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Author: Subject: The trials & tribulations of Thorium production
careysub
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[*] posted on 20-1-2015 at 13:48


Quote: Originally posted by Dan Vizine  

Saudi Arabia has some of the most restrictive travel policies in the world, and advance visas are required for all foreigners desiring to enter............ Nationals of Israel and those with evidence of visiting Israel will be denied visas, although merely being Jewish in and of itself is not a disqualifying factor.[/color]

I don’t understand what this means. I’ll be coming from Israel. Which is very clear evidence of visiting Israel. But there are airlines that fly from Israel to Saudi Arabia, so I'm completely confused.


I don't believe there are any airlines flying direct between Israel and Saudi Arabia.

Muslims from Israel or Palestinian Territories wishing to go on Hajj must take buses to Jordan and fly from there.

In the past when people were travelling to Israel and then going to Saudi Arabia the Israelis would not stamp your passport as having entered Israel. Saudis might be able to infer that you had come through Israel, but without the stamp they could officially be ignorant.
Quote:
(Oh, and police officers often decide accident responsibilities and punishments at the scene).[/color] Getting pretty weird now.....

Public and private hospitals in Saudi Arabia, by law, do not admit foreigners even with health insurance and during a life threatening emergency. What?!! Are you kidding me? Now, it would seem they've crossed the line into institutionalized inhumanity.

All western joys are forbidden, except to the wealthy, who can flaunt the laws.


Saudi Arabia ranks almost at the very bottom of The Economist's ranking of totalitarian states, beaten only by North Korea (last I checked).

They've been good buddies of the U.S. though ever since, well, oil.

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Israel might be interesting if I were religious, and so it won't be in the slightest.


Not interested in history? Lots of it there - from prehistoric times, ancient civilization, to Medieval and later civilization.
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[*] posted on 20-1-2015 at 20:59


Quote: Originally posted by careysub  


Not interested in history? Lots of it there - from prehistoric times, ancient civilization, to Medieval and later civilization.


On the contrary, when I was in China and Belgium, the history was fascinating. And the buildings and everything were phenomenal from Brugge to Shanghai. I walked Chinese streets built in 1500 AD and climbed steeples in Brugge halfway to the sky. The history was overwhelming, being American and all.

In fact, since seeing Belgium, I've seen a life I'd rather have lived than being an American (well, after the 60's anyway, the 60's in the US was the single most exciting time and place to live in the world if you're of a particular persuasion). But the history of the area of the middle east that I'll be in...well, first word that pops into my mind is strife. You may be right, and it may have attractions but I just don't know of anything that I'm anxious to see there. I hope I'm surprised.


[Edited on 21-1-2015 by Dan Vizine]





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[*] posted on 21-1-2015 at 12:58


Quote: Originally posted by Dan Vizine  
You may be right, and it may have attractions but I just don't know of anything that I'm anxious to see there. I hope I'm surprised.


Some notable examples:
Jericho - the oldest continuously occupied city in the world (and one of the oldest, period).
Excellent Roman ruins in Caesarea, and Roman roads throughout Israel.
Crusader fortresses - Belvoir near the Sea of Galilee, Nimrod in the Golan (my favorite - spectacular view)
Jerusalem itself is a 3000 year old city, with excavated sites of interest spanning the entire period (the underground passage to the Siloam Spring dug 2800 years ago is impressive). Much impressive religious architecture of course, starting with the whole Temple Mountain (Mount Moriah). Impressive ancient tombs galore.
The Nabatean city of Avdat in the Negev (also spectacular).
Masada is very impressive - a palace/fortress of Herod I on top of a dramatic pinnacle, with the siege ramp built by the X Roman Legion still in place.
Lots of famous ancient battle sites.

Natural wonders: the Dead Sea (and whole Jordan Rift Valley); Makhtesh Ramon - a huge erosion crater, a landform apparently unique to Israel and the Sinai.
Bird watchers like Israel as it is a crucial migration corridor between Africa and northern Eurasia.

