Op imiza ion o he syn hesis o Magne ic Nanopa icles by Solid Sampling High
Resolu ion Con inuum Sou ce G aphi e Fu nace A omic Abso p ion Spec ome y and
Mul i-Response Su ace Me hodology
Elisa Isabel Ve eda Alonso (1), M. Ma López Gue e o (1), Ampa o Ga cía de To es (1), José
Manuel Cano Pa ón (1), M. Te esa Siles Co de o (1)
(1) Uni e si y o Málaga
Campus de Tea inos Málaga Spain
Email: ei e [email protected]
P esen ing au ho : M. Ma López Gue e o
Type:
O al
Theme:
E. Ma e ials, De ices and Nanochemis y
Topic:
E3. Analy ical Techniques, Cha ac e isa ion and P ope ies
Keywo ds:
Magne ic nanopa icles, Solid sampling HR-CS-ETAAS, Mul i- esponse su ace
me hodology
SUMMARY:
Magne ic nanopa icles (MNPs) a e a new kind o nanome e -sized ma e ials supe pa amagne ic wi h
po en ial applica ions as magne ic ca ies o a ious biomedical uses, was ewa e emedia ion,
p econcen a ion o a ious anions and ca ions, e c.1 The excellen p ope ies o MNPs a e s ongly
in luenced by he size o he nanopa icles. Ano he impo an ac o is he amoun o i on p esen . In
his wo k a simple, apid and inexpensi e app oach was de eloped o di ec de e mina ion o Fe
concen a ion and pa icle size o solid MNPs by solid sampling high esolu ion con inuum sou ce
g aphi e u nace a omic abso p ion spec ome y (SS-HR-CS-GFAAS). A new s a egy in e alua ing
a ea and slope o he ob ained abso bance signals o a line o Fe (352.614 nm) wi h low sensi i i y
was de eloped o bo h de e mina ions. Fo his pu pose, i e u nace p og am pa ame e s,
a omiza ion hea ing a e, a omiza ion empe a u e, py olysis hea ing a e, py olysis empe a u e and
hold py olysis ime, we e op imized wi h he employ o wo mul iple esponse su ace designs. The
esponse a iables chosen we e: a omiza ion signal a ea/weigh ed mass o MNPs and he in e se o
he upslope o he a omiza ion signal/weigh ed mass o MNPs. Wi h he op imized u nace pa ame e s,
good calib a ion cu es (R > 0.997) we e ob ained wi h liquid i on s anda ds ( o Fe de e mina ion)
and wi h MNPs samples wi h ce i ied size pa icle ( o size pa icle de e mina ion). The de e mina ion
o he MNPs size was alida ed by ansmission elec on mic oscopy (TEM).
The de eloped me hod was used in he op imiza ion o he syn hesis o MNPs by a mul i- esponse
su ace me hodology. The MNPs we e syn hesized by a modi ied chemical co-p ecipi a ion me hod,
whe e h ee ac o s ( eac ion ime, olume and concen a ion o NH3) we e in es iga ed using wo
esponses a iables (Fe concen a ion and 1/size o MNPs). F om his s udy was concluded ha he
highes Fe concen a ions we e ob ained wi h low olumes o NH3, and he smalles sizes o MNPs
we e ob ained wi h high NH3 concen a ions. The e o e, he op ima espe imen al condi ions ob ained
we e: eac ion ime: 55 min; NH3 olume: 10 mL; and NH3 concen a ion 30%. The syn hesis o
MNPs wi h he op imized pa ame e s esul in MNPs wi h a ound 65% in Fe and a size o 17 nm.
Op imum size anges om 13 o 18 nm a e p e e able o hei use as abso ben in solid phase
ex ac ion because o hei highe magne ic momen pe pa icle.2
[1] M.H. Mashhadizadeh, Z. Ka ami, J. Haza d Ma e ., 2011, 190, 1023.
[2] M. Ma ciello, V. Conno d, S. Vein emillas-Ve dague , M.A. Ve gés, J. Ca ey, M. Respaud, C.J.
Se na, M. P. Mo ales, J. Ma e . Chem. B, 2013, 1, 5995.