shady shady biz

[flenser]

What is your specific procedure? Are you filtering hormone dissolved solvent solution?

No, I'm recrystallizing using mixed solvents: methanol and cold water. It works well, but while they are wet the crystals are more like glue than powder.

It doesn't pass through the filter with the rest of the solution. I use about 5psi vacuum on the filter, or it would take forever to drain. Quite a bit of it sticks to beaker. When it dries, scrape it off the beaker and the filter, crunch it up and it looks like test e raws again.

 

[iintensity]

How many times did you recrystallize? What was your final yeild?

My concern is what the starting purity of the powder actually is. Meaning is the testosterone itself an impurity due to the majority of the substance serving as a filler?

I can do this project and send it out for testing myself. I'm just not certain on the exact analysis that should be preformed and don't want to waste $300.

My friend says LC/MS is the proper method, he gave me some long drawn out reason that I didn't fully understand. He pretty much said he believes the majority of the impurities would most likely be of a related substance very close but not identical to the compound. This can show as a pure substance with a seperation method such as cromatography but highly impure with LC/MS.

If you know the exact analysis that should be used let me know.

 

[swim15]

Ive got a connection for legitimate testing. That said its $400 a sample and not always available. Im going to have a sample tested at the next time available using LC/MS and that should show everything...which will give me and idea if its, say, a 70% pure sample because there are lots of related substances (other hormones that are byproducts or just did not make it to target hormone) or if there are actual contaminants in the raw.

Not sure about the hormones but if there are specific contaminants, then it will be much easier to figure out what is soluble with what and go about the purifying process. Hope to be able to have something to go off of in the next 2-3 weeks.

 

[flenser]

How many times did you recrystallize? What was your final yeild?

My concern is what the starting purity of the powder actually is. Meaning is the testosterone itself an impurity due to the majority of the substance serving as a filler?

I can do this project and send it out for testing myself. I'm just not certain on the exact analysis that should be preformed and don't want to waste $300.

My friend says LC/MS is the proper method, he gave me some long drawn out reason that I didn't fully understand. He pretty much said he believes the majority of the impurities would most likely be of a related substance very close but not identical to the compound. This can show as a pure substance with a seperation method such as cromatography but highly impure with LC/MS.

If you know the exact analysis that should be used let me know.

I've only done it once. I need to get more raws before I try it again. But then I will recrystallize the same material twice. The difference between what is lost the first time and what is lost the second should be a reasonable measure of what impurities are removed. At least that's the theory...

I do plan on testing the raws before and after recrystallization. That's assuming there IS a difference in what's recovered the second time. Otherwise I will assume it's not effective and look for different extraction methods.

 

[devildog93]

Just wanted to bump this info. up so that we might have a bit more input on things. I really do think this is going to be a good way to go for some of us.

I wonder if this is something Basskiller has experimented with as well. Anyone ever run into him on other boards?

 

[flenser]

I have plans for additional extraction methods, but I am currently stalled because I lack the means to test my results. Hopefully, Capt. Forest's lab will produce reliable output.

 

[devildog93]

Ok Flenser, i came across this today and was wondering if this was what you had originally tried:

Courtesy of Overburdened.





I've removed lye after removing esters from test prop.... this wont work here, but I think, as long as you are willing to lose up to 10% of your product by 'washing' it, you could do this:

**dissolve the test e in the least amt of methanol you can(you can get pure methanol heet(gas line anti-freeze)the yellow bottle)
**add 1 teaspoon per 10g of test e, of backing soda(sodium bicarbonate)
**swirl , you may have a little test e come out of solution, if you do, add enough more methanol to redissolve all of it.
**let it sit a few min, then swirl again, repeat about 5 times
**run the solution through a double coffee filter. you should have ALL THE baking soda out of the methanol/test e solution.

**you need to get a big jar, using COLD DISTILLED WATER, add to the methanol/test solution(this will precipitate the test out of the methanol, you should have a PURE product precipitating out)

**Keep adding COLD(this water should be ice cold!)distilled water till all of your test precipitates out. then you will run the first time with a single coffee filter. then run the solution again through double coffee filter. let the test dry completely(the methanol will evaporate completely.), the water will take at least 24 hours in a warm(75-78 degrees(you don't want the enanth to melt) place....

