Determination of Aluminum(III) in Minerals, Sludges, Soils and Plant Extracts using 2-Hydroxy-3- Methoxybenzaldehyde-P-Hydroxybenzoic Hydrazone

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1 Intrntionl Journl of Sintifi n Rsrh Pulitions, Volum 2, Issu 12, Dmr Dtrmintion of Aluminum(III) in Minrls, Slugs, Soils n Plnt Extrts using 2-Hyroxy-3- Mthoxynzlhy-P-Hyroxynzoi Hyrzon S.Stysr, V. Krishn Ry & P. Rvnr Ry Dprtmnt of Chmistry, Sri Krishnvry Univrsity, Anntpur (A.P), Ini Astrt- Highly snsitiv n sltiv irt n rivtiv sptrophomtri mthos r propos for th trmintion of luminium in vrious mtrils. 2-hyroxy-3- mthoxynzlhy-p-hyroxynzoi hyrzon rts with Al(III) forming yllow olour solul omplx in quous imthyl formmi whih hs λmx t 410 nm in th ph rng Snsitivity of th mtho hs signifintly inrs in th prsn of 0.02% of tyl pyriinium hlori misllr mium. Th systm oy Br s lw in th rng μg ml-1 of Al(III). Th molr sorptivity (4.19 x 104 L mol-1 m-1), ttion limit (3.8 x 10-3 μg ml-1) n trmintion limit (1.16 x 10-2 μg ml-1) init th snsitivity of th propos mtho. Th stuis on fft of ivrs ions show lmost ll th nions (xpt F-) n mjority of th tions o not intrfr in mor thn 50 fol xss. Th intrfrn from Ni(II), F(III), Cu(II) n Ti(IV) ws limint y using suitl msking gnts. Th irt mtho ws ppli for th trmintion of luminium in silit minrls, inustril slugs n in soils. Th snsitivity n sltivity of th propos mtho is furthr nhn in th first fourth orr rivtiv sptrophomtri mthos vlop. Son orr rivtiv mtho ws ppli for th trmintion of Al(III) in plnt xtrts, hir, t n wtr smpls. T I. INTRODUCTION h inustril n iologil pplitions of luminium r quit unnt. Its pplitions rng from rosp inustry, trnsporttion, uiling n ltril trnsmission, pkging n wtr trtmnt. Crtin luminium slts srv s n immun rspons oostr llow th protin in vin hiv suffiint potny s n immun stimulnt. Th othr si of its ffts is inrs mounts of itry luminium ru skltl minrliztion (ostophni) rsulting in growth rtrtion. Aluminium n us nuroxiity in vry high oss whih n ltr th funtion of loo rin rrir 1. Aluminium inrss strogn rlt gn xprssion in humn rst nr lls grown in th lorry 2. Mrury thrmomtrs r not llow on mny irlinrs s it unrgos mlgmtion with luminium mging prottiv oxi surf film on luminium mtl. Hn, trmintion of luminium in tr quntitis in vrious nturl systms is n importnt tsk. Among th first rport sptrophomtri mthos, th xtrtion mtho using 8-hyroxy quinolin is not snsitiv ut highly sltiv 3. Th propos y Mrznko t l 4 Sfvi 5, n Ahm t t 6 r highly snsitiv ut thy suffr from th intrfrn of som ivrs ions. Th mthos propos y Nsimn t l 7., r lss snsitiv. W r now rporting snsitiv n rsonly sltiv irt n rivtiv sptrophomtri mthos for th trmintion of luminium in numr of nturlly ourring omplx mtrils. II. EXPERIMENTAL Th hromogni rgnt, 2-hyroxy-3- mthoxynzlhy-p-hyroxynzoi hyrzon ws synthsiz in th lorry y onnsing 2-hyroxy-3- mthoxynzlhy n p-hyroxynzoi hyrzon. A DMF solution of th rgnt in suitl onntrtions ws us in th stuis. 