filtering ur test powder to a 99% purity
- Thread starter adammac
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Viciouscycle w
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I think this is what you want. From another forum.
I only studied Testosterone, never got really far with it as I was occupied with other things. You can check different solubillities of steroids in the Merck Index or CRC. The police kept mine unfortunately. steroids are lipids and as such are hydrophobic (water fearing) I don`t think any of them dissolve in water. You can find out what solvents are used for purification by reading chemical abstracts.
What I would do is a dual solvent recrystallization using ethanol + water. Methanol is preferred, but it would make me nervous since I wouldn`t have the right equipment to test for any trace solvent left behind. In theory, it would all evaporate past its boiling point.
Here`s patent on the subject:
Japanese Patent JP56002999
Abstract: PURPOSE: To increase the crystal size and the bulk density of crystallized testosterone enanthate, and to improve the efficiency of extraction and filtration of slurry, by crystallizing crude testosterone enanthate in a mixed solvent comprising specific amounts of water and alcohol.
CONSTITUTION: Crude testosterone enanthate of formula is dissolved in an aliphatic lower alcohol (pref. methanol). The solution is cooled near the crystallization temperature, and mixed with 10W50wt%, pref. 20W30wt%, based on the alcohol, of water, and recrystallized at ***8804;0°C, pref. ***8804;-10°C.
PURIFICATION OF TESTOSTERONE ENANTHATE - MITSUBISHI CHEM IND LTD
Not sure what this terminology means 10W50wt%, pref. 20W30wt%...
I would start out heating the water and placing the testosterone enanthate in the liquid under magnetic stirring. Use a magnetic stirring hotplate. I would keep temperature of the water at 60-70C or so, not to damage the testosterone. I`m going by speculation here, as I`ve never done it.
After a little while I would add methanol or ethanol which I`ve already been heating on the same hotplate in a seperate beaker. WARNING! boiling alcohol can cause fires. Fumes are flammable so be careful and take the necessary precautions.
I would add it in increments slowly to my testosterone/water mix. For 100g of Testosterone, I would be using something like 600ml of water and I would start with maybe 50ml of methanol. I would take note of how it is dissolving and add methanol by 10ml increments. When it seems to be practically dissolved (not as cloudy, more clear) I would start adding the methanol by pipette, drop by drop until it is completely clear. Take it off the heat wrap it in foil and let it sit at room T without disturbing it. The next day, put it in the freezer.
You should see mass crystals forming at the bottom. If not, you used too much solvent, so boil some off using the hotplate and repeat process. You need a source of vacuum and bucher funnel with filteration funnel. Wet your filter paper with fridge cold water using a squirt bottle. Apply vacuum, run your mix through and rinse with ice cold water. Do this fast as you want it as cold as possible to minimize product loss. The fresh water washes should technically remove all traces of the alcohol.
Let your crystals air dry by spreading them out on a tray.
If there are weird impurities like pubes, you would need to perform a hot filtration. If you have decoloration, you will need to use activated carbon.
I only studied Testosterone, never got really far with it as I was occupied with other things. You can check different solubillities of steroids in the Merck Index or CRC. The police kept mine unfortunately. steroids are lipids and as such are hydrophobic (water fearing) I don`t think any of them dissolve in water. You can find out what solvents are used for purification by reading chemical abstracts.
What I would do is a dual solvent recrystallization using ethanol + water. Methanol is preferred, but it would make me nervous since I wouldn`t have the right equipment to test for any trace solvent left behind. In theory, it would all evaporate past its boiling point.
Here`s patent on the subject:
Japanese Patent JP56002999
Abstract: PURPOSE: To increase the crystal size and the bulk density of crystallized testosterone enanthate, and to improve the efficiency of extraction and filtration of slurry, by crystallizing crude testosterone enanthate in a mixed solvent comprising specific amounts of water and alcohol.
