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Author: Subject: The trials & tribulations of Thorium production
j_sum1

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Mood: Metastable, and that's good enough.

Congratulations Dan. This has been a monumental effort and your results have been hard-won.

Is it my imagination or is your holding of that jar a posture of triumph?

I am looking forward to a write-up but in the meantime I must set aside some time to re-read this whole thread.
I presume the write-up will go in prepub?

Magpie
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Nice going Dan.

I know what you mean about some of these obsessions costing a lot of money. My autoclave construction comes to mind, ~$550. My homemade hood ran about$2000.

But it is sweet to be at a point in one's life when you have the option of taking on these projects. And the man hours? That's all just fun!

[Edited on 2-8-2016 by Magpie]

The single most important condition for a successful synthesis is good mixing - Nicodem
Dan Vizine
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After 3 re-suspensions in 1.5 L distilled water (fines decanted off include calcium hydroxide and very fine thorium particles)....

On to dilute nitric acid washes.

"All Your Children Are Poor Unfortunate Victims of Lies You Believe, a Plague Upon Your Ignorance that Keeps the Youth from the Truth They Deserve"...F. Zappa
Dan Vizine
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First wash with 1 L (Distilled H2O - HNO3) (8:1) shows a distinct darkening as residual Ca impurities are dissolved.

"All Your Children Are Poor Unfortunate Victims of Lies You Believe, a Plague Upon Your Ignorance that Keeps the Youth from the Truth They Deserve"...F. Zappa
Dan Vizine
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Subsequent washes, washing time, settling time before decantation

1.0 L DI H20 3 hours 10 min.
1.0 L (DI H2O - HNO3) (8:1) 8 hours 10 min.
6 x 1.0 L DI H2O 1 hour 5 minutes

Settling: https://www.dropbox.com/s/4khwojlye381a80/2016-08-03%2019.34...

Attached pics show final supernatant H2O and comparison of pH of this liquid and the virgin DI H2O. I can't see a difference. Final washes and drying tomorrow.

[Edited on 3-8-2016 by Dan Vizine]

"All Your Children Are Poor Unfortunate Victims of Lies You Believe, a Plague Upon Your Ignorance that Keeps the Youth from the Truth They Deserve"...F. Zappa
Dan Vizine
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THE PREPARATION OF PURE THORIUM METAL BY THE SYLVANIA PROCESS

1. Th(NO3)4 (H2O)4 + NH4OH ---> Th(OH)4 ------>ThO2

2. ThO2 + Ca ------> Th

Anhydrous thorium dioxide (1)

To a stirred, clarified, room-temperature solution of thorium nitrate tetrahydrate (227 g, 411 mmol) in distilled H2O (2.5 L) was added 28% aqueous NH3 (317 mL, 285 g, 4.60 mol) in one portion. The temperature of the resultant white slurry was found to rise slightly (~35 C). Stirring was continued under ambient conditions for 1.0 h and then the precipitate was collected by filtration and washed in succession with distilled H2O (3 x 500 mL), dilute aqueous NH3 (0.6 M, 5 x 500 ml) (note 1) and additional distilled H2O (5 x 500 mL) to give crude thorium hydroxide (note 2). The extremely bulky bright white solid was air-dried to give a dense, friable off-white solid of approximately 15 - 20% of its original volume. After drying to constant weight at 80 - 90 degrees C for 15 h, the solid was pulverized to give127 g (103 %, TY= 123 g) of a very heavy white powder. The excess weight is residual water and ammonium nitrate. Calcining in a 2 inch diameter Mullite tube, with one closed end and the other end vented to the atmosphere, was started. At about 400 C, a small amount of brown gas was seen, supporting the presence of a small amount of ammonium nitrate. The colored gas disappeared after 10 minutes and water vapor was noted to be evolving slowly . After a total of 12 hours at 1000 C, the material was recovered from the process tube and finely ground with a mortar and pestle. The resulting off-white, heavy powder was packaged under argon to give 108 g (99.5%, T.Y. = 108.5 g) of anhydrous thorium dioxide (1).

