QUYT NH CA B TRNG B NNG NGHIP V PHT TRIN NNG THN S 26/2002/Q-BNN, ngy 15 thng 04 nm 2002 V/v ban hnh tiu chun ************** B TRNG B NNG NGHIP V PHT TRIN NNG THN

- Cn c Ngh nh s 73/CP ngy 01 thng 11 nm 1995 ca Chnh ph quy nhchc nng, nhim v, quyn hn v t chc b my ca B Nng nghip v Pht trin Nng thn; Cn c Ngh nh 86/CP ngy 08 thng 12 nm 1995 ca Chnh ph quy nh phn cng trch nhim qun l Nh nc v cht lng hng ho; pht trin nng thn ban hnh ngy 1/10/1999 v vic ban hnh quy ch lp xt duyt v ban hnh tiu chun ngnh Xt ngh ca ng V trng V Khoa hc Cng ngh v Cht lng sn phm QUYT NH iu 1: Nay ban hnh tiu chun ngnh sau: 1. 10TCN 499-2002 thnh phm thuc bo v thc vt 2. 10TCN 500-2002 thuc tr su cha hot cht triazophos 3. 10TCN 501-2002 thuc tr bnh cha hot cht triadimenol 4. 10TCN 502-2002 thuc tr bnh cha hot cht propineb 5. 10TCN 503-2002 thuc tr bnh cha hot cht imibenconazole 6. 10TCN 504-2002 thuc tr bnh cha hot cht oxolinic acid 7. 10TCN 505-2002 thuc tr c cha hot cht trifluralin 8. 10TCN 506-2002 thuc tr c cha hot cht cinmethylin 9. 10TCN 507-2002 thuc tr c cha hot cht sethoxydim iu 2: Quyt nh c hiu lc sau 15 ngy k t ngy k

- Cn c quyt nh s : 135/Q-BNN-KHCN ca B trng B Nng nghip v

iu 3: Cc ng Chnh Vn phng, V trng V Khoa hc Cng ngh v Cht lng sn phm, Cc trng cc bo v thc vt, Th trng cc n v lin quan chu trch nhim thi hnh quyt nh ny. KT. B TRNG B NNG NGHIP V PHT TRIN NNG THN Th trng Bi B Bng : k

Nhm C TIU CHUN NGNH 10 TCN 499 -2002

THNH PHM THUC BO V THC VT Phng php xc nh tnh cht ho l Plant Protection Product Testing methods of Physical and Chemical Properties

I. PHNG PHP TH RY T 1. Phm vi p dng Tiu chun ny qui nh phng php th ry t p dng cho: -Thnh phm thuc bo v thc vt (BVTV) dng bt thm nc (WP); -Thnh phm thuc bo v thc vt (BVTV) dng huyn ph (SC); -Thnh phm thuc bo v thc vt (BVTV) dng ht phn tn trong nc (WG). 2. Phng php th 2.1. Nguyn tc Mu sau khi c thm t hon ton (hoc to huyn ph) vi nc c chuyn ton b vo ry c kch thc xc nh. Mu trn ry c ra di dng nc my cho n khi phn cn li trn ry khng i. Xc nh khi lng phn cn li trn ry sau khi c sy kh ti trng lng khng i. 2.2. Dng c Cc thu tinh dung tch 250 ml. a thu tinh u bt cao su. Ry c kch thc l 75 m, 45 m (hoc kch thc theo yu cu) Giy lc.

Bnh ht m. ng cao su ng knh trong 10 mm. 2.3. Tin hnh 2.3.1. Thuc BVTV dng bt thm nc v huyn ph Cn khong 20 g mu chnh xc ti 0,1 g vo cc 250 ml. Va thm nc va khuy bng a thu tinh cho n khi c khi bt nho. Thm nc vo cc pha long khi bt nho ti 150 ml, chuyn sang ry c thm t, trng cc nhiu ln v ln ry. Ra mu trn mt ry di dng nc my (chy chm) trong 4 pht. Chuyn nh lng phn cn trn ry ln ming giy lc bit trng lng, kh v sy 65 5oC n khi lng khng i, cn v xc nh phn cn thu c. 2.3.2. Thuc BVTV dng ht phn tn trong nc Cn khong 10g mu chnh xc ti 0,1 g vo cc 250 ml. Thm 100 ml nc, yn 1 pht, khuy nh bng a thu tinh u bt cao su trong 30 giy vi tc khuy 3-4 vng /giy. Chuyn ton b bt nho ln ry, trng cc nhiu ln v ln ry. Ra mu trn mt ry di dng nc my qua ng cao su. (tc chy 4-5 lt/pht). Hng dng nc theo vng trn t thnh cho n tm ca ry v gi khong cch gia u ng cao su v b mt ry 3-5 cm. Ra mu trong 10 pht. Chuyn nh lng phn cn cn li trn ry ln ming giy lc bit trng lng, kh v sy 65 5oC n khi lng khng i. Cn v xc nh phn cn thu c. 2.3.3. Tnh kt quX (%) = m x100 w

Phn cn li trn ry (X) tnh bng phn trm theo cng thc: Trong : m: khi lng cn cn li trn ry, g. w: Khi lng mu, g II. PHNG PHP TH RY KH

1. Phm vi p dng Phng php ny p dng cho thnh phm thuc bo v thc vt (BVTV) dng ht s dng trc tip. 2. Phng php th 2.1. Nguyn tc Mu c tch nh lng thnh nhng phn khc nhau qua cc ry c kch thc xc nh. 2.2. Dng c, thit b Ry c kch thc: 850 m, 710 m , 500 m, 420 m, 355 m, 250 m, 150 m. y ry v np ry. My ry, ry 300 dao ng /pht, bin rung 4 mm, tc quay 2,5 vng/pht. Chi lng Cc dung tch 300 ml. Cn c chnh xc 0,1 g. Giy nhn bng c din tch khng nh hn 38 cm2 2.3. Tin hnh Lp ry theo th t ry c kch thc l nh hn di, y ry di cng. Ly khong 300 g mu cho vo cc dung tch 300 ml bit trng lng. Cn cc v mu, chnh xc ti 0,1 g. Chuyn mu ln ry, ly chi lng qut ht bi dnh trn cc ln ry. Tnh khi lng mu. y np ry, t b ry vo my ry v cho ry 45 pht, yn 2 pht cho lng bi ri ly ry ra khi my. Tho tng ry ra v p ngc mi ry ln 1 ming giy vung trn, bng c cn trc. p nh thnh ry ln ming giy, dng chi lng qut nh ln mt ry trn cho bong nhng ht bi bm vo l ry. Lt ry li qut nh mt ry di. Cn li ming giy cha mu chnh xc ti 0,1 g v tnh khi lng mu tng ng vi mi ry. Cng lm nh vy vi y ry. T l ht c kch thc 850 - 250 m (X) tnh bng % theo cng thc :X (%) = m 100 M

T l ht bi qua ry 250 m v cn li trn ry 150 m (Y) tnh bng % theo cng thc: T l ht bi lt qua ry 150 m (Z) tnh bng % theo cng thc:n Y (%) = 100 l M Z (%) = 100 M

Trong : m: Khi lng mu cn li trn cc ry c kch thc l 850 m n 250 m, g n: Khi lng mu trn ry 150 m, g l: Khi lng mu trong y ry, g M: Khi lng mu ban u, g III. PHNG PHP XC NH T SUT L LNG 1. Phm vi p dng Tiu chun ny quy nh phng php xc nh t xut l lng ca dung dch huyn ph c nng ng vi nng s dng (nng hot cht khng ln hn 1%) ca: -Thuc BVTV dng bt thm nc (WP); -Thuc BVTV dng huyn ph (SC); -Thuc BVTV dng ht phn tn trong nc (WG).

