h). 7.7 Diatomit 7.8 Chat amin - céc amin tir 4 dén 4, 7 dén 21 (nh duoc néu trong Bang 4), anilin va 1.4- phenylendiamin — tt cd déu la chat chudin finh khiét cdp cao nhét. 7.9 Dung dich chuan 7.91 Cac dung dich amin géc cé ndng 46 bang hogc lén hon 300 jxg 461 voi mai amin trong 1 mi dung mdi phi hyp. CHUTHICH Axetontl lt dung mai ph hop 48 pha dung coh ge, kim cho co amin ob dn nh th. 7.9.2, Cac dung dich amin higu chudn 48 str dung thong I. Pha loding tir dung dich géc (7.9.1) dén ndng 46 p = 15,0 ug d6i voi mdi amin trong 1 ml dung mdi thich gp. 7.9.3 Cac dung dich amin higu chuan d& dinh legng, dai nang d6 tir 2 ug lan dén 50 jg d6i voi mdi amin trong mot millit dung mdi phu hop. Néu sir dung sac ky khi, thém vao 10 pl dung dich chuan 1ndi (7.9.4) cho mdi millt trréee khi tid, CHO THICH Trach nhigm ci ting phiong thir nghigm lé Ilva chon céc néng d phi hep 4 higu chun, 7.9.4. Chat chudn ngi dang dung dich (IS), p= 1,0 mg/m! trong dung méi phi: hgp. rong truing hep phan tich GC-MS, od thé sir dung m6t trong cac chat chudn ndi sau : — S14: naphtalen-d8, s6 CAS: 1146-65-2 — 182: 2,4,5- tricloanilin, 36 CAS: 636-20-6 — 183: antraxen-d10, 86 CAS: 1719-06-8 7.9.8 Chat chi thj 48 sau dé rita giai cdc amin: benzidin-d8, s6 CAS : 22890-63.6. ‘p= 0,5 mg/ml benzidin-¢8 trong dung dich (7.9.4). benzidin-d8 (CAS: 92890-63-6) la m@t chét chi thj phd hyp 48 gay nhiéu phan sau cla séc ky GC (10.5) 7.10 Dung dich nude natri hydraxit, 41g kh6i kugng 10%. cla néng a6 xitrat pla ndng 46 khdi tugngTCVN 12512-1:2018 7.11 Nuc loai 3, phi hop voi TCVN 4851 (ISO 3696). 8 Thiét bj, dung cy 8.1 Thiét bj chiét, theo Hinh 1, gdm 06: ~~ Ong sinh han cd nhdm NS 29/32, — Méc duge lam bang vat ligu tro 68 gitr mau thir tai vj tri d8 cc giot dung mi ngung ty nhé vao mu thir, — Binh cdu 100 mi NS 29/32, va — Nguon nhiet. Hinh 1—Thiét bi C6 thé sir dung thiét bj trong ty néu thu duge cing két qua. 82 Bésiéuam 8.3. Binh phan dng (20 mi dn 50 ml) bang thi tinh chiu nbigt, o6 np kin. 8.4 Ngudn nhigt, tao duge nhigt 46 (70 + 2) °C. 8.5 — Cét thuy tinh hoac cét polypropylen, c6 duéng kinh trong tir 25 mm dén 30 mm, chidu dai tir 130 mm dén 150 mm, duye nhdi bang 20 g diatomit (7.7), 06 dau ra lép voi phéu Igc bang xo thuy tinh. Cé thé mua cae oft diatomit nhdi sdn hoac nhdi 20 g diatomit vao c6t thuy tinh hay ct polypropylen én kich thu6e xéc dinh, 8.6 — Thiét bjcé quay chan khéng cé kiém sodt chan khéng va bé cach thily. C6 thé sir dyng foai Khdc ctia thiét bj bay ho’, vi dy: b& cach thily 06 dng nite dug kiém soat phia trén chat l6ng. 8.7 Pipet cé kich c& yéu cau hodc pipet didu chinh duge, 8.8 — Thiét bj sac ky duge chon nhu sau:‘TCVN 12512-1:2018 8.8.1 Sac ky lop méng (TLC) hodc sc ky lop méng higu nang cao (HPTLC), 06 bd phat hign phil hop. 8.8.2 Sdc ky long higu ning cao (HPLC) cb rita giai gradien va detector mang diot (DAD) hoac detector khdi phé chon Ipc (MS). 8.8.3 Sée ky khi (GC) cd detector ion héa ngon liza (FID) hoiic detector khéi phd chon toc (MS). 8.8.4 Bign di mao quan (CE) c6 detector mang diot (DAD). 8.8.4.1. Bé loc mang PTFE (polytetrafioetylen), kich thc 15 0,2 um, thich hyp véi éign di mao quan (8.84), CHU THICH MO td ode dibs hide adc ky dag cho rong Phy Wye A 9 L4y mau va chuan bi mau thir 9.4 Yéu cdu chung (Cac mau thir phai dugc lya chon dita trén cdc tiéu chi sau : — cc phan cia hang dét (9.2) ; — ban chat ca cdc thanh phan xo (hgp phan xo) (9.3 va 9.4) ; — vat igu durgc to mau (9.6), de bigtkhi sit dung pigment (9.6). Chuan bj cdc mau thir bang céch cét cac hang dét thanh céc dai ho’ manh (xem phia dudi) dé co duoc ting khdi krong Id 4 g. ‘D4i voi c&c mau th dua vao chiét cht mau (10.1), — dt c&c hang dét thanh cdc dai néu sir dung thiét bj mé ta trong 8.1, hoe ~ ct hang dét thanh cdc manh nhé néu sty dung cdc thiét bi khac hoc néu chi dua cdc méu thir ‘vao qui trinh tach khir (10.3). 9.2 Hang dét Néu hang dét la ban thanh phdm, vi dy: soi, vai v.v... thl cdt hang dét thanh céc m&u thi. Néu hang dét cd mét s6 phan bing vat ligu dét, vi dy: quan do, ct mu thir ti tat c& cdc phan cla hang d6t, 06 thé la: — (cée) vai chinh, — (cae) lop Ist, — (cée) vai tam tai, — cc hin théu, . — (c4e) nhan mac trén mat hang dét, — (cc) day rit, — (cée) khéa kéo,TCVN 12512-1:2018 — long gid, hoae — chi may. Néu kn6i hugng cia mot s6 phan (vi dy: nhan mc, chi may, hinh théu o6 kich thuée nhd) khéng Gat (1g) kh6i lrgng 48 thir, thu gom cac phan giéng hét nhau,-néu cé thé. Néu ting khdi hrong cila vat ligu nhé hon 0,5 g thi vat itu nay duge xée dinh I& mot thanh phan thie yéu. (xem C.1.) Cac vat figu 0 khdi lugng nhd hon 0,2 g thi khéng cn phan tich, Hinh théu phai dug c4n cling voi vai nén. 9.3. Hop phan xo Do vige 4p dung tiéu chuan nay mét phan dya trén phuong phap chiét chét mau nén cn nhgn biét ban chat cia cdc thanh phan xo dét 48 06 thé xéc dinh duoc kha nang sir dung thudc nhudm phan tan. Bang 2 t6m tat bin trong hyp: Bang 2 - Ap dung phwong phdp chiét chat mau cho thuéc nhugm phan tan (10.1) ¢6 lién quan én ban chat xo Ban chat xo Siedyngthudc | Trvénghep | Cé can chiét chdt mau cho thuéc nhugen phan tan nhugm phan tén (40.4) khong? Xo ty nhién Khong A Khong Xo nhan tao Khong B Khéng Chua xéc dinh c C6 © D ce Néu cdc xo Khéng due nh ti Khéng phi thir Logi thuée nhugm dug sir dung cho xo tyr nhién hoa xo nhan tgo durge giai thich trong Phy lye D. 9.4 Trudng hyp hén hop x0 Trong trong hep cc loai xo khéc nhau duge trén vao nhau, tham khdo Bang 3 dé quyét dinh phai ap dung phurong php chiét chdt mau nao cho thuéc nhudm phan tan (10.1)TCVN 12512-1:2018 Bang 3~ Ap dyng phurong phap chiét chat mau cho thude nhugm phan tan (10.1) hoc cae ‘thudc nhudm khéc (10.2) c6 Hlén quan dén hon hyp x7 Qui trinh nao phai ‘Thanh phan cia hon hop xo ap dung A 8 ¢ D Thanh phan} a? 10.2 10.2 08 10.1,va10.2 | 0810.1 va 10.2 ta hén hop | pe 10.2 10.2 c&10.1va102 | 08 10.1 va 10.2 ~ co | cdt01vato2 | cdt0.1vat02 | cA 10.1va102 | oA 10.1va 102 Qo 8 10.1 va 10.2 4 10.1 va 10.2 4 10.1 va 10.2 10.1° * Khi st» dyng pigment hoiic khi khdng xéc Jinh duge sy cb mat cia pigment, cling ép dung 10.2 (xem 9.5). ° Xam Bang 2 48 biét ¥ nghTa cia A,B, C va D 9.5 Vat ligu durge tao mau bang pigment Néu vat ligu durge in hodc nhudm bang pigment (Phu lye G) cling nhur d6i voi vat ligu bat ky, néu khéng hdc chén céch sir dyng pigment, phai thyc hin phurong phép trong 10.2. 