0.01M sk solution of Al(III) ws prpr y issolving rquisit mount of luminium mmonium sulpht in istill wtr n stnriz volumtrilly 8. Th working solutions wr prpr y iluting th sk solutions with istill wtr. Buffr solutions of ph wr prpr y mixing 0.2M CH 3 COON n 0.2M CH 3.COOH in suitl proportions n hking th ph y ph mtr. Th misllr mium, tyl pyriinium hlori (1%) ws prpr y issolving 1 grm of slt (SRL Chmils) in 100 ml of oil istill wtr. Th sorn n rivtiv mplitu msurmnts wr m on SCHIMADZU 160-A UV-visil sptrophomtr. Th ph of th uffr solutions ws msur y Elio ph mtr (LI 610). All othr hmils us wr of nlytil or gurnt rgnt gr. III. PROCEDURE To 4 ml of uffr solution (ph 5.0) 1 ml of HMBAHBH (1 x 10-2 M), 0.2 ml of.p. (1%) 1 ml of DMF tkn in h of st of 10 ml volumtri flsks, vril mounts of Al(III) wr n ilut th volum with istill wtr. Th sorn of ths solutions ws msur t 410 nm ginst rgnt lnk n plott ginst th mount of luminium. A stright lin with rgrssion qution A= ε (μg ml -1 ) [Al(III) ] ws otin in spifi onntrtion rgion of Al(III). For th rivtiv sptrophomtri trmintion of luminium, first, son, thir n fourth orr rivtiv sptr wr ror in th wvlngth rgion nm with sn sp of 2400 nm pr minut n with 9 grs of from. For th xprimntl solutions ontining iffrnt mounts of th mtl ion unr optiml onitions n

2 Intrntionl Journl of Sintifi n Rsrh Pulitions, Volum 2, Issu 12, Dmr th rivtiv mplitus wr msur t th suitl wvlngths n plott ginst th mount of luminium vlut th trminl rngs in vrious orr rivtiv mthos. IV. RESULTS AND DISCUSSION Th sorption sptrum [Al(III) HMBAHBH] omplx show mximum sorn t 410 nm whr th rgnt show ngligil sorn. Th sorn ws foun mximum n onstnt in th H rng Thrfor, th nlytil stuis wr rri out t ph 5.0. A 15 fol molr xss rgnt ws foun nssry otin mximum olour intnsity for givn mount of mtl ion. Th sorn of th mtl omplx signifintly inrs in th prsn of tyl pyriinium hlori n tyl tri mmonium romi tioni surftnts ut slightly rs in th prsn of soium oyl sulpht, polyvinyl lohol n Trin-X-100. Btwn th two tioni surftnts tyl pyriinium hlori gv mximum sorn. Hn, th nlysis ws rri out in th prsn of 0.02%.p.. Th rivtiv sptr ror in th wvlngth rgion nm for th xprimntl solutions show mximum n proportionl vril sorns t 427 nm (1 st orr), t 444 nm (2 n orr), t 424 nm n 457 nm (3 r orr) n t 409 nm, 445 nm n 474 nm (4 th orr) s shown in Figurs 1 4. Th nlytil rsults otin in irt n first fourth orr rivtiv mthos r tult in