[Edited on 21-1-2015 by careysub]
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[*] posted on 22-1-2015 at 20:59


Well, if this is a typical trip, It's 18 hrs flying time and I won't sleep, I'll arive, get to Haifa, eat and sleep. Next day work into early evening, a few hours off, sleep, repeat 1X. Travel to Tel Aviv, have a few hours, pack, sleep and return in a %^&$* middle seat. My opportunities for sightseeing will be really limited. I didn't arrange any extra time. Sightseeing usually depends on if I go out drinking with the grad students (Bless you my Belgian Friends!) on most trips, when I go to industries, we never,ever end up partying after work.

I so hope the next long trip is to Europe or thereabout, we're putting units into Berlin (M. Braun's backyard...prolonged snicker), Sweden and another in Great Britain, but none of them ordered the installation package, me.

NOW...for the news. I found a young, highly skilled welder who has welded SS tanks for the pharma companies. He said a few days, $100. I'll finally have the reactor I need.





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[*] posted on 25-1-2015 at 14:25


And done.....

He asked for $150, took $130 instead of estimated ~$100 because he had to buy the wire and refill his argon tank. I kinda thought it was implied that he had this stuff when he took the job. I probably would have looked for another welder who would only charge for labor and the materials used, but we agreed to $130 and I thanked him. I pressure tested it. Perfect. He inerted the inside during the weld, gave a real clean product.

There's not much more to do except consider my newly acquired ability to do possible ball-milling of the ThO2. I have mixed feelings. It sounds good, I think the best way to avoid ThO2 contamination of the product, besides the obvious, is to minimize particle size. I just don't want my grinding media to end up in the product.

I'm getting excited about this, all of the real challenges have been addressed to the best of my [practical] abilities. Cost overruns have appeared from time to time. Investment is now around $800 but shouldn't go much higher.

And, I now I have a glovebox to handle the product powder in. Good stuff.

I'm just hoping people will be interested in powdered or room temp "pressure-sintered" forms. It's pretty much going to be the only stuff around, except for those very infrequent ebay offerings (the last one I saw was about 0.1 g for $200). Ridiculous. Fingers crossed.

Now, if I didn't have an appointment in Israel followed by Ga. again, it would be clear sailing. Stay tuned, it WILL happen...

SS 309 Reactor.JPG - 2MB

[Edited on 26-1-2015 by Dan Vizine]





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[*] posted on 26-1-2015 at 08:02


While I normally avoid powders, I'd make an exception here knowing the extreme time and effort you put into making this product. Sign me up for a sample when it's finally finished! Really great work here.
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[*] posted on 27-1-2015 at 12:40
Thorium from oxide


The most efficient method to produce thorium metal is reducing the thorium dioxide with combined powder of an alkali metal and an alkaline earth halide.
Thorium of a purity greater than 99 % by weight can be prepared by reacting thorium dioxide at 900-1000°C with calcium halide and alkali metal.
Optimal results can be obtained if these amounts are used, for every mole of thorium dioxide, at least 6 moles of calcium halide and at least 8 moles of alkali metal.
Following equation:
2 CaX2 + 4M +ThO2 → Th + 2CaO + 4 MX
2 CaCl2 + 4 Na + ThO2 → Th + 2 CaO + 4 NaCl
If reducing agents are used less than the above stated amounts, then usually the purity of the thorium falls to 90%.
Heat the mixture in an electric furnace temperature of 900-1000°C. Under a nobel gas atmosphere, let it react for 30 minutes, and turn off the heat and let it cool.
Then wash the mixture with 30% acetic acid with continuous stirring until bubbling stops, then filter it and wash the precipitate with alcohol and few times with hot water and filter it. Now you should have thorium powder, it should look like platinum powder.
The thorium powder should be stored in nobel gas atmosphere or melted to solid chunk because in it’s powder form it is pyrophoric.


