University of Puerto Rico in Cayey

Chemistry Department
Synthesis and characterization of low-melting mixed-metal oxides
Melizabeth Santana Silverio
804-10-8040
Prof. !"asz #ociels"i
$%&M 4'''
(heme) Synthesis and characterization of low-melting mixed-metal oxides
*bstract)
Solid-state chemistry is the st!dy of the synthesis+ str!ct!re and ,ro,erties of solid
,hase materials. &n this investigation the main goal is to ma"e new ternary low-melting
mixed-metal oxides. (he elements !sed are arsenic -*s.+ tell!ri!m -(e.+ lead -Pb.+
bism!th -/i. and antimony -Sb. have the ,ro,erty of having low-melting ,oints. (his
,rocess !sed was synthesis even tho!gh the characterization co!ldn0t be com,leted it is a
goal that its ho,e to achieve in f!t!re wor"s.
&ntrod!ction)
Solid state chemistry is the st!dy of the synthesis+ str!ct!re+ and ,ro,erties of
solid ,hase materials and its also referred as the chemistry of materials. (here are
different "inds of solid states) amor,ho!s+ crystalline or ,olycristalline. 1haracterization
is the analysis of identifying the ,ro,erties of a com,o!nd. 2-ray crystallogra,hy is a
techni3!e that allows the 45 determination of molec!lar str!ct!res. * synthesis reaction
or direct combination reaction is one of the most common ty,es of chemical reactions. &n
a synthesis reaction two or more chemical s,ecies combine to form a more com,lex
,rod!ct. &norganic synthetic methods can be classified ro!ghly according the volatility or
sol!bility of the com,onent reactants+ in this case low melting mixed metals.
&n this Pro6ect of solid state we wor"ed with some elements in the 14+ 17 and 18
col!mn of the ,eriodic table. 9e wor"ed with them beca!se those elements were the
ones we had in the inventory. (he elements !sed are arsenic -*s.+ tell!ri!m -(e.+ lead
-Pb.+ bism!th -/i. and antimony -Sb.. (his elements have low melting ,oints and some
of them need to be handled with ,reca!tion beca!se of they0re toxic ,ro,erties. &n the
table below is shown the ,hysical and ,ro,erties of each element with its health handle
effects.
Table 1 ) Physical and 1hemical descri,tion of the elements !sed
1

Element Group Period Oxidation
State
Physical
properties
Chemical
properties
Health Effects
As 15 4 3, 5
Molar mass:
74.92g/mol
Stable
Poisonous
CARCINOGENIC
EFFECTS:
Melting
Point:
Sublimation
temperature:
615C
material Classified A1
Toxic
Te 16 5 4, 6, -3
o!ar mass"
1#$%6&'(mo!
)o!i*
e!tin'
point" 450C
)ta+!e
,on-
f!amma+!e
Very hazardous in
case of ingestion.
Slightly
hazardous.
P+ 14 6 #, 4
o!ar mass"
#&$%#'(mo!
Boiling
Point:
1740C
Melting
Point:
327.43C
)ta+!e
,on-
corrosive
Slightly hazardous
in case of skin
contact
(permeator).
CARCINOGENIC
EFFECTS:
Classified A3
(Proven for
animal.)
-i 15 6 3, 5
o!ar mass"
#&.%/.'(mo!
Boiling
Point:
1560C
Melting
Point:
271.3C
)ta+!e Hazardous in case
of ingestion.
Slightly hazardous
in case of eye
contact (irritant),
of inhalation.
)+ 15 5 3, 5
o!ar mass"
1#1%$6'(mo!
Boiling
Point:
1635C
Melting
Point: 630C
)ta+!e Very hazardous in
case of ingestion.
Hazardous in case
of skin contact
(irritant).
0 16 # -#
o!ar mass"
15%//'(mo!
Boiling
Point:183C
Melting
point:218.4C
,on-
f!amma+!e
Acute or chronic
respiratory
conditions may be
aggravated by
overexposure to this
gas.
9ith the elements selected reactions were made with different ratios. (he ratios
were selected by n!meric order. Some of the ratios with low n!meric order were already
discovered so & selected higher n!meric ratios. &n the following gra,hs yo! can a,,reciate
the elements that have been discovered and the ones to be discovered.
Table 2: 5iscovered com,o!nds
:

Oxygen content
Same group
15/15
3 AsSbO
3
4 AsSbO
4
AsBiO
4
SbBiO
4
5 AsSbO
5
7 SbBi
3
O
7
Table 3) 1om,o!nds to be discovered
Ratio Mix Elements Possible products
1): *s/i; *s
:
/i
4
;
'
*s
:
/i
4
;
11
*s
:
/i
4
;
14
*s
:
/i
4
;
17
Pb(e; Pb(e
:
;
7
Pb(e
:
;
8
Pb(e
:
;
<
Pb(e
:
;
8
Ratio Mix Elements Possible products
:)1 *s/i; *s
4
/i
:
;
'
*s
4
/i
:
;
11
*s
4
/i
:
;
14
*s
4
/i
:
;
17
Pb(e; Pb
:
(e;
4
Pb
:
(e;
7
Pb
:
(e;
8
Pb
:
(e;
<
Ratio Mix Elements Possible products
1)4 *s/i; *s
4
/i
7
;
1:
*s
4
/i
7
;
17
*s
4
/i
7
;
1<
*s
4
/i
7
;
:0
Pb(e; Pb
4
(e
7
;
14
Pb
4
(e
7
;
18
Pb
4
(e
7
;
18
Pb
4
(e
7
;
:4
Sb/i; Sb
4
/i
7
;
1:
Sb
4
/i
7
;
17
Sb
4
/i
7
;
1<
Sb
4
/i
7
;
:0
Ratio Mix Elements Possible products
4)1 Sb/i; Sb4/i;8
Sb4/i;<
Sb4/i;'
Sb4/i;10
Some elements can have similar ,ro,erties beca!se of the gro!, or family they
are in the ,eriodic table. #nowing this+ & searched to see what com,o!nds were analog!es
and new. (he ma6ority of the com,o!nds are new exce,t fo!r that are analog!es. *n
analog!e com,o!nd is a com,o!nd that has the same ,hysical and chemical ,ro,erties as
another com,o!nd b!t they differ in one element. &n the following table there is showed
the analog!e com,o!nds.
Compounds Analogue
Pb(e
:
;
7
Pb(e
:
;
8
Pb(e
:
;
<
Pb(e
:
;
8
SnPb(e
:
=ePb(e
:
Methodology)
(he ,rocess for ma"ing inorganic com,o!nds first we need ma"e silica t!bes with
carbon coating to load the reactions. >or this we need to Meas!re a 48inch silica t!be
with a mar"er each 8cm. 1!t with a glass c!tter each 1:inches. %sing a /!nsen b!rner
se,arate each t!be and close the end in a circ!lar way. 9ait !ntil its room tem,erat!re
and insert a small amo!nt of acetone to ma"e the carbon coating. (he carbon coating is
necessary beca!se it ,revent the reactants to react with the glass of the t!be. ?eat the t!be
with acetone !ntil the lower ,art t!rns blac". 5o a tri,licate of carbon coating in each
t!be.
(o determine how m!ch of reactant we need we have to calc!late the amo!nt of
each element. >or this calc!lation we need :0mg of the element with higher weight+ !se
the ratio and then !se the molar mass of the other element. /elow there is an exam,le of
this calc!lation.
Illustration 1: ?ow to calc!late de amo!nt of element for the reaction
*
:
/;
7
@ Molec!lar weight of) *A100.7gBmol and /A70.8gBmol
?aving the t!bes done and "nowing the amo!nt of elements what0s left is to start
the reaction. Co! ,o!r the reactants into the t!bes with a f!nnel and ,lace them in the
oven with the tem,erat!re it needs. 9hen the time of the reaction sto,s+ leave the t!bes at
room tem,erat!re so they can cool off. &dentify the ,rod!ct with the techni3!e of 2-ray
crystallogra,hy.
>!t!re wor")
/eca!se of lac" of materials and time o!r ,ro6ect have a different method of
heating or synthesizing+ we ,o!red the elements in the t!bes witho!t oxides and let them
react with the oxygen that the atmos,here ,rovides.
*s f!t!re wor" in this investigation & wo!ld li"e to com,lete the reactions made
with the oven and learn the techni3!e of 2-ray crystallogra,hy. &n addition wor" with
analog!e reactions of thori!m with hafni!m.
Deferences)
1. MSDS, http://sciencelab.com (accessed May 2014)
:. !"asz #osciel"i+ Solid state research table MxMEy$x.
4. J., Blascovich; J., Loomis; A.C. Beall; K. R. Swinth; C. L., Hoyt; J. N., Bailenson, Inorganic
Journal Crystal Research and Technology, (1984), 19, 109-112, DOI:
10.1207/S15327965PLI1302_01, Tandfonline,
http://www.tandfonline.com/doi/abs/10.1207/. U4Zu_164nFI (accessed May 2014)
4. S. =.+ Par"er@ F. G.+ Pinnell@ . H.+ Swin"+ Fo!rnal of Material Science Determination of the
liquidus-solidus curves form the system PbTe-GeTe, -1'<4.+ '+ 18:'-184:+ S,ringerin"+
htt,)BBlin".s,ringer.comBarticleB10.100<I :>/>00741<74 -accessed May :014.