2. Nguyn tc Dung dch huyn ph ca mu th vi nc theo nng s dng trong ng ong c duy tr nhit v thi gian xc nh. Loi b 9/10 th tch dung dch huyn ph pha trn v xc nh lng hot cht trong 1/10 th tch cn li trong ng ong. 3. Ho cht, dng c

Nc cng chun: theo TCVN 3711 - 82 Cc c dung tch 250 ml ng ong nt nhm dung tch 250 ml, chia ti 1ml c khong cch gia vch 0 v vch 250 ml l 20 - 21,5 cm (hnh 1) ng ht thu tinh di 40 cm, ng knh trong 5 mm, mt u nhn c ng knh trong 2 - 3 mm, u kia ni vi ngun ht. B n nhit 30 1oC.

Hnh 1 4. Tin hnh Chuyn lng mu th ( pha 250 ml dung dch huyn ph c nng ng vi nng s dng) vo cc dung tnh 250 ml cha sn 50 ml nc cng chun nhit 30 1oC, khuy trong 2 pht vi tc 2 vng/ giy. Chuyn nh lng dung dch huyn ph vo ng ong dung tch 250 ml. Thm nc cng chun nhit 30 1oC vo ti vch 250 ml. y nt, o ngc ng ong 30 ln. t ng ong vo b n nhit 30 1oC, trnh rung v trnh nh nng mt tri trc tip chiu vo. Sau 30 pht ht 225 ml dung dch pha trn bng ng ht trong 10 - 15 giy, ch ng ht sao cho u ng lun lun nhng di mt cht lng vi mm, trnh ng ti lp di ng ong. Lng hot cht trong 25 ml cn li di y ng ong c xc nh theo phng php ring ca tng loi thuc. 5. Tnh tonX (%) = 111(c q ) c

T sut l lng (X) tnh bng % theo cng thc: Trong : q-khi lng hot cht trong 25 ml dung dch huyn ph cn la trong ng ong, g c-khi lng hot cht trong mu, gc= a b 100

a-Hm lng hot cht trong mu, % b-khi lng mu, g IV. PHNG PHP XC NH THM T 1. Phm vi p dng Tiu chun ny qui nh phng php xc nh thm t ca: -Thuc BVTV dng bt thm nc (WP)

-Thuc BVTV dng ht phn tn trong nc (WG) -Thuc BVTV dng bt ho tan trong nc (SP) 2. Nguyn tc Cho mt lng mu th xc nh vo nc cha trong 1 cc thu tinh c kch thc nht nh. Xc nh thi gian thm t hon ton ca mu th. (khng khuy) 3. Ho cht, dng c ng ong dung tch 100 ml Cc thu tinh dung tch 250 ml, c kch thc ng knh: 6,5 0,5 cm chiu cao : 9,0 0,5 cm Cc cn ng h bm giy Nc cng chun: theo TCVN 3711 - 82 4. Tin hnh Dng ng ong ly chnh xc 100 ml nc cng chun vo cc thu tinh 250 ml. Cn khong 5 g mu chnh xc 0,1g vo cc cn (sao cho mu khng b nn cht). Chuyn ton b mu vo cc thu tinh cng mt lc sao cho b mt ca nc trong cc khng b xo ng. Thi gian thm t tnh bng pht t khi mu c chuyn ht vo cc thu tinh cho n khi lng mu c thm t hon ton (ch cn li lp mng ht mn trn b mt nc) V. PHNG PHP XC NH TO BT 1. Phm vi p dng Tiu chun ny qui nh phng php xc nh to bt i vi thuc BVTV phi pha long vi nc trc khi s dng. 2. Nguyn tc

Dung dch huyn ph vi nc ca mu th theo nng s dng c chun b vo ng ong c kch thc xc nh. o ngc ng ong 30 ln, xc nh lng bt to thnh. 3. Ho cht, dng c, thuc th ng ong c nt nhm dung tch 250 ml, chia vch n 2 ml, kch thc qui nh nh hnh 1. ng h bm giy Nc cng chun: theo TCVN 3711 - 82 4. Tin hnh 180 ml nc cng chun vo ng ong 250 ml v t trn cn v cn vo ng ong lng mu to huyn ph vi 200 ml nc cng chun theo nng s dng. Thm nc cng chun khong cch gia b mt cht lng v y ca ming ng ong l 9 0.1 cm. y nt, o ngc ng ong 30 ln, t ng ong trn bn v lp tc bm ng h . c th tch bt to thnh sau 10 1 giy; 1,3, 12pht 10 giy. VI. PHNG PHP XC NH T TRNG 1. Phm vi p dng Tiu chun ny qui nh phng php xc nh t trng ca thuc BVTV dng k thut v thnh phm.

2. Qui nh chung T trng k xc nh t trng ca thuc BVTV dng lng Bnh t trng xc nh t trng thuc BVTV dng lng v rn Mu phn tch tin hnh ng thi trn 2 php o i vi phng php dng t trmg k v 2 lng cn i vi phng php bnh t trng. Nc ct theo TCVN 2217 - 77 3. Phng php bnh t trng

3.1. Nguyn tc T trng ca mu th c xc nh bng cch so snh khi lng mu th v nc trong cng 1 bnh t trng 200C. 3.2. Dng c Bnh t trng thu tinh nt nhm c ng mao qun gia. C hoc khng c np y thu tinh. Dung tch 5,10, 25, 50 hoc 100 ml; bnh t trng khng c np y khng s dng xc nh t trng ca cht lng r bay hi. (hnh 2, hnh 3) B n nhit , iu chnh c nhit 20 0,50C Nhit k chia n 0,10C Cc thu tinh dung tch 250 ml Nc ct theo TCVN 2217 - 77 Dung dch kh bt silicon: 1% silcolapse 5000 (khi lng/th tch)

Hnh 2 3.3. Tin hnh

Hnh 3

3.3.1. Xc nh khi lng nc ct Cn bnh t trng sch v kh (c nt) chnh xc n 0,0001 g (m 0), y nc ct un si, ngui v t vo b n nhit (nhng ngp n c bnh) nhit 20 0,5 0C t nht 20 pht. Ly bnh t trng ra y nt, lau kh bnh, cn v xc nh khi lng (m1). Khi lng nc 200C (mn) c tnh bng gam theo cng thc : mn = ( m1 - m0) Trong : m0 - Khi lng bnh t trng, g m1 - Khi lng bnh t trng v nc ct, g 3.3.2. Xc nh t trng ca thuc BVTV dng lng Xc nh khi lng ca mu th trong bnh t trng 20 0C (m2) nh phn 3.3.1 T trng ca mu th 20 0C (d20) c tnh bng g/ml theo cng thc:d 20 =n d 20 m2 mn

Trong : dn20 = 0,9982 g/ml l t trng ca nc 20 0C. T trng tng i ca mu 20 0C (S20) c tnh theo cng thc:S 20 = ( m 2 m0 ) mn

