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Author: Subject: The Short Questions Thread (4)
Molecular Manipulations
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[*] posted on 31-5-2015 at 22:55


Quote: Originally posted by Brain&Force  
Will the use of a steel file impart any significant amount of steel contamination to the powder?
Certainly some, but for most purposes it's not a big deal. Run a magnet over the shaving to be sure.
xfusion, I've heated potassium nitrate above that temp before. No bang to speak of (hard to speak with one's face covered in molten oxdizers and glass shards [JK]). In large amounts and/or confined, I'd stay away.




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[*] posted on 1-6-2015 at 07:12
delta H/G for absorption of water by concentrated sulfuric



Does anyone know where to find quantitative data for enthalpy/free energy changes from absorption of water by sulfuric acid? This would be useful for predicting reactions such as

CH3CHOHCH3 <----> CH2=CHCH3 + H2O

in acidic media.

Edit: NIST has reaction energetics for both sulfuric acid and water. Calculations would need to take into account concentration and the exact ionic species involved, but the data is there.

[Edited on 6/1/2015 by Insanus]

[Edited on 6/1/2015 by Insanus]
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[*] posted on 3-6-2015 at 19:45


Does anyone know what diameter capillary tube I need to use for a theile tube/ non mel-temp machine melting point determination? I don't have a mel-temp machine so it has to be the older fashioned sample tied to a thermometer in a theile tube/ oil bath route..I'm stumped and I don't know if the diameter of the capillary tubing is important to the accuracy or not. I really appreciate any advice.



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[*] posted on 4-6-2015 at 02:06


Silica gel from cat litter
There are brands of cat litter claiming to be 100% silica gel (according to MSDS). However, not all of the crystals are clear -- there is perhaps 5% blue crystals in the mix. The label says that it is scented for some of the brands.

Does anyone have any experience with cat litter as a source for silica gel? It seems like it might be a useful thing to have on hand and rather cheap and simple to obtain.
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[*] posted on 4-6-2015 at 03:24


ok as a spill kit perhaps...




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[*] posted on 4-6-2015 at 17:10


@Funkerman23: diameter shouldn't matter much, as long as it is fairly thin. I was unaware that melting point capillaries even came in different diameters. I think the ones I use (also with a Thiel tube and thermometer) have an inner diameter of 1.0 mm.
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[*] posted on 4-6-2015 at 17:19


Quote: Originally posted by j_sum1  
Silica gel from cat litter
There are brands of cat litter claiming to be 100% silica gel (according to MSDS). However, not all of the crystals are clear -- there is perhaps 5% blue crystals in the mix. The label says that it is scented for some of the brands.

Does anyone have any experience with cat litter as a source for silica gel? It seems like it might be a useful thing to have on hand and rather cheap and simple to obtain.



Ali baba... $600.00 a ton.

The blue crystals you see may be the color indicator. WallMart sells it as a flower desiccant, and it turns blue as it absorbs moisture. It's about 5 bucks a pound there.

I never saw it in cat litter.




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[*] posted on 5-6-2015 at 05:52


Quote: Originally posted by blogfast25  
Quote: Originally posted by DraconicAcid  
It's chelated to make it sound more nutritious.


That won't work with chemophobes! :D

But wel with chemophages :D...

Just tell chemophobes that:
Proteins are polyaminoacids, polypeptides very similar to polyamide plastic...they wont eat anything but starch...
--> Starch is a polymer of glucose similar to cellophane and cellulose.
--> They die starving :D and Darwin wins :P




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[*] posted on 10-6-2015 at 12:13


When chlorinating solutions of, say, dyes, how necessary is it to absorb excess chlorine? I don't have a fume hood.



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Loptr
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[*] posted on 11-6-2015 at 09:32


Since potassium fluoride had a melting point around 858*C, can I assume that I can easily dehydrate the dihydrate to the anhydrous form without it decomposing?
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[*] posted on 11-6-2015 at 10:09


Quote: Originally posted by Loptr  
Since potassium fluoride had a melting point around 858*C, can I assume that I can easily dehydrate the dihydrate to the anhydrous form without it decomposing?