CONSTITUTION: Crude testosterone enanthate of formula is dissolved in an aliphatic lower alcohol (pref. methanol). The solution is cooled near the crystallization temperature, and mixed with 10W50wt%, pref. 20W30wt%, based on the alcohol, of water, and recrystallized at ***8804;0°C, pref. ***8804;-10°C.
PURIFICATION OF TESTOSTERONE ENANTHATE - MITSUBISHI CHEM IND LTD
Not sure what this terminology means 10W50wt%, pref. 20W30wt%...
I would start out heating the water and placing the testosterone enanthate in the liquid under magnetic stirring. Use a magnetic stirring hotplate. I would keep temperature of the water at 60-70C or so, not to damage the testosterone. I`m going by speculation here, as I`ve never done it.
After a little while I would add methanol or ethanol which I`ve already been heating on the same hotplate in a seperate beaker. WARNING! boiling alcohol can cause fires. Fumes are flammable so be careful and take the necessary precautions.
I would add it in increments slowly to my testosterone/water mix. For 100g of Testosterone, I would be using something like 600ml of water and I would start with maybe 50ml of methanol. I would take note of how it is dissolving and add methanol by 10ml increments. When it seems to be practically dissolved (not as cloudy, more clear) I would start adding the methanol by pipette, drop by drop until it is completely clear. Take it off the heat wrap it in foil and let it sit at room T without disturbing it. The next day, put it in the freezer.
You should see mass crystals forming at the bottom. If not, you used too much solvent, so boil some off using the hotplate and repeat process. You need a source of vacuum and bucher funnel with filteration funnel. Wet your filter paper with fridge cold water using a squirt bottle. Apply vacuum, run your mix through and rinse with ice cold water. Do this fast as you want it as cold as possible to minimize product loss. The fresh water washes should technically remove all traces of the alcohol.
Let your crystals air dry by spreading them out on a tray.
If there are weird impurities like pubes, you would need to perform a hot filtration. If you have decoloration, you will need to use activated carbon.
I wouldn't recommend any novice brewer attempt recrystallization, especially with methanol. As an alternative, why not use an LC-MS testing service to get the molecular mass of the Tesosterone Enanthate that have. Not only will you get the molecular mass of the Testosterone Enanthate, but you'll get it's concentration versus any impurities. You may also find out that you don't have Testosterone Enanthate at all 
When people talk about "filtering test powder"....It's not really a thing. There are situations where certain compounds can break down, and de-crystallize (Tren in pure form can crash after a short period of time with poor storage), but in this situation your overall purity is decreasing, because the molecule is breaking down. There are still MANY crystals still in the solution, but it's on the way down.
Most Universities will offer LC-MS testing for a fee. I'm also excited about advancements in NIR Spectometry, it's going to continuously get better, and eventually, I believe there will be a consumer model that would allow us to bypass the expensive, time consuming testing.
When people talk about "filtering test powder"....It's not really a thing. There are situations where certain compounds can break down, and de-crystallize (Tren in pure form can crash after a short period of time with poor storage), but in this situation your overall purity is decreasing, because the molecule is breaking down. There are still MANY crystals still in the solution, but it's on the way down.
Most Universities will offer LC-MS testing for a fee. I'm also excited about advancements in NIR Spectometry, it's going to continuously get better, and eventually, I believe there will be a consumer model that would allow us to bypass the expensive, time consuming testing.
I would expect some of the side reaction products and decomposition products of testosterone to have similar solubility characteristics to testosterone. That is the problem you run into. Basically you just have to trust your supplier, unless you have a serious lab where you can run chromatography and analytical equipment. I have cleaned up testosterone enanthate before with methanol and water, its a very good way to remove heptonic acid which causes pain. When Test E powder gets old (about a year at RT) it turns yellow with heptonic acid. Keep it in the freezer, else it will decompose to yellow goop. Dissolving it in methanol and flooding with water is a good way to reclaim what is left if the goop shit.
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