NGHIEN CffU Sir TAO PHffC DA PHOI TUf CUA La(lll) VQfl 1-(2-<br />
PYRIDYLAZ0)-2-NAPHTH0L(PAN) VA NaSCN B A N G PHIATNG<br />
PHAP TRIET - T R A C QUANG, UfNG DUNG KET QUA NGHIEN CUfU<br />
XAC DINH HAM LirOlNG LANTAN TRONG MAU DirOlC PHAM<br />
• • •<br />
<br />
NGUYIN KHAC NGH^A^ THAI HUE TAM^<br />
^Khoa Hda - Dai hpc Vinh<br />
'Cao hpc 15 - Hda phin tich - Dai hpc Vinh<br />
<br />
<br />
SUMMARY<br />
In this study, the multiligand complexation in the system of 1- (2-pyridylazo)- 2-Naphthol(PAN)-<br />
La(III)-SCN- was studied by using refringent-photometry method. The optimal conditions, composition,<br />
mechanism, quantitative parameters of these coplex have been determined( for instance: pHpa,=5,00;<br />
optimal extraction solvent: izoamylie; composition!: 1:2; e = 4,0346. Iff*). This result can be used into<br />
determination the lanthanum content in pharmaceutical product.<br />
<br />
1. Md DAU<br />
<br />
Vigc sQ dgng cae nguygn td hidm dd che tao cac chi Vigc nghien cQu phQc daligan eua La(lll) vdi thudc<br />
tiet may trong cac dieu kign lam vigc khac nghigt dang thQ hOu ed 1-(2-pyridylazo)-2-Naphthol(PAN) va thioxi-<br />
dupc xem la giai phap tdi uu nhat cho nganh ky thuat ^nua tronp dung mfli hQu ed izoamylie blng phUdng<br />
hien dai. Ngoai nhOng Qng dgng quan trpng nhQ cac S ' ^ ? ' ' * ' - - ''^'"^- " ^ l " - ^ '^-'' ' °J !!??^-^ "S-<br />
n„ R„\A-h- ,u-, , • - u-> - / ^ ,u- khoa hpc ma con CO y nghia ve mat thgc tien boi<br />
nguyen to hiem thi lantan con co nhQng Qng dgng khac phuong phap cd dp nhgiy, dp chfnh xac cao, dgng eg,<br />
nhu: Cong nghiep vat ligu, cong nghigp hoa chat, vi thiet bj may mde ddn giln re tidn, mjt khac lai thoi<br />
lupng phan bon, mpt sd phQc chit eua lantan ed kha man di/pc yeu clu cho vigc phan tfch vi nguygn td lan-<br />
n5ng khang khuan,.. tan trong mflt sd ddi tupng khac nhau.<br />
<br />
II. THI/C NGHIEM<br />
<br />
Dung cu va hoa chat: mufl'i La(N03)3.6H20 99.9%, blng axft HNO3 0.01 IVI).<br />
a) Dung cp: Cac hoa chit dupe can trgn can phan ?""9 djch 1-(2-pyridylazo)-2-Naphthol(PAN)10-;M<br />
tich cd dfl chfnh xac +0 01 mo cuvet thach anh rn hp' '^^^^^ ^^^ ^^"9 ^'^^^°'})- °""9 ^^-^^ ^^^^^ ^° 1^<br />
<br />
2 so le sau dau phay. May do quang WPA Light Wave (dung dieu chlnh pH)<br />
S 200 Diode Array Spectrophotometer do mat dO quang , v',,-,-. /-i-^<br />
vdi tin higu 3 sd le sau dIu phay . '^^ ^^ '^ '^^^ ^"^- ^'"^^ *°2n va xu ly sfl ligu bang<br />
,, ,, . ,.-, r, J. u , r . „ , . . z\\\id^q trinh Descriptive statistic. Regression trong<br />
b) Hoa chat: Dung djch La'*10-'M (dupe pha tQ phan mdm Ms-Excel, phln mdm dd hpa Matlab 7.5.<br />
<br />
<br />
i n . KET QuA VA T H A O L U A N<br />
<br />
1. Nghien ctfu hi$u iJng tao phtfc PAN-La(in)-SCN"<br />
