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DubaiAmateurRocketry
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Titanium IV Perchlorate Ti(ClO4)4
I recently got interested into Titanium IV perchlorate.
In the preview of this report, (I wish some one could purchase this and give it to us for free)
http://link.springer.com/article/10.1007/BF00922105
It stated that Ti(ClO4)4 decompose into TiO2 and the rest chlorine and oxygen, this is such a high amount of oxdizier released !!
Only 17.9% of this compound is turned into solid upon decomposition, and the rest is oxidizers, even the TiO2 could react with aluminum !
It contains more oxidizer by weight than AP and denser. However its reported that it explode at 130 degree, but i dont think it would be that
dangerous, since decomposition is endothermic.
I also found a place to purchase this, extremely expensive though.
[Edited on 15-6-2013 by DubaiAmateurRocketry]
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Fantasma4500
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interesting, i think what approach you would want would be dilute HClO4 + Ti as Ti even reacts with HCl of what ive heard
whats the price for say.. 100g Ti(ClO4)4?? sounds expensive, not only by the idea that titanium compounds are pricey but tetraperchlorate..??
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DubaiAmateurRocketry
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Quote: Originally posted by Antiswat  | interesting, i think what approach you would want would be dilute HClO4 + Ti as Ti even reacts with HCl of what ive heard
whats the price for say.. 100g Ti(ClO4)4?? sounds expensive, not only by the idea that titanium compounds are pricey but tetraperchlorate..??
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In your dreams bro, Titanium Tetra perchlorate reacts with water.
Making it, you need a solution of 98% Anhydrous perchloric acid and 2% Cl2O7 as catalyst. Which is why it is so expensive.
The price for 250 grams of TP is almost one dollar per gram..
[Edited on 15-6-2013 by DubaiAmateurRocketry]
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Trotsky
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That's actually pretty cheap. I mean, comparably. Try buying gaboxadol or anything cool for that price.
Someone should tell the coke dealers that a dollar per gram is expensive 
If it's as good as it looks a few grams will pack a powerful punch. I'd worry about ddt if you're thinking of it as a propellant. That won't work
well
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DubaiAmateurRocketry
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| Quote: Originally posted by Trotsky | That's actually pretty cheap. I mean, comparably. Try buying gaboxadol or anything cool for that price.
Someone should tell the coke dealers that a dollar per gram is expensive
If it's as good as it looks a few grams will pack a powerful punch. I'd worry about ddt if you're thinking of it as a propellant. That won't work
well |
It might be, I will try purchase around 50 gram first, It is not reactive at all, if it had a reactivity NFPA it would be maximum 2.
Also the decomposition composition is..
Ti(ClO4)4 + Heat = TiO2 + 7O2 + 2Cl2
Although it first makes some chlorine oxides, it will furthur decompose.
[Edited on 15-6-2013 by DubaiAmateurRocketry]
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hyfalcon
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| Quote: Originally posted by DubaiAmateurRocketry | | Quote: Originally posted by Antiswat | interesting, i think what approach you would want would be dilute HClO4 + Ti as Ti even reacts with HCl of what ive heard
whats the price for say.. 100g Ti(ClO4)4?? sounds expensive, not only by the idea that titanium compounds are pricey but tetraperchlorate..??
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In your dreams bro, Titanium Tetra perchlorate reacts with water.
Making it, you need a solution of 98% Anhydrous perchloric acid and 2% Cl2O7 as catalyst. Which is why it is so
expensive.
The price for 250 grams of TP is almost one dollar per gram..
[Edited on 15-6-2013 by DubaiAmateurRocketry] |
Correct me if I'm wrong, but 98% perchloric acid is explosive in and of itself. Anything over 70% and you're asking for an explosion.
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Trotsky
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Does anyone know if you could form phenyl titanium triperchlorate? Or perhaps trinitro phenyl titanium triperchlorate? Or perhaps some other organic
substitutent to make for a more neutral OB, remove the need for an additional fuel source.
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franklyn
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Bretherick's Handbook of Reactive Chemical Hazards Vol 1
[ 4 1 7 0 ] Titanium Tetraperchlorate
Kirk Othmer, 4th. Edn., 1996, Vol. 18, 161
The compound sublimes from 70 °C and explodes on heating to 130 °C
at atmospheric pressure. US Patent 3157464
Described as insensitive to heat or shock, this powerful oxidant explodes
on contact with Diethyl ether , and ignites with Formamide , or Dimethylformamide.
