TIU CHUN QUC GIA TCVN 9292 : 2012 PHN BN - PHNG PHP XC NH AXIT T DO Fertilizers - Method for determination

for free acid Li ni u TCVN 9292 : 2012 c chuyn i t 10 TCN 303-2005 theo quy nh ti khon 1 iu 69 ca Lut Tiu chun v Quy chun k thut v im b khon 2 iu 7 Ngh nh s 127/2007/N-CP ngy 1/8/2007 ca Chnh ph quy nh chi tit thi hnh mt s iu ca Lut Tiu chun v Quy chun k thut. TCVN 9292 : 2012 do Vin Th nhng Nng ha bin son, B Nng nghip v Pht trin Nng thn ngh, Tng cc Tiu chun o lng Cht lng thm nh, B Khoa hc v Cng ngh cng b. PHN BN - PHNG PHP XC NH AXIT T DO Fertilizers - Method for determination for free acid 1. Phm vi p dng Tiu chun ny quy nh phng php xc nh hm lng axit t do c trong cc loi phn c d axit. 2. Ti liu vin dn Cc ti liu vin dn sau y l rt cn thit p dng tiu chun ny. i vi cc ti liu vin dn ghi nm cng b th p dng phin bn c nu. i vi cc ti liu vin dn khng ghi nm cng b, th p dng phin bn mi nht, bao gm c cc sa i, b sung (nu c). TCVN 4440 - 2004, Supe pht pht n. TCVN 4851 - 89 (ISO 3696 - 1987), Nc dng cho phn tch trong phng th nghim Yu cu k thut v phng php th. TCVN 9297 : 2012, Phn bn - Phng php xc nh m. 3. Thut ng v nh ngha Tiu chun ny s dng cc thut ng v nh ngha sau: 3.1. Axit t do (free acid) Axit cn d (quy v H2SO4) trong phn bn. 4. Nguyn tc Chun lng axit t do c trong phn bn bng dung dch natri hydroxit, s dng ch th mu hn hp metyl , metyl xanh. 5. Ha cht v thuc th

Ha cht s dng pha cc cht chun t loi tinh khit ha hc, ha cht s dng phn tch t loi tinh khit phn tch. 5.1. Nc ct, TCVN 4851-89 (ISO 3696-1987). 5.2. Natri hydroxyt (NaOH). 5.3. Ch th mu metyl , metyl xanh. 5.4. Dung dch tiu chun NaOH 1 M v NaOH 0,5 M: Cn 40 g NaOH chnh xc n 0,0002 g ha tan bng 600 ml nc ct, chuyn vo bnh nh mc dung tch 1000 ml, thm nc ct n vch nh mc. Pha long dung dch NaOH 1 M 20 ln thu c dung dch NaOH 0,05 M. Dung dch NaOH c bo qun kn trong bnh nha PE kim tra li nng dung dch trc khi s dng bng dung dch HCl c nng tng ng. 5.5. Hn hp ch th mu metyl , metyl xanh: Ha tan 0,200 g metyl trong 100 ml etanol (dung dch 1). Ha tan 0,100 g metyl xanh trong 100 ml etanol (dung d ch 2). Trn dung dch 1 v dung dch 2 vi t l 1 : 1 theo th tch (V/V). 6. Thit b, dng c S dng cc thit b, dng c thng thng trong phng th nghim v cc thit b, dng c nh sau: 6.1. Bnh nh mc, dung tch 50, 100, 1000 ml. 6.2. Bnh tam gic chu nhit, dung tch 250, 500 ml. 6.3. Buret, dung tch 50 ml, chnh xc 0,1 ml. 6.4. Cn phn tch, chnh xc 0,0002 g. 6.5. Cc chu nhit, dung tch 250, 1000 ml. 6.6. Pipet, dung tch 2 ml. 6.7. Phu lc, ng knh 8 cm. 7. Ly mu v chun b mu 7.1. Mu em n phng th nghim c o trn u, tri phng trn khay nha hoc tm nilng, ly mu trung bnh theo phng php ng cho gc, trn u, ly hai phn i din v loi b dn cho n khi cn khong 500 g. 7.2. Chia mu trung bnh thnh hai phn bng nhau, cho vo hai ti PE buc kn, ghi m s phn tch, ngy, thng, tn mu (v cc thng tin cn thit), mt ti lm mu lu, mt ti lm mu phn tch. 7.3. Nghin mn mu ri qua ry 2 mm, trn u lm mu phn tch. 7.4. Cc mu c m cao c th cn mt lng mu xc nh, sy kh nhit 70 oC, xc nh m nghin mn mu kh qua ry 2 mm lm mu phn tch. Lu khi tnh kt qu phi nhn vi h s chuyn i t khi lng mu kh sang khi lng mu thc t ban u.

7.5. Cc mu khng th x l theo 7.3, 7.4 c th ly mt lng mu khong 20 g, nghin tht mn lm mu phn tch. 7.6. Trong trng hp phn bn l supe pht pht n c th p dng TCVN 4440-2004. 8. Cch tin hnh 8.1. Cn 5 g n 10 g 0,0001 g mu c x l theo (7) cho vo bnh tam gic dung tch 500 ml. 8.2. Thm 250 ml nc ct, lc u trong 60 min. 8.3. Lc qua giy kh, thu c dung dch lc vo bnh dung tch 250 ml. 8.4. Ly 100 ml dung dch lc cho vo cc dung tch 250 ml. 8.5. Thm 3 git ch th mu (mc 5.5). 8.6. Chun bng dung dch tiu chun NaOH 0,05 M cho n khi dung dch t mu tm chuyn sang mu xanh lc. 8.7. Ghi li s ml dung dch NaOH 0,05 M s dng. 9. Tnh kt qu 9.1. Cng thc tnh 9.1.1. Hm lng axit t do quy v H2SO4, tnh theo phn trm (%), khi lng phn thng phm c tnh theo cng thc: % Axit t do = Trong : a Th tch dung dch tiu chun NaOH s dng, tnh bng mililt (ml). M Nng dung dch tiu chun NaOH s dng, tnh bng mol (M); P Khi lng mu tng ng vi lng dung dch mu ly chun , tnh bng gam (g); 0,04904 l h s biu th s gam H2SO4 tng ng vi 1 ml dung dch NaOH 1 M (g), h s ny s dng vi phn bn l supe pht pht v amoni sunphat. CH THCH 1: Trong trng hp phn bn l amoni nitrat th h s l 0,06302 (tnh theo HNO3). Nu hm lng axit t do quy v P2O5 th s dng h s 0,071. 9.1.2. Hm lng axit t do quy v H2SO4, tnh theo phn trm (%) khi lng phn kh kit c tnh theo cng thc: % Axit t do = Trong K H s kh kit (theo TCVN 9297 : 2012) 9.2. Kt qu php th l gi tr trung bnh ca t nht hai ln th c tin hnh song song. Nu sai lch gia cc ln th ln hn 5 % gi tr tng i th phi tin hnh th nghim li.
0,04904 x a x M x 100 x K P 0,04904 x a x M x 100 P

10. Bo co th nghim Bo co th nghim cn bao gm nhng thng tin sau: a) Vin dn tiu chun ny; b) c im nhn dng mu; c) Kt qu xc nh axit t do; d) Nhng chi tit khng quy nh trong tiu chun ny hoc nhng iu c coi l ty chn v cc yu t c th nh hng n kt qu th nghim.