r^AM^? Inll^nif^'^'^M^^ P^° '^^P thg electron eua thudc thQ PAN, phQc ddnligan La(lll)-PAN va phQc dalioan<br />
PAN-La(lll)-SCN- d pH = 5,00 dQpc thd hign d hlnh 1 va bing 1. v > ^ vd pnuc oaiigan<br />
<br />
<br />
<br />
Hoa hpc & LTng dung<br />
CD) Si 22 (io6)/2oog<br />
Bing 1: Cic thOng sfl' v^ p\\6 ciJa thuO'c thUr PAN, phijrc danllgan, phufc daligan<br />
(H = 0,1; I = 1,001cm; pH = 5,00)<br />
<br />
Dung dich nghien cifu pH >-wax(nm) AA[to< A'-Max(nm)<br />
<br />
PAN 5,00 470 0,560<br />
<br />
PAN-La(lll) 5,00 560 0,619 90<br />
PAN-La(lll)-SCN 5,00 570 1,014 100<br />
<br />
<br />
<br />
1.1 •<br />
3^<br />
1.0 •<br />
0.9'<br />
0.8<br />
0.7'<br />
0.5 1 Li \<br />
0.5<br />
0.4<br />
0.3 \ . . . _ ^ \ / J \ \<br />
0.2<br />
0.1 •• __^.^^^^,.,-^ ~~-~~ ^"^<br />
<br />
400 450<br />
W.tvi- loiitflh (11<br />
<br />
1 -PAN 2 - PAN - La^* 3 - PAN - La^* - SCN"<br />
<br />
Hinh 1: Pho hap thu cua thuoc thuf PAN, phtfc dofnligan La(III)-PAN,<br />
phtfc daligan PAN-La(III)-SCN•(^ = 0,1; I = 1,001cm; pH = 5,00)<br />
<br />
Ket qua cho thly: PAN cd >.„« = 470nm; phQc La(lll)-PAN cd ).„„ = 560nm; phQc PAN-La(lll)-SCN cd ^Max =<br />
570nm. Dieu nay loai trQ dUpc anh hudng ciJa thudc thQ PAN va phQc La(lll)-PAN den phd ciJa phQc daligan. Vl<br />
vay chung tdi chpn X = 570nm de do quang trong qua trlnh nghien cQu tiep theo.<br />
<br />
2. Dieu ki^n tao phtfc tdi lAi<br />
a) Anh hudng ciJa pH den s y hinh thanh phClc PAN- La(lll)-SCN'<br />
Ke't qui khao sat khoang pH tfl'i QU cua phQc daligan trong dung mdi izoamylie dupc the hign d hlnh 2.<br />
<br />
1,2n^<br />
<br />
H<br />
0.8<br />
<br />
0,6<br />
<br />
0,4<br />
<br />
0.2<br />
pH<br />
<br />
<br />
Hinh 2: Do thj bieu dien stf phu thupc mat dp quang cua phtfc PAN-La(III)-SCN'<br />
vao pH (^ = 0,1; I = 1,001cm; X = 570nm)<br />
<br />
<br />
Hoa hpc & Ung d u n g<br />
Si 22 (io6)l2oog<br />
m<br />
TQ dd thj cho ta thay: Mat dp quang cua phQc dali- b) Ban chat dung moi hOu cd<br />
gan tQdng dd'i cao va dn djnh trong khoing pH: 4-^6. De khIo sat dung mfli chidt tfl'i uu, chung tfli tidn<br />
Vay trong qua trlnh tidn hanh nghien cQu tiep theo hanh chidt phQc daligan trong cae dung mdi hQu cd<br />
chung tfli tidn hanh d pH = 5,00. khac nhau, kdt qui thu dupc thd hign 6 hlnh 3.<br />
<br />
<br />
<br />
<br />
cr<br />
<br />
<br />
<br />
<br />
600 650<br />
Wave length (nm)<br />
<br />
(1) Phd hip thg phan tQ cua phQc daligan trong clorofom<br />
(2) Phd hip thg phan tQ cua phQc daligan trong axeton<br />
(3) Phd hap thy phan tQ cua phQc daligan trong n-butylic<br />
(4) Phd hap thu phSn tQ cua phQc daligan trong izoamylie _<br />
<br />
Hinh 3: Do thi bieu dien stf phu thupc mSt dp quang cua phtfc daligan<br />
vao dung moi chie't (n = 0,1; 1 = 1,001cm; pH = 5,00)<br />
<br />
<br />
TQ dd thj cho ta thay: PhQc PAN-La(lll)-SCN" dupe 2. Xac djnh thanh phln, ctf che'va cac tham<br />