Studies of Complex Perchlorates
www.dtic.mil/dtic/tr/fulltext/u2/430803.pdf
www.dtic.mil/dtic/tr/fulltext/u2/607947.pdf
www.dtic.mil/dtic/tr/fulltext/u2/634105.pdf
___________________________________
Another Oxidizer of Interest
The reaction between zinc and liquid dinitrogen tetroxide involves the evolution of
nitric oxide, and the formation of a compound Insoluble In the tetroxide havlng the
empirical formula Zn(NO3)2 • 2N2O4. Tha action of heat on this compound, and its
reactions with organIc solvents ( particularly ethyl ether ) are considered in the light
of possible structures for the compound. Heating at 100 º results In the removal of
the two moIocuies of dinltrogen tetroxide, leaving zinc nitrate in the pure anhydrous
form. This method of preparation is simpler than methods previously described.
Zinc nitrate is stable at 100 º, but decomposes slowly in the temperature range
100 - 240 º, and rapidly above 240 º.
For this abstract and first page , of part VII , the first cited below.
http://pubs.rsc.org/en/content/articlelanding/1951/jr10.1039...
The Liquid Dinitrogen Tetroxide Solvent System
Part VII. Products of reaction of zinc with liquid dinitrogen tetroxide
J. Chem. Soc. , 1951 , 2829 - 2833
Part VIII. Rates, and possible mechanisms, of reaction of zinc with liquid dinitrogen tetroxide
J. Chem. Soc. , 1951 , 2833 - 2838
Part IX. Products, rates, and possible mechanisms of the reaction of zinc with liquid dinitrogen trioxide–tetroxide mixtures
J. Chem. Soc. , 1951 , 2838 - 2843
This whole series of papers related to N2O4 are cited here , if you have access _
www.sciencemadness.org/talk/viewthread.php?tid=19098&pag...
____________________________________
Ti(ClO4)4
As you point out produces 17.9 % solid ( TiO2 )
9 mols of gas and one mol of TiO2 or 10 %
LiClO4
produces just 14 % solid ( Li2O )
9 mols of gas and 2 mols of Li2O or 18.2 %
Zn(NO3)2 • 2N2O4
produces 21.8 % solid ( ZnO )
21 mols of gas and 2 mols of ZnO or 8.7 %
The density of the final pyrotechnic mixture will
also factor significantly in the performance derived.
.
[Edited on 16-6-2013 by franklyn]
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AndersHoveland
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| Quote: |
Nonsolvated titanium perchlorate was produced by the action of TiCl4 on anhydrous perchloric acid (containing up to 2% Cl2O7). Titanium perchlorate
possesses an appreciable intrinsic vapor pressure and can be repeatedly sublimed at 70 °C under vacuum. The properties of sublimed Ti(ClO4)4 differ
from the properties of the starting material.
It was established by the method of differential thermal analysis that Ti(ClO4)4 melts with partial decomposition at 85–95 °C, and above 110°C
under vacuum it decomposes to TiO2, O2, and oxides of chlorine. The heating of Ti(ClO4)4 at atmospheric pressure ends in explosive decomposition at
∼130 °C.
Ti(ClO4)4 dissolves vigorously in water, it dissolves with decomposition in nitromethane and acetonitrile - the solution turns yellow. It is insoluble
in CCl4 but above 25 °C it reacts, forming a yellow solution.
Titanium perchlorate is a colorless hygroscopic crystalline substance. ... The density of Ti(ClO4)4 ... is equal to 2.35 g/cm3.
"Volatile titanium perchlorate", V. P. Babaeva, V. Ya. Rosolovskii,
Bulletin of the Academy of Sciences of the USSR, Division of chemical science, November 1974, Volume 23, Issue 11, pp 2330-2334
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| Quote: Originally posted by Trotsky | | Does anyone know if you could form phenyl titanium triperchlorate? Or perhaps trinitro phenyl titanium triperchlorate? Or perhaps some other organic
substitutent to make for a more neutral OB, remove the need for an additional fuel source. |
It seems that Ti(ClO4)4 spontaneously reacts with any organic compound (much like anhydrous Al(ClO4)3 does). I do not think it would be any less
oxidizing if it just had 3 perchlorate groups.
However, it might be possible a Lewis adduct could be formed. US patent 2,363,684 describes an aduct (6:1) between DMSO and Al(ClO4)3, though it can
be noted that the reaction did not involve the anhydrous form of aluminum perchlorate, but rather the DMSO was used to displace the water of
hydration. Anhydrous Al(ClO4)3 immediately oxidizes most organic solvents, though it did react to form 1:3 adducts with both nitromethane and
tetrahydrofuran.