Tl 1. Prmtr Br's lw rng (μg ml -1 ) Molr sorptivity, ε (L mol -1 m -1 ) Snll s snsitivity (μg m -2 ) Angulr offiint (m) Y - intrpt () Corrltion offiint (r) Rltiv stnr vition (%) Dttion limit (μg ml -1 ) Dtrmintion limit (μg ml -1 ) Composition (Mtl : Lign) Dirt mtho Tl 1. Anlytil hrtristis of [Al(III) HMBAHBH] I rivtiv II rivtiv III rivtiv IV rivtiv 410 nm 427 nm 444 nm 424 nm nm 409 nm 445 nm 474 nm , : Stility onstnt x Th molr sorptivity Br s lw rngs, ttion limit, trmintion limit shown in th tl init th high snsitivity of oth th irt n rivtiv mthos. Howvr th rivtiv mthos r foun muh mor snsitiv thn th irt mtho. Th fft of ivrs ions on th sorn of th xprimntl solution show tht ll th nions tst (xpt F - ) o not intrfr in mor thn 100 fol xss. Fluori is lrl up 45 fol xss. Among th tions P(II), L(III), Hg(II) n Th(IV) o not intrfr in mor thn 100 fol xss. Y(III), Bi(III), Mo(VI) n Zr(IV) r lrl up 50 fol xss. Th lrn limits of othr mtl ions r 30 fol C(II), S(IV), 26 fol (Au 3+, Ru 3+ n Zn 2+, 20 fol (Tl 3+, Ag +, Mn 3+, Cr 6+, C 4+ ) n 10 fol (Co 2+, W 6+, P 2+ ). Th lrn limits of Ni 2+, F 3+, Cu 2+, n Ti 4+ whih intrfr sriously, r nhn mor thn 100 fol in th prsn of EDTA or I s msking gnts. Th rsults prsnt in Tl 2 rvl tht in th 1 st n 2 n rivtiv mthos, th lrn lvls of numr of mtl ions whih show srious intrfrn in zro orr mtho r grtly inrs. In th thir n fourth rivtiv mthos lso th lrn limits of som mtl ions r foun highr thn in zro orr mtho. This is n vin of th grtr sltivity of th rivtiv mthos ovr zro orr mtho.

3 Intrntionl Journl of Sintifi n Rsrh Pulitions, Volum 2, Issu 12, Dmr Tl. 2 Tolrn limits of Forign ions Amount of Al(III) tkn = μgml -1 ; ph = 5.0 Forign ion Tolrn limit (μgml -1 ) Forign ion Tolrn limit (μgml -1 ) Asort 875 P(II) 104 EDTA 760 L(III) 70 Ioi 390 Hg(II) 40 Thio ur 380 Th(IV) 24 Trtrt 266 Y(III) 15 Phospht 260 Bi(III) 15 Thio sulpht 250 Mo(VI) 10 Citrt 244 Zr(IV) 9 Sulpht 240 C(II) 8 Bromi 202 S(IV) 8 Thioynt 154 Au(III) 7 Cront 140 Ru(III) 7 Nitrt 110 Zn(II) 7 Chlori 90 Tl(III) 6 Oxlt 74 Ag(I) 6 Fluori 15 Mn(II) 6 Cr(VI) 5 C(IV) 5 U(VI) 3 Co(II) 3 W(VI) 3 P(II) 2 Ni(II) F(III) Cu(II) Ti(IV) <1, 75 <1, 90 <1, 45 <1, 60 Tl.2.. Tolrn limits of forign ions Forign ion Tolrn limits (in fols) Zro Orr First rivtiv Son rivtiv 427 nm 444 nm 424 nm Thir rivtiv nm Fourth rivtiv 409 nm 445 nm 474 nm Cu(II) < intrfrs intrfrs Ni(II) <