Attachment: thorium dioxide reducion.pdf (134kB)
This file has been downloaded 225 times

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[*] posted on 27-1-2015 at 19:57


Thanks, analog. If you look earlier in the thread I'm following a method developed by Westinghouse for the AEC or whatever the acronym in use in the 40's was.

Your contribution looks great! If the few sentences that I read are really the case, this beats my existing prep. My Na is only 99% but the impurity is probably just other group 1 metals.

The boiling point of pure Na metal is 892 C.

The temp is marginally lower, the reaction time is markedly shorter. It complicates the hydrolysis step a lot, re. H2 liberated, possible dispersion of finely divided Th powder.

I don't see any particular reason that I couldn't start with 99% 2-PrOH, proceed to 70% 2-PrOH and then to water before proceeding to mild nitric acid washes, more water, more 99% PrOH, then acetone.

I tried for the melted chunks, VAR, but nobody is willing to contaminate their machine.

[Edited on 28-1-2015 by Dan Vizine]





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[*] posted on 27-1-2015 at 20:08


Quote: Originally posted by MrHomeScientist  
While I normally avoid powders, I'd make an exception here knowing the extreme time and effort you put into making this product. Sign me up for a sample when it's finally finished! Really great work here.

Ditto.
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[*] posted on 28-1-2015 at 18:12


Quote: Originally posted by anolog  
The most efficient method to produce thorium metal is reducing the thorium dioxide with combined powder of an alkali metal and an alkaline earth halide.....


entropy,

So, your very first post has turned out to be a real splash...It's potentially going to change the very nature of a project I started early last year.

I LOVE the idea of milling while reacting, and the high expected fluidity at temperature! The inclined configuration is genius. One way or another, that will be used.

I'm really fond of the possibly lower temperature range and of the potentially somewhat shorter reaction period.

But, I'm wary of the excess Na hydrolysis...it's about on par with my worries about trying to distill the sodium off first. That requires construction of another air-tight metal device.

I was already a bit concerned about just the simple calcium hydrolysis. Naturally, not about the hydrolysis itself, but because it combines lots of evolved gas with powdered alpha emitters. I guess that the alcohols will tame the rate. But, that's got it's own complications...

And finally, most chemists realize that while some patents are pretty good, some leave out crucial details and some are almost lies. This doesn't appear to probably one of the last two options. But you never know.

So many new things to ponder and a little math. Want to get j_sum1's sample right.



[Edited on 29-1-2015 by Dan Vizine]





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[*] posted on 31-1-2015 at 13:31


The preferred route leads to this overall transformation:

2.05 CaCl2 + 4.43Na + 0.411 ThO2 --> 0.411 Th + 0.822 CaO + 1.64 NaCl + 1.23CaCl2 + 2.79 Na

That includes 2.5 X the number of moles of CaCl2 and 2.7 X the number of moles of Na needed stoichiometrically.

The weights of reactants for my 108.5 g of ThO2are:
227.7g of CaCl2
101.9 g Na
for a total mass of roughly 438.1 g.

That leaves a metal/salt mixture containing 64.1 g of Na to hydrolyze while keeping the temperature and air-exposure low and controlling the particulate flow within that stream to avoid aerosols.

Physical removal of solidified reaction mixture from my vessel will essentially be impossible, meaning the "hydrolyze in place" technique needs to be used. The volume of potentially Th-laden hydrogen ought to be about a little over 30 L.

I could try to just distill the excess sodium off. It's about like distilling cesium except with different geometries for the "condenser".

But the main hitch to this is the volume of reactants and products. It really necessitates several runs. Since I anticipate that the reactor will be at or near its limits (per earlier discussion with rep from SS company), each re-run will require a lot of clean-up.

Yeah, I also know that I appear to want to violate the smart way to do things where you do scouting runs, identify your chosen method, then do scale-up. Truth is, I do want to violate it. That's why I've been trying to examine every avenue, every way it can fail, etc. I want to perform the reaction in, as close as I can come to, 1 time.

