Sciencemadness Discussion Board

The Problem with SynthSource

Praxichys - 27-4-2017 at 05:48

Hi everyone,

In lieu of dredging up an old thread where we breathed life into SynthSource over a year ago, I have some announcements of changes/revitalization.

Many of you have noticed that the domain has been broken for quite a while; this is because proboards decided that being forwarded to from a custom domain should be a paid service. Not willing to fork over $14 per month (in addition to the domain registration), and considering the relatively small amount of traffic, the website has sat defunct for some time.

I've recently come into a massive bulk buy (no joke, over 3 metric tons of something secret, exciting, and inexpensive) and I will be making all the transactions through SynthSource, which will go to support full functionality of the site for the foreseeable future.

Of course, all discussions regarding the chemical uses of such things is reserved for ScienceMadness; SynthSource is only designed to act as a firewall to protect SM in the event legal action is taken against a site engaging in this potentially risky endeavor.

In the interim, http://synthsource.proboards.com/ can be used to get to SS, and I will be updating my signature to reflect that.

Texium - 27-4-2017 at 06:01

3 metric tons! How are you going to sell all of that to SM members? Either way, I await with anticipation.

Dr.Bob - 27-4-2017 at 07:07

3 tons, I have more books than that already. I hope you found something more exciting than that. Good luck.

Praxichys - 27-4-2017 at 08:36

Haha, thanks. It's not books!

I'll give some hints: There are 7 varieties, it's packed in 31 fiber drums, and I'm getting it shipped to MI as surplus from a nuclear power plant in Tennessee. It's not classified as hazardous or radioactive, however some of the varieties have nonradioactive singular isotopes involved. Some of these varieties are very expensive to purchase directly from a supplier, however I managed to pick all of it up for rather cheaper, and I can certainly repack it in such a way that everyone can afford a few pounds.

Many labs can benefit from having this around, and certainly a good number of labs already use this in some form or another to do a very important job. Of course, in the nuclear industry, the job this stuff performs is rather more critical, so the varieties I have are either of extreme purity, high effectiveness, or are monoisotopic.

Can anyone guess what it is?

Magpie - 27-4-2017 at 09:36

Boron, lead, cadmium

TheNerdyFarmer - 27-4-2017 at 09:45

Is it potassium permanganate? Or possibly a dichromate salt?

Melgar - 27-4-2017 at 10:46

Sodium metal? From one of those old breeder reactors that ended up not being designed so well?

[Edited on 4/27/17 by Melgar]

PirateDocBrown - 27-4-2017 at 10:52

Lithium 6 or 7? Or just heavy water?

Amos - 27-4-2017 at 10:56

Quote: Originally posted by Melgar  
Sodium metal? From one of those old breeder reactors that ended up not being designed so well?

[Edited on 4/27/17 by Melgar]


Somehow I feel as though an individual can't just purchase 3 metric tons of elemental sodium from a nuclear company, but here's to hoping! But then again, it would definitely be qualified as hazardous, and there aren't multiple stable isotopes.

[Edited on 4-27-2017 by Amos]

Praxichys - 27-4-2017 at 11:04

Some more clues:

It's not a singular element, nor does it contain any transition metals. A halogen is involved in one of the versions, and Lithium-7 in another. Some are air-sensitive and all of them are shipped wet.

Cryolite. - 27-4-2017 at 11:35

FLiBe?

Melgar - 27-4-2017 at 12:02

Quote: Originally posted by Amos  
Somehow I feel as though an individual can't just purchase 3 metric tons of elemental sodium from a nuclear company, but here's to hoping! But then again, it would definitely be qualified as hazardous, and there aren't multiple stable isotopes.

At first I guessed "heavy water", but that's not really useful in a lab. And as far as what he was talking about, I was guessing that the category might be "alkali metals" and the single variety he had was sodium.

Maybe something a little broader like "deuterated solvents" or "solvents without any light hydrogen in them, that are suitable for proton NMR" though? Although the lithium clue kind of makes that untenable.

TheNerdyFarmer - 27-4-2017 at 12:52

Is it something like lithium fluoride for liquid fluoride nuclear reactors? As well as lithium hydroxide to basify the coolant in a pressurized water reactor.



[Edited on 27-4-2017 by TheNerdyFarmer]

XeonTheMGPony - 27-4-2017 at 16:32

I'll say flourienart from 3M or how ever it is spelt

Praxichys - 28-4-2017 at 07:06

All right, since nobody is getting it, I'll spill the beans.

It's ion exchange resin!

Kiss water distillation goodbye because you can make your own water deionizing system for super cheap. Forget eBay resin prices... I got this stuff at a steal.

I also have specialized strong acid and base resins. The strong acid resin is so good that you can run a salt solution through it and get 28% HCl out the other end. You can probably make 20% nitric straight from KNO3, distillation not required! (videos pending) Want HCN or HN3 but don't want to put your life on the line distilling it? Use resin!