chie't tot trong dung mfli izoamylie. so^ djnh ItfcTng cua phtfc daligan PAN- La(III)-<br />
SCN-<br />
c) Thdi gian lac chie't, the tich dung moi chiet<br />
va thdi gian do mat do quang to'i Uu a) Xac djnh thanh phan phUc daligan PAN-<br />
Khi nghien cQu cac yeu td trgn dg'n sg tao phQc La(lll)-SCN-<br />
Chung tdi da xac djnh dupc thdi gian lie chidt tfl'i uu la SQ dgng cac phQdng phap chuyen djch can blng,<br />
6 phiit, thdi gian do mat dp quang tfl'i uu la 20 phut, the phUdng phap ty sd mol, phUdng phap hg ddng phan tQ<br />
tfch dung moi chig't tdi Uu la 5ml (cho 10ml mlu phan<br />
mol, phUdng phap Staric-Baebanel. Chung tfli da xac<br />
tfch), sd lan chie't 1 lan vdi higu suit R = 98,14%.<br />
djnh dupc cung mflt gia trj vd ty Ig PAN: La(lll): SCN'<br />
d) Anh hudng cCia nong do SCff la 1:1:2 phQc tao thanh la daligan va ddn nhan.<br />
<br />
Khi ty Ig ndng dp tang tQ 800 trd Ign thl mgt b) Cd che t^o phUc daligan PAN- La(lll)-SChf<br />
De xac djnh dQpc dang ion La(lll) va thuO'c thQ di<br />
dp quang cija phQc tang dat cgc dai va dn djnh. VI vay vao pjiQc Chung tfli sQ dgng doan tuyg'n tfnh trong dd<br />
thj bieu dign sg phg thupc mgt dfl quang vao pH (hlnh 2)<br />
Chung tfli chpn 1.000 cho qua trlnh nghien cQu. va xac djnh cae gia trj CK; (CR - C^); (CSCN- - CK); -IgB<br />
^La(lll) ket qui xac djnh dupc:<br />
<br />
<br />
<br />
<br />
m Hoa hpc & Lfng dung<br />
Si 22 (io6)/20og<br />
Qng vdi i = 0 cd tga = q.n + p.n' = 3,078 ~ 3 vdi e ,M, = (4,0346 ± 0,0029).10' (vdi p = 0,95; k = 4), ke't<br />
q = 1, p = 2 ^ n = 1, n' = 1. qua nay hoan toan phu hpp vdi ke't qua tfnh theo<br />
Qua day chung tfli rut ra kdt luan phQdng phap dudng chuan.<br />
* Dang ion kim loai di vao phQc la La^*; Hg sd can blng Kp va hIng sd ben p cua phQc cung<br />
* Dang ligan thQ nhat di vao phQc la R"; dupc xac djnh theo phuong phap Komar, ke't qua thu<br />
* Dang ligan thQ hai di vao phQc la (SCN)'; dupc la: IgK = 5,7758 ± 0,0971; Igp =17,9756 ± 0,1060<br />
(vdi p = 0,95; k = 4).<br />
* Cong thQc gia djnh cua phQc la: (R)La(SCN)2.<br />
c) Xac dinh cac tham sd dinh lUdng cua phUc<br />
3. Phtftfng trinh dtfc^ng chuan phu thuoc m§t<br />
daligan PAN- La(lll)-SCN- dp quang vao nong dp phtfc<br />
Hg sd hap thg phan tQ mol cua phQc dQpc xac djnh Kg't qua nghien cQu thu dUpc phUdng trlnh dUdng<br />
theo phUdng phap Komar. Ket qua xac djnh dQpc ia: chuan cd dang:<br />
i6 r3+<br />
AAj = (0,1095 ± 0,0049).10°.C;': + (0,1649 ± 0,0215)<br />
La<br />
1,2 M<br />
<br />
1<br />
<br />
0,8<br />
y = 0,1019x +0,1649<br />
0,6 F? = 0,9873<br />
<br />
0.4<br />
<br />
0,2<br />
CjMO'M<br />
0<br />
0 9 10<br />
<br />
Hinh 4: Stf phy thupc mSt dp quang vao nong dp cua phtfc daligan<br />
PAN-La(III)-SCN-(n = 0,1; I = 1,001cm; X = 570nm; pH = 5,00)<br />