("Solvation, Solvolysis, and Complexing of Anhydrous Aluminum Perchlorate in Anhydrous Media", Z.K. Nikirina, V. Ya. Rosolovskii, Izvestiya
Akademii Nauk SSSR, Seriya Khimicheskaya, No. 6, pp. 1223–1227, June, 1980.)
Another possibility is mixed azide-perchlorate complexes. Both Ti(ClO4)62‒ and
Ti(N3)62‒ exist.
Though consideration would be needed, because anhydrous Ti(ClO4)4 would likely immediately oxidize any free azide ions (though once the azide groups
are part of the complex they will no longer be vulnerable to oxidation, as they will be electron donating).
And I also doubt Ti(N3)4 would be a strong enough Lewis acid to form an adduct with perchlorate ions, so the resulting complex ion would probably have
to contain at least 3-4 perchlorate groups.
[Edited on 16-6-2013 by AndersHoveland]
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DubaiAmateurRocketry
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| Quote: Originally posted by franklyn | Bretherick's Handbook of Reactive Chemical Hazards Vol 1
[ 4 1 7 0 ] Titanium Tetraperchlorate
Kirk Othmer, 4th. Edn., 1996, Vol. 18, 161
The compound sublimes from 70 °C and explodes on heating to 130 °C
at atmospheric pressure. US Patent 3157464
Described as insensitive to heat or shock, this powerful oxidant explodes
on contact with Diethyl ether , and ignites with Formamide , or Dimethylformamide.
Studies of Complex Perchlorates
www.dtic.mil/dtic/tr/fulltext/u2/430803.pdf
www.dtic.mil/dtic/tr/fulltext/u2/607947.pdf
www.dtic.mil/dtic/tr/fulltext/u2/634105.pdf
___________________________________
Another Oxidizer of Interest
The reaction between zinc and liquid dinitrogen tetroxide involves the evolution of
nitric oxide, and the formation of a compound Insoluble In the tetroxide havlng the
empirical formula Zn(NO3)2 • 2N2O4. Tha action of heat on this compound, and its
reactions with organIc solvents ( particularly ethyl ether ) are considered in the light
of possible structures for the compound. Heating at 100 º results In the removal of
the two moIocuies of dinltrogen tetroxide, leaving zinc nitrate in the pure anhydrous
form. This method of preparation is simpler than methods previously described.
Zinc nitrate is stable at 100 º, but decomposes slowly in the temperature range
100 - 240 º, and rapidly above 240 º.
For this abstract and first page , of part VII , the first cited below.
http://pubs.rsc.org/en/content/articlelanding/1951/jr10.1039...
The Liquid Dinitrogen Tetroxide Solvent System
Part VII. Products of reaction of zinc with liquid dinitrogen tetroxide
J. Chem. Soc. , 1951 , 2829 - 2833
Part VIII. Rates, and possible mechanisms, of reaction of zinc with liquid dinitrogen tetroxide
J. Chem. Soc. , 1951 , 2833 - 2838
Part IX. Products, rates, and possible mechanisms of the reaction of zinc with liquid dinitrogen trioxide–tetroxide mixtures
J. Chem. Soc. , 1951 , 2838 - 2843
This whole series of papers related to N2O4 are cited here , if you have access _
www.sciencemadness.org/talk/viewthread.php?tid=19098&pag...
____________________________________
Ti(ClO4)4
As you point out produces 17.9 % solid ( TiO2 )
9 mols of gas and one mol of TiO2 or 10 %
LiClO4
produces just 14 % solid ( Li2O )
9 mols of gas and 2 mols of Li2O or 18.2 %
Zn(NO3)2 • 2N2O4
produces 21.8 % solid ( ZnO )
21 mols of gas and 2 mols of ZnO or 8.7 %
The density of the final pyrotechnic mixture will
also factor significantly in the performance derived.
.
[Edited on 16-6-2013 by franklyn] |
\
Are you sure Lithium Perchlorate decomposes to Li2O instead of LiCl ? , because wiki says LiCl. Which is 40% Solid.
I just checked some reported most did not state or stated LiCl.
Titanium perchlorate is some times dangerous with some types of liquid though.
