melizabeth santana oral presentation may2014

8/12/2019 Melizabeth Santana Oral Presentation May2014

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Melizabeth Santana Silverio

QUIM 4999 Inorganic Investigation

Prof. L. Koscielski

Synthesis and characterization oflow-melting mixed-metal oxides

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University of Puerto Rico in Cayey


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Contents:

Introduction

Elements of the reactions

Descriptions

Compounds known

Investigation

Methodology

Conclusion

Futures work References

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Introduction: What is solid statechemistry?

Solid state chemistry is the study of the synthesis, structure,and properties of solid phase materials.

Solid state is also referred as the chemistry of materials.

Different kinds of solid states amorphous, crystalline orpolycrystalline.

1Google image, http://googleimage/amorphous(accessed May 2014)

Figure 1: Kinds of solid states1

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http://googleimage/amorphoushttp://googleimage/amorphous


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Characterization is the analysis of identifying theproperties of a compound.

X-ray crystallography is a technique that allows the 3Ddetermination of molecular structures.

A synthesis reaction or direct combination reaction is oneof the most common types of chemical reactions.

In a synthesis reaction two or more chemical speciescombine to form a more complex product.

Inorganic synthetic methods can be classified roughlyaccording to the volatility or solubility of the componentreactants, in this case low-melting mixed-metals.

Introduction: What is solid statechemistry?

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Oxides are binary or tertiary compounds of oxygen withanother element or group.

The elements used are arsenic (As), tellurium (Te), lead(Pb), bismuth (Bi), and antimony (Sb).

They have the properties of all having low melting points.

Elements of reaction

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Table 1: Physical and Chemical description of the elements used2

2MSDS, http://sciencelab.com(accessed May 2014) 6
http://sciencelab.com/http://sciencelab.com/


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With the elements selected reactions were made withdifferent ratios.

The ratios were selected by numeric order.

Some of the ratios with low numeric order were alreadydiscovered so I selected a higher numeric ratio.


Table 2: Discovered compounds3

Oxygen contentSame group

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3 AsSbO34 AsSbO4

AsBiO4SbBiO4

5 AsSbO5

7 SbBi3O7

3Lukasz Koscielki, Solid state research table MxM'yQx.7


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Table 3: Compounds to be discovered

Ratio Mix Elements Possibleproducts

1:2 AsBiO As2Bi4O9

As2Bi4O11

As2Bi4O13

As2Bi4O15

PbTeO PbTe2O5

PbTe2O6

PbTe2O7

PbTe2O8


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2:1 AsBiO As4Bi2O9

As4Bi2O11

As4Bi2O13

As4Bi2O15

PbTeO Pb2TeO4

Pb2TeO5

Pb2TeO6

Pb2TeO7



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1:3 AsBiO AsBi3O6

AsBi3O7

AsBi3O9

AsBi3O10

PbTeO PbTe3O4

PbTe3O8

PbTe3O10

PbTe3O11



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3:1 SbBiO Sb3BiO6

Sb3BiO7

Sb3BiO9

Sb3BiO10



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Ratio Mix Elements Possible products

1:3 AsBiO As3Bi5O12

As3Bi5O15

As3Bi5O17

As3Bi5O20

PbTeO Pb3Te5O13

Pb3Te5O16

Pb3Te5O18Pb3Te5O24

SbBiO Sb3Bi5O12

Sb3Bi5O15

Sb3Bi5O17

Sb3Bi5O20


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The elements to be synthesized most of them are newcompounds and analogues.

Analogues have a structure similar to that of anotherone, but differing from it in respect of a certain

component.

The only analogue compounds are:

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Compounds Analogue

PbTe2O5PbTe2O6PbTe2O7PbTe2O8

SnPbTe2

GePbTe2


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Making silica tubes

1. Measure a 48inch silica tube with a marker each 6cm.

2. Cut with a glass cutter each 12inches.

3. Using a Bunsen burner separate each tube and closethe end in a circular way.

4. Wait until its room temperature and insert a small

amount of acetone to make the carbon coating.

5. Heat the tube with acetone until the lower part turnsblack.

6. Do a triplicate of carbon coating in each tube.

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Methodology


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Methodology


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Methodology


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Synthesizing the reaction

1. Calculate the amount of reactants your going to use likethis example equation:

Note: The element with higher molar mass is always20mg

2. Weight the elements and insert them in the tubes withcarbon coating through a funnel and a rubber handle.

3. Put the funnel and the rubber handle in a beaker withaqua regia 3HCl: 1HNO3.

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Methodology


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4. Repeat steps with al reactions, using a new rubberhandle and funnel in each one.

5. After a day remove the aqua regia and put the funnelsin base for another day and clean the rubbers.

6. Put the tubes in the oven.

7. Characterize the product with X-ray crystallography.

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Methodology


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Methodology


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Load reactions in oven and characterize them.

Learn the technique of X-ray crystallography.

Make analogue reactions of Thorium with Hafnium.

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Future work


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University of Puerto Rico at Cayey

BRIC

Dr. L. Koscielski

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Acknowledgements


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Google image, http://googleimage/amorphous(accessed May 2014).

MSDS, http://sciencelab.com(accessed May 2014)

Lukasz Koscielki, Solid state research table MxM'yQx. J., Blascovich; J., Loomis; A.C. Beall; K. R. Swinth; C. L., Hoyt; J.

N., Bailenson, Inorganic Journal Crystal Research andTechnology, (1984), 19, 109-112, DOI:10.1207/S15327965PLI1302_01, Tandfonline,http://www.tandfonline.com/doi/abs/10.1207/.U4Zu_164nFI

(accessed May 2014)

S. G., Parker; J. E., Pinnell; L. N., Swink, Journal of MaterialScience Determination of the liquidus-solidus curves form thesystem PbTe-GeTe, (1974), 9, 1829-1832, SpringerLink,http://link.springer.com/article/10.1007%2FBF00541753

(accessed May 2014)22

References
http://googleimage/amorphoushttp://sciencelab.com/http://www.tandfonline.com/doi/abs/10.1207/.U4Zu_164nFIhttp://link.springer.com/article/10.1007/BF00541753http://link.springer.com/article/10.1007/BF00541753http://www.tandfonline.com/doi/abs/10.1207/.U4Zu_164nFIhttp://sciencelab.com/http://googleimage/amorphous


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Melizabeth Santana Silverio

QUIM 4999 Inorganic Investigation

Prof. L. Koscielski

Synthesis and characterization oflow-melting mixed-metal oxides

University of Puerto Rico in Cayey

melizabeth santana oral presentation may2014

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