9.6 Mau 9.6.1 Yeu cau chung Phai thir tét c& c&c mau Xe, soi hoc vai “mau trdng” va khéng tao mau dug coi la kh6ng chira cht mau azo va do vay khong can phai thi, Mat khac, nén chi y dén céc vat ligu “in mau nhat” bdi vi chting c6 thé chéra chét mau azo. 9.6.2 Trréng hep gép mau C6 thé thir ba mau cling véi nhau. 88 gop ba mau, phai 4p dyng céc qui téc sau. Cac qui tic dug ligt ké theo the ty wu tien: — Lya chon ba mau tt cing mét phn cla hang dét; — Néu ba mau khéng Idy tir cing mét phan cia hang dét, va chon ba mau nay tir cdc phan vat ligu dét durgc lam ti cling mét loal xo dét; — Néu ba mau khong ldy tir cling mét phan cia hang dét va khéng lay tt cling mot logi xo dét, ta chon ba mau nay tly ofc phan vatligu dét, khi d6 phai 4p dung cing mét qui tinh. 9.6.3 Chuan bj mau thir c ba mau ‘Tung mau phai cé khdi long x4p xi bang nhau dé c6 dug ting khdi lugng 1g.TCVN 12512-1:2018 Néu két qua cla mu thir két hop ném trong khoding tir 5 mg/kg dén 30 mg/kg amin bat ky 64 néu, can thi’ ring bai vi két qua thir ca mau thir mgt mau c6 thé vugt qua 30 mg/kg. Gi6! han dinh lugng cla ting amin phai cé tai ligu kém theo cac quy trinh xac nhan gid tr str dyng ndi bd. 10 Cach tién hanh 10.1 Qui trinh chiét chat mau cho thuéc nhugm phan tén bang xylen Mau thir dét nhugm bang thude nhugm phan tan dug git? trong thiét bi chiét (8.1), dat mau phia trén 25 ml xylen dang s6i trong khodng 40 min hoc cho dén khi thay cdc giot dung mai tir mau thi? khong mau. D8 ngudi dich chiét xylen xudng nhiét 4 phang trvdc khi ldy dich chiét ra kh thiét bj chiét, Néu dich chiét khong mau, diéu 46 cé nghTa la mau thé vat ligu d@t khong duge nhudm bang cac thudc nhudm phan tan, khéng can tiép tye qui trinh nay. Cé de dich chit xylen trong thidt bi 0B quay & nhigt a tie 45 °C dn 75 °C cho t6% Kho, Can nay duge chuyén mt céch dinh lugng vdo binh phan Ging cing véi cde phan cia metanol, sir dyng b8 siéu am 48 phan tan ch&t mau (néu thé tich cu6i cing I6n hon 2 mi thi glam thé tich xubng khong 2 mi) va ‘thyec thign tach Khir (10.3). Ngoai ra, néu mu thir vat figu dét khng mét mau hodn toan sau khi chiét ‘hi phai thir mu thir thé hai theo 10.2. 10.2 Vat liéu d@t dug tao mau bang pigment va/hoge nhudm bang chdt mau khéng phai a thude nhugm phan tan Néu mu thir vat ligu dét 06 chira céc xo chi thuge trudng hgp A vashode B (9.4) hoc dugc tao mau ‘bang pigment thi cho tnvc tiép mau thir vao binh phan tng. Néu mau thir wat i@u dét khéng mét mau hodn toan sau khi p dung qui trinh trong 10.1 thi phai cét va cchudin bj mau thir thé hai theo 9.1 va cho tryc tigp vao mét binh phan img méi. 10.3. Tach khir ‘Thém 16 mi dung dich Gém xitrat (7.5) 6 gia nhiét dn 70 °C vo binh phan tng. Day kin binh phan ting va xiv ly trong (30 # 1) min & (70 + 2) °C. ‘Sau G6, thém 3,0 ml dung dich nurée nats dithiont (7.6) vao binh phan tmng, 48 tach Khir céc nhém azo, sau 45 lc manh hén hop va I ngay & (70 4 2)°C trong (30 + 1) min fiép theo, va lim aguoi dén nhi8t do phong (tir 20°C dén 25 °C) trong ving 3 min. 104 Tach vi c6 die cée amin ‘Thém 0,2 ml dung dich NaOH (7.10) vao dung dich phan ing va lic manh. Chuy&n dung dich phan ting vao oft diatomit (8.5) va 68 c6t hép thy trong 15 min, rong khi €, them 10 mi tbutyl metyl ete vo binh phan dng, tSc manh va sau Khong thai gian 15 min, Gan tbutyl metyl ete (trong trrémg hop 10.2, cing véi xo) lén dinh cbt va thu gom dung mél ra gid trong binh cdu 100 mi cé 8 néi nam chudn hodc binh thi tinh cho thiét bj cd quay (8.6). 14TCVN 12512-1:2018 Binh phan (rng duge rita bang 10 mi tbuty! metyl ete va dung moi duoc chuyén vao Ot. Sau a6, 8 tryc tiép 60 mi butyl metyi ete lén oft. 8 phat hién va dinh krong amin, 06 dac dich chiét Hbutyl metyl ete & nhigt a khong qué 50°C dén khoding 1 ml (khdng dé khd). Néu cAn ddi dung mdi khac, loai bd phan dung mdi cén (ai that cdn than bang dong nhe cia khi trot. CHU THIGH 1 Vige loa ba dung mal (c6 trong thiét bi quay chan khong, bay hot dén Kho) co thd dn dn tht host ‘céc amin quan wong néu thyc hin trong ce du kign khong dug kim sodt Cho ngay axetonitil hog ete butyl mety! (hose chi metanol khi sir dung dign di mao quan) vao dich chiét ho&c phan can dé dat dén 2,0 mi, phan tich ngay lap tic. Néu qua trinh phn tich khong hoan thanh trong vong 24 h, gidr dich chidt & nhigt d6 dui — 18 °C. CHU THICH 2 Nhi od nén, cc amin ing I, vi dy: 2.4-ieminatoluen va 2.4-diaminoanison thuémg rt kbm bn ving, S36 ‘igt trong metanol. Néu vgc phan ich iti han, oh King ph hii dg ec amin ray bng thi bj do sau Khodng thd sian dai hon, 10.5 Phat hign va dinh lweng amin Co thé sik dyng cac ky thuat sdc ky durge liét ké (8.8) d8 phat hién amin. Cling cé thé sir dung phuong phép phat hign khdc. Néu trong khi higu chuan thuéng Ié (7.9.2) phat hign dug lang amin bat ky kin hon 5 mg/kg, phai thyc hign quitrinh dinh long béing céch st? dung durang cong higu chudn dudi dang dé thj higu chudn nhiéu diém (7.9.3) vai it nhat ba diem. 10.5.1 Phat hign anilin va 1,4-phenylenediamin (chat chi thi ciia 4-aminoazobenzen) Dui didu kién olla phuong phdp nay, céc chét mau azo c6 kha nding tgo thanh 4-aminoazobenzen, tao ra anilin va 1,4-phenylendiamin (vi dy : C.J, Disperse Yellow 23). Do cdc gidti han phat hign va thu hii 1,4-phenylenediamin, chi 6 th® dug phat hign anilin, Néu anilin dug phat hién én hon § mg/kg trong mu thir (9.6.2) thi phai thir sy c6 mat cita ch&t mau giai phéng ra 4-aminoazobenzen theo TCVN 42612-9 (ISO 14362-3). 