Thorium metal (2)

A full-penetration TIG-welded SS 309 reactor (2 in dia., 4 in long, 0.125 walls) fitted with machine-cut female1/2" NPT threads on the top surface was inerted with UHP argon and then charged with (1) (87.5 g, 331 mmol), anhydrous CaCl2 (35 g), and high-purity Ca (99.9%) filings (34.5 g, 861 mmol). The reactor was immediately closed (note 3) with a male 1/2" machine cut NPT threaded adapter that transitions to 1/4 " SS 304 pipe 10 inches long terminated with a SS 316 Swagelok valve. The reactor was supported at an angle of ~15 degrees off the vertical, inside of an electrically heated oven, and slowly rotated by the pipe/valve (note 4) which was attached to a SS 316 7 micron in-line filter and then to an axially mounted, new 00 rubber stopper. The rubber stopper was pierced down its axis by a silicone grease-lubricated syringe needle (4 in length, 14 gauge) which connected to a three-way valve which allowed for its routing to either a mechanical vacuum pump or UHP argon (supplied at a pressure of 5 inches Hg using a bubbler). In operation, the lubricated stopper revolves around the syringe needle creating a rotating gas-tight seal. The reactor valve was opened and a series of six evacuation/refill cycles was performed. The oven was heated to 950 C over an hour and stirred for an additional 5 hours under the UHP argon at 5 in. Hg. The heating was stopped, the reactor valve was closed and the reactor was separated from the upstream components and cooled. The reactor exhibited heavy scaling (note 5). After exterior cleaning and inspection the reactor was opened, fitted with a threaded-to-fit plastic funnel and put into a ice-water bath under an inverted acrylic dome (note 6). Water (~ 150 mL) was added, dropwise at first, to the reactor. The presence of unreacted calcium was confirmed by hissing and bubbling. After two hours, the reactor's contents were emptied into a large glass reactor (1 gal bottle). A rinse, close, shake, open and empty sequence was repeated 8 times on the reactor by which point inspection revealed it to be empty. The closed glass reactor's contents were mechanically stirred for 18 hours and then allowed to settle for 5 minutes. All suspended solids were then removed by decantation. A further 3 re-suspensions in 1.5 L distilled water, decanting off the suspended solids in-between, were performed. The solids were then stirred with 1 L (distilled H2O - HNO3) (8:1), recovered by decantation after 5 minutes, then the process was repeated with 1.0 L distilled H20 for 3 hours followed by a 10 min. settling, 1.0 L (distilled H2O - HNO3) (8:1) for 8 hours followed by a 10 min.settling, and finally with six identical 1.0 L distilled water washes for 1 hour with 5 minute settling periods. The final aqueous decantate had a pH identical to the original distilled H2O and was totally transparent and colorless. The solids were collected by filtration, washed in succession (under argon) with acetone (3 x 300 mL) and petroleum ether (30 - 60 degree) (3 x 300 mL) then dried to constant weight in vacuo for 18 hours to give (2) as a heavy gray powder (63.0 g, 82.0%, T.Y. = 76.8 g)

Notes

1. Prepared by dilution of 103 mL 28% aqueous NH3 to a volume of 2.5 L with distilled H2O.

2. The solid is also referred to as ThO2 dihydrate in some sources.

3. Vibra-TITE compound, nickel platelets in a graphitic base, rated for 2600 F service

4. The valve was connected to the hollow shaft of a stirring motor which was then attached to the in-line filter and 00 stopper.

5. A few grams of a material resembling gray stone was recovered from the furnace floor. Upon standing in 25 mL H2O overnight it disintegrated into a mixture of a white precipitate and gray flakes. The pH was quite basic. The postulated cause is a pin-hole leak at the reactor floor allowing a tiny amount of molten Ca/CaCl2 to push through it under the argon pressure and dislodge some of the scale from the reactor exterior. The utterly pristine, silver colored metal surfaces inside the cooled reactor are good evidence for no significant back-diffusion of oxygen.

6. A clear plastic waste basket about 1.5 feet tall and a foot in diameter with a 1/8" inch hole drilled in the center bottom.

[Edited on 6-8-2016 by Dan Vizine]

"All Your Children Are Poor Unfortunate Victims of Lies You Believe, a Plague Upon Your Ignorance that Keeps the Youth from the Truth They Deserve"...F. Zappa
Magpie
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Very nice work on such a challenging project.