4 Intrntionl Journl of Sintifi n Rsrh Pulitions, Volum 2, Issu 12, Dmr Y(III) < 1 68 > 100 > 100 > 100 > 100 > 100 > 100 L(III) < 1 > 100 > 100 > 100 > 100 > 100 > 100 > 100 V(V) < intrfrs intrfrs intrfrs In(III) < intrfrs intrfrs intrfrs intrfrs intrfrs F(II) < Ti(IV) < G(III) < intrfrs intrfrs intrfrs intrfrs intrfrs Applitions Th irt mtho ws ppli for th trmintion of luminium in ront n silit minrls, inustril slugs n soil smpls. Th smpl solutions wr prpr s pr th rommn prours for silit minrls 9, inustril slugs 10 Vril liquots of th smpl solutions wr trt with suitl mounts of HMBAHBH n.p.. (surftnt) unr th prsri onitions n th sorns wr msur t 410 nm. Th mounts of luminium prsnt in ths smpls wr omput from prtrmin lirtion plots n prsnt in Tl 3, 4 n 5. Tl 3. Dtrmintion of Al(III) in ront n silit minrls Aluminum (%) Smpl Crtifi Foun* Vlu Sili rik (NBS 1.99 ± ) ± Glss frit (NBS 128) Optil glss (BSC 0.76 ± /644) Optil glss (NBS 1.87 ± ) ± Lim sn * Avrg of four trmintions ± S.D. Rltiv Error (%) Th rsults otin in th prsnt mtho with rgr slugs wr ompr with thos otin y flm mi sorption sptrophomtri mtho n prsnt. Tl 4. Dtrmintion of luminum in Slug smpls Prsnt mtho AAS mtho ± ± ± ± ± ± * Avrg of four trmintions ± S.D. Tl 5. Dtrmintion of luminium in Soil smpls Smpl Grlinn (groun nut ultivtion soil) Tiptri (Bngl grm ultivtion soil) Rpthu (Sunflowr ultivtion soil) Amount of luminium (µg ml -1 ) A Foun* Rovry (%) ± ± ± ± ± *Avrg of four trmintions ± S.D ± Th son orr rivtiv sptrophomtri mtho ws mploy for th trmintion of luminium in plnt xtrts, humn hir, t n wst wtr smpls. Th solutions of plnt, xtrt 11, humn hir n t 12 wr prpr oring th rommn prours n thir luminium ontnt wr trmin y th propos son orr rivtiv mtho. Th plnt xtrt smpls wr lso nlys y flm mi sorption sptrophomtri mtho n ompr with thos of prsnt mtho n IPE 13 rport t. Th rsults r prsnt in Tl 6 n 7. Slug smpl Amount of luminum (mg/g)*

5 Intrntionl Journl of Sintifi n Rsrh Pulitions, Volum 2, Issu 12, Dmr Tl 6. Dtrmintion of luminum in plnt xtrts Smpl Amount of luminium (µg ml -1 ) Prsnt mtho* AAS mtho* Ros ± 3 55 ± Sprouts ± ± Grss 298 ± ± Miz ± ± * Avrg of fiv trmintions = Smpls from Intrntionl Plnt nlytil xhng progrmm (I.P.E.) IPE rport 43 t pt rng (mg g -1 ) Tl.7. Dtrmintion of luminium in humn hir, t n wst wtr Amount of luminium (µg ml -1 ) Smpl Rovry Rfrn 44 Rltiv A Foun* RSD (%) (%) Mtho rror (%) T Humn hir Wst wtr * Avrg of four trmintions = Thr ross t smpl, Brook Bon Ini Lt., = Domsti swg wtr. Th propos irt n rivtiv sptrophomtri mthos r simpl, snsitiv, lss tious, rsonly sltiv n r pplil for th nlysis of omplx mtrils. Th prsnt irt mtho is foun mor snsitiv thn thos propos y Nmov t l 13, Zhong fng t l 14., n Srgio t l 15. Th son rivtiv mtho ws foun mor sltiv. REFERENCES [1] Bnks,W.A.;Kstin,A.J. Aluminium inu nuroxiity:ltrtions in mmrn funtion t th loo-rin rrir..nurosi BiohvRv 13(1) ;1989; 47. [2] Mttllostrogns : n mrging lss of inorgni xnostrogns with potntil th ostrogni urn of th humn rst