<br />
TQ dd thi tren chung tfli rut ra ket luan: Khoang ndng ham lupng lantan trong mlu nhan tao bang phUdng<br />
dfl cija phQc PAN-La(lll)-SCN" tuan theo djnh luat Beer<br />
la: (0,2 + 7,0).10'^M. Khi ndng dfl cija phQc Idn hdn thl phap chig't trie quang cho thly: tjN < t,o,95;4) nen X ^<br />
xay ra hign tupng Igch khdi djnh luat Beer. Hg sd hap a, la do nguyen nhan nglu nhien (p = 0,95; k = 4) vdi<br />
thg phan tQ mol tfnh theo phgdng trinh dudng chuan la: sai sd tUdng do'i q% = 0,4712% < 5%. VI vay cd the<br />
Ephjc = (4,0346 ± 0,0029).10^ Kdt qua nay hoan toan ap dgng ket qua nghien cQu de xac djnh ham iQpng lan-<br />
phii hpp vdi phUdng phap Komar. tan trong mlu that.<br />
De Qng dgng ket qua nghign cQu trgn vao xac djnh<br />
ham lupng lantan trong mau that va dga vao thanh - Tig'n hanh xac djnh ham IQpng lantan trong mau<br />
phln mlu that chung tfli da xay dgng phddng trlnh that (vign nen Fosrenol®). Ke't qua nghign cQu dQpc<br />
dudng chuln khi ed mat ion cln nhu: Mg^*, Ca^*, Fe^* ham iQpng cua lantan cacbonat trong mfli vign nen<br />
ke't qua thu dupc phUdng trlnh: Fosenol la:<br />
AA| = (0,1096 ± 0,0059).10^C^^ + (0,1650 ± 0,0012) 484,398 < mLa2,co3)3 ^ 548,887<br />
Trong khi tren nhan cua san phlm ma nha san xult<br />
4. Xac dinh ham ItfoTng lantan trong vien nen da ghi la moi vign nen Fosenol® cd chQa 500mg<br />
Fosrenol® (dtf^fc ph§m cua Cannada)<br />
La2(C03)3. NhQ vay ket qua nghign cQu dQpc la phu hpp.<br />
- xac djnh ham lupng lantan trong mlu nhan tao<br />
blng phuong phap chiet - trie quang. Ket qua xac djnh (Xem tiep trang 35)<br />
<br />
<br />
<br />
<br />
(m<br />
Hoa hpc & Lfng d u n g<br />
.5^22 (io6)/20og<br />
Hlnh 3 cho thly, sQ phg thuflc cua IgD vao IgCrppo Thanh phln phQc cua Y^* dupc chidt trong hg TPPO-<br />
la tuydn tfnh va hg sd gdc cua dudng thing IgD = toluen tQ mfli axit nitric dupc xac djnh la Y(N03)3.3TPP0<br />
t(lgCTPpo). tga = X = 1,8. Do dd phQc cua Gd^* dupe<br />
chidt vao pha hOu cd la GdCl3.2TPP0. Vay qua trinh [2], tQ mfli trudng axit tricloaxetic la Y(CCl3C0O)3.2TPP0<br />
chidt Gd'* blng TPPO trong mfli trudng HCI xly ra theo [3]. Nhu vgy, thanh phln phQc cua NTDH dupc chidt<br />
phUdng trinh phln Qng:<br />
trcng hg TPPO-toluen tQ mfli trudng axit clohydric tuong<br />
Gd3;, + 3CI(n) + 2TPP0(hc) « LnCl3.2TPP0(hc) tg nhu tu mfli trodng axit tricloaxetic.<br />
<br />
rV. KET LUAN<br />
- Da khio sat higu Qng tao phQc cua Gd'* vdi tac - Da xac djnh dupe thanh phln cua phQc khi chidt<br />
nhan chidt TPPO-toluen trong mOi trudng axit clohydric Gd'* blng TPPO-toluen tQ mfli trQdng axit clohydric la<br />
blng phd tQ ngoai va hdng ngoai, kdt qui cho thly cd<br />
higu Qng tao phQc giQa chung. 6dCl3.2TPP0.<br />
<br />
TAI LI?U THAM KHAO<br />
1. LUU Minh Dgi, Dao Ngpc Nhigm (2006), Chiit trudng axit tricloaxetic, Tap chf Hda hpc va Lfng- dgng.<br />