Need aqueous ammonia? No problem, just shake some ammonium sulfate fertilizer solution with some of the strong base resin and BOOM. Done. Freebasing methylamine? No problem. And the best part about all of this is that the resin is totally regenerable. (I will supply the information from the manufacturer about exactly how to do this, although the stuff is so cheap that you might as well just toss it)

I also have some awesome specialty resins. I have chloride-loaded strong anion exchange resin which actually has applications in organic synthesis. I have lithium-7 loaded resin specifically designed to strip radioisotopes from the cooling loops of pressurized water reactors, which could help purify your drinking water in a nuclear emergency. Or, you could wash the lithium right out of it and make yourself a sample of Li-7, which goes for $10,000/kg. Your call. I have antimony and bismuth-chelating resin which has high selectivity for certain metals and may have applications in the purification metals and salts.

Anyway, I'm getting info packets put together about the care and feeding of such resins. I expect that for SM members I will be able to get this out the door as low as $5 per kg depending on the type. Stay tuned!

elementcollector1 - 28-4-2017 at 07:19

Quick question about the acid-generating resins: How long of a life do they have? As in, can they do that indefinitely?

Amos - 28-4-2017 at 07:54

Quote: Originally posted by elementcollector1  
Quick question about the acid-generating resins: How long of a life do they have? As in, can they do that indefinitely?


And how picky are they about the source of H+ during regeneration?

Magpie - 28-4-2017 at 08:19

Quote: Originally posted by Praxichys  

It's ion exchange resin!

Anyway, I'm getting info packets put together about the care and feeding of such resins. I expect that for SM members I will be able to get this out the door as low as $5 per kg depending on the type. Stay tuned!


This is awesome!

Praxichys - 28-4-2017 at 08:41

@elementcollector1

Pretty much. They need to be regenerated with a stronger acid though. So, you'd use the resin to make HNO3, and then regenerate it with concentrated HCl or something like that. Usually you can't make HNO3 from a nitrate salt and HCl, but with the resin it is possible. It's nice because HCl is usually super cheap, and you don't have to do any distillation as long as you don't mind a bit of residual KNO3 in your acid. Although, you could essentially eliminate all the KNO3 if you used enough of an excess of resin.

The number of cycles varies by application, and production of acids is probably one of the harshest things you can do to the resin. I'm just guessing here but considering standard resins can be regenerated a few thousand times, I'd estimate you'd get at least 50 or 100 cycles. At $5/kg-ish, you're not going to find a way to get that much HNO3 any cheaper.

Here is some tech data for Amberlite IRN77: http://www.lenntech.com/Data-sheets/Amberlite-IRN-77-L.pdf

At 1.9eq/L, you'd need a liter of wet resin to make 1.9 mol of HNO3, or 119g. To make a liter of 68% nitric, you would mix KNO3 and 5.7 liters of resin into a bucket, slosh it around, and let it sit overnight. After that, strain the resin and rinse with a minimum of distilled water. The resin has about 35-40% recoverable water around it, so once drained you'd now have 2.3 liters of 29.5% acid plus whatever wash water you used, so probably 15-20%. (It would be easier to do this with a column for obvious reasons, if you have one) You can just boil this until the vapor reaches the azeotrope temp, at which point you have a liter of 68% nitric minus some vapor losses, with maybe a percent or two KNO3 mixed in. (Using excess resin will help with this)

The regeneration process is about the same, but you'd just be washing the resin in strong HCl and then washing the KCl solution out of it with water.

Also, the stronger the acid, the less conversion you will have. I doubt, for instance, that you could reliably make HBr this way, but HF is probably not a problem. Check out this PKa chart: http://www.ochemonline.com/PKa_data If it needs HCl to regenerate, it probably has a similar effective PKa, which means excellent conversion percentages to most other common acids.


@Amos - It will depend on the resin. Once the drums get to MI, I will be able to pull the manufacturer specs and recommendations for use and regeneration. I know classifications and brands, but I will not know actual part numbers until I have them on-hand. There are lots of factors to be considered like resin swelling and osmotic shock. I will be developing methods for amateur use.

[Edited on 28-4-2017 by Praxichys]

JJay - 28-4-2017 at 08:42

Definitely very cool. I've read a lot of posts over the years suggesting ion exchange resins, and I've always been a little baffled as to where to obtain them, what kind to get, and how to use them.

Sulaiman - 28-4-2017 at 09:00

Definitely interesting.
Do you think that you may be able to ship internationally ? (UK specifically)
If so, I would like some sort of sample kit, a usable ammount of each type, and greater quantity for DI water generation.

Over my three years of this hobby, I have purchased an equivalent 600 ml/day,
so I'd like something like 1 to 2 litres per day continuously,
could someone advise how much resin I would need ?

The idea of strong acid and base resins able to geberate such useful reagents on demand is exciting !

CharlieA - 28-4-2017 at 11:37

The amount of resins needed depends in great part upon the quality of the water you start with. You could probably make an estimate by knowing the TDS (total dissolved solids) and their nature of your source water.


[Edited on 4-29-2017 by CharlieA] If I could type I would be dangerous.

[Edited on 4-29-2017 by CharlieA]

CharlieA - 28-4-2017 at 11:41

Praxichys: I am probably in the market for some of each (cation and anion exchange resins).