 

[hotdog23]

Bump. This is a good thread.

If someone be kinda enough to school me -

What advantages does the extraction hold over a water wash? Both are removing water soluble impurities right?

 

[fightingfires]

Hotdog...I think someone mentioned that a straight water was only removes water soluble impurities from the surface from each grain, while the majority is held within the crystal. Solvent water extraction gets out a larger percentage of water impurities

 

[iintensity]

Bump. This is a good thread.

If someone be kinda enough to school me -

What advantages does the extraction hold over a water wash? Both are removing water soluble impurities right?

That will work fine if you know the impurities are water soluble.

The above is called recrystallization. The impurities will be dissolved in the solution leaving the desired compound behind.

I'm not sure how useful what described above is because I don't know what the impurities are.

 

[dredd09]

That's why doing both polar and nonpolar filtrations are necessary. That way you at least get rid of water soluble and solvent soluble contaminates . First i would dissolve the good stuff with an appropriate solvent and filter. Then i would go polar, with dihydrogen monoxide , or MEOH .

 

[hotdog23]

Hotdog...I think someone mentioned that a straight water was only removes water soluble impurities from the surface from each grain, while the majority is held within the crystal. Solvent water extraction gets out a larger percentage of water impurities

Ohh k, much more effective and worth the time then

That will work fine if you know the impurities are water soluble.

The above is called recrystallization. The impurities will be dissolved in the solution leaving the desired compound behind.

I'm not sure how useful what described above is because I don't know what the impurities are.

Ya we really need quantitative analysis on the yield, this is a discussion that should be pursued.

To make some contribution to this thread. If you store methanol hormone solution in heavy duty ziplock while adding your chilled water. You can easily catch test in the corner and snip the rest of the bag away from it. Saves a lot of hassle of filtering, and makes drying much easier

 

[hotdog23]

That's why doing both polar and nonpolar filtrations are necessary. That way you at least get rid of water soluble and solvent soluble contaminates . First i would dissolve the good stuff with an appropriate solvent and filter. Then i would go polar, with dihydrogen monoxide , or MEOH .

I can't keep up on the chem bro. What has been discussed primarily is our non polar filter (recrystallization), at which point we will add our remaining hormone to a solvent... MEOH or dihydro and then what?

 

[dredd09]

Dihydrogen monoxide sounds like an exotic chem i know. Most the world is covered in it though. Also seen as dh2O, or distilled water. Lol. The other is methyl alcohol. Commonly available in your local auto zone or equiv.

 

[dredd09]

Yields will be affected greatly by actual raw purity and technique used to filtrate solutions. Vacuum filtration with filter paper would be best, but presoaked coffee filters and a funnel could do the job.

 

[iintensity]

Ohh k, much more effective and worth the time then



Ya we really need quantitative analysis on the yield, this is a discussion that should be pursued.

To make some contribution to this thread. If you store methanol hormone solution in heavy duty ziplock while adding your chilled water. You can easily catch test in the corner and snip the rest of the bag away from it. Saves a lot of hassle of filtering, and makes drying much easier

Methanol is normally the first solvent of choice because of its polarity (5:1 index). Steroids also have a good solubility in methanol.

I would never use a ziplock bag. A beaker would be best to use or at least some sort of jar will work. The methanol must evaporate.

 

[dredd09]

Not to mention all the finer material you could lose.

 

[iintensity]

Paging @Bill Roberts

This would be a good question for his Q&A. He's a chemist.

 

[hotdog23]

Dihydrogen monoxide sounds like an exotic chem i know. Most the world is covered in it though. Also seen as dh2O, or distilled water. Lol. The other is methyl alcohol. Commonly available in your local auto zone or equiv.

Lmao ok gotcha now. I saw you mentioned acetone earlier, what about letting raw crack back after dissolving in small amount of tone? I've used it on something else before and it didn't require a wash afterwards.

Methanol is normally the first solvent of choice because of its polarity (5:1 index). Steroids also have a good solubility in methanol.

I would never use a ziplock bag. A beaker would be best to use or at least some sort of jar will work. The methanol must evaporate.

You can leave the bag open NP, I get how it looks but trust me very easy to deal with

 

[hotdog23]

Paging @Bill Roberts

This would be a good question for his Q&A. He's a chemist.

He should answer. He works here