Trong : m2 - Khi lng mu th , g

3.3.3. Xc nh t trng ca thuc BVTV dng huyn ph

Cn v xc nh khi lng bnh t trng cha khong 20 ml mu th (m2). Thm khong 20 ml dung dch kh bt, trn bng cch xoay nh bnh. y vo bnh t trng dung dch kh bt, t vo b n nhit (nhng ngp n c bnh) nhit 20 0,5 0C t nht 20 pht. Ly bnh t trng ra y nt, lau kh bnh, cn v xc nh khi lng (m3). Ch : Mu th, dung dch kh bt gi nhit 20 0,5 0C. T trng ca mu 20 0C (d20) c tnh bng g/ml theo cng thc:

d 20 =Trong :

m2 m0 mn m3 m2 d n 20 D

D-t trng 200C ca dung dch kh bt g/l, xc nh theo 3.3.2. m2 - Khi lng bnh t trng v mu th, g m3 - Khi lng bnh t trng, mu th v dung dch kh bt, g 3.3.4. Xc nh t trng ca thuc BVTV dng rn khng ho tan trong nc nhng thm t Cn v xc nh khi lng bnh t trng c cha lng mu rn chim khong 1,5 ml (m1). Thm 1 lng nc ct un si, ngui n na bnh v t vo desicator chn khng cho n khi ht bt kh. Ly ra, y nc ct un si ngui vo v t vo b n nhit (nhng ngp bnh t trng n c) nhit 20 0,5 0C t nht 20 pht. Ly bnh t trng ra y nt, lau kh bnh, cn v xc nh khi lng (m4g). T trng ca mu 20 0C (d20) c tnh bng g/ml theo cng thc:

d n 20 (m1 m0 ) d 20 = mn (m4 m1 )

Trong : m1 - Khi lng bnh t trng v mu th, g

m4 - Khi lng bnh t trng, mu th v nc ct, g 3.3.5. Xc nh t trng ca thuc BVTV rn ho tan trong nc nhng khng thm t Tin hnh theo 3.3.4. vi cht lng khng ho tan mu nhng thm t mu. T trng ca mu 20 0C (d20) c tnh bng g/ml theo cng thc:d 20 = 0.9982 (m1 m0 ) S .mn ( m4 m1 )

S - t trng tng i ca cht lng xc nh theo 3.3.2.

4. Phng php t trng k 4.1. Nguyn tc T trng ca thuc BVTV dng lng c o bng t trng k nhit nht nh. 4.2. Dng c T trng k chia n 0,001 g/ml ( loi I) hay 0,0005 g/ml ( loi II) B n nhit Bnh hnh tr thu tinh khng mu c ng knh ln hn ng knh ln nht ca mt k t nht 25 mm. Cc thu tinh dung tch 250 ml

4.3. Tin hnh Cho mu th vo bnh hnh tr thu tinh n cch ming bnh 4 cm, t vo b iu nhit nhit 20 0,5 0C t nht 20 pht, dng nhit k va khuy va o nhit ca cht lng. Khi nhit ca cht lng t 200C 0,50C th nh t trng k vo bnh sao cho khng chm y v thnh bnh (khong cch ca t trng k vi y bnh khng c nh hn 3 cm ). Sau 3 -4 pht, ghi t trng ca mu th trn vch t trng k.

T trng ca mu th ng vi vch chia ca t trng k theo im di ca mt cu lm i vi cht lng trong sut, sng mu v gii hn trn ca mt cu lm i vi cht lng hi c v sm mu. Kt qu o l trung bnh ca hai ln o lin tip. S chnh lch ca hai ln o khng ln hn 0,001 g/ml i vi t trng k loi I v 0,0005 g/ml i vi t trng k loi II. i vi thuc BVTV dng huyn ph: Cn 100 g nc ct un si ngui chnh xc ti 0.01 g vo cc thu tinh 250 ml. Vn cc trn cn thm mu t t n100 g. Trn u bng cch rt i rt li sang mt cc thu tinh 250 ml khc cho n ng nht - dung dch A. Xc nh t trng ca dung dch A bng t trng k nh trn. T trng ca mu 20 0C (d20) c tnh bng g/ml theo cng thc:d 20 = a 2 a

a -t trng o c ca dung dch A 20 0C VII. XC NH HM LNG NC 1. Phm vi p dng Tiu chun ny qui nh phng php xc nh hm lng nc ca thuc BVTV dng k thut v thnh phm. 2. Phng php chun Karl Fischer 2.1. Phng php chun th tch 2.1.1. Nguyn tc Lng nc trong mu c xc nh bng phng php chun th tch vi dung dch Karl Fischer.

2.1.2. Ho cht, dng c, thuc th Methanol kh (hm lng nc khng c ln hn 0,03% ) Dung dch Karl Fischer (KF) Nc ct theo TCVN 2271-77 My chun Karl Fischer vi in cc platin kp Xylanh bm mu dung tch 10 ml, chia vch n 0,1 ml. 2.1.3. Tin hnh 2.1.3.1. Xc nh h s (F) ca thuc th Karl Fischer Thm chnh xc 20 ml methanol vo bnh phn ng, chun bng ung dch KF. Cn v chuyn bng xylanh khong 0,05 g nc ct chnh xc n 0,00001 g (m) vo bnh phn ng, chun bng dung dch KF n im tng ng, (V). Lp li 3 ln.F ( g / ml ) = m V

Trong : m - Khi lng mu th, g V- Th tch dung dch KF s dng, ml 2.1.3.2. Xc nh hm lng nc ca mu th a/Mu thuc BVTV dng lng Thm chnh xc 20 ml methanol vo bnh phn ng, chun bng thuc th KF n im tng ng. Cn v chuyn bng xy lanh lng mu (m 1) vo bnh phn ng, khuy 1 pht v chun bng dung dch KF trn my cho n im tng ng (V1) b/ Mu dng rn Lng mu th (m1) c ho tan (hoc chit thnh phn nc ca mu) bng dung mi thch hp - dung dch A. Cn v xc nh khi lng dung dch A (m2). Cn v chuyn bng xylanh lng dung dch A (m3) vo bnh phn ng, khuy

trong 1 pht v chun bng dung dch KF trn my cho n im tng ng (V1). Xc nh tng t vi mu trng. 2.1.3.3. Tnh ton kt qu Hm lng nc (X) trong mu lng c tnh bng % theo cng thcX (%) = 100 V1 F m1

Hm lng nc (X) trong mu rn c tnh bng % theo cng thcX (%) = 100 (V1 V0 ) m2 F m3 m1

Trong : m1 - Khi lng mu th, g m2 - Khi lng dung dch A, g m3 - Khi lng dung dch A a vo bnh phn ng, g V1 - Th tch dung dch KF xc nh dung dch A trong bnh phn ng, ml V0- Th tch dung dch KF xc nh mu trng, ml

2.3. Phng php chun in lng 2.3.1. Nguyn tc Lng nc trong mu c xc nh bng phng php chun vi dung dch in cc Karl Fischer. 2.3.2. Ho cht, dng c, thuc th Methanol kh (hm lng nc khng c ln hn 0,03% ) Dung dch in cc Karl Fischer (KF)

Nc ct theo TCVN 2217 - 72 My chun Karl Fischer vi in cc platin kp Xylanh bm mu dung tch 10 ml, chia vch n 0,1 ml. 2.3.3. Tin hnh a/ Mu dng lng Cn v chuyn bng xylanh lng mu (m) vo bnh phn ng, khuy v chun trong thi gian 1-10 pht (tu theo tng loi thuc BVTV c th). Ghi kt qu lng nc xc nh c trn my (M1) b/Mu dng rn Lng mu th (m) c ho tan (hoc chit thnh phn nc ca mu) bng dung mi thch hp - dung dch A (m1). Cn v chuyn bng xylanh lng dung dch A (m2) vo bnh phn ng, khuy v chun trong thi gian 1-10 pht (tu theo tng loi thuc BVTV c th). Ghi kt qu lng nc xc nh c trn my (M1). Xc nh tng t i vi mu trng. 2.3.4. Tnh ton kt qu Hm lng nc (X) trong mu lng c tnh bng % theo cng thcX (%) = 100 M1 m