1. What are machine cut NPT threads? Is this something you did or did you hire this out? In my experience it is next to impossible to get NPT threads gas tight. Why did you choose NPT? Wouldn't some type of fine thread be easier to seal. But since your reactor is vented anyway maybe this makes no difference?

2. What has been your experience with pin-hole leaks in stainless steel? Is this a common experience with 0.125" wall steel? Especially under low pressure (5" Hg).

The single most important condition for a successful synthesis is good mixing - Nicodem
Dan Vizine
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Bezaleel
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Congratulations, Dan! Great work in the engineering part in particular.
Do you plan to continue on a follow-up project of melting your Th into a single lump? (MP = 2023 K ​(1750 °C))

 Quote: Originally posted by Magpie Very nice work on such a challenging project. 1. What are machine cut NPT threads? Is this something you did or did you hire this out? In my experience it is next to impossible to get NPT threads gas tight. Why did you choose NPT? Wouldn't some type of fine thread be easier to seal. But since your reactor is vented anyway maybe this makes no difference? 2. What has been your experience with pin-hole leaks in stainless steel? Is this a common experience with 0.125" wall steel? Especially under low pressure (5" Hg).

I supposed Machine Cut as opposed to Die Cut. However, on pg. 7 Dan mentions Precision Cut as opposed to Rolled. Wouldn't even consider using a rolled thread for a purpose like this, so yes. Rolled threads are good when it comes to mechanical strength, but not when it comes to precision fitting, as required in this case.

One thing I wonder about is why no copper flange gasket has been used instead of a precision thread, but probably the operating temperature is too close to the melting point of copper (1084.62 °C per Wiki).
Dan Vizine
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Thanks Bezaleel.

Yes, you're right, Die-cut may be what the lower quality NPT threads are. I'm really no expert, but the threads on the LHS are visibly superior to those on the RHS.

The reason for not using flanges is as simple as cost. Precise flanges would require welds but then machining to eliminate warping caused by welding. Copper could have been usable at 950 C if thin stock was used.

There are so many things that COULD be done....
An inert-atmosphere furnace
Induction heating
Specialty crucibles like Mo (in inert atmospheres)

In any case, I think one metric by which we could say this was sufficiently protected is that the Th doesn't blacken in air readily. This usually signifies a purity in excess of 99%.

I cannot find an arc-furnace operator interested in contaminating his chamber with thorium. I obviously can melt it here, but not without destroying it in the process. That only leaves pressing as an option. That's a poor option with this powder, without real precision tooling, which I don't possess. Thus, the contamination possibility is unacceptable.

[Edited on 7-8-2016 by Dan Vizine]

"All Your Children Are Poor Unfortunate Victims of Lies You Believe, a Plague Upon Your Ignorance that Keeps the Youth from the Truth They Deserve"...F. Zappa
Dan Vizine
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The Dropbox link to the above-referenced clip has been deleted.

Instead, here is a Dropbox link to all of the sources, pictures and movies that I accumulated over the course of this project. It's over 300 MB. The link will be good for several months. Please download anything that you might want to save.

And this link is a chronological ordering of the most important pictures. Each picture is titled by a description of what it's about :

https://www.dropbox.com/sh/5mjwdsnm0mhs7r2/AABCONsCnSInHQRFD...

[Edited on 8-8-2016 by Dan Vizine]

"All Your Children Are Poor Unfortunate Victims of Lies You Believe, a Plague Upon Your Ignorance that Keeps the Youth from the Truth They Deserve"...F. Zappa
Dan Vizine
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Sometimes it's easy to overlook things you take for granted.

Say, for instance, the above calciothermic reaction. The temperature controller said that the furnace temp. was ~ 950 C. The color of the reactor says something different. It's yellow to my color-challenged eyes. This suggests why the pinhole leak make have happened. This steel was at 1200+ C and being pushed to its limits.

So, the placement of the thermocouple wasn't as good as it could have been. But perhaps that's part of the reason for the thorium having apparently very low ThO2 content (judging, again, from resistance to darkening in air).