neodym vi ytri bing triphenylphosphin oxit (TPPO) td 5. Nguyin Dinh Luygn, TrIn Hoang Khanh, Nguyin<br />
mdi trudng axit nitric, Tgp chf Hda hpc, T.44 (5), Thj Hdno Md, Nguyin Thj Trang (2009). ChiSt La, Nd<br />
tr.571-573. Gd, Er bang triphenylphotphin exit til mdi trUdng cirua<br />
2. Luu lyiinh Dai, Dao Ngpc Nhigm (2007), Xic djnh vi thioxianat. Tap chf Khoa hpc & Giao dgc, Trudng<br />
thinh phin cua phdc chat triphenylphosphin oxit-ytri DHSP, Dai hpc Hud (Da nhan dang).<br />
til mdi trudng axit nitric. Tap chf Hda hpc, T.45 (2), tr. 6. Nguyin Dinh Trigu (2001), Cic phUdng phip phin<br />
195-198. tich vit ly vi hda ly, NXB Khoa hpc v l Ky thudt. Ha Nfli.<br />
3. Nguyin Dinh Luygn, Nguyin HQu Hidn, Pham Quy, 7. Barbara Stuart (2004), Infrared Spectroscopy:<br />
Vo Tidn iJung (2009), Chiit fim giiu ytri vi xic djnh Fundamentals and Applications, Wiley, Chichester, UK.<br />
thinh phin phdc cua nd vdi triphenylphosphin oxit til<br />
mdi trudng axit tricloaxetic. Tap chf Khoa hpc & Giao 8. T.S. Lobana, F.R. Hartley (1992), The Chem-<br />
dgc, Trudng DHSP, Dai hpc Hug, sd 01(09), tr.19-23. istry of Organophosphorus Compounds, Wiley, New<br />
York, USA. *<br />
4. Nguvin Dinh Luygn, Pham Quy (2009), ChiS'tcic<br />
nguySn todit hiim bing triphenylphosphin oxit til mdi NgUttiphin biin: TS NGUviN V A N H A I<br />
<br />
<br />
<br />
NGHIEN cufu Sir TAO PHUfC DA PHOI TUf...<br />
(Ti^p theo trang 39)<br />
<br />
TV. KET LUAN<br />
SQ dgng phuong phap chidt - trie quang dd nghign - Da xac djnh dope cac tham sd djnh lopng cua phQc.<br />
cQu sg tao phQc PAN-La(lll)-SCN' trong dung mfli hOu<br />
cd izoamylie. Chung tfli dua ra kdt luIn: - Da xac djnh dupc phUdng trinh dudng chuln va<br />
- Da nghign cQu mflt each cd hg thdng sg tao phQc, khoing ndng dfl phQc tuan theo djnh luat Beer.<br />
cac didu kign tao phQc va chidt phQc tdi QU.<br />
- Da xac djnh dupc ham lupng lantan trong mlu<br />
- Da xac djnh dQpe thanh phln, cd chd ciia phln<br />
Qng tao phQc daligan. nhan tao va mlu that cho kdt qui phii hpp vdi thgc td.<br />
<br />
TAI LitU THAM KHAO<br />
1. Hd Vidt Quy (1999): Cic phUdng phip phin tich 3. Bhoon Y. K, Pandeya K. B. (1974) "Metal com-<br />
quang hpc trong hoi hpc. NXB. OHQG Ha Nfli. plexes of 1- (2- Pyridylazo)- 2- Phananthrol (PAP) as<br />
2. TrIn COng Vigt (1993), luan an tidn sy, "NghiSn Visual Indicators in acid- Base Titrations" J. Indian<br />
cdu stf hlnh thinh vi chief phdc da phCfi tit cua mdt Chem. Soe, Vol. LI, pp. 960-962. «<br />
s6 nguySn t6 dit hiim vdi PAR - axit axetic vi din<br />
xu5?cua/?d". tr.16-19. NgUtiphin bifn: PGS, TS DINH XUAN DJNH<br />
<br />
<br />
<br />
H6a hpc & tfng dyng<br />
S r 2 2 (io6)/20og<br />
m<br />
Thêm vào BST
Báo xấu
Download
Vui lòng tải xuống để xem tài liệu đầy đủ