Hm lng nc (X) trong mu rn c tnh bng % theo cng thcX (%) = 100

( M 1 M 0 ) m1m m2

Trong : m - Khi lng mu th, g m1 - Khi lng dung dch A, g

m2 - Khi lng dung dch A a vo bnh phn ng, g M1- Lng nc trong dung dch A a vo bnh phn ng, g M0- Lng nc xc nh c trong mu trng, g Ch : Tnh ton lng cn mu th xc nh hm lng nc bng phng php chun KF c th cn c theo bng sau: STT` 1 2 3 4 5 6 Hm lng m 10-50% 1 - 10% 0,1 - 1% 0,01 - 0,1% 0,001 - 0,01% 0,0001 - 0,001% Lng cn mu 0,02 - 0,01 g 0,05 - 0,01g 0,1 - 0,01g 1,0 - 0,1g 5 - 1,0 g 10 5 g

3. Phng php Dean Start 3.1. Nguyn tc Lng nc trong mu c xc nh bng phng php chng ct ng si vi toluene hoc naphtha. Phng php ny ch p dng cho mu c hm lng nc ln hn 0,1%. 3.2. Ho cht, dng c Toluene hoc naphtha Dng c Dean - Start (hnh 4) ng thu dung tch 2 ml chia vch n 0,05 ml, u ni c nhm Bnh cu c nhm dung tch 500 ml ng ong dung tch 100 ml Cn k thut, chnh xc 0,01g

Hnh 4 3.3. Tin hnh Cn lng mu thch hp (sao cho th tch nc thu c t 0,5 - 1,8 ml) vo bnh cu 500 ml, thm khong 100 200 ml toluene hoc naphtha lng mu trong bnh ngp di lp dung mi, cho vo bnh vi vin bt. Tin hnh chng ct trn bp sao cho tc chng ct t 2-5 git trong 1 giy. Tip tc un cho n khi khng thy nc ng trn thnh bnh v th tch bnh thu khng tng thm trong 5 pht. Ngng chng ct, yn 30 pht, ghi th tch nc thu c. 3.4. Tnh ton kt qu Hm lng nc A trong mu tnh bng % theo cng thc:A = 100 V m

Trong : V- Th tch nc bnh thu, ml m-Khi lng mu, g VIII. PHNG PHP XC NH BN BO QUN 1. bn bo qun nhit 0C 1.1. Phm vi p dng Tiu chun ny qui nh phng php xc nh bn bo qun nhit 0C ca thnh phm thuc BVTV dng lng. 1.2. Nguyn tc Mu th c bo qun 0 1 0C lin tc trong 7 ngy, xc nh th tch cht rn hay cht lng tch lp . 1.3. Ho cht, dng c, thit b ng ong 100 ml, chia vch n 0,1 ml Pipet 100 ml T lnh c kh nng duy tr nhit 0 1 0C ng ly tm dung tch 100 ml c kch thc (mm) nh hnh 5

Hnh 5 1.4. Tin hnh Dng pipet ly 100 ml mu th chnh xc n 1.0 ml vo ng ly tm, t vo t lnh nhit 0 1 0C trong 1 gi. Trong thi gian , 15 pht khuy mu 1 ln ( mi ln khuy 30 giy). Tip tc bo qun mu nhit 0 1 0C lin tc trong 7 ngy. Sau ly mu ra, nhit 20 0C trong 3 gi, o ngc ng ly tm mt ln, ly tm 15 pht v ghi li th tch cht rn hoc cht lng tch lp y ng ly tm. Ch : Tc ly tm V (vng / pht)V = 98 ,45 10 3 d

d - Khong cch gia hai ng ly tm i din, cm 2. bn bo qun nhit 54 C 2.1. Phm vi p dng Phng php ny qui nh p dng xc nh bn bo qun nhit 54 C cho cc dng thnh phm thuc thuc BVTV. 2.2. Nguyn tc Mu th c bo qun 54 2 0C lin tc trong 14 ngy (hoc nhit v thi gian xc nh theo yu cu), xc nh tnh cht ca mu th d n nhit thng sau 24 gi. 2.3. Dng c Thit b iu chnh c nhit 54 2 0C.

Desicator khng c cht ht m L dung tch 100 ml, nt xoy, c ming lt polyetylen. Cc dung tch 250 ml, ng knh trong 6,0 - 6,5 cm. Ming knh trn dng y trn mt mu trong cc c th to ra p sut khong 25 g/cm2. 2.4. Tin hnh 2.4.1. Thuc BVTV dng nh du Cho khong 50 ml mu th vo l, y ming lt polyetylen, t l vo thit b iu chnh nhit 54 0C. Sau 30 pht y nt xoy vo l v l trong iu kin nhit 54 2 0C trong sut 14 ngy ( hoc thi gian khng lin tc tng ng). Sau ly l ra, m nt xoy, l ngui t nhin nhit phng ri y nt xoa li. Xc nh cc ch tiu vt l v ho hc ca mu th sau 24 gi k t khi ly mu th ra khi thit b iu chnh nhit. 2.4.2. Thuc BVTV dng bt thm nc Cho khong 20g mu th vo cc, dn u mt mu. t ming knh ln mt mu trong cc v t cc vo thit b iu chnh nhit 54 2 0C trong sut 14 ngy ( hoc thi gian khng lin tc tng ng). Sau ly cc ra, b ming knh ra, ngui cc trong desicator. Xc nh cc ch tiu vt l v ho hc ca mu th sau 24 gi k t khi ly mu th ra khi thit b iu chnh nhit. KT. B TRNG B NNG NGHIP V PHT TRIN NNG THN Th trng Bi B Bng : k

GII THIU HOT CHT TRIAZOPHOS

Cng thc cu to:

Tn ho hc: 0,0 - dimethyl 0-1- phenyl-1-H-1,2,4-triazol-3-yl phosphorothioat Cng thc phn t: C12H16 N3O3PS Khi lng phn t: 313,3 ho tan ( 200C) trong: Nc: Ethyl acetat , acetone : Hexane: 0,03 0,04 g/l > 1000g/kg 9 g/kg

Ethanol, toluen: Dng bn ngoi : Cht lng c dng du , mu vng xm

> 330g/kg

bn: Bn vi nh sng , b thu phn trong mi trng axit v mi trng kim

Nhm B&C TIU CHUN NGNH 10 TCN 500-2002

THUC TR SU CHA HOT CHT TRIAZOPHOSYu cu k thut v phng php th Insecticide containing triazophos Technical requirements and test methods

1. PHM VI P DNG Tiu chun ny p dng cho: - Triazophos k thut; - Thuc bo v thc vt (BVTV) c cha hot cht triazophos dng nh du dng lm thuc tr su hi cy trng. 2. QUI NH CHUNG 2.1. Ly mu Theo 10TCN 386 - 99 2.2. Ho cht Ho cht phn tch phi l loi TKPT 2.3. Mc sai lch cho php ca hm lng hot cht Hm lng hot cht ng k Mc sai lch cho php % g/kg hoc g/l 200C

T 2,5 tr xung T trn 2,5 n 10 T trn 10 n 25 T trn 25 n 50 T trn 50 tr ln

T 25 tr xung T trn 25 n 100 T trn 100 n 250 T trn 250 n 500 T trn 500 tr ln

15% hm lng ng k 10% hm lng ng k 6% hm lng ng k 5% hm lng ng k 2,5% 25g/kg hoc g/l

2.4. Cn phn tch Cn s dng c chnh xc n 0,00001g 3. YU CU K THUT 3.1. Triazophos k thut Triazophos k thut l cht lng c mu vng nht n nu vi thnh phn chnh l triazophos v tp cht sinh ra trong qu trnh sn xut. 3.1.1. Hot cht Hm lng triazophos ng k, khi xc nh phi ph hp vi qui nh trong mc 2.3. 3.1.2. Tnh cht vt l axit (tnh theo H2SO4) Khng ln hn 0,2 g/kg