"All Your Children Are Poor Unfortunate Victims of Lies You Believe, a Plague Upon Your Ignorance that Keeps the Youth from the Truth They Deserve"...F. Zappa
NEMO-Chemistry
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Finally a product that dosnt resemble crud!! Superb read and work!! A real challenge and some fabulous engineering.

I found the whole thread totally inspiring, not that i am ever likely to be good enough to even contemplate something like this, i think the mere fact it was done outside of a special laboratory makes it special.

Dunno how others feel or view it, but personally i think projects like this prove amateur science projects have a place still within society.

It shows even the most challenging projects can be done by in non professional settings safely, as long as the project is handled in a professional such as this one was.

Getting a thorium sample for a element collection is one thing, but to actually make a sample is on another level, congratulations! And yes i can finally see it , i was starting to think you was fobbing me off with green gunk lol
Dan Vizine
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The product is really rather beautiful after all the extensive washing. My greatest fear was that the powder would blacken readily, meaning that ThO2 was >1%. Because, if it's more than 1%, I have no way to say it's not %5. The powder is a light steel gray. Acid washing of ThO2-free samples is said to improve purity to 99.6 to 99.8%. I likely have several hundred ppm of both chromium and nickel.

"All Your Children Are Poor Unfortunate Victims of Lies You Believe, a Plague Upon Your Ignorance that Keeps the Youth from the Truth They Deserve"...F. Zappa
NEMO-Chemistry
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63! Only the good or very lazy chemists reach that age . So i guess you must be good.

Yes i have a way to go before i reach 'old age', although Darwin seems to be constantly on my shoulder .

I have started to read up on Marie Curie and others who first started to isolate such metals. Absolutely mind blowing what they did with what i would consider pretty primitive equipment!

Ok Curie paid the price but the work to process vast amounts of ore is mind blowing.

It might be my age but i still live in a bubble that says one day an amateur will discover something significant in his shed, i think without that i would view science differently and maybe loose interest.

But i am still at the nice stage where even the very simple is extremely exciting! Salt from sodium and chlorine reacted in a flask with sand on the bottom still fascinates me (welders mask etc ).

Manganese and changes in oxidation state still amaze me. I am not into big bangs as such, but i am developing an interest in flashes of different colour .

Over here things like that get you into alot of trouble, so my ventures with black powder using different oxidizer's is very very small scale and limited.

Loud bangs and blowing things up dosnt really interest me. The Thorium interests me because i am fascinated by cloud chambers and watching the decay process. But thats is all for when i am confident i can keep Darwin at bay.
Dan Vizine
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Interestingly, although Marie Curie witnessed the premature deaths of several workers in the nascent field of radioactivity, she never admitted that there was a direct connection. She never even acknowledged that there was a relationship between her work and her ultimately radiation-related (my words) death.

"All Your Children Are Poor Unfortunate Victims of Lies You Believe, a Plague Upon Your Ignorance that Keeps the Youth from the Truth They Deserve"...F. Zappa
Dan Vizine
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A final close-up.

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phlogiston
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Thanks a lot for sharing the inspiring and captivating story of making this! I can't tell you how much I enjoyed reading about your meticulous planning, problems, solutions and final success with us. Looking at the history of the element, it appears likely that you are the very first -amateur- scientist in the world to isolate this metal in the last century (if not ever, depending on whether you count well-to-do victorians). There ought to be an olympic medal or noble price for amateur chemistry, but alas.

Is the cleaning effort purely precautionary or have you actually detected some contamination?
From the perspective of an interested element collector: are you planning to recover some of the cost by selling some of the metal? (or make a well-deserved profit, I don't care about the financial details, just if you are planning to sell samples of it)

[Edited on 23-8-2016 by phlogiston]

-----
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j_sum1

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Mood: Metastable, and that's good enough.

I agree. This has been fascinating to watch. It has been a lot of hard work. Your excellent results are truly well-deserved.