10.5.2 Lién quan dén thiét bj djnh lugng/cdc ngudn khdc c6 két qua dwong tinh gia Khi si? dyng GC, thém 10 pl dung dich chuan ngi (7.9.4. va 7.9.5) trén 1 ml dich chiét (10.4) trdc khi tigm. ‘Néu thyc hign phan tich xe nhgn benzidin bing DAD hoc TLC, vige stv dyng benzidin-6 (7.9.5) la khéng kh thi boi vi Khong thé t4ch peak khai benzidin khdng doteri héa. Tach dich chit thanh hai phan truéc khi thém dung dich chudn ndi (7.9.4) vao mét phan dé phan tich GC-MS. Trong phan tich GC-MS, néu 46 thu hdi cht chi thi benzidin-d8 (7.9.5) nhd hon 30 % gid tr] ky vong {do c&c Anh hurdng nén hoge céc ly do chura biét), o6 thé khong phat hién duoc céc amin, sau 46 phai thyec hign phan tich HPLC d8 tiép theo rive gidi céc amin: 2, 9, 10, 11, 12, 13, 15, 16 va 17 (Bang 1).TCVN 12512-1:2018 Néu mot mau thir chira benzidin sau Khi téch khir, nén tinh ham hrgng benzidin bing benzidin-d8 (7.95) giéng nh chat chudn néi. \Khi sir dung dién di vang mao quan (CE), 200 il dich chiét, v6i dung moi duepe chuyén thanh metanol (10.4), tron ngay (do tinh khdng én dinh cua mét sé amin trong metanol) voi HCI 50 ul (c = 0,07 mol/l) vva cho qua bé loc mang (0,2 ym). Dung djch nay duge phan tich b&ng phurong php dign di ving mao quan. Néu mét amin bat ky duege phat hién bang mot phuong phap sdc ky thl phdi xc nhgn bang cach sir ‘dyng mét hoc nhidu phurong phép khac, Két qua la duong tinh cht Khi tdt c8 cde phurong phdp kya chgn cho két qua duong tinh. Truéc khi két luan, phai xem xét trvéng hyp cdc két qué durong tinh gid. Khi quan sat th4y c6 sy khdc nhau gitra cdc két qua thu duge tlr céc kf thuat sdc ky khac nhau, cdc gid tri chénh léch vé két qua od thé do cdc nguyén nhan khac nhau (xem Phy luc C), vi dy: — cc két qua duvong tinh gid (vi dy: do nhiét 40 cao 6 dau vo, hoe do sy ich khong hon toan ‘cdc chat ding phan theo mé ta trong Bang C.1), va. — c&c két qua 4m tinh gid [vi du: thay d6i dung mdi (chi thich 1 trong 10.4) hodc dung méi urge si dung (cht thich 2 trong 10.4) hoge sy nhiéu trong cdc chét nn (xem bén dui). Céc két qué duong tinh gid cing 06 thé do cde amin duge gial phong tr cdc nguén khéc (vi dy : polyuretan hode chét lién két ngang). Xem Phy lye C. Néu cc amin 68 nhgn biét 06 c4c chat déng phan, c&n thén vé c&ch nhén biét ding. 10.6 Qui trinh kiém tra 10.6.1 Yéu cau chung 8 kim tra qui trinh, thém 100 jul dung dich géc amin (7.9.1) (ho&c mét lugng dé dat duge 30 yg cla ting amin trong binh phan (ng) véo trong binh phén tng (8.3) 06 chira 15 mt dung dich dm xitratinatr hhydroxyt (7.5) 6 gia nhigt. Qui trinh kiém tra nay phai durge thyc hign vét ting 16 mA the ‘Sau 46, thye hign theo qui trinh dug cho trong 10.4 va 10.5. Binh lugng chuain ibm tra nay dya trén dung dich higu chudn thudng [6 (7.9.2). 10.6.2. Higu chudn bang chdt chudn ngi (dinh Lvgng duge thy hign bing sc ky khi) AsxAise YS Pe Pe eae © a Trong 46 néng d cla amin trong dung dich mu thi, tinh bang yim! ; ‘A. difn tich peak cita amin trong dung dich mu thi, tinh bang don vj dign tich; Ae dign tich peak cia amin trong dung dich higu chudn, tinh bang don vj dign tich ; ‘Ass _diénttich peak cita ch&t chudn n6i trong dung dich mu thir, tinh bang don vi din tich; 16TCVN 12512-1:2018 Asc din tich peak ca chét chudin ndi trong dung dich hiéu chudi, tinh baing don vj dién tich; V thé tich mau thi cudi cling durgc tao ra theo 10.4, tinh bang ml ; V, thé tich dung dich amin durgc sir dung cho qui trinh kiém tra, tinh bang mi; P — ndng dé ca amin trong dung dich higu chuan, tinh bang ysg/mi. 10.6.3 Higu chudn khéng cé chat chudn ngi Py DXERE @) Trong 66 ‘P ndng 46 clia amin trong dung dich mu thir, tinh bang pg/ml ; A, dién tich peak ctia amin trong dung dich mu thir, tinh bang don vj dién tich; A. dign tich peak cia amin trong dung dich higu chuan, tinh bang don vj dign tich; V thé tich mau thir cubi cing duigc tz0 ra theo 10.4, tinh bang ml; V, thé tich dung dich amin étrgc sir dung cho qui trinh kiém tra, tinh bang ml; Pe ndng 46 cita amin trong dung dich hiéu chudn, tinh bang pg/ml 10.64 Thu hdi amin TY Ig thu hdl amin phai tudn theo cdc yéu cu téi thiéu sau : — C&c amin 96 1 dén 4, 7,9 d8n 17 va 2046n21: 70% — Amin 56 8: 20% — Amin sé 18 va 18: 50% — Amin 95 5, 6 va 22: xem chi thich trong Bang 1 — Anilin: 70% CHO THICH Higa nay, cha 6d di kn nghim dB diva ra cc you chu ti thibu cho cc amin urge Lk & tn (vf dy: 14 phenylenediarnin). Néu sy thu hdi amin khéng tuan theo céc yéu cau téi thiéu phi hgp thi kiém tra qui trinh va thir lai bang céc mdu thir méi. 11 Banh gid 14.4 Yéu edu chung Theo qui dinh trong 10.5, néu trong khi higu chudn thudng Ié (7.9.2) phat hién amin bat ky lon hon 5 mg/kg thi phai thyc hin qui trinh dinh luigng bang dé thj hiéu chun nhigu diém (7.9.3) véi it nhAt ba idm. Néu 4p dung ca 10.1 va 10.2 ma thu duge hai két qua khac nhau thi sau dé ghi Iai gid trj cao nhat cla tung amin.TCVN 12512-1:2018 ‘V6 dd thi Gung chudn cika tinh G4p tng so voi ndng 46 chudn da biét (durgc higu chinh vé tinh dap tng a6i voi chét chudn noi néu st dung). Ti d3 thi higu chudn, ngi suy nding 66 clia amin, tinh bang pot! (a). 