3.2. Thuc tr su c cha hot cht triazophos dng nh du Sn phm dng nh du l hn hp cht lng, ng nht trong sut, mu vng nht n nu, c mi c trng ca este phosphoric, khng lng cn ca triazophos k thut, dung mi v cc cht ph gia

. 3.2.1. Hot cht Hm lng triazophos ng k, khi xc nh phi ph hp vi qui nh trong mc 2.3 3.2.2. Tnh cht vt l 3.2.2.1. axt (tnh theo H2SO4) Khng ln hn 3.2.2.2. pH Trong khong 3.2.2.3. bn nh tng t nh ban u bn nh tng sau 30 pht, lp kem ln nht bn nh tng sau 2 gi : lp kem ln nht ti nh sau 24 gi Hon ton 2 ml 4 ml Hon ton 4 ml 3,5 0,5 2 g/kg

bn nh tng cui cng sau 24 gi 30 pht: lp kem ln nht

3.2.3. bn bo qun 3.2.3.1. nhit O0C Sau khi bo qun 0 + 10C trong 7 ngy, th tch cht lng hoc cht rn tch lp khng ln hn 0,3 ml. 3.2.3.2. nhit 540C Sau khi bo qun 54 + 20C trong 14 ngy, sn phm phi ph hp vi qui nh trong mc 3.2.

4. PHNG PHP TH 4.1. Xc nh hm lng hot cht triazophos 4.1.1. Nguyn tc: Hm lng triazophos c xc nh bng phng php sc k lng cao p, vi ct pha thun. Kt qu c tnh da trn s so snh gia s o din tch hoc chiu cao ca pic mu th v s o din tch hoc chiu cao ca pic mu chun .

4.1.2.

Ho cht, dng c, thit b.

Isooctan Dioxan Cht chun triazophos bit hm lng Bnh nh mc dung tch 10 ml Cn phn tch My sc k lng cao p vi detector t ngoi My tch phn k hoc my vi tnh Ct pha thun Lichrosorb Si 60, 5 m , (250 x 4 mm) hoc tng ng Micro xylanh bm mu 50 l, chia vch n 1 l 4.1.3. Chun b dung dch 4.1.3.1. Dung dch mu chun Cn khong 0,010 g cht chun triazophos chnh xc ti 0,00001 g vo bnh nh mc 10 ml . Ho tan v nh mc ti vch bng dung mi pha ng. 4.1.3.2. Dung dch mu th Cn lng mu cha khong 0,010 g hot cht chnh xc ti 0,00001 g vo bnh nh mc 10 ml. Ho tan v nh mc ti vch bng dung mi pha ng. 4.1.4. Thng s my Pha ng : iso octan : dioxan ( thm 0,15% nc) 90:10

Bc sng: Tc dng :

254 nm 1 ml /pht

Th tch vng bm mu:

20 l

4.1.5. Tin hnh phn tch trn my Bm dung dch mu chun cho n khi s o din tch hoc chiu cao ca pic mu chun thay i khng ln hn 1%. Sau , bm ln lt dung dch mu chun v dung dch mu th lp li 2 ln. (s o din tch hoc chiu cao ca pic mu chun thay i khng ln hn 1% ). 4.1.6. Tnh ton kt qu Hm lng hot cht triazophos ( X ) trong mu c tnh bng phn trm theo cng thc: Sm mc X= Sc mm Trong : Sm : Trung bnh s o din tch hoc chiu cao ca pc mu th Sc : Trung bnh s o din tch hoc chiu cao ca pc mu chun mc : Khi lng mu chun, g mm : Khi lng mu th, g P : tinh khit ca cht chun, % 4.2. Xc nh axt Theo 10TCN - 409 - 2000, mc 4.2 4.3. Xc nh pH Theo 10TCN 389-99, mc 4.2 P

4.4. Xc nh bn nh tng: Theo TCVN - 3711 - 82, mc 3.5 4.5. Xc nh bn bo qun 4.5.1. nhit 0oC Theo 10TCN - 433 - 2001, mc 4. 5..2.1 4.5.2. nhit 54oC Theo 10TCN - 105-88

TI LIU THAM KHO

1. TCVN - 3711- 82 2. 10TCN - 105 - 88 3. 10TCN 386 99 4.10TCN 389-99 5. 10TCN - 409 2000 6. 10TCN 433-2001 7. Hoechst , Application for registration triazophos, January 30th-1992 8. FAO Panel of Expert on Pesticide Specification, Registration Requirements and Application Standards and Prior Informed Consent, Manual on Development and Use of FAO Specifications for Plant Protection Products-fifth edition, 1999. 9.The British Crop Protection Council & The Royal Society of Chemistry, UK, The pesticide Manual, tenth edition, 1994. KT. B TRNG B NNG NGHIP V PHT TRIN NNG THN Th trng Bi B Bng : k

GII THIU HOT CHT TRIADIMENOL

Cng thc cu to:

Tn ho hc: (1RS,2RS;1RS,2SR )-1-(4-chlorophenoxy)-3,3-dimethyl-1-(1H1,2,4-triazol-=1-yl)butan-2-ol. Cng thc phn t: C14H18 ClN3O2 Khi lng phn t: 295,5

ho tan ( 200C) trong: ng phn quang hc A B Nc Dichlormethane, isopropanol Toluene Hexane: 62 mg/l 100-200 g/l 20-50g/l 0,1-1g/l 32mg/l 100-200g/l 10-20g/l 0,1-1 ng phn quang hc

Dng bn ngoi : dng tinh th, khng mu . bn : C 2 ng phn quang hc u bn nhit thng .

Nhm B&C TIU CHUN NGNH 10 TCN501-2002

THUC TR BNH CHA HOT CHT TRIADIMENOL Yu cu k thut v phng php th Fungicide containing triadimenol Technical requirements and test methods

1. PHM VI P DNG Tiu chun ny p dng cho: - Triadimenol k thut; - Thuc bo v thc vt (BVTV) c cha hot cht triadimenol dng nh du dng lm thuc tr bnh hi cy trng; - Thuc BVTV c cha hot cht triadimenol dng bt thm nc dng lm thuc tr bnh hi cy trng. 2. QUI NH CHUNG 2.1. Ly mu Theo 10TCN 386 99. 2.2. Ho cht Ha cht phn tch phi l loi TKPT Nc cng theo TCVN 3711-82 2.3. Mc sai lch cho php ca hm lng hot cht

Hm lng hot cht ng k Mc sai lch cho php % g/kg hoc g/l 200C

T 2,5 tr xung T trn 2,5 n 10 T trn 10 n 25 T trn 25 n 50 T trn 50 tr ln

T 25 tr xung T trn 25 n 100 T trn 100 n 250 T trn 250 n 500 T trn 500 tr ln

15% hm lng ng k 10% hm lng ng k 6% hm lng ng k 5% hm lng ng k 2,5% 25g/kg hoc g/l

2.4. Cn phn tch Cn s dng c chnh xc n 0,00001g. 3. YU CU K THUT 3.1. Triadimenol k thut Triadimenol k thut l cht rn dng tinh th khng mu vi thnh phn chnh l triadimenol v mt phn tp cht sinh ra trong qu trnh sn xut. Hot cht : Hm lng triadimenol ng k, khi xc nh phi ph hp vi qui nh trong mc 2.3. 3.2. Thuc tr bnh c cha hot cht triadimenol dng nh du Sn phm dng nh du l hn hp cht lng, ng nht trong sut, khng lng cn ca triadimenol k thut, dung mi v cc cht ph gia. . 3.2.1. Hot cht