[Edited on 16-6-2013 by DubaiAmateurRocketry]
[Edited on 16-6-2013 by DubaiAmateurRocketry]
[Edited on 16-6-2013 by DubaiAmateurRocketry]
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AndersHoveland
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I would suspect a mixture of byproducts is produced upon initial reaction. That is the problem with some of these energetic propellants, the
byproducts themselves can absorb energy or be slow to fully react and release all their energy. However, as the byproducts cool away from the initial
reaction zone, the end product would indeed tend to be LiCl, though below a certain activation temperature Li2O, Cl2, and H2O can no longer combine,
and I am sure some HCl manages to escape also.
The decomposition of some of these compounds is not always stoichiometric.
With magnesium perchlorate, I would expect much higher ratios of MgO to form, rather than the chloride.
I'm not saying let's go kill all the stupid people...I'm just saying lets remove all the warning labels and let the problem sort itself out.
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DubaiAmateurRocketry
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| Quote: Originally posted by AndersHoveland |
I would suspect a mixture of byproducts is produced upon initial reaction. That is the problem with some of these energetic propellants, the
byproducts themselves can absorb energy or be slow to fully react and release all their energy. However, as the byproducts cool away from the initial
reaction zone, the end product would indeed tend to be LiCl, though below a certain activation temperature Li2O, Cl2, and H2O can no longer combine,
and I am sure some HCl manages to escape also.
The decomposition of some of these compounds is not always stoichiometric.
With magnesium perchlorate, I would expect much higher ratios of MgO to form, rather than the chloride. |
Oh yes i do agree that LP does form some Li2O and decompositions are not really stoichiometric, but i was just trying to make sure the main product is
LiCl, although some traces of Li2O may be found.
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Fantasma4500
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this thread surely grew quickly haha...
98% is do-able infact, but i would only handle that in drop-amount treating it as liquid NI3, or in other words NCl3..
theres a video of anh. HClO4 reacting with paper tho
explodes on contact..
but i expected a much much higher price really..
octanitrocubane has a price that exceeds the price of gold per gramme before the 30% gold price drop just recently
now a 100g charge of that would be very expensive, despite that it exceeds 10000m/s VoD
in any possible way you wouldnt want this for rocket propellants anyways
with the price of this perchlorate, i suppose you want this as a catalyst more than main oxidizer..?
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franklyn
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You are right — too late to edit now though
I just assumed 4 LiClO4 => 2 Li2O + 7 O2 + 2 Cl2
It actually is LiClO4 => LiCl + 2 O2
produces 39.8 % solid ( LiCl )
2 mols of gas and 1 mols of LiCl or 33.3 %
The higher heat of formation determines the product
ΔfH solid LiCl = −409 kJ/mol
ΔfH solid Li2O = −300 kJ/mol
http://books.google.com/books?id=13sMAQAAIAAJ&pg=PA16&am...
Lithium: Theoretical Studies and Practical Applications
http://books.google.com/books/download/Lithium.pdf?id=13sMAQ...
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virgilius1979
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What would be the result of reaction between Ti(ClO4)4 and H2O ?
Because I was thinking at the first time one could synthesize Ti(ClO4) by electrolysing concentrated HClO4 with Ti electrodes.
a bit off topic question: Did anyone produced some AgClO4 ? Do you also need anhydrous HClO4 ?
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DraconicAcid
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| Quote: Originally posted by virgilius1979 | What would be the result of reaction between Ti(ClO4)4 and H2O ?
Because I was thinking at the first time one could synthesize Ti(ClO4) by electrolysing concentrated HClO4 with Ti electrodes. |
Probably TiO2 and HClO4. Perchlorate is a very poor ligand, and titanium is very oxophilic.
Please remember: "Filtrate" is not a verb.
Write up your lab reports the way your instructor wants them, not the way your ex-instructor wants them.
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DubaiAmateurRocketry
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| Quote: Originally posted by DraconicAcid | | Quote: Originally posted by virgilius1979 | What would be the result of reaction between Ti(ClO4)4 and H2O ?
Because I was thinking at the first time one could synthesize Ti(ClO4) by electrolysing concentrated HClO4 with Ti electrodes. |
Probably TiO2 and HClO4. Perchlorate is a very poor ligand, and titanium is very oxophilic. |
The link i gave already stated the best route to it.
TiCl4 and anhydrous HClO4, with few drops of Cl2O7, containing at least 2% of the solution, could help give a good yeild of TiCl4O16. Make more there
are 4 HClO4 at least for each TiClO4, and add some extra would be better.