J. Appl. Toxiol;26(3); 2006; 191. [3] A.Clssn, L Bstings n J.Vissr, A highly sltiv prour for th sptrophomtri trmintion of luminium with 8-hyroxy-quinolin n its pplition th trmintion of..,anlyti Chimi At, 10,1954,373. [4] Z.Mrznko, M.Jrosz, Formtion of trnry omplxs of luminium with som triphnyl mthn rgnts n tioni surftnts, Anlyst,107,1982,1431. [5] A.Sfvi,t l Simultnous sptrophomtri trmintion of F (III), Al (III) ncu(iii)y prtil lst- squrs lirtionmtho Sp.Chimi.At;63(1); 2006; 196. [6] M. Jmluin Ahm n Jml Hossn, Sptrophomtri trmintion of luminium y morin; Tlnt,;42(8); 1995; 1135 [7] C.Pulo Nsimn, L. Cristini Jost;t.l, Simultnous trmintion of Al(III) n F(III) in post hmoilysis fluis y sptrophomtry n multivrit lirtion Tlnt,;70;(3 )2006; 540. [8] A.I. Vogl A Txt ook of Quntittiv Anlysis 4th n, Longmns, Lonon, 1978, 389. [9] N.L.Bnrj n B.C. Sinh,Extrtion sptrophomtri mtho for trmintion of luminium in silits; Tlnt; 37(10);1990; [10] Environmntl prottion Agny, USA, Mtho, 3050B [11].O.C Btgli, A.M.C.Furlni, J.P.E.Tixir, P.R.Furlni, J.R.Gllo, Thnil Bulltin No.78, 1983, 9. [12] Ronghun H n Jinhu wng, Novl tlyti sptrophomtriprour for th trmintion of tr- lvl luminium;anlyti Chimi At, 2000, 412, 241. [13] Annul Rport, Intrntionl plnt-anlytil Exhng (IPE) Wgningn Agriulturl Univrsity, Th Nthrlns, [14].I. Nmov, B. Evtimov, n I. Hrhovsk, Sptrophomtri Dtrmintion of Aluminium (III) n Fluori ions with Bromopyrogllol R in th prsn of Ctioni SurftntsSpnx,C.R.A.Bulg.Si. 43(2), 45,1990. [15] Liu Zhongfng, Liu Shopu n Wng Xuho,Sptrophomtri trmintion of Aluminium in Coppr Alloys with Croxyzo I,Chmistry prtmnt,southwst Chin Thrs Univrsity ;10(4), 1990, 9. [16] SrgioL.C. Frrir Ni.O.Lit,AlilsonF.Dnts t l.,sptrophomtri n rivtiv sptrophomtri trmintion of luminium with Hyroxynphthol Blu,Tlnt, 41(10), 1994,1631.

6 2 A/ 2 A/ Intrntionl Journl of Sintifi n Rsrh Pulitions, Volum 2, Issu 12, Dmr AUTHORS First Author S.Stysr, Dprtmnt of Chmistry, Sri Krishnvry Univrsity, Anntpur (A.P), Ini Son Author V. Krishn Ry, Dprtmnt of Chmistry, Sri Krishnvry Univrsity, Anntpur (A.P), Ini, Emil : vkry_sku@yhoo.o.in Thir Author P. Rvnr Ry, Dprtmnt of Chmistry, Sri Krishnvry Univrsity, Anntpur (A.P), Ini Wvlngth (nm) Fig. 1. First orr rivtiv sptr of [Al(III) HMBAHBH] Amount of Al(III)(μgmL -1 ) ; ; ; ; ; Wvlngth (nm) Fig. 2. Son orr rivtiv sptr of [Al(III) HMBAHBH] Amount of Al(III)(μg ml -1 ) ; ; ; ; ; -

7 4 A/ 4 3 A/ 3 Intrntionl Journl of Sintifi n Rsrh Pulitions, Volum 2, Issu 12, Dmr Wvlngth (nm) Fig. 3. Thir orr rivtiv sptr of [Al(III) HMBAHBH] Amount of Al(III)(μgmL -1 ) ; ; ; ; ; Wvlngth (nm) Fig. 4. Fourth orr rivtiv sptr of [Al(III) HMBAHBH] Amount of Al(III)(μgmL -1 ) ; ; ; ; ; -