Hm lng triadimenol ng k khi xc nh phi ph hp vi qui nh trong mc 2.3. 3.2.2. Tnh cht vt l bn nh tng t nh ban u bn nh tng sau 30 pht, lp kem ln nht bn nh tng sau 2 gi, lp kem ln nht ti nh sau 24 gi bn nh tng cui cng sau 24 gi30 pht, lp kem ln nht 3.2.3. bn bo qun 3.2.3.1. nhit O0C Sau khi bo qun 0 + 10C trong 7 ngy, th tch cht lng hoc cht rn tch lp : Khng ln hn 0,3 ml. 3.2.3.2. nhit 540C Sau khi bo qun 54+ 20C trong 14 ngy, sn phm phi ph hp vi qui nh trong mc 3.2. 3.3. Thuc tr bnh c cha hot cht triadimenol dng bt thm nc Sn phm l hn hp bt mu kem vi thnh phn chnh l triadimenol k thut v cc cht ph gia. 3.3.1. Hot cht Hm lng triadimenol khi xc nh phi ph hp vi qui nh trong mc 2.3. Hon ton 2 ml 4 ml Hon ton 4 ml

3.3.2. Tnh cht vt l T sut l lng : Sau khi to huyn ph ca sn phm trong nc chun D 30 + 10C trong 30 pht, hm lng triadimenol trong dung dch huyn ph: Khng nh hn 60%. 3.3.3. bn bo qun nhit 540C: Sau khi bo qun 54+ 20C trong 14 ngy, sn phm phi ph hp vi qui nh trong mc 3.2. 4. PHNG PHP TH 4.1. Xc nh hm lng hot cht triadimenol 4 4.1.1. Nguyn tc: Hm lng triadimenol c xc nh bng phng php sc k kh vi detector ion ho ngn la (FID). Dng di-butyl phtalate lm cht ni chun. Kt qu c tnh da trn s so snh gia t s s o din tch ca pic mu th vi pic ni chun v t s s o din tch ca pic mu chun vi pic ni chun. 4.1.2.Ho cht, dng c, thit b. Cht chun triadimenol bit hm lng Cht ni chun di-butyl phtalate Dimethyl acetamide Bnh nh mc dung tch 10 ml Cn phn tch My sc k kh, detector ion ho ngn la My tch phn k hoc my vi tnh Ct mao qun SE54 (25 m x 0,53 mm x 0,32 m) hoc tng ng Microxylanh bm mu 5 l, chia vch n 1 l Kh Nit 99,9% Kh hydr 99,9% Khng kh nn dng cho my sc k kh.

4.1.3. Chun b dung dch 4.1.3.1. Dung dch mu chun Cn khong 0,01 g cht chun triadimenol v 0,01 g cht ni chun chnh xc ti 0,00001 g vo bnh nh mc 10 ml. Ho tan v nh mc n vch bng dimethyl acetamide. 4.1.3.2. Dung dch mu th Cn lng mu th cha khong 0,01 g hot cht triadimenol v 0,01 g cht ni chun chnh xc ti 0,00001 g vo bnh nh mc 10 ml. Ho tan v nh mc n vch bng dimethylacetamide.

4.1.3.3. Thng s my Nhit ct: Nhit bung bm mu: Nhit detector: Kh nit : Kh hydr : Khng kh: Kh N2 b tr detetor 2200C 2800C 3000C 10ml/pht 35ml/pht 300ml/pht 30ml/pht

4.1.4. Tin hnh phn tch trn my Bm dung dch mu chun cho n khi t s s o din tch ca pic mu chun v pic ni chun thay i khng ln hn 1%. Sau , bm ln lt dung dch mu chun v dung dch mu th, lp li 2 ln . Sai lch gia cc ln bm khng ln hn 1%. 4.1.5. Tnh ton kt qu

theo

Hm lng hot cht triadimenol ( X ) trong mu c tnh bng phn trm cng thc: Fm mc X= Fc mm Trong : Fm : Trung bnh t s gia s o din tch ca pic mu th v pic ni chun Fc : Trung bnh t s gia s o din tch ca pic mu chun v pic ni P

chun mc : Khi lng mu chun, g mm : Khi lng mu th, g P : tinh khit ca chun, % 4.2. Xc nh bn nh tng: Theo TCVN - 3711 - 82, mc 3.5. 4.3. Xc nh t sut l lng Theo 10 TCN 102-88. Xc nh lng triadimenol trong 25 ml dung dch cn li di y ng ong: Sau khi ht 225 ml pha trn, chuyn nh lng ton b dung dch cn li di y ng ong vo mt a bay hi. Cho bay hi nhit 54 oC trong t sy chn khng ti trng lng khng i. Xc nh hm lng hot cht triadimenol trong cn theo mc 4.1 trong tiu chun ny. Tnh ton kt qu : T sut l lng (Y) tnh bng phn trm theo cng thc :

111 Y = c

( c-q )

Trong : q : khi lng hot cht triadimenol trong 25 ml dung dch cn li di yq= p l 100

ng ong, g. p: l hm lng cn trong 25 ml dung dch trn l: l khi lng cn trong 25 ml dung dch trn c : khi lng hot cht triadimenol trong lng mu dng xc nh t sut l lng, g. 4.4. Xc nh bn bo qun 4.4.1. nhit 00C Theo 10TCN 433-2001, mc 4.5.2.1. 4.4.2. nhit 540C THEO 10TCN 105-88 .

ti liu tham kho 1. TCVN - 3711- 82. 2. 10TCN 102-88. 3. 10TCN - 105 88. 4. 10TCN 386 99.

5. 10TCN - 433 2001.6. Ti liu ng k thuc Triadimenol ca hng Bayer. 7. Ti liu ng k thuc triadimenol ca hng Thuc tr su Si gn.

8. 8.FAO Panel of Expert on Pesticide Specification, Registration Requirementsand Application Standards and Prior Informed Consent, Manual on

Development and Use of FAO Specifications for Plant Protection Products-fifth edition, 1999. 9. 9.The British Crop Protection Council & The Royal Society of Chemistry, UK, The pesticide Manual, tenth edition, 1994. KT. B TRNG B NNG NGHIP V PHT TRIN NNG THN Th trng Bi B Bng : k

GII THIU HOT CHT PROPINEB

Cng thc cu to:

[-SC(S)NHCH2CH(CH3)NHCS2Zn-]x

Tn ho hc: Polymeric zinc propylenebis(dithiocarbamate) Cng thc phn t: (C5H8N2S4Zn)x Khi lng phn t: 289,8 ho tan 20 oC Trong : nc Toluen, hexane, dichloromethane Dng bn ngoi: cht rn dng bt, mu trng. Bn diu kin kh. Phn hy trong mi trng m, axit v kim trung tnh. 0,01 g/l < 0,1 g/l

NHM B&C TIU CHUN NGNH 10TCN 502 -2001

THUC TR BNH CHA HOT CHT PROPINEB Yu cu k thut v phng php th Fungicide containing propineb Technical riquirements and test methods

1. PHM VI P DNG Tiu chun ny p dng cho: - Propineb k thut; -Thuc bo v thc vt c cha hot cht propineb dng bt thm nc dng lm thuc tr bnh hi cy trng. 2. QUI NH CHUNG 2.1. Ly mu Theo 10TCN 386-99. 2.2. Ho cht Ho cht phn tch phi l loi TKPT. Nc cng theo TCVN 3711-82. 2.3. Mc sai lch cho php ca hm lng hot cht

Hm lng hot cht ng k Mc sai lch cho php % T 2,5 tr xung T trn 2,5 ti 10 T trn 10 ti 25 T trn 25 ti 50 T trn 50 tr ln T trn 500 tr ln g/kg hoc g/l 200C T 25 tr xung T trn 25 ti 100 T trn 100 ti 250 T trn 250 ti 500

15% hm lng ng k 10% hm lng ng k 6% hm lng ng k 5% hm lng ng k 2,5% 25g/kg hoc g/l

2.4. Cn phn tch Cn s dng chnh xc 0,0001g; 0,1g.

3. YU CU K THUT 3.1. Propineb k thut Propineb k thut l bt ri, mu kem vi thnh phn chnh l propineb v mt phn tp cht sinh ra trong qu trnh sn xut. 3.1.1. Hot cht Hm lng propineb ng k, khi xc nh phi ph hp vi qui nh trong mc 2.3. 3.1.2. Tp cht Hm lng nc: Khng ln hn 2,5%. 3.2. Thuc tr bnh c cha hot cht propineb dng bt thm nc Sn phm l hn hp ng nht dng bt mn, mu kem vi thnh phn chnh l propineb k thut v cc cht ph gia.

