TIEU CHUAN NGANH 10 TCN 365-99 PHAN TICH PHAN BON Phuong phap xac dinh axit humic. va axit fulvic (Yén cau kf thuat) Pham vi ap dung: Tigu chuan nay quy dinh phuong phép xéc dink axit humic va axit fulvic 4p dung cho than bin va céc loai phan hén hop hitu co-khodng. Nguyen tae: Hoa tan axit humic va axit fulvic bing dung dich kiém, xée dinh téng s6 axit humic va | axil fulvic hoa tan trong kiéra bing phuong phip xéc dinh cacbon hitu co Walkley- 3.1. 3.L.1. 3.1.2. 3.1.3. 3.1.4. 32. 3.2.2. 3.2.3, Black. Dua vio tinh chat khong tan trong, axit clia axit humic ¢6 thé tach riéng axit humic va xéc dinh ham lugng bing phuong phép Walkley-Black. Thiet bi va thudc tha. ‘Thiet bi: Can phan tich c6 46 chinh xc 0,0002g. Buret 6 46 chinh xc 0,1 mb. Pipet Sml, 10ml. C8 250ml. . Phéu loc dudng kinh Som. . Bép cach thuy. Thude thir: Dung dich chudn kali bicromat M/6: Can chinh xéc 49,04g K,Cr,O, (TK) di say kho a 105°C, hoa tan vao nuéc thanh J lit trong binh dinh miic. Axit sunfuric dac TK (d= 1,84) Dung dich mudi Mhor 0,5M: Can 196g mudi Mo FeSO,.(NH,). 6H,0 vio 50m! HS, dac va thém nude dén 1 lit, Dé ling trong. Loc néu duc. Ban hanh kom theo quyét dink x0: 4HQD-BNN-KHCN ngay 24 thing 2 nim 1999 esia Bo Nong nghiép va Phat trién néng thon. 100THRU CMUAN PHAN BON 10 TCN 365-99 3.2.4, 3.2.5. 3.2.6. 3.2.7, 3.2.8. 3.2.9, 4 4d. 4L2 4.1.3. 4.4. 4.15. 4.1.6; 4.2. 421 4.2.2. 4.2.3, 4.24. 4.2.5, 4.26. 4.2.7, Hon hop natri hydroxit-pyrophotphat pH=13: Hoa tan 44,6g Na,P,O; . 10H,O va 4g NaOH thinh 1 lit dung dich bing nude cat (dung dich 6 néng d6 0,1 M cho méi Lozi) Dung dich H,SO, IN Dung dich H,SO, 0,05N. Dung dich NaOH 0,05N Cc chi thi mau - Chi thi mau Ferroin; Hod tan 0,695g FeSO,.7H,O va 1,485g 0 phenaltrolin monohydrat (C,;H,N, -H,O) trong 100ml nude cat. ~ Chi thj mau Barri dipheny] amin sunfonat néng d6 0,16% trong nude - Chi thi mau axit N.diphenyl anthranilic 0,1% cling 0,1% Na,CO, trong nuéc Nude c6 d6 din dign < 2p.S/em. * Cach tién hanh: Chiét mau, Can chinh xc 3-5g méu phan di dugc chudn bi theo 10 TCN-301-97 va nghién nho qua ray 0,20mm, cho vio binh tam gidc 250ml. Rita va gan nhiéu Kin bang nude néng cho hoa tan céc hop chat ho’ tan trong nude (cdc loai phan khodng, cde chat khit vo co nhu Fe*?, Mn*?, $2...) Co miu cho déin gain kho (khong dé chay). Rot vao 100m! hén hop natri hydroxit-pyrophotphat pH=13. Lac déu va dé qua dem Loe qua gidy loc min, néu duc ciin loc lai Xéc dinh téng s6 axit humic va axit fulvic. Dang pipet lay Sl hoac 10ml dung dich loc (Smt véi than bin va LOml véi hén hop hitu co-khoang) cho vio cde chiu nhigt 250ml. Trung hda bing dung dich H;SO, IN cho dén khi xudi hign ket tha. Co can dén gén kho ten bép cach thuy. Dimng pipet cho vao e6e 10ml dung dich chun K,Cr,0, M/6, tic tron déu can vao dung dich. Thém nhanh 20m! H,SO, dam dac. Lic tron déu hén hop. é yen 30 phut. Them 100ml nude va 10m! H,PO, va dé that ngudi. 10110 TEN 365.99 TIEU CHUAN PHAN BON 4.2.8. Cho 0,3ml mot trong chi thj mau va chudn 49 bing mudi Mhor dén khi mau chuyén. * Chi thi mau Bari diphenyl sunfonal chuyén tir mau tim sang miu xanh kd cay * Chi thi mau axit N.penyl anthranilic chuyén tit mau tim sang mau xanh ld cay * Chi thi mau Ferroin chuyén tir mau ti sang mau dd. 4.2.9, Tién hanh déng thei mau tring (10ml K,Cr,O, M/6) 43. Xe dinh axit humic. 4.3.1. Ding pipet lay 5-10ml dung dich chiét ritt cho vio ede. 4.3.2. Cho timg giot H)SO, IN va khudy déu. Su két tia sé hodn toin khi dung dich 06 pH=1,0 (kiém tra bang pH met). 4.3.3. Dun céc tren bép céch thuy 1-2 gid dé thic day keo tw axit humic. 4.3.4, Dé ngudi va loc. Vat bd dung dich loc. 4.3.5. Két tia tren gidy loc duoc hoa tan bang dung dich NaOH 0,05N néng va chuyén dung | dich loc vao ede 250ml. Trung hoa dung dich bing H,SO,0,05N . Co can dén gin kho trén bép each thuy . Tin hanh xéc djnh axit humic theo Walkley-Black (tit 4.2.4 déin 4.2.8) 5. Céch tinh két qua: Tinh % khdi luong quy vé C cba téng sé axit humic va axit fulvic (hoae cia riéng phan axit humic) yc = @zb4 am a: Thé tich dung dich mudi Mhor chudn do mau trang (ml) +b: Thé tich dung dich mudi Fhor chun do mau wich (ml) m: Khéi {uong mau tong tg véi-mau trich (g) Chi thich: Solasit fulvic) = %C téng s6 (axit humic va axit fulvic) - % C (axit humic). 102