No. The dihydrate has an MP of only 41 C (Wiki). On melting it becomes a saturated solution of KF in water.

Heavily dissociated into K<sup>+</sup> and F<sup>-</sup>, the fluoride ions reacts with water, because HF is a weak acid (pK<sub>a</sub> = 3.17, Wiki):

F<sup>-</sup>(aq) + H<sub>2</sub>O(l) < === > HF(aq) + OH<sup>-</sup>(aq). Water soluble fluorides do indeed yield alkaline solutions.

Since as HF is volatile, on heating it will partially 'boil off'. You end up with KOH, or at least KF heavily contaminated with KOH.

[Edited on 11-6-2015 by blogfast25]




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[*] posted on 11-6-2015 at 10:18


Quote: Originally posted by blogfast25  
Quote: Originally posted by Loptr  
Since potassium fluoride had a melting point around 858*C, can I assume that I can easily dehydrate the dihydrate to the anhydrous form without it decomposing?


No. The dihydrate has an MP of only 41 C (Wiki). On melting it becomes a saturated solution of KF in water.

Heavily dissociated into K<sup>+</sup> and F<sup>-</sup>, the fluoride ions reacts with water, because HF is a weak acid (pK<sub>a</sub> = 3.17, Wiki):

F<sup>-</sup>(aq) + H<sub>2</sub>O(l) < === > HF(aq) + OH<sup>-</sup>(aq). Water soluble fluorides do indeed yield alkaline solutions.

Since as HF is volatile, on heating it will partially 'boil off'. You end up with KOH, or at least KF heavily contaminated with KOH.

[Edited on 11-6-2015 by blogfast25]


Yeah, that's what I was afraid of, and I don't feel like working with HF at this time.

Thanks blogfast!

[Edited on 11-6-2015 by Loptr]
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[*] posted on 21-6-2015 at 00:37


Quick question, just concentrated some 70% Nitric acid via distilling with 98% Sulphuric acid and continued until no more nitric came over. The sulphuric acid obviously has a large quantity of water in it now, is it fine to boil the water back off on heat so its reconcentrated for re-use again.

[Edited on 21-6-2015 by greenlight]
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[*] posted on 21-6-2015 at 19:03


At the very least, do it in a fume cub., as the dense vapours of the sulfuric acid will form on heating, and are rather unpleasent.



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[*] posted on 25-6-2015 at 17:29


closely related question :

How long (approx.) should it take for ~94% sulfuric acid to reach 98%? I think I tried once, and yes got nasty clouds of acid, but the concentration didn't change much. Seems like a lot of acid evaporates, not just the water?



[Edited on 26-6-2015 by learningChem]
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[*] posted on 25-6-2015 at 20:39


Try what I have been doing by just heating at 110-120.C in a beaker or other glass container on a hotplate instead of boiling the acid as well by heating strongly. This will boil the water which will evaporate off but leave the acid so no acid clouds.
You can put a watch glass or beaker bottom or anything that has a glass surface over the acid heating container to tell when all the water is gone (I use a glass saucepan with glass lid). If the glass surface becomes fogged up with condensation, there is still water in the acid. It will also tend to lightly fume white fumes when all the acid is nearly gone but these fumes will not fog up the glass.
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[*] posted on 26-6-2015 at 11:52


Thanks greenlight! I'll give your method a try. I was under the impression that, as the acid became more concentrated, more energy was needed to get rid of the remaining water, but experiment should clear this up =)
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[*] posted on 26-6-2015 at 20:40


I have used this method many times usually starting with clear 60% Sulphuric acid and afterwards it is much darker yellow and thicker and will char paper towel black on contact.
Just periodically check for water condensation and when none is visible let it heat for an additional 10 minutes to ensure good concentration
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[*] posted on 27-6-2015 at 03:53