44.2 Tinh amin trong mau Méc amin dug tinh bang phan khéi lugng wy, tinh bang mg/kg, cla mau thir theo ofng thire sau : xe Trong a ‘Ax ning 46 ndi suy ca amin, tinh bang pg/ml ; V thé tich cudi cing ca dich chiét duye tao ra theo 10.4, tinh bang m! ; ime _khéi lvgng cila mau thir dét, tinh bang g. 11.388 tin ody ca phuong phép 186 tin c@y cla phurong phép, xem Phy tye B. 12 Bao céo thir nghigm ‘Bao cdo thir nghigm phai gdm tdi thiéu céc théng tin sau: a) vign dan tiéu chudn nay; b) loai, ngudn géc va sur chon mBu thir (mot phan méu thie, néu o6 thé); ©) ngay nhén mu va ngay phan tich; 4) quitrinh dy mau va qui trinh chudn bi durgc thye hign theo 10.1 vashogec 10.2; ©) phurong phap phat hign va phuong phap dinh Iurong; ) giéi han phat hign cho tt¢ng amin, tinh bang mg/kg: 9) kB qua duge ghi tal a mre arylamin, tinh bang mg/kg. CHU THICH Cdn cdn than khi bibu thi céc amin nhd hon 30 mgikg bot vi cdc gid tr ndy 06 thd do ce két qua dueng tinh ‘18, BB bidu thi kt qua, xem Phy lye C.TCVN 12512-1:2018 Phu luc A {tham khao) Phan tich sc ky AA Nhan xét ban dau Do thiét bj (8.8) ola céc phéng thir nghiém o6 thé khc nhau, khOng 06 hung dn 4p dung chung cho phan tich sdc ky. Cac théng s6 duéi day da duyge thir nghiém thanh cdng va sir dung A.2 Sac ky lop mong (TLC) Ban (HPTLC): silica gel 60 véi chdt chi thi phat huynh quang F254, 20 cm x 10 em ‘Thé tich mu chdm: (2.66n 5) ul, dang ciém Dung mai pha déng 4: clorofonvaxit axetic (90 + 10) phan thé tich Thude thi 1: ‘Béi voi sy hinh thanh NOx, dat trong budng tring mét céc cd md véi khodng 4 ml dung dich axit sulfuric va them mét thia nhd natri nitrit ran, Bong cira budng ‘va 08 phan ing xdy ra, D&t ban khé vao trong bung. Sau 5 min, ldy ban ra va 4m khé trong ding khi fanh. Thudc the 2; ‘Sau 46 phun fn ban dung dich a-naphtol 0,2 % dure chudn bj trong KOH (c= 1 mot) trong metanot Phat hign: 41) C&c ban TLC v6i chét chi thi phat huynh quang F254 2) Bén UV vashoac sau khi xir ly tiép bang thude thi 1 va 2, thdi gian phan ung. Khong § min Ban (TLC): silica gel 60 v6i chdt chi thi phat hujnh quang F254, 20 cm x 10 cm Thé tich mu chém: 10,0 pl, dang vach Dung mdi pha déng 2: cloroformietyl axetat/axit axetic (60 + 30 + 10) phan thé tich Dung mi pha déng 3: cloroformimetanol (95 + 5) phn thé tich Dung méi pha dong 4: n-butyl axetattoluen (30 + 70) phan thé tich Phat trién: Bubng bao ha Dung m6i pha dong 2 va 3: lién tiép ma khdng lam khé cac ban Phat higa: 1) Cac ban TLC v6i chat chi thi phat huynh quang F264 2) Bén UV valhode sau hi xi Ij tiép bang thudc thir 4 va 2, thai gian phan img khong Simin 19TCVN 12512-1:2018 Ban (TLC): silica gel 60, (20 x 20) cm? Thé tich mu chém: 10,0 ul, dang vach Dung mi pha dng 2: cloroformetyl axetat/axit axetic (60 + 30 + 10) phan thé tich Dung méi pha dgng 3: doroform/metanol (95 + 5) phan thé tich Dung méi pha dng 2 va 3: fin tiép ma kh6ng lm khé céc bn Phat trién: budng bao hda A3 Sc kj léng higu nang cao (HPLC) A341 Sdc ky léng higu nang cao/detector mang diot (HPLC/DAD) Dung moi riva giai 1: metanol; Dung méi rira gi 2: héa tan 0,68 g kali dihydrogen photphat trong 1 000 ml nuéo, sau d6 thm 150 mi metanol Pha tinh: Zorbax Eclipse XDB C186" (3,5 ym); (150 x 4,6) mm Tée 46 dong: 0,6 mifmin dn 2,0 miimin (dang gradien, xem bén dui) Nhigt 46 cbt: 32°C Thé tich tigm: Sul Phat hign: DAD, ghi quang phd Binh lugng: tai 240 nm, 280 nm, 305 nm va 380 nm Giedian Tho’ gian (min) Dung méirixa gidi 1(%) Tée 4 dong (ml) 0,00 10,0 08 22,50 55,0 0,8 27,50 100,0 06 28,50 100.0 0,95 28,51 100,0 20 29,00 100,0 20 29,01 10.0 20 31,0 10,0 06 36,00 10,0 06 > Zorbax Ealpse XDB C18 @ 1d métvl dy ala sn phm phi hop oof mai. ThOng tin nay duva ra ‘nha tgo thu€n i cho ngurdi st dung ti8u chudn va khong phai a chi thi cla ISO v8 sén phémm nay. 20TCVN 12512-1:2018 Xem vi dy trong Hinh A.1. CHU DAN 1 4,4-phenylendiamin 2 Anilin X thai gian, tinh bang phat Y hp thy quang, tinh bing mAU * amin thom 1 dén 21 (xem Bang 1) Hinh Al - HPLC/DAD-sac ky 4d A.3.2 Sic ky léng higu nang cao/detector khdi phd chan Ic (HPLC/MS) Dung moi riva gigi 1: axetonitril Dung mei riza gidl 2: 5 mmol ammoni axetat trong 1000 ml nude, pH = 3,0 Pha tinh: Zorbax Eclipse XDB C18 © (3,5 wm); (2,1 x 50) mm The a dong: 300 phim Gradien: bt dau tir 10 % dung mi nira giai 1, ting lén dén 20 % dung moi riva giai 1 trong ving 1,5 min; téng tuyén tinh fen 90% dung mai rira gidi 1 trong véng 6 min; Nhi6t d6 cot: 40°C; Thé tich tigm: 2.0 pk Phat hién: detector khdi phd tir crc va/hodc bay ion, ché d6 quét va/hoac MS ion con MS phat hin 24TOVN 12512-1:2018 khi phun: nitor (due dng chaifmay tao kh); {on hoa: phun dign tly dong API, bd phan manh 120 V Ad Sic ky khi mao quanidetector khél phé chon loc (GC-MS) Cot mao quan: DB-35 MS (J & W)®, dal: 35 m, 6izdng kinh trong 0,25mm, 4 day mang: 0,25 um He théng tiem: chia ding hoc khéng chia ding Nhigt 46 cBng tém: 260°C Khi mang: helt Chuong trinh nhigt dG: 100°C (2 min), 100 °C dén 310 °C (15 °Cimin), 310°C (2 min) Thé tich tim: 1,0 wl, chia dang 1:15 Phat hign: Ms. AS Bign di mao quan (CE) Mao quan 1: 56 om, khong nhéi, duéng kinh trong 50 yl, voi khe sang mé rong (Aglient®”y; Mao quan 2: 56 om, nhdi bing polyvinyl alcohol (PVA), dung kinh trong 50 pi, voi kha sang mé réng (Aglient®); Dung dich 46m: dung dich agm photphat (¢ = 50 mmol!), pH = 2,5 Nhigt 66 cot: 25°C Bign ap: 30KV Thos gian tim: 4s Thoi gian riva: 58 Phat hign: DAD 214 nm, 254 rm, ghi quang phd "Ages bid dsde cai 5 i Aglient® la met vi dy cia sin phdm phit hop eb gid tr thuong mal. Théng tin ndy dura ra him tao thugin li ‘cho ngudi sir dung tidu chudn va khdng phai la ch! thi cila ISO v8 san pham nay. 22Phy luc B (tham khao) 6 tin efy ctha phirong phdp (Céc 40 ligu sau thu dugc trong phép thir lién phéng trén vai potyete®: Bang B.1 —Két qua tir phép thir tién phong A. TCVN 12512-4:2018 Qui trinh phan tich xo Amin * ‘ et R al molkg | ma/kg (%%) | mg/kg | mgfkg (%) | markg Qui irinh chidt bang xylen, 19.8 iin 6 | 7,6 (26,6) , if fe polyeste | pelorcanitin | 28, @8) | 27 | gga) | 7° ‘Qui trinh chiét bang xyien, 16,8 in }. 30,1 | 8.7 (28,0) | 3, coms polyeste | p-cloroanilin }. 