CHT LNG T PHNG PHP XC NH KALI D TIU Soil quality - Method for determination of bio-available potassium Li ni u TCVN 8662:2011 c chuyn i t 10 TCN 372 - 99 thnh Tiu chun Quc gia theo quy nh ti khon 1 iu 69 ca Lut Tiu chun v Quy chun k thut v im a khong 1 iu 6 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 8662:2011 do Vin Quy hoch v Thit k Nng nghip 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.
CHT LNG T - PHNG PHP XC NH KALI D TIU
Soil quality - Method for determination of bio-available potassium 1. Phm vi p dng Tiu chun ny quy nh phng php xc nh hm lng kali d tiu ca t da theo phng php quang ph pht x. 2. Ti liu vin dn Cc ti liu dn sau y l cn thit p dng tiu chun ny. i vi cc ti liu vin dn ghi nm cng b th p dng 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 7538-1 (ISO 10381-1) Cht lng t - Ly mu - Phn 1: Hng dn thit k chng trnh ly mu. TCVN 6647 (ISO 11464), Cht lng t - X l s b t phn tch ha l. 3. Nguyn l Dng dung dch amoni axetat 1,0 mol/l (pH = 7,0) ha tan cc dng kali d tiu trong t. Xc nh hm lng kali trong dch chit mu t bng phng php quang ph pht x. 4. Ha cht v thuc th 4.1 Ha cht Khi phn tch, ngoi tr trng hp c nhng ch dn ring, ch dng cc thuc th tinh khit phn tch v nc ct hoc nc tinh khit tng ng. 4.1.1 Amoni axetat (CH3COONH4); 4.1.2 Axit axetic (CH3COOH). 4.1.3 Axit nitric (HNO3) 70%; 4.1.4 Amoni hydroxyt (NH4OH) 25%; 4.2 Cc dung dch thuc th 4.2.1 Dung dch amoni axetat 1 mol/l (pH = 7,0) Ha tan 77,08 g amoni axetat vo 400 ml nc trong bnh nh mc dung tch 1000 ml, sau thm nc n vch mc v lc u. Kim tra pH ca dung dch bng my o pH trc khi s dng v iu chnh pH = 7,0 (s dng dung dch amoni hydroxit 3 mol/l hoc axit axetic 10%). 4.2.2 Dung dch gc kali 1000 mg/l c sn trn th trng. 4.2.3 Dung dch tiu chun kali 100 mg/l pha t dung dch gc kali. Dng pipet ly 10,0 ml dung dch gc kali (4.2.2) vo bnh nh mc dung tch 100 ml, thm 1 ml axit nitric, thm nc n vch mc 100 ml v lc u. 4.2.5 Dung dch amoni hydroxyt (NH4OH) 3 mol/l Pha long 21,3 ml amoni hydroxyt (4.1.4) bng nc ct vo bnh nh mc dung tch 100 ml. Thm nc n vch mc 100 ml. 4.2.6 Dung dch axit axetic (CH3COOH) 10% Pha long 10 ml axit axetic (4.1.2) bng nc ct vo bnh nh mc dung tch 100 ml. Thm nc n vch mc 100 ml. 4.2.7 Dung dch axit nitric (HNO3) 0,5 mol/l Pha long 10 ml axit axetic (4.1.2) bng nc ct vo bnh nh mc dung tch 100 ml. Thm nc n vch mc 100 ml. 4.2.8 Dy tiu chun kali Chun b 6 bnh nh mc dung tch 100 ml c nh s th t t 0 n 6. Dng pipet ln lt ht dung dch chun kali (4.2.3) vo cc bnh theo th tch ghi trong bng di y. Thm 1 ml axit nitric (4.2.7) vo tng bnh v cho thm dung dch amoni axetat (4.2.1) n vch mc 100 ml ri lc u. S th t 0 1 2 3 4 5 Th tch dung dch chun kali (4.2.3) 0 5 10 15 20 30 (ml) Nng