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2. XC NH CC THNH PHN TRONG QUNG APATT 2.2.1 Xc nh hm lng P2O5 trong qung apatit (Phng php th tch Molipdat) 2.2.1.1. Nguyn tc: Ph mu Apatit bng dd HNO3 chuyn hon ton cc mui photphat trong mu vo dd di dng H3PO4 Ca5 ( PO4 )3 F + 10 HNO3 = 5Ca ( NO3 ) 2 + 3H 3 PO4 + HF - Sau kt ta hon ton gc Photphat di dng kt ta vng Amoni Photphat molipdat trong mi trng axid dd nng H 3 PO4 + ( NH 4 ) 2 MoO4 + 21HNO3 = ( NH 4 )3 H 4 P ( Mo2O7 ) 6 (mauvang ) + 21NH 4 NO3 +10 H 2O Lc ra kt ta cho sch axid, ho tan kt ta bng 1 lng NaOH tiu chun 0,14N cho d chnh xc ( NH 4 )3 H 4 P ( Mo2O7 ) 6 + NaOH = 23 Na2 MoO4 + ( NH 4 ) 2 MoO4 + 2( NH 4 ) 2 HPO4 +26 H 2O Chun lng kim d bng dd H2SO4 tiu chun 0,14N theo ch th PP, im tng ng dd mt mu hng H2SO4 + NaOH = Na2SO4 +2H2O 2.2.1.2. Ho cht, dng c: 2.2.1.2.1 Ho cht: - Dung dch NaOH 0,14N - Dung dch H2SO4 0,14N - HNO3 2/3, NH4NO3 30% - Dung dch (NH4)2MoO4 7,5 % - Ch th PP 0,1% cn - Dung dch NH4OH 1:1 - Dung dch Citrat Amon (17% 2.2.1.2.2 Dng c - Cc thu tinh chu nhit 250ml - Bnh col 250ml - Bnh nh mc 250ml - ng ht c bu 10ml - Mt knh ng h 8cm Ngy 21/03/2011
Cng ty CP ho cht Phc Lm - ng ong chia vch 50ml - Cn phn tch, bp in - Buret chun 25ml, 50ml - Phu lc 8 cm - Bng + giy lc v nt 2.2.1.3. Tin hnh:
Cn chnh xc 1g ( 0,0001)g mu qung apatt nghin mn v sy kh 105oC chuyn vo bnh col chu nhit 250ml. Tm t mu bng nc ct + 30ml HNO3 2/3, y cc bng mt knh ng h, un si nh mu 30 pht. Ly ra ngui trng mt knh ng h. Chuyn ton b vo bnh nn 250ml, nh mc ti vch - xc trn u. em lc kh qua giy lc thng b 2 ln nc lc u trng ra dng c. Dng ng ht c bu ht chnh xc 10ml dd lc chuyn vo bnh col 250. Dng NH4OH 1:1 trung ho n kt ta trng + 2ml dd Amon Citrat 17% + 15ml NH4NO3 30% (NH4)2MoO4 7,5% ( 30ml), lc k 30 pht lng 1: 2 gi. em lc kt ta qua bng lc v giy lc nt, ra kt ta n ht phn ng axid (th 20ml nc ra bng 1 git NaOH 0,14N + 3 git ch th PP 0,1% m mu hng khng mt i trong 20ml nc ra l sch). Chuyn giy lc v kt ta vo bnh col va lm kt ta trn, dng NaOH tiu chun 0,14N ho tan kt ta vi lng d chnh xc sau thm vi git ch th PP 0,1% v chun lng d NaOH bng H2SO4 tiu chun 0,14N. im tng ng dd mt mu hng. Ghi th tch NaOH v tiu tn trong qu trnh chun + Tnh kt qu: % P2O5 = mDgP2O5 ( NV ) NaOH ( NV ) H 2 SO4 Vdm 100 G Vxd mDg P2O5 = 142 46 1000
Ngy 21/03/2011