30,1 (28,9) 4 (65,8) 59 Trong 66 Fa} Rplai R aptailgp gid ti trung binh S946 lech chudn ofa 46 lap lal Sy 4 Kich chudn cla 66 tal fp 9 _amliche Sammlung von Untersuchungsverfahren nach §35 LMBG, saber, naa. set +1998: Nachwois der Verwendung bestimmter Azofarbstoffe aus textlen Bedarfsgegenstaenden, 23‘TCVN 12512-1:2018 Céic dir igu sau thu duge trong thir nghiém lién phang trén vai en, vai béng va vai viseo duoc thyc hign bi 11 phong thir nghiér. Bang B.2 - Két qua ti? cdc thir nghiém lién phong auieinn TS amin ¥ 7 * R Sa phan tich mgkg | mokg(%) | maka | maka (%) | mara HPLC | ten | 33)-dimetybenzan 2s | sates) | 17 | iar | 48 HPLC | bong | Beran 7 | saqa | 18 |tsean| 41 HPLC] Visco | 33-dimalhonybenzicin ms | 2a(ea) | 10 | Toes | 28 HPLC_| len | 4A-daminodiphenyimetan | 17.7 | s0(ies) | 14 | Vo2a) | 26 HPLC | ten | o-totuidin ze |aanss| i | 8 | 40 (61.1) Trong a6 1 Alpi Rapti lap 2 gid tj rung binh 44 46 Ich chun oda 6 Kip ai ‘5996 lech chudn cia 69 ti tgp %TCVN 12512-1:2018 Phy yc (tham khdo) Huréng din dnh gid — Giai thich két qua phan tich C.1 Yéu cau chung Phy luc nay dura ra huréng dan ky thuat bé sung nhung khéng ban dén céc két qua dat duge theo qui trinh duoc m6 ta trong tiéu chudn nay. Vi chi voi mot lrgng rét nhé cdc amin cling cé thé dln dén két qué durong tinh gid, qui dinh REACH 1907/2006/Phy luc XVII dinh 16 gid tr gidi han cla vat ligu mu 14 30 mglkg. Gid tri nay chi dp dung ‘cho mét mau thi den, nhung khdng 4p dung cho cac mu thir két hop (9.6.2). Néu phat hign lugng amin vot qué 30 mg/kg thi phai khang dinh la c6 str dung chat mau azo (xem ‘Bang 1). Néu dui 30 mg/kg thi khéng thé khang dinh chac chan ngay duge viéc c6 sir dung cac chat mau azo (xem Bang 1) hay khéng khi khong ¢6 thong fin bd sung nhy fogi vashodc d6 tinh Khi8t cba chat mau hoae cac nguyén ligu khdc 44 sir dyng. An dinh mot mau thir 66 khdi lugng giam nhu 14 mét thanh phan thi yéu va dura ra théng tin vé 65 ‘khOng chac chan lén hon do vat ligu o6 tinh ddng nhat thap hon. Do sy tn tai oa cc ehdt déng phén déi v6i m6t s6 amin myc tiéu (xem Bang C.1), phong thir nghigm hai dm bdo 1a cdc dac tinh sc kh 48 va phé cila chat phan tich dugc phat hign la tuong dong voi eae chat amin chuan, CAA Xéc dinh 4-aminoazobenzen Dui cac diéu kign cla phuong phap nay, cdc chat mau azo cé thé tgo thanh 4-aminoazobenzen, tg0 ra anilin va 1,4-phenylenediamin (vi dy: C.l Disperse Yellow 23). Do céc gi6i hen phat hién va syy thu hdi 1,4-phenylenediamin, chi phat hin éuge anilin. Néu anilin duge phat hign én hon 5 mg/kg trong mot mau thir két hgp gdm ba phan, sau do phai thir sy 06 mat cla cac chdt mau gidi phong 4- aminoazobenzen theo TCVN 12512-3:2018 (ISO 14362-3:2017). C.1.2 Két qua dwong tinh gia Bang C.1 cho thay cdc chat 06 thé tao ra két qua duong tinh gid (bao gdm sy nhiéu bdl cae chdt dng phan).TCVN 12512-1:2018 Bang C.1 — Ligt ké cc ly do cho két qua dirong tinh gia “ Taha gi asc sant Ha ae Sas xét 8) cas |, | CRT TOE RES TRATES cE diiiiaiee =F ye cde bng phan Salven Yalow 7 eves cH im ty pharaictenct= aminkipheny! a Kiting + inh turing, hrydenyaznbenzen (cto tm Kb nh vy fae . ob thd bit au tr tbe - | vo 1 ff etwtm to thanh 4 67-4 | aminabipheny! amareas oR) | quake aminotipheny! rong pranvamin | Cm SOL, feta bp a % phan Bi atk ba thd nhupn Direct back 168 oy oe hin: we Wang cine Sg ? | ars [mm wm the, a | && [eee mm | Tae oh 10 chat L aeel 602 | towel t a ‘dng phan cht déng phan CHET ahem Reactive Red 474 hye surat - ob gié tH ‘hang mai tp ot Cae tude nue | ‘Cin thin cic fap chat 4 | sag | Areenytemin wy | eb ni te ant do cia 2-naphthymin CO | ries Tak ed 2 one Bing Cla hen Wt ach cE phan chit ang phan = & o7 | 3 Buge phat hign la o- 56.3 | cimethyazsbe totuin, xm 36 18 ren 40> toyiezo-0- ‘oui | & wee a ‘Bunge phat hi 18 2.4 Pa ea ee ae pen, nirotowen | | T_[ 108 Feioreaniin | THE 3 ca Bog 1 Gln tn WaT ich ce a8 a. | pdt bg phan phanTCVN 12512-1:2018 Bang 1 (tiép theo) Danke che anita | U2 WHE cho Era 86 duong tinh gid cine Tanke Nndn xét Ténhéa chit | Chutrichéa hoe | chéued chét | chu tie héa hee og phin Far bbe ig? |) pe aoe 2 Pioment Red 23 eg rmethonyS-ntroanin, 2) bute to rm 4 et, reonyaenaen 4emeth-onym- amin, 8 615- | phenylenediami w. Hai thudc nhugm vei 2- 054 | te Set methoxy-S-nitroanlin azo diaminoarisole Come oO my Wen bt duge Het ke ben Orshon's to ah fem C241 va 2.1.23). THE SR Cha thin Bi ch ede dng phn chdt ing phn a Chit xip va ehdt gin nme ae hovoy| mau in, cfc ibn chit A-metyened | PY" Ty J | polyme, sy tach & nhiét sarmeryen- | pores: | Prenvt 8 cao xtc ohn Kt qu g | 1% | dana ae cc 6C tang ky tuatLc 774 | daminos- NN“{inelylen- phenytmetan sho |g OME, | fo wo tn tt lene)bis: wr TN | ngang ding cho ang {aziridine-t- ‘dung in carbox-amide) eng cine Sing 3,3-di-cloro- peg . . i tham thao au kdthop o- benzidin 3.3.4 cba Pigment Black 7 vol 10 loro tighony- oe | 8 Pigment Orange 19 hog ee Pigment Orange 24 éu9e bit gi phdng amined lién quan 118 ‘3,3'dimethoxy- Khong cn tic ang thém " eran 90-4 anisginTCVN 12512-1:2018 Bang 1 (tiép theo) ‘Sy ch ode amin & vet Cap aot azo ct} | cus wns Gil “Thanh phn 5 “fog GC bang kg trust LC. aig [seme [SO Om | ae Thi BS aT 92 | ag. | bonetin 4. nit en 09 | 24 | 8 cp ati azo Cl thanh xs 88 cp 601 220 | HEEL | phn 5, sy ch cbc amin Thanh phn 5 {itt 60 cao, xe nig bt qud GC bang hp ust i Wing cin dong bm . (chi ¥ rang mot hop chat ag | 82 | 44-mettene- as we erg 889 | éroroudn tung 08th 8 the gan eu Khe hav) “ae. | SmetroAE : E10 cet ‘Cha iin WH ae wd ty fetid weQrenes | adng prin cht bg phn. resin Famer bs Farmelyrene= Ban than amin a mot (2-re-niin) bis-2-lor>- hll ding rin cho TO 101. | 2.2-hioroa aniin) peyuretan, ya | 124 | metendianin aeaane | SOO" | payor va va 4a-metytene- poy ania ‘Ban than amin ta mot tlt 6g rén cho ahve ‘epoxy va nhya nhiet rén, OO | ana ttn pn tn 101- | 44-oxydan- . chlt polyme dang nhot, "| a0 | tine seer bidn dBi Khng. phe hal fhish mang pobine kheng néng chay bai .d6ng rn nhigt hoge birc a ee era Tam ing en te ng henTCVN 12512-1:2018 Bang 1 (tiép theo) Tash ede arin & AGTH gy [680 185 obey om mB * GC hai thube nhugm che mamta? | or Chet 2 ot ce ct on, Xtc han Két qua GC bang ky thus Le. 95 | othiin 2 oy | pgment Red} a om_ som) 0/ Sime) ot [mM gar Can thén khi tach cdc chit adng phi. Tat c& ba chbt Kh6 téch bing GC, oft ‘ing phn shan eye Khe hoBe the 68 gla nhigt 4 thdp hobo. tach bing kj thug C. Setotayen d= Poljuretan min polyme cia 24+ Chit nfp va chit gin 953 (2,4-diaminotol- toluylen- mau in, c&c tien chat 19 | oy | vere sisocyenta polymne (}) Ta Stin [Tat ed su chat Cla When ch che lantine og pan chit ang phn 20 [Tar [2a saimehy MC, | Tat cd sau chat Cin than khi tach cdo 12-7 | tania wong ‘@Bng phan chit ang phan wh Tech & ah Bh cao tat ao ‘du phun GC 06 thé xB ay | 2% [eens hn kat qua GC bling ky 04.0 | methoxyanitine uate. Tat c& ba chat Cin thn Kl tach che ‘dog phén cndt ing phn Ono Bin han - aminoazobenen 18. mot 22) © bom thude nhuen azo o8 tan 09-3 a” * “solvent yellow 1", ‘Thy hign theo TCVN 125123 (80 14362-3) ‘Cac amin cd fan quan khac 62- ‘anilin HN 4D “Thye hign theo TCVN: 533 425123 (ISO 14362.3) 106- | té-phenyien - | Tat ca ba chat Gong Cin than Khi téch cac iN hy eos [aon | ces ‘Trong myc nay, khuyén ngh] bao cdo cdc két qua phan tich nhur sau: 2TCVN 12512-1:2018 6.1.3. Trong trémg hyp mize cho méi thanh phan amin $30 mg/kg ‘Theo phan tich da thy hign, khéng phat hign trong hang héa c6 chat mau azo cé thé gidi phéng mot hogc nhidu amin duge ligt k8 cy thé (xem Bang 1) bang cach tach (cdc) nhém azo. C.1.4. Trong trémg hyp mire cho méi thanh phan amin > 30 mg/kg 1) Chita (cdc) thanh phan amin o6 mire > 30 mg/kg. 2) Két qua phan tich cho thdy hang héa da dug sdn xudt hod xir ty bang (cdc) chét mau azo cd thé gidi phéng mét hogc nhidu amin dug liét ké cy thé (xem Bang 1) bang céch téch (cdc) nhém azo ella ching, 3) C6 thd 66 cdc két qua dung tinh gia va Bang C.1 dura ra danh myc cdcly do. Néu cdn nghi ng&r cdc két qua durong tinh gid, xem huéng dan vé qui trinh va cach gidi thich trong C.2. €.2. Huéng dan vé qui trinh va cach gidi thich néu c6 két qua diong tinh gla €.2.1 Két qua durong tinh gia do cdc van dé sac ky C.2.1.1. Két qua dong tinh gia do cdc chat ddng phan Phan tich 24 amin va nhidu chat ding phan c6 thé cb 1a mét cBng vic khé khén (Bang C. 1), Nhidu amin c6 cdc cht dng phan c6 thé tao ra cdc két qua duong tinh gia néu ky thuat tach khéng duc téi wu héa. Luu ¥ khi tach amin myc tiéu, phal chi y dén cdc chat déng phan ola né. Cac amin c6 nhidu hon mét hé théng vong thom cling c6 cdc chat déng phan, nhung hiém hon va throng tach dé dang hon, Cac phéng thi nghiém phai dam bao két qua dung. €.2.1.2 Két qua duong tinh gid do cdc nguén khdc khéng phai chdt mau azo €.2.1.2.1 Két qua dwong tinh gia do nhigt 49 cao trong b6 phan tiém GC Amin 12, 18 va 21 d6i khi tao ra mot s6 két qua duong tinh gid trong GC do sy tach lién két amin cla cdc chat mau & nhigt d@ cao, amin 9 va 19 do kam dist gay cdc tién chat polyme polyuretan & nhiégt 40 cao. Can khang dinh dinh lugng cac két qua vai ky thuat khdng phai GC. €.241.2.2 Két qua dwong tinh gid duegc tgo ra tir qui trinh héa hoc Cac amin 9, 18, 16 va 19 thinh thoang cho ode két qua duong tinh gia do ede nguén khée nh polyuretan, c&c chat tao lign két ngang va céc chat khéc. MOt qui trinh dy mau don gidn 48 thy sy khdc nhau gitta lién két hoge khdng lin két azo la thyc hién lai qui trinh bang nuée thay cho dung dich natri dithionit. Néu két qua 06 thé so sénh duge voi mat két ‘qua G8 06 bd sy téch kh thi amin tir ngudn khong phai la chét mau azo. Néu cn thi, céch ii thich dui day lé mot vi du: “amin” (tén amin) duge phat hién thdy & murc (két qua tinh bang mg/kg) theo qui trinh duge mé ta trong tiéu chun nay. Tuy nhién, khi thie hign quy trinh phan tich nay ma Khéng o6 mat chdt khie cling 30TCVN 12512-1:2018 thu duge két qua tong duong. Bi vay, amin hinh thanh tie nguén khéng phai chat mau azo. Khong sir dyng chét mau azo bi cém giai phéng ra céc amin (Bang 1). C.2.1.2.3 Két qua durong tinh gid do cac chat mau Cac amin 1, 4 va 8 0d thé dug tao ra gién tiép trong qui trinh (tach khir bang dithionit) tir mét 96 chat mau khéng chtva cdc amin 06 lién két azo. Khéng 06 sy phan biét ro rang cdc chat mau nay va chdt mau azo bj c4m gial phéng ra céc amin (Bang 1). Phai ching minh sy khéng c6 cc ch&t mau azo bj c&m trong méu thir bang bing chirng (vi dy: hd so truy sudt ngubn géc tir thuédc nhudm hoae nha san xudt thudc nhugm), diva trén thong tin vé cdu tric thudc nhudm, dé xdc inh cdc két qua c6 lién quan Ia oc két qua duong tinh gid. Néu cn thiét, c4ch giai thich dudi day la mét vi dy: Cac ngubn khac cia amin durge phat hin *(t8n ca amin)” od thé dura vao két qua bao cdo, ma ngudn g6c cla chting khéng thé ching minh dya trén phan tich phong thir nghiém. 4-aminobiphenyl, 2-naphthylamin, 4-methoxy-m-phenylenediamin: khdng thé x4c dinh chdc chan sy vang mat lia cde chat mau azo bi cdm gidi phéng ra cdc amin (Bang 1) ma khéng 06 théng fin bd sung, vi dy: cdu tric héa hoc cia céc chat mau dugc si dyng. CHU THICH 1 4-eminobipheny, 2-naphthytamin: sn phim mdu thir 06 thé durge nhugm mau bang ede chdt mau 0 chu tric che cdc amin ahung khong pha én kt azo. 4-methoxy-m-phenylenediamin: san phdm mau thir o6 thé d& duge tao mau bang cdc cht mau azo ma cu tric khéng chéza 4-methoxy-m-phenylenediamin 04 tao thanh tir traée nhung o 2-amin-4- nitroanisol, trong qua trinh thyc hign phan tich, chét mau azo giai phéng 2-amin-4-nitroanisol sé bién 446i thanh dang 4-methoxy-m-phenylenediamin. aTCVN 12512-1:2018 Phy luc D (tham khao) Bang giai thich cac thuéc nhugm duc str dung trong cac vat ligu dét khaéc nhau Bang D.1 — Cac thuéc nhugm st dung trong cdc vat gu dét khéc nhau Thude nhugm Loal chat mau Pate Tryc| Phan iu Hoat| pigment Bane | anit | orom | ohdtim | | | amo | a | Ya | Jogi Xe ty nhién Xe dng | Len x | mx 7 ® x x vat [Tom [wy foo [x x |e wm fw pxt x Bong Gai dau Noudn a 6c x wx} mx | x | x x xellulo Be ‘Sidal Gai day Xo nhan tao Polyeste * x Polyamit =] x | «x fey x |x |x] x Triaxetat x x cw aw] x lo] @ | wl] « Acrylic x &) x Visco 7 ml x [alex] « Xo clo x x [khong phat thude nhugm azo x nghfa la logi thude nhugm sir dung ()_ nigh 1a oa thuéc nhuom sir dung trong céc trong hep ngoal le Xx nghTa lé foal thude nhugm thudng sir dung. Chi cdc