Loptr - 28-4-2017 at 11:53

I will definitely be getting in on this one.

Very nice!

Melgar - 28-4-2017 at 12:00

I seem to recall a thread on one of those sites that's archived on Erowid, where someone ground up some pills, dissolved them in a large amount of distilled water, let the insoluble stuff settle out, then filtered the rest and ran it through an acidified ion exchange resin. Yields of the amine salt were nearly quantitative. This might be useful for anyone attempting to isolate a useful monoamine reagent from some OTC dietary supplement. You can run as much solution as you want to through it, to rinse it off, and as long as it doesn't form ions, it won't rinse off any of the ions already there.

Of course, this dashes my hopes to sell my five pounds of strong-acid ion exchange resin to users here. :(

Texium - 29-4-2017 at 05:47

Ha! Doug made the ion-exchange resin market crash.

XeonTheMGPony - 30-4-2017 at 05:33

my water is hideous would love to buy 5 gallons of water DI resin! be easy enough to make a recirculating batch purifier system to make pure water at 250gal a shot!

j_sum1 - 30-4-2017 at 05:38

I'd need to learn how to use these but I would definitely be in for a decent amount to deionise some water -- enough to make international shipping worthwhile.

XeonTheMGPony - 30-4-2017 at 06:27

It is pretty easy to make a DI system, and I prefer the batch system to thoroughly clean it up Vs an open flow system.

The Volatile Chemist - 30-4-2017 at 11:02

Wow. Very cool. As others have said, I will definitely be 'in on this'...

TheNerdyFarmer - 30-4-2017 at 17:00

Can't wait until they are up for sale. And now we wait in excitement.

Dr.Bob - 1-5-2017 at 05:54

Neat, I have used a few of them, it is a broad area, but some of those are pretty specific uses. It will be nice to see a list once you get them all.

Praxichys - 3-5-2017 at 11:22

All right, the resin has arrived!

I have the following:

- Purolite NRW 3560Li7
- Purolite NRW 3560
- Purolite NRW 5010
- Purolite NRW 160Li7
- Energy Solutions CN100 (I think this is Chelex-100, hydroxide form)
- Dowex 550A

And also one more, but it's stacked so deep into the storage unit that I need to pull out a bunch of drums to get at it, so I'm going to wait!

All of them are a few months past their expiration dates, which explains why I was able to secure $50k worth of resin for a small fraction of that price. The expiration doesn't really mean a whole lot considering that's when they lose their certification to successfully treat nuclear waste, which requires very strict performance requirements from the resin. Tests are pending to ensure activity on the older samples.

Unfortunately there are no isolated samples of strong cation resin. The Purolite NRW 3560 is the only version that has any cation resin at all, and it is mixed with the anion. The industry standard for regeneration on this type involves a carefully prepared solution of NaCl which causes one type to float and the other to sink, so I believe it is possible to hack it DIY-style. Regardless, this is the one you want for building your own DI water system, and happens to be one of the most abundant resins I have, so it will be dirt cheap.

I'm working on an inventory and a SM-specific price list. I may also offer a full purchase refund to anyone willing to make a Youtube video with the resin that helps me get all of this out the door. I can already think of a myriad of things I can do with this stuff, and the list on the way.

Quick pic:
https://drive.google.com/open?id=0B_16NzkNoL75Vm96QnlKMHIyZl...

If anybody has some suggested uses, post them below and I will add them to the list, and I might be able to send you some samples to try it on!

TheNerdyFarmer - 3-5-2017 at 12:34

Are you gonna record your experiments if they are a success? I have a slight feeling some people would like to see more vids from you. Especially on something as different as this.

Cryolite. - 3-5-2017 at 13:11

It's a shame that these resins aren't Li-6 enriched... owning a solid sample of Li-6 carbonate would be really cool.

Praxichys - 4-5-2017 at 04:30

Why Li-6 and not Li-7? They are both stable isotopes. Li-6 is the rarer of the two by something like 16x but it's susceptible to neutron capture so it cannot be used for radwaste treatment. Hence, the resin is loaded with Li-7, which is still something like $10,000/kg to produce.

Cryolite. - 4-5-2017 at 07:49

Lithium 6 is the isotope of lithium found in hydrogen bombs. I wanted some specifically because it was the rare isotope, and because it has this application so far removed from its chemistry.

TheNerdyFarmer - 18-5-2017 at 09:52

Any update on how this stuff works or when you will post it for sale?

Cryolite. - 20-6-2017 at 13:52

Still no updates on when this will go up for sale?

Praxichys - 21-6-2017 at 05:43

It's coming, I promise. The resin is sitting in my storage unit at the moment. I had to make an emergency 2-week trip to Mexico for work and I've been back for four days. The containers are on their way and I should have it up for sale this weekend.

Thanks for hanging in there!

Dr.Bob - 22-6-2017 at 12:44

I understand your challenge, trying to do this type of work, along with a day job and family issues is often a bigger challenge that you would think. Good luck on the sales.

TheNerdyFarmer - 24-7-2017 at 08:14

Any update on this?