 Quote: Originally posted by phlogiston From the perspective of an interested element collector: are you planning to recover some of the cost by selling some of the metal? (or make a well-deserved profit, I don't care about the financial details, just if you are planning to sell samples of it) [Edited on 23-8-2016 by phlogiston]

Actually, I think you deserve to keep every single hard-won microgram to yourself. You have bragging rights over Theo Gray on this one.
(Actually, now that I think about it, it wouldn't hurt to let him know what you have accomplished. I am certain he would be interested and probably enjoy a photo. For thorium, he might even pay a visit.)

But on the off-chance that you are in the sharing mood, I know I would pay good money for two or three sand-sized particles in an ampoule under argon or embedded in glass. I think for my element collection, having a miniscule sample would be testament to the extreme difficulty in obtaining the element.

Dan Vizine
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That's high praise, thank you!

An eBay seller forwarded me this NRC ruling...(he sells thorium compounds on eBay without too much trouble from his store or "firm")...

As my status as a "commercial firm", simply because I sell items on eBay, is not on firm ground, I won't be selling individual samples to anybody. I'm sorry, but I don't think I'm allowed to sell under these rules.

Ownership of this material was transferred last night to a bona fide commercial firm specializing in element samples. They pay to have it legally shipped to them. They can legally sell natural thorium for purely commercial purposes under the small quantities of source material "General License" rule. This is automatically granted simply by virtue of being one of the below groups, no application needed.

§ 40.22 Small quantities of source material.

(a) A general license is hereby issued authorizing commercial and industrial firms; research, educational, and medical institutions; and Federal, State, and local government agencies to receive, possess, use, and transfer uranium and thorium, in their natural isotopic concentrations and in the form of depleted uranium, for research, development, educational, commercial, or operational purposes in the following forms and quantities:

(1) No more than 1.5 kg (3.3 lb) of uranium and thorium in dispersible forms (e.g., gaseous, liquid, powder, etc.) at any one time.

It wasn't clear from the regulations if private individuals can even possess source materials other than a few specific items, U glass, U & Th ore, tritium signs, the usual suspects.

Once they have packaged it, I'll let the forum know here.

Again, several people expressed interest in samples and I apologize for promises I made before I knew the regulations.

"All Your Children Are Poor Unfortunate Victims of Lies You Believe, a Plague Upon Your Ignorance that Keeps the Youth from the Truth They Deserve"...F. Zappa
j_sum1

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Mood: Metastable, and that's good enough.

 Quote: Originally posted by Dan Vizine Ownership of this material was transferred last night to a bona fide commercial firm specializing in element samples.

Wait! does that mean you have done all of that work and not kept any for your own element collection??

I can't see that I would ever have done that. I am not saying I would do like Scrooge McDuck does with gold but -- I would at least admire my work for few weeks.

Dan Vizine
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No, I didn't. I kept 5 grams. Nobody will bother you for that. They just don't want private individuals selling it, I think most probably because it will be shipped improperly. But other factors come into play. Owners of "source material" may not abandon it. Ever. They must technically ship it in accordance with law to one of four long-term nuclear repositories and pay for disposal. This is the lowest level waste so all four sites accept it.

This law is obviously violated frequently. Dozens of us here have DU. A friend who was selling DU on eBay sent me this message:

I'd be very careful with selling this material on ebay. I'm not sure if I ever told you what happened to me when I was selling DU samples on ebay. A few years ago I was contacted through ebay from someone claiming to be from the MA department of public health radiation control program. They told me to cease all sales of DU. It was very unprofessional and I shrugged it off as someone harassing me on ebay. A few weeks later I got letter in the mail from the same place. It was a cease and desist letter stating that I had to delist all my DU samples. Apparently the NRC had saw them and tipped off the MA DPH radiation control. MA is an NRC agreement state which means they relinquish all regulatory requirements to the state. I took down my listings but they sent me another letter asking for the specs on my storage facility, leak testing, calibration data for my detection equipment, etc. I explained to them that I was just a private citizen at a residence and not a big company. They sent another letter saying that the matter was closed. It didn't end there though. About two months later I was paid a visit from two FBI agents! They started by saying that DU was some pretty serious stuff and asked what I was doing with it. I told them no, it's depleted you can't do much with it at all and I explained how I was selling small samples on ebay to collectors for educational purposes. They started asking me crazy questions like did I support terror, was I a member of isis, did I want to hurt US citizens. I swear it was like something from a movie! Long story short is that the MA DPH said that by selling DU on an online auction site, I can't guarantee that it will end up with someone properly licensed or properly stored. I never heard back from the FBI. They said they were just "checking up" on me because MA DPH was worried. I know ebay seller Hudaho was selling Th foil samples and he was harassed by ebay into taking them down as well. Anyway, just thought I'd warn you, I don't know what the laws are like in your state regarding stuff like that but I don't want anyone to have to go through what I went through. It was just so ridiculous and unbelievable! All over some tiny DU samples.