thuée nhugm phan tan phi hgp véi qui trinh chiét chat mau (10.1). Céc mu c6 thé duge sang loc 48 xde inh liu c6 thuéc nhuém phan tan hay khdng bang cAch chiét xo trong xylen s6i trong 20 min. Néu dung m6i cé mau, c6 thé sir dung cdc thudc nhudm phan tan; mét sb pigment tan mot phan cing lam thay di mau dung méi. 32TCVN 12512-1:2018 Phy lye E (tham Khao) Qui trinh chiét léng/léng khéng c6 diatomit EA Luu y ban du Qui tinh nay mé t8 phuong phép sang loc cho céc amin durgc lit ké trong Bang 1 bang qui trinh chiét lengfténg khong ob cdl diatomit (8.5). Phat hign amin bat ky duege ligt kB ob lrgng Kon hon 5 mgikg va ‘nhé hon 100 mg/kg phai dugc phan tich lai theo phyong phép duge m6 té trong tiéu chudin nay bang qui trinh chiét Iéng/léng ¢6 o6t diatomit. Sy mé t& hoan chinh qui trinh nay bao gdm cdc phan a8 chudn bi mu dure m6 t8 & phan trén cia tidu chudn nay dé tranh sy tim kiém cdc tai ligu tham khdo chéo. C6 thé sit dung phuong phép sang loc tong ty nhu phuong phép duge mé ta trong tigu chudn nay, néu cho thay cac két qua so sanh duc vei phuong phap durgc mé td trong phy tye nay. Xem Diu 9 48 4p dung céc hung dan chudn bi mau thi. E.2 Thudc thir bd sung dugc sir dung E21 Géc dung dich amin higu chudn d& sir dung thueémg 16 Pha long dung dich géc (7.9.1) d6n ndng 9 p= 6,0 4g méi amin trén millit cua mot dung méi phi hep. 8 phan tich GC-MS, pha loding bang dung dich chuan ngi (E.2.2.2). E.22 Cac dung dich amin higu chuan a6 djnh lng, dai ndng 46 tir 0,8 9 dén 20 yg tig amin trén militia mot dung méi phir hep. 1B phén tich GC-MS, pha long bang dung dich chudn n6i (E.2.2.2), CHUTHICH Trdch nhifm cba ting phing thir nghitm Iya chon ede ng 6 phi hap ob higu chun, E.2.2.1 Chét chudn ngi dang dung dich (1S), p = 10 yg cita [Simi t-butyl metyl ete (6.4). Trong truéng hep phan tich GC-MS, o6 thé sir dung mét trong cac chat chudn noi sau: — St: naphthalen-d8, s6 CAS: 1146-65-2; — 1S2: 2,4,5-tricloanilin, s6 CAS: 636-30-6; — 183: antraxen-d10, s6 CAS: 1719-06-8. £.2.2.2 Chét chuda ndi dé sau 46 riva gidi céc amin: benzidin-d8, s6 CAS: 92890-63-6. ‘p= 5 jig benzidin-d8/ml trong dung dich E.2.2.4. benzidin-d8 (s6 CAS: 92890-63-6) la mét chat chi thi ph hyp cho céc nhiéu trong phan sau cilia sic dd cc. 33TCVN 12512-4:2018 CHU THICH — Néu ode phan tich xé¢ nhén benzidin dugc thye hign bang DAD hoge TLC, sir dyng benzidin-d8, s6 CAS: '92890-63-6 la khéng kha thi bai vi khéng thé téch peak khdi benzidin khong toteri hoa. E23 Dung dich nude natri hydroxit 40 % wiw, E.24 Natri clorua E.3. Thiét bi, dung cy bé sung duge sir dung E31 May lic ngang, cé tan sudt 5 s”, va khodng lc tir 2 om dén 5 cm. E.3.2. May ly tam, téc d6 lén hon 3 000 véng/phut E4 Céchtién hanh £41 Chun bj mau Chun bj mu thir (9.1) bang cach cat d8 c6 Guge ting khéi lugng 0,6 g. E42. Chiét chdt mau bing xylen d6i v6i thude nhugm phan tan Mu thir vat ligu dét nhudm bang thudc nhugm phan tan duge gift trong thiét bj chiét theo 8.1, dat & phia trén 25 ml xyien s6i trong khoang 40 min hoe cho d&n Khi cdc giot dung mdi khéng mau. B& mat dich chiét xylen dén nhiét 4 phong. Néu dich chiét khéng mau, khéng c&n tiép tyc qui trinh. C6 dac dich chiét xylen trong thiét bj 06 quay & nhiét d6 tir 45 °C dén 75 °C cho dén khi dn Iai lurgng can nhd. Phan cn nay durge chuyén dinh lweng sang binh phan teng véi c&c phan metanol, ding bé siéu am dé phan tan chat mau (thé thich cudi cling gidm cdn khodng 1 mi), va tiép tyc tach Khir (E44), Néu mu thir vat liu dét khong mét mau hoan toan sau khi chiét thi phai thir mu thé? thi hai theo £43. E43 Vat ligu dét durge nhugm bang thuée nhum khong phai thude nhugm phén tan Néu méu thir vat igu d6t 66 chira cde xo’ chi thudc truéng hop A vashode B (9.4) hoe khéng mat mau hoan toan, theo mé 8 trong E.4.2, thi phai ct va chudin bj mu thir thir hai theo E.4.1 va 9.1 va cho try tiép vo trong mot binh phan ding mai. E44 Tach khir Cho 8 ml dung dich dém xitrat (7.5) 6& gia nhiet ti truéc dén 70 °C vao binh phan tng. Bay kin binh phan ding va xi ly trong (30 + 1) min & (70 42) °C. ‘Sau dé, &8 tach khir céc nhém azo, thém vdo binh phan ng 2,0 ml dung dich nutte nats dithionit (7.6), lc manh binh va ngay lap tirc lai gir & (70 + 2) °C trong (30 + 1) min tiép theo, 48 ngudi dén nhigt 46 héng (tir 20 °C dén 25 °C) trong ving 2 min, E45 Tach va cé dic cdc amin 34TCVN 12512-1:2018 Thém 0,5 mi dung dich nude natri hydrovit (E.2.3), 7 g natti clorva (E,2.4), va 3 ml chat chun ngi dang dung dich (E.2.2.1) vao dung dich phan tng va lac trong 15 min (+ 1 min) bang may lac ngang (E.3.1). Bé hoan thanh vige téch pha sau khi léc, nén quay ly tam (E.3.2) hn hyp. Néu c6 thé, si dung pha trén 48 xac dinh céc amin ma khong can bude 06 dc. B& phat hién va dinh lung amin (xem E.4.6), dich chiét t-butyl metyl ete c6 thé duge cb dac dén Khodng 1 mi (chwa khé) & khéng qué 50 °C. Néu can thiét, thay dung mai khdc, Jogi bd rét can than phan cn lai cia dung mi ra bang dang yéu khi tro (xem 10.4). CHU THICH Vige agi ba dung méi (c8 69c trong hit bj & quay chan Khdng, cB quay dn kho} cb th8 dn dé sy tht thot amin quan tng nu thy hign dud cdc idu kin Kg Kido Soak, Ngay sau 9, dich chiét hogc phan cn duge ldy ra bang dung mdi phus hgp, vi dy: axetonitri hoge & butyl metyl ete, va phan tich ngay. Néu khéng thé hoan thanh phan tich trong vong 24 h, phai gid’ mu thi & dugi-18°C. CHU THICH 2 Do chit nbn, cde amin riéng 8 nhu 2,4-daminololuen vé 2.4-daminaarislenhidu Kha ning b 4 bn din rt kém, &e bi6t trong metanol. Néu chm ché trong phan tich, ob thé khGng phat hig duge ofc amin tal thoi didm do ting thidt bi E.4.6. Phat hign va dinh kreng amin Phat hign amin c6 thé dug thye hign bang cac kf thut sdc ky dugc ligt ké trong (8.8). Cé thé sir dyng phuong phap da xéc nhén khao. Néu nhén biét bat ky aryl amin nao dugc ligt K8 trong Bang 14 cae ndng dé tir 5 mg/kg 4én 100 mg/kg, can phan tich Iai m&u bang phuong phap mé ta trong