Also, because we're not talking about a complex, or simply expensive organic reactant, the Th isn't going anywhere if this reduction fails to live up to expectations. If the product isn't exactly what I want, the logical fall-back is to convert any thorium/thoria to the fluoride and go that route, or more likely, re-react it with more Na and calcium chloride.

So, minimizing exposure and producing the best quality product seem to be at odds with one another. Isn't that a shocker?

These issues in no way diminish my appreciation for the new posting. It's great, but how well I can adapt my available resources to it is uncertain.
Rotation of the tilted reactor is inspired*, although I do need to make a leak-tight gas swivel to apply argon to the end of the revolving tube from the reactor. My planned approach is to use a long, slender lubricated hypodermic needle piercing a rubber stopper along its axis.

Since it was mentioned a while back, my reactor has a volume of 11 cubic inches (about 180 mL to those of you almost anywhere else in the world who are not still mired in the English system).

* Almost all synthetic chemists look at unstirred reaction mixtures as being highly suspect, with good reason usually.

[Edited on 31-1-2015 by Dan Vizine]





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[*] posted on 20-5-2015 at 12:16


Well, I was relieved to note that the only reason that the Na method was used was economy. They just generated the Ca in situ because of the high cost of Ca metal. The reaction is still just the calciothermic reduction of the oxide. I may increase the molar proportion of Ca to improve the product.

Did you think I'd been swallowed by the earth? I was, in a way. That's what traveling constantly feels like.

So, I'm over budget and behind schedule. SNAFU in the literal sense.

But summer is here, outside work is possible and only two more trips (that I know of) stand between me and time for Th.

[Edited on 20-5-2015 by Dan Vizine]





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[*] posted on 20-5-2015 at 12:36


Still, good to have you back! :)



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[*] posted on 7-6-2015 at 16:13


Thanks....now....I'm in Wisconsin....so, that's another week.

Well, anyway it's set. The reaction will employ a larger than normal Ca/ThO2 ratio, in an inclined SS 309 reactor (~20 - 25 degrees from vertical) which will be slowly rotated, with a few large lumps of SS 309 in the mixture to stir it, for the required time at a minimum of 900 - 950 C under a 5 in Hg pressure of argon. The cooled reactor will be rigorously cleaned of scale and wire wheel brushed/ sanded to a clean metal surface in preparation for in in situ hydrolysis. The 1/4" pipe and the 1/4-to-1/2" adapter will be removed under argon. OK, here's where it becomes tricky. How best to do it?

As a first solution, I'm thinking this is glovebag work under argon with a respirator for good measure. But you know how glovebags never totally seal at the open end? I'll heat seal this open end shut along its entire length. This project has really boiled down to meeting one engineering problem after another. It's time consuming.





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[*] posted on 7-6-2015 at 18:23


Quote: Originally posted by Dan Vizine  
This project has really boiled down to meeting one engineering problem after another. It's time consuming.


This explains adequately why there's only one Dan Vizine! :D




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[*] posted on 2-7-2015 at 17:38


I think that sounded very complimentary, my friend, thanks! I have weeks of solid travel ahead (at least I'll get to check off another National Lab, Argonne, this time).

But, I've managed to spend some time redesigning the apparatus into it's final form. The scavenging of a discarded stirring motor spurred this. Now the reaction can truly be stirred. That warms and reassures me.

Now, this is just a mock-up to see if the stirring motor was up to the task, and it is. The final reaction set-up will be a bit more substantial and outside.


Thorium set-up.jpg - 231kB

[Edited on 3-7-2015 by Dan Vizine]





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[*] posted on 2-7-2015 at 18:47


Lookin' good. Can't wait for the final push...



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[*] posted on 10-8-2015 at 17:37


OK....I'm on vacation, after traveling most of the friggin' summer.

Time for this to come together. Proof of my sincerity is evidenced by the fact that I lugged that #&^%$*165 pound tank up 11 cellar stairs with no railings and followed that up with the vacuum pump. The second picture shows the rotating vacuum/gas seal I devised. It's a 2-way valve arranged to deliver either vacuum or argon to the reactor through a syringe needle inserted down the central axis of a rubber stopper and lubricated with silicone oil.