3.2.1. Hot cht Hm lng propineb ng k, khi xc nh phi ph hp vi qui nh trong mc 2.3. 3.2.2. Tp cht Hm lng nc: Khng ln hn 2,5 %. 3.2.3. Tnh cht vt l 3.2.3.1. pH ( dung dch 1% trong nc ) Trong khong 5,0 - 9,0. 3.2.3.2. Th ry t Lng cht cn li trn ry 75 m: Khng ln hn 2%. 3.2.3.3. Thi gian thm t Thi gian thm t hon ton: Khng ln hn 2,0pht. 3.2.3.4. T sut l lng Sau khi ta huyn ph ca sn phm trong nc chun D 30 1oC trong 30 pht, hm lng propineb trong dung dch huyn ph: Khng nh hn 60%. 3.2.3.5. to bt Th tch to bt sau 1 pht: Khng ln hn 2,5ml. 3.2.4. bn bo qun nhit 54 oC Sau khi gi nhit 54 + 2oC trong 14 ngy, sn phm phi c hm lng hot cht bng 95% tr ln so vi hm lng ban u v tnh cht vt l ph hp vi quy nh ti 3..2.3.

4. PHNG PHP TH 4.1. Xc nh hm lng hot cht propineb 4.1.1. Nguyn tc Propineb b phn hy bng axit sulfuric nng gii phng ra carbondisulfit. Carbondisulfit c hp ph vo dung dch KOH trong methanol. Lng kali xanthogenate to thnh c xc nh bng phng php chun it. 4.1.2. Ho cht dng c Ch axetat, dung dch 10% trong nc Kali hydroxit, dung dch 2N trong methanol Axid axetic, dung dch 30% Axid sulfuric c It, dung dch chun 0,1N Phenolphtalein, dung dch 1% trong ethanol Bnh cu 3 c, dung tch 250ml ng dn kh Phu nh git ng sinh hn nc Bnh sc kh, dung tch 50ml Ht thy tinh B to chn khng nc Cc thy tinh dung tch 500ml Buret 50ml Bp in Cn phn tch, cn k thut Lp dng c nh hnh v

4.1.3.

Tin hnh

Cho dung dch ch axetat vo ti na 2 bnh sc kh 1v 2. Cho ht thy tinh vo ti na bnh3, dung dch KOH n ngp ht thy tinh. Ni u ra ca bnh 3 vi b to chn khng . Cn lng mu th c cha khong 0,4g hot cht propineb chnh xc ti 0,0001g vo bnh cu ba c, cho 80ml nc ct vo bnh cu, ni sinh hn, to chn khng. Cho t t 20ml axit sulfuric c qua phu nh git vo bnh ba c. un si bnh trong 1 gi. Tt bp in. Chuyn dung dch kali hydroxit t bnh 3 vo cc 500ml, trng bnh nhiu ln bng nc ct (300ml). Trung ho bng dung dch axit axetic, dng ch th phenolphtalein. Thm 1ml h tnh bt v chun ngay lp tc bng dung dch it chun 0,1N cho n khi xut hin mu xanh tm (V1). Lm nh trn vi mu trng (V2). 4.1.4. Tnh ton Hm lng hot cht propineb (X) c tnh bng phn trm theo cng thc (V1 - V2) 1,449 X =

m Trong 0,01449 : Lng propineb tng ng vi 1 ml dung dch ide 0,1N. V1 V2 m : Th tch dung dch iode 0,1N dng chun mu trng, ml. : Th tch dung dch iode 0,1N dng chun mu th, ml. : Lng cn mu th, g.

4.2. Xc nh hm lng nc Theo 10TCN 231-95, mc 3.7. 4.3. Xc nh pH Theo 10TCN 389-99, mc 4..2. 4.4. Th ry t Theo 10TCN 103-88. 4.5. Xc nh thi gian thm t Theo 10TCN 389-99, mc 4.4. 4.6. T sut l lng Theo 10TCN-231-95. Xc nh lng propineb trong 25 ml dung dch cn li di y ng ong: Sau khi ht 225 ml dung dch pha trn, chuyn ton b dung dch cn li di y ng ong vo bnh cu ba c 250 ml, trng ng ong bng lng nc ti thiu v xc nh khi lng hot cht propineb theo mc 4.1.3 ca tiu chun ny.

Tnh ton : T sut l lng Y tnh bng phn trm theo cng thc : 111 (c -q) Y = c Trong c: Khi lng hot cht propineb trong 250 ml dung dch huyn ph, g. q: Khi lng hot cht propineb trong 25 ml dung dch huyn ph cn li di y ng ong c tnh bng gam theo cng thc : q = 0,01449 x V V: Th tch dung dch I2 0,1 N dng ht chun , ml. 4.7. Xc nh bt 4.7.1. Ho cht, dng c Nc cng chun ng ong c nt nhm 100 ml, khong cch gia vch 100 ml vi y ca nt nhm khng nh hn 35 ml v khng ln hn 40 ml. 4.7.2. Tin hnh Cn 0,2g mu vo ng ong, thm nc cng chun n vch100ml. y nt, o ngc ng ong 30 ln. yn 1 pht v xc nh th tch bt. 4.8. bn bo qun nhit 54oC Theo 10TCN-105-88. Ti liu tham kho 1. 10TCN 103-88, 1988. 2. 10TCN 105-88, 1988. 3. 10TCN 231-95, 1995. 4. 10TCN 386-99,1999. 5. 10 TCN 389-99, 1999. 6. CIPAC Handbook 1. 7. Fao specifications for plan protetion products, 1980.

8. Ti liu ng k thuc propineb ca hng Bayer. KT. B TRNG B NNG NGHIP V PHT TRIN NNG THN Th trng Bi B Bng : k

GII THIU HOT CHT IMIBENCONAZOLE

Cng thc cu to:

Tn ho hc 4-chlorobenzyl N-(2,4-dichlorophenyl)-2-(1H-1,2,4-triazol-1yl)=thioacetamidate Cng thc phn t: C17H13Cl3N4S Khi lng phn t: 411.7 ho tan trong: Nc: Acetone Xylene Methanol : : : 1,7 mg/l (20C) 1063 g/l (25C) 250 g/l (25C) 120 g/l (25C)

Dng bn ngoi: Tinh th mu vng nht. Bn nhit thng.