kali trong bnh chun (mg 0 5 10 15 20 30 K/l) 5. Thit b v dng c S dng cc dng c thng thng trong phng th nghim v cc thit b dng c sau: 5.1 Cn phn tch c sai s khng qu 0,0001 g; 5.2 Cn k thut c sai s khng qu 0,01 g; 5.3 My lc; 5.4 My quang k ngn la hoc my quang ph hp th nguyn t; 5.5 Bnh tam gic dung tch 100 ml, 250 ml; 5.6 Bnh nh mc dung tch 50 ml, 100ml, 1000 ml; 5.7 Phu lc c ng knh t 5 cm n 10 cm; 5.8 Pipet dung tch 1 ml, 2 ml, 5 ml, 10 ml; 5.9 Cc chu nhit dung tch 1000 ml. 5.10 Giy lc chm. 6. Ly mu v chun b mu Ly mu t i din theo TCVN 7538 - 1 (ISO 10381 - 1). X l s b mu t theo TCVN 6647 (ISO 11464). 7. Cch tin hnh 7.1 Chit mu Dng cn k thut (5.2) cn 10,0 g mu t, cho vo bnh tam gic c dung tch 250 ml. Cho vo 50 ml dung dch amoni axetat 1 mol/l (4.2.1). Lc bnh trong 5 min, lc qua giy lc (5.10) v thu ly dch lc. Ra t trn phu 5 ln, mi ln dng 10 ml dung dch amoni axetat (4.2.1). Dung dch ra c gom cng dch lc, gi chung l dch lc. Chuyn ton b dch lc qua bnh nh mc dung tch 100 ml v thm dung dch amoni axetat (4.2.1) n vch 100 ml. Lc u dung dch. Chun b mu trng v mu lp. 7.2 Lp ng chun o cng pht x ca dy tiu chun kali trn my quang k ngn la dng knh lc mu kali, hoc o trn h pht x ca my quang ph hp th nguyn t ti bc sng 766,5 nm. Lp ng chun: trc honh ghi nng ca cc dung dch chun, trc tung ghi cng pht x tng ng o c. Xc nh ta tng mu chun v v ng chun. 7.3 o hm lng kali o cng pht x ca dung dch mu trn my quang k ngn la dng knh lc mu kali, hoc o trn h pht x ca my quang ph hp th nguyn t ti bc sng 766,5 nm. Tin hnh tng t i vi mu lp v mu trng. Cn c cng pht x o c ca tng dch chit mu t v da vo ng chun suy ra nng kali trong dch chit mu t. CH THCH: Khi dng quang k ngn la, n nh thp ca my l yu t nh hng v my khng c h thng t ng chng trnh ha kim sot tc dng khng kh v kh nhin liu, knh lc mu c di nh sng cho i qua rng ( 10 nm), cn lin tc kim tra n nh ca tr s cng pht x o c. t nht c sau 10 mu li cn kim tra cng pht x o c ca thang chun. Khi dng h pht x ca my quang ph hp th nguyn t: nhy qu cao ca my l yu t nh hng, cn chn khe o hp (0,2 nm), pha long mu v xoay u t mc thch hp. 8. Tnh kt qu Hm lng kali d tiu trong mu t (mg K/mg) c tnh theo Cng thc (1): K(mg/kg) = (1) Trong a l nng kali trong dch chit mu t, tnh bng miligam trn lt (mg/l); b l nng kali trong dung dch mu trng, tnh bng miligam trn lt (mg/l); V l ton b th tch dung dch chit mu, tnh bng mililit (ml); f l h s pha long ca dung dch mu; m l khi lng mu, tnh bng gam (g); k l h s chuyn thnh t kh tuyt i. 9. Bo co th nghim Bo co th nghim cn bao gm nhng thng tin sau: - Vin dn tiu chun ny. - c im nhn dng mu - Kt qu php xc nh hm lng kali d tiu - Mi thao tc khng quy nh trong tiu chun ny, hoc c coi l ty chn v cc yu t c th nh hng n kt qu th nghim.