Just need final leak testing, a possible dummy reaction with a SS reactor containing molten calcium (would hate to have intragranular attack, failure, and an ensuing Ca fire loaded with Th), whipping up a 5 in Hg bubbler and this can start.

2015-08-10 21.20.30.jpg - 887kB2015-08-10 21.20.56.jpg - 803kB





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[*] posted on 10-8-2015 at 17:58


I can't wait!
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[*] posted on 10-8-2015 at 18:01


Quote: Originally posted by j_sum1  
I can't wait!


Totally seconded.




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[*] posted on 20-9-2015 at 11:27


Well, the dummy reaction with only 20 g Ca and 20 g CaCl2 in a 304 SS bomb is currently stirring at 950 - 960 C. After an hour or so, I'll cool the reactor and see just exactly what to expect during hydrolysis.

This gave me a chance to see what, if anything, is problematic before the real thing.

Incidentally, I solved the "time" issue which has kept me out of circulation so much. I gave 6 months notice this week. Plenty of time for them to find a replacement and have me train that person. I'm done with the soul-crushing grind.

2015-09-20 15.17.53.jpg - 2.3MB

[Edited on 20-9-2015 by Dan Vizine]





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[*] posted on 20-9-2015 at 14:23


The trial reaction was largely uneventful, it revealed one weakness in the setup which was solved by a small piece of silica board.

The pictures show how the SS 304 reactor fared both immediately post-reaction and after clean-up with a 7" SS wire wheel. Not bad, actually, better than I expected.

I'll try the hydrolysis of the Ca/CaO/CaCl2 mixture as soon as I get a chance. It will be interesting to see how easily the top threads unscrew, perhaps giving some indication of the gas-tightness at elevated temperatures.

post reaction.jpg - 1.3MBcleaned.jpg - 824kB





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[*] posted on 20-9-2015 at 14:36


Quote: Originally posted by Dan Vizine  
I'm done with the soul-crushing grind.





Self-employment or massive lottery win?




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[*] posted on 20-9-2015 at 15:42


Combination of many factors.
I'm old enough, I'll be 63 in a couple months.
Our mortgage will be paid off in 8 months, yearly expenditures drop by $8-9 k.
Three of my closest friends for >40 years have died within the past year. That can focus your values and choices quite profoundly.
I can just make and sell whatever I want (tax free up to, like, $15k). If I sell $6k per year, on top of SS, I'll have the same income as now, but with the mortgage thing, lower bills. I'll enjoy what I do, have time, which is much more valuable than money, and have no boss but myself.

A true no-brainer. My job currently has no end, it consumes all my time. I'm often still answering e-mails at midnight. No, thanks. Not for me.

[Edited on 20-9-2015 by Dan Vizine]





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[*] posted on 22-9-2015 at 07:33


I've been giving some thought to the "hydrolysis in place" step, which is next. My original plan was cleaning the reactor, post reaction, placing in a large beaker and surrounding by and eventually submerging under ice-water. This has all kinds of obvious down sides and it's abandoned.

I'm now thinking of a deep plastic funnel (or similar) adapted to screw into the reactor. The reactor can still be ice-cooled. and by adding an exhaust line to the upper wall of the funnel and a lid, I should keep mist from carrying off too many fine suspended particles. Perhaps a HEPA filter in the funnel lid? I'd love to find a consumer product which could be repurposed for this part.

This is actually where things become tricky, all the solution processing. This is also where I considered buying a Geiger counter. Units start at a hundred or two. The problem is that they aren't all that good for alpha particles. Counters that are really good for alpha particles have large, special detectors and the units are typically $1500 to $2000. So, back to relying on favorable engineering, I guess.

I suppose equipping my respirators with HEPA filters would be in order, too.

[Edited on 22-9-2015 by Dan Vizine]





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