Nhm B&C TIU CHUN NGNH 10 TCN 503-2002

THUC TR BNH CHA HOT CHT IMIBENCONAZOLE Yu cu k thut v phng php th Fungicide containing imibenconazole Technical requirement and test methods

1. PHM VI P DNG Tiu chun ny p dng cho: -Imibenconazole k thut; -Thuc bo v thc vt (BVTV) c cha hot cht imibenconazole dng bt thm nc, dng lm thuc tr bnh hi cy trng. 2. QUI NH CHUNG 2.1. Ly mu Theo 10TCN 386-99 2.2. Ho cht Ho cht l loi tinh khit phn tch Nc cng chun, theo TCVN 3711 -82 Nc ct, theo TCVN 2217 -72 2.3. Mc sai lch cho php ca hm lng hot cht

Hm lng hot cht ng k % T 2,5 tr xung T trn 2,5 n 10 T trn 10 n 25 T trn 25 n 50 T trn 50 tr ln T trn 500 tr ln g/l hoc g/kg 20o C T 25 tr xung T trn 25 n 100 T trn 100 n 250 T trn 250 n 500

Mc sai lch cho php 15 % hm lng ng k 10 % hm lng ng k 6 % hm lng ng k 5 % hm lng ng k 2,5 % 25 g/kg hoc g/l

2.4. Cn phn tch Cn s dng c chnh xc n 0,00001 g 3. YU CU K THUT 3.1. Imibenconazole k thut Sn phm c dng tinh th mu vng nht, vi thnh phn chnh l imibenconazole v tp cht sinh ra do qu trnh sn xut. Hot cht: Hm lng imibenconazole ng k khi xc nh phi ph hp vi qui nh trong mc 2.3. 3.2. Thuc tr bnh c cha hot cht imibenconazole dng bt thm nc Sn phm l hn hp ng nht dng bt mn, vi thnh phn chnh l imibenconazole k thut v cc cht ph gia. 3.2.1. Hot cht Hm lng imibenconazole ng k khi xc nh phi ph hp vi qui nh trong mc 2.3.

3.2.2. Tp cht Hm lng nc: Khng ln hn 1% 3.2.3. Tnh cht vt l 3.2.3.1. pH (dung dch 10 % trong nc) Trong khong: 8,0 - 9,5 3.2.3..2. Thi gian thm t Thi gian thm t hon ton: Khng ln hn 1,0 pht 3.2.3.3. T sut l lng Sau khi to huyn ph trong nc cng chun ( theo TCVN 3711-82) 30 1 C trong 30 pht, hm lng imibenconazole trong dung dch huyn ph khng nh hn 60 %. 3.2.4. bn bo qun nhit 54 C: Sau khi bo qun 54 2 C trong 14 ngy, sn phm phi ph hp vi qui nh trong mc 3.2. 4. PHNG PHP TH 4 4.1. Xc nh hm lng hot cht imibenconazole 4.1.1. Nguyn tc Hm lng imibenconazole c xc nh bng phng php sc k lng cao p vi detector t ngoi (UV), ct pha o, dng fluoranthene lm cht ni chun. Kt

qu c tnh ton da trn s so snh gia t s s o din tch ca pic mu th vi pic ni chun v t s s o din tch ca pic mu chun vi pic ni chun. 4.1.2. Ho cht, dng c, thit b Cht chun imibenconazole bit hm lng Cht ni chun fluoranthene Acetonitril Nc ct Bnh nh mc dung tch 10 ml My sc k lng cao p, detector UV My tch phn k hoc my vi tnh Ct sc k lng cao p pha o Lichrosorb RP 18 5 m (250 x 4 mm) hoc tng ng Microxylanh bm mu 50 l chia vch n 1 l Cn phn tch 4.1.3. Chun b dung dch 4.1.3.1. Dung dch ni chun Cn khong 0,060 g cht ni chun fluoranthene chnh xc ti 0,00001 g vo bnh nh mc 100 ml, ho tan v nh mc ti vch bng acetonitril. 4.1.3.2. Dung dch mu chun Cn khong 0,010 g cht chun imibenconazole chnh xc ti 0,0001 g vo bnh nh mc 10 ml, ho tan v nh mc ti vch bng acetonitril - dung dch A. Dng pipet ly chnh xc 1 ml dung dch A v 1 ml dung dch ni chun vo bnh nh mc 10 ml. Ho tan v nh mc ti vch bng acetonitril. 4.1.3.3. Dung dch mu th Cn lng mu th c cha khong 0,010 g imibenconazole chnh xc n 0,00001g vo bnh nh mc 10 ml, thm 5 ml acetonitril, lc trong b siu m 10 pht. n nhit phng, ho tan v nh mc ti vch bng acetonitril - dung dch B. Dng pipet ly chnh xc 1 ml dung dch A v 1 ml dung dch ni chun vo

bnh nh mc 10 ml. Ho tan v nh mc ti vch bng acetonitril, lc qua mng lc 0,45 m trc khi bm vo my. 4.1.4. Thng s my Pha ng: Acetonitril + Nc = 75 + 25 (V/V) Tc dng: 1 ml/pht Bc sng: 254 nm Th tch vng bm mu: 20 l 4.1.5. Tin hnh phn tch trn my Bm ln lt dung dch mu chun cho n khi t s s o din tch ca pic mu chun vi pic ni chun thay i khng ln hn 1%. Sau , bm ln lt dung

dch mu chun v dung dch mu th lp li 2 ln (sai lch gia cc ln bm khng ln hn 1%). 4.1.6. Tnh ton kt qu Hm lng hot cht imibenconazole (X) trong mu c tnh bng phnX = Fm mc P Fc mm

trm theo cng thc: Trong : Fm : Trung bnh t s s o din tch ca pic mu ni chun vi pic mu th Fc : Trung bnh t s s o din tch ca pic mu ni chun vi pic mu chun mc : Khi lng mu chun, g mm: Khi lng mu th, g P : tinh khit ca cht chun, %

4.2. Xc nh hm lng nc Theo 10TCN 231-95, mc 3.7. 4.3. Xc nh pH Theo 10TCN 389-99, mc 4..2 4.4. Xc nh thi gian thm t Theo 10TCN 103 - 88 4.5. Xc nh t sut l lng Theo tiu chun ngnh s 10TCN- 102-88 Xc nh lng imibenconazole trong 25 ml dung dch cn li di y ng ong. Sau khi ht 225 ml pha trn v chuyn nh lng ton b dung dch cn li di y ng ong vo mt a bay hi. Cho bay hi nhit 54 0C trong t xy chn khng ti trng lng khng i. Xc nh hm lng hot cht imibenconazole trong cn theo mc 4.1. trong tiu chun ny. Tnh ton kt qu: T xut l lng y tnh bng % theo cng thc:y= 111 ( c q ) c

Trong : q: Khi lng hot cht imibenconazole trong 25ml dung dch cn li di ng ong, g c: Khi lng hot cht imibenconazole trong lng mu dng xc nh t xut l lng, g 4.6. bn bo qun nhit 54C: Theo 10TCN 105 - 88

TI LIU THAM KHO 1. TCVN 2217 -72 2. TCVN 3711-82 3. 10TCN 102-88 4. 10TCN 103-88 5. 10TCN 386-99 6. 10TCN 325-95 7. 10TCN 389-99 8.The British Crop Protection Council & The Royal Society of Chemistry, UK, the pesticide Manual, tenth edition, 1994. 9. FAO Panel of Expert on Pesticide Specification, Registration Requirements and Application Standards and Prior Informed Consent, Manual on Development and Use of FAO Specifications for Plant Protection Products-fifth edition, 1999. 10. Hokko Chemical indty Co. Ltd, Technical information of manage 5% Wettable powder, 1994

KT. B TRNG B NNG NGHIP V PHT TRIN NNG THN Th trng Bi B Bng : k

GII THIU HOT CHT OXOLINIC ACID

Cng thc cu to:

Tn ho hc: 5- ethyl- 5,8- dihydro-8-oxo [1,3] dioxolo [4,5-g] quinoline-7cacboxylic acid Cng thc phn t: C13H11 N O5 Khi lng phn t: 261,2 ho tan ( 200C) trong: Dung dch NaOH 1M Xylen n - hexane 20-33%