Whats the best way to produce AlBr3 in a solvent? Mixing Al with bromine will form AlBr3 but the reaction is very exhotermic. In a solvent water or oxidation could be avoided as much as possible. I have doubts about what type of solvent would be adequate and what type of precaution should I take since the reaction is so exhothermic (which is what keeps me from just trying it).
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[*] posted on 27-6-2015 at 21:13


Quote: Originally posted by lenner  
Whats the best way to produce AlBr3 in a solvent? Mixing Al with bromine will form AlBr3 but the reaction is very exhotermic. In a solvent water or oxidation could be avoided as much as possible. I have doubts about what type of solvent would be adequate and what type of precaution should I take since the reaction is so exhothermic (which is what keeps me from just trying it).

I think Dichloromethane would be ideal here as it is non-flammable, bromine is miscible in it and does not react with bromine. Just use an ice bath and/or a reflux condensor to catch the inevitable DCM fumes.
Provided the reaction is spontaneous (It might not be) this should be a very safe way to do it, as the bromine will always be quite dilute. The only issue you might have is adding a whole bunch of bromine at the start and then having the reaction take off and boiling away all your DCM.
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[*] posted on 28-6-2015 at 00:30


Can mineral spirits (white spirit) go bad? I have (probably) pretty old can of it and it should be colourless, but mine seems to be a little bit brown/orange (maybe there's some rust in can, which causes that?) and it's also imposible to ignite it, but it should burn... I'm confused.

Thanks for answer




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[*] posted on 28-6-2015 at 12:50


Quote: Originally posted by Molecular Manipulations  
Quote: Originally posted by Brain&Force  
Will the use of a steel file impart any significant amount of steel contamination to the powder?
Certainly some, but for most purposes it's not a big deal. Run a magnet over the shaving to be sure.
xfusion, I've heated potassium nitrate above that temp before. No bang to speak of (hard to speak with one's face covered in molten oxdizers and glass shards [JK]). In large amounts and/or confined, I'd stay away.


Thanks :)




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[*] posted on 29-6-2015 at 11:07


lenner, see US patent 2975214 for preparation of AlBr3 in different solvents.

learningChem, concentrated sulfuric absorbs water from air as crazy. Some moisture guard is a must, the highest concentration I've obtained without using the protection is something like 92% in a receiver and 96% in a source pot.

greenlight, 98% sulfuric acid can be dehydrated above 300°C, 90% needs more than 270°C, 80% needs at least 210°C.
You need to make at least 50% sulfuric acid content in a resulting mixture (120°C dehydration temperature for H2SO4-H2O system) to leave no way for the nitric acid to come dilluted from the mixture. Of course, I'm supposing you have azeotropic or higher initial concentration of nitric acid.
http://www.qvf.com/qvf-process-systems/mineral-acids/concent...

[Edited on 29-6-2015 by byko3y]
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[*] posted on 6-7-2015 at 23:42


Thanks byko3y.

So I did a quick test. Heated a few mls of ~94% sulfuric acid in a small beaker. At ~120C white fumes can already be seen, but I don't think there's any water in them. I tried to condense the vapor on a piece of glass and didn't see any kind of droplets. I did see condensation/refluxing on the inside walls of the beaker, a few milimeters above the acid surface, but I suppose that's just acid (though it's a bit strange that the drops 'climb' the wall at that low temperature?).

Anyway, just as I originally thought, removing water from already concentrated acid does require a fair amount of heat/time? (apart from some sort of moisture guard)

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[*] posted on 10-7-2015 at 11:05


Quote: Originally posted by xfusion44  
Can mineral spirits (white spirit) go bad? I have (probably) pretty old can of it and it should be colourless, but mine seems to be a little bit brown/orange (maybe there's some rust in can, which causes that?) and it's also imposible to ignite it, but it should burn... I'm confused.

Thanks for answer

Red-orange stuff is probably rust, and it may not burn because it has collected a lot of water from the air over the years. Try distilling it and see how much water's in it. The distillate should definitely a-flame.




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