Diéu 10, sau d6 ding it nhdt mét duéng cong higu chudn ba diém dé dinh lvgng ham lugng amin, Thyre hién inh lweng bing phuong phép HPLC hoae GC-MS. Néu trong phan tich GC-MS, sy thu hdi cdc chat chi thi benzidin-d8 (7.9.5) thép hon 30 % so véi gia tr ky vong (do cae anh huréng cia chét nén hoge cc ly do chua biét), ¢6 thé khéng phat hién dugc cao amin thi phai thy hign phan tich HPLC 42 sau 46 na gidi cdc amin: 2, 9, 10, 11, 12, 13, 15, 16 va 17 (Bang 4). E47 Quitrinh kiém tra ‘Dé kiém tra qui trinh, cho 60 pl dung dich gc amin (7.9.1) (hoe thé tich ft hon dé tao duge 18 pig ting amin trong binh phan (ng) va 2,0 ml nude, thay cho dung dich nur6¢ natri dithionit (7.6), vao binh phan ing (8.3) 06 chira 8 ml dung dich dém vitratinatri hydroxyt (7.5). Sau 66 thyc hign theo quitrinh trong E.4.5 va E.4.6. Néu dung dich mau thir khéng c8 dac, sv thu héi cdc amin khac nhau [a khéng déi, cn bang vat ly; trong treéng hop nay, qui trinh kiém tra la mét phan xac nhan phuong phdp cia ting phong thir nghigm. Néu cdn ¢8 dc cde amin, phai thyc hign qué trinh kiém tra véi ting 16 m&u. Binh leong chuan kiém tra nay dya trén dung dich higu chudn thuémg i (E.2.1). ‘Ty Ié thu hoi amin phai tuan theo cdc yéu cdu t6i thiéu sau: 35TCVN 12512-1:2018 Cac amin 6 1 dén 4, 7, 9 dén 17 va 20 dén 21: ‘Amin s6 8: Amin s6 18 va 19: Amin s6 5, 6 va 22: Anilin: 36 70% 20% 50% xem chdi thich trong Bang 1 70%TCVN 12512-1:2018 Phy lye F (qui ginh) Ch&t mau Phuong php x4e dinh mét s6 amin thom Fa Yéu cdu chung Trong phy ye may mé ta qui trinh dé x4c dinh tnyc tiép mt sé amin thom tir cac cht mau, CHO THICH —Céc chét mau gid phéng nhiéu hom 200 mg/kg amin eo thé lim vat ligu dt éuxge nhudm mau Khéng dat. F.2 Nguyén tac Nguyén tac tong ty nhu 44 mé td trong Bidu §, loal trir céng doan chiét (10.1 va 10.2) bj logi bé khi mu thir 18 mot chét mau. Tach khis (10.3), tach va 03 dae cdc amin (10.4), phat hign va dinh lung amin (10.5) va qui trinh kiém tra (10.6) van gir tong ty, cing nhu d4nh gid (Bidu 11). Néu cdn phan tich ban cht ca chat mau, phai sir dung phuong phap trong Phy luc F. F.3. Chudn bj mau thir F.3.1. Yéu cau chung Mau thir la chét mau do nha sén xudt cung cp. F.3.4 Binh lwgng mu thir ‘Chudn bj mau thir tir chat mau dé 06 duc khdi lwgng 200 mg. F.4. Cach tién hanh ‘Cho mau thi? vo trong binh phn ig, thém 2,0 ml metano! va thy hign theo qui trinh nh mé'ta trong Biéu 10 nhung bat dau dp dung céc huéng dan durge cho trong 10.3. F.5 Banh gia Mic amin durge tinh bing ty I kh6i lrgng w, tinh bang mg/kg mAu thir theo céng thirc (3), trong 6 me 1a kh6i long cia mau thir cht mau, tinh bang g. F.6. Bao céo thie nghigm Bao cdo cdc két qua theo yéu cau trong Digu 12. 37TCVN 12512-1:2018 Phy luc G (tham kno) Pigment G.1. Nhu6m pigment G.1.1 Nhugm khdi Nhudm khéi la nhudm pigment cé polyme nh&n tzo trong qué tinh ép din true khi hinh thanh xo. Cac. xo dién hinh la polyamit, acrylic, polyeste va polyolefin. Kh8ng thé phan biét b&ing dyng cy quang hoc gira polyme nhudm pigment va polyme nhudm phan tan. Mat chi dan tét polyme nhudm pigment van con mau Khi chiét bang xylen. G.A.2_ Nhugm xo Nhugm xo’ c6 th8 4p dung cho tét ca cac logi xo’ (gdm ca xorthiy tinh), Bay la qué trinh mot ong doan khéng c&n xi? Iy sau, oO thé lam cho san ph4m 6 gid thanh ré va théng dung. Pigment durge 4 dinh bang cht keo ho&c chat két dinh. Theo kinh nghiém, c6 thé phan biét cdc xo nay véi xo’ nhugm phan tan bang kinh hién vi. C6 thé thay d6i do dam mau cia polyme nhudm khéi (6.1.1) sau d6 bang qua trin mhugm xo ) Hinh G.1 —Nhugm xo G43 In pigment Pigment deg sit dung phd bién dé in vat fiéu dét. Vat ligu dét durgc in bang pigment voi sy hé tro otra. chat tao mang cho pigment, céc tac nn lam mém, c&c chét bién tinh ding, chat khit bot, chat lam dic. Tuy thude vdo chat lung cla chat tao mang, cém giéc cimg cla vai in chi ra vigc sir dung pigment do 06 46 b&n mau thp véi cha xat. Pigment “dure gan” véi xo bang keo.TCVN 12512-1:2018 Hinh G.2 -In pigment G.2_ Cac tiéu chi d6i véi vat ligu durge in 6.2.1 Cac tiéu chi déi v6i in pigment Hinh in duegc gan mau bang chét tao mang van cén trén xo; ‘Céc chi tiét nhé dug dinh voi xo; ‘Cam gid sé tay ofmg hon so véi khu vire xo’ khong dug in; Khi vat ligu dt mam duge kéo cng, cd thé nhin thay cdc soc mau trang hodc sang. Néu cé vai pha cila céc xo khéc nhau, qui trinh in ré nhat la in pigment. Cac hinh in pigment 06 6 b&n mai mon kém hon khi in bang thudc nhugm. Chi c6 thé in cdc mau trdng va sang hon vat ligu nén bang in pigment. Cac tiéu chi dé in bang thuéc nhugm: ‘Thudc nhudm khong durgc gén mau bang cht to mang. ‘Thue nhudm thém vao x0, Néu kéo céng, cdc vat ligu det mém thudrg khdng cho thy céc soc tréng hode sang. Kh in vai pha ir céc xo khac nhau, vi cdc xo khéc nhau bigu hign d6 dém mau khéc nhau.. {89 bén mai mén oa hinh in bang thudc nhudm t6t hon nhidu so voi in bang pigment. G3 Chi dan a6i voi pigment ‘D6 voi polyeste nguyén chat, vat ligu dét van cn mau sau khi chiét bang xylen. ‘Sau khi chiét bang xylen va thay di dung méi sang metanol, cé céin mau khéng hda tan. ‘Cac ti8u chi 8 in pigment (G.2.1). 39TCVN 12512-1:2018 q i) Thu myc tai ligu tham khdo TCVN 12512-3:2018 (ISO 14362-3:2017), Vat ligu dét — Phuong php xée dinh mét sé amin thom giai phong tir chdt mau azo - Phan 3: Phét hign vigc sir dung mét s6 chét mau azo 06 thé gi8i phéng 4-aminoazobenzen Regulation (EC) No 1907/2006 of the European Parliament and of the Council of 18 December 2008 concerning the Registration, Evaluation, Authorisation and Restriction of Chemicals (REACH) and establishing a European Chemicals Agency ‘Schneider, G.: Verwendungsverbot bestimmter Azofarbstoffe fir Bedarisgegenstande: Analytik und Bewertung von Analysenergebnissen Application Ben of Certain Azo colorants for ‘commodities: Analysis and Interpretation of Analytical Resulls, Deutsche Lebensmittel- Rundschau, 93 (3), 69-102 (1997)