So, this arrived after the Th was done. I decided to try to do the most cooperative thing and that was get it out of my possession and keep everything within the legal boundaries.

Concerning an earlier question of thorough clean-up, here is part of the complete write-up. Since you can never say nothing is there (thickness of detector window deflects some alphas), it seemed prudent to re-paint the garage floor. What if a drop splashed that I didn't notice? I wet-mopped. The thing about alpha particles, you just need to immobilize trace amounts to make them safe. I didn't find floor areas above background levels but I'm not trained on the instrument. I used the most careful techniques that I could. I'm comfortable with it.

I can't see myself ever repeating this experiment because of the potential for official intervention. If they want to be unsympathetic, it can be a nasty gray area.

"All Your Children Are Poor Unfortunate Victims of Lies You Believe, a Plague Upon Your Ignorance that Keeps the Youth from the Truth They Deserve"...F. Zappa
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Mood: Metastable, and that's good enough.

Sounds like someone needs to learn what the word, "depleted" means.

I guess that is a reasonable outcome all things considered. And nice that you could get rid of all of your collectable waste in a straightforward fashion.

There is, as always, a double standard here. I can buy 2% thoriated welding rods OTC, burn them up in use, release unknown quantities of Th into the air (more rather than less knowing my welding), catch some in my respirator (or not!) and no one will bat an eyelid. I could even let the rods rust and have the Th enter the environment.

But you, because you are doing some actual science and concentrating the thorium are subject to all kinds of regulations regarding waste as well as the product formed. The safety standards you impose on yourself with respect to cleaning up alpha sources in your garage are far more rigorous than any imposed regulation, and yet for all that, you cannot be trusted to package and distribute in a responsible manner.

Such are the delights of red tape and a litigious society.

For my element collection I intend to buy a welding rod and maybe a lantern mantle (if I can find one). In the short term. In the long term I hope to have a tiny scrap of actual metal. But I won't be making it myself.

violet sin
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ya unfortunately it looks like you have invested time and effort in creating a road map that will be appealing to those FAR FAR FAR FAR less competent individuals that abound on the internet. Yet you, did all the learning, processing, clean-up in QUITE the respectable manner, and get shafted...

rules is rules, gotta respect them. just a darn shame. guess I am gonna have to make due with my welding rod and mantle for samples. been looking into some mineral specimens to round out the set. but there will be no chem experiments, refining or otherwise. beyond irresponsible with my income, lab space and location( not a whole hearted tragedy, just not a bright idea)

well you learned a lot, have an epic of a tale, bragging rights to the moon and a personal sample for your collection. So the half full side of the chalice is still looking pretty darn good. gotta stay positive thanks for a hell-ava journey

-=>}[ ⊙¥⊙ ]{<=- 15-23-12
NEMO-Chemistry
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Yeah the bragging rights and pictures are worth a shit load more than some grey powder. Plus if your hit by a bus (I hope not), then no one careless gets to handle it.

Shame you couldnt keep more but having said that, its probably better that way in the long run.

No one can argue you didnt do it, to me what you had to overcome to get it done and the pics of the steps are worth way way more.

I know your a professional but you were not in a multi million £ facility with a open ended budget! So it makes it really special.

I agree about the prize, there really should be some kind of prize for doing stuff like this. My favourite picture is the heat pic showing the hot spot. Every time i look at it i think 'damn that was trying hard to get out'.

SO whats next on the list? I dont see how you can stop now at Thorium . Honour dicates you have to top that lol . I am only goading you into another fabulous write up but i doubt your going to fall for it.
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