Reaction must been done under -10 degree, a bit lower is ok.
Heating of TiCl4O16 releases large amounts of gas, could lead to explosions, although the decomposition is endothermic.
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AndersHoveland
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For those who are not aware of the dangers, anhydrous HClO4 is not stable in storage. In fact, if left in a jar it gradually decomposes, increasing in
temperature until there is a runaway decomposition and it finally explodes.
| Quote: | | Pure perchloric acid is unstable. If left standing at room temperature for between 10 and 30 days, at some point the temperature of the acid will
spontaneously rise to 90 °C, at which point there will be an explosion. |
72% perchloric acid is completely stable, however. It is just that the chemical properties of perchloric acid change markedly over 72% concentration.
We can think of this concentration threshold as actually being hydroxonium perchlorate, H3OClO4.
[Edited on 18-6-2013 by AndersHoveland]
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DubaiAmateurRocketry
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| Quote: Originally posted by AndersHoveland | For those who are not aware of the dangers, anhydrous HClO4 is not stable in storage. In fact, if left in a jar it gradually decomposes, increasing in
temperature until there is a runaway decomposition and it finally explodes.
| Quote: | | Pure perchloric acid is unstable. If left standing at room temperature for between 10 and 30 days, at some point the temperature of the acid will
spontaneously rise to 90 °C, at which point there will be an explosion. |
72% perchloric acid is completely stable, however. It is just that the chemical properties of perchloric acid change markedly over 72% concentration.
We can think of this concentration threshold as actually being hydroxonium perchlorate, H3OClO4.
[Edited on 18-6-2013 by AndersHoveland] |
Titanium perchlorate react with water, so it have to be prepared at temperature below -10 degree. -15 would guarantee no accidents, since that's how
the Russian team performed and synthesized it
Can you distillate water from 72% HClO4 ?
[Edited on 18-6-2013 by DubaiAmateurRocketry]
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woelen
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Please use full words and not slang like 'u' where you should put 'you'.
It makes u l00k l1ke a k3wl.
Back to topic, you cannot distill off the water from 72% HClO4. This is the azeotrope of perchloric acid with water and when you boil this liquid,
then water and acid escape in exactly a 28 to 72 ratio.
If you want to concentrate perchloric acid beyond 72%, then you need a strong drying agent to bind the water. Concentrated sulphuric acid in large
excess amount does the job. P4O10 also does the job. I, however, STRONGLY advice against trying this. Distilling anhydrous perchloric acid is insanely
dangerous and leads to violent explosions very easily. In professional labs this usually is not allowed at all, or if people need anhydrous perchloric
acid, then they have to work in pairs, using blast shields and personal protection gear. You cannot store anhydrous perchloric acid. It explodes after
appr. 1 month of storage if kept cool, it explodes earlier when kept at room temperature or when not entirely pure.
Acid at 72% concentration is the highest stuff which can be obtained commercially. Anything above 75% is dangerous to have around. It is really
remarkable to see how much the properties of perchloric acid change with increasing concentration. At 70% it is actually amazingly inert and not even
capable of oxidizing fairly strongly reducing stuff like Na2SO3 or KI, while anhydrous acid explodes on contact with nearly any reductor (e.g. dust,
people, animals, plants  ).
@AndersHoveland: The 72% acid is the azeotrope, it is not hydronium perchlorate. The 72% acid does not have some well-defined stoichiometry, it just
is a mix of water and acid. Hydronium perchlorate, H3O(+)/ClO4(-) is a solid and it contains appr. 85% by weight HClO4.
[Edited on 18-6-13 by woelen]
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watson.fawkes
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| Quote: Originally posted by woelen | | In professional labs this usually is not allowed at all, or if people need anhydrous perchloric acid, then they have to work in pairs, using blast
shields and personal protection gear. |
Not only that, there's a specific class of fume hoods for working with
perchloric acid. They have integral washdown systems on the interior walls.
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Nitro-esteban
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What would happen if titanium were reacted with 60% HClO4?
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woelen
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Titanium most likely does not react with 60% HClO4. Or, if it does, then I expect formation of purple titanium(III) ions in solution. On boiling down,
the titanium is oxidized by air and hydrous TiO2 will separate from the liquid.
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DubaiAmateurRocketry
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Guys I purchased the paper, here it is 
Page 1
[Edited on 21-6-2013 by DubaiAmateurRocketry]
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DubaiAmateurRocketry
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[Edited on 21-6-2013 by DubaiAmateurRocketry]
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