maybe weight the first portion and see what kind of yield you got…if yield was good, I would discard it.
Just a thought, I really have no idea what you got going on there.
Okay, ist crop yielded 7.12grams, second 1.1grams. Big different in the two…first was fibery crystaline and broke up easily, second was like crusted over talc powder and tends to stick to the container moreso. No crystaline feel at all. Both felt astringent-like with the little bit that ended up on my fingers after scraping filter with razor. Could the second crop be the powder that people speak of versus crystals from the drip method?
It sure looked weird, but I saw it the first time too with the kit versus now with naoh. Looked like spit in the mix floating around just sub-surface. The methanol/hormone mix had been filtered crytal clear before naoh addition and after the hour, it was yellowish and slightly hazy, but had no precip. If the two are taken together, I have around 8.2 grams. Does this sound right?
[quote]K_D wrote:
Okay, ist crop yielded 7.12grams, second 1.1grams. Big different in the two…first was fibery crystaline and broke up easily, second was like crusted over talc powder and tends to stick to the container moreso. No crystaline feel at all. Both felt astringent-like with the little bit that ended up on my fingers after scraping filter with razor. Could the second crop be the powder that people speak of versus crystals from the drip method? It sure looked weird, but I saw it the first time too with the kit versus now with naoh. Looked like spit in the mix floating around just sub-surface. The methanol/hormone mix had been filtered crytal clear before naoh addition and after the hour, it was yellowish and slightly hazy, but had no precip. If the two are taken together, I have around 8.2 grams. Does this sound right?[/quote]
I’m stumped. 8.2 is probably a reasonably yield for the first recrystallization, but I suppose that as cheap as it is to make test from syno, I would just pitch the second part. I mean, you’re going to inject this stuff, so why even take a chance?
agreed. I was thinking the same thing.
Okay, so I let it dry for a few days and it didn’t loose any weight, so I assume I’m good. Mixed with 5%ba and 15%bb and the rest grapeseed oil to 100mg/ml. I think I see it is very important to thoroughly heat before filtering, as the first few ccs clogged the whatman fast.
Probably loaded up the whatman with hormone! Let the mixing vial sit in boiling water for a few minutes and it filtered easily, so I might have lost a little bit to the first whatman. I’m curious if I have finally done enough right to get it to hold…we’ll see in a few days. Thanks for all the help. It sure do look purdy.
with 5% I think you may find it a bit painful.
Be careful about heating too much as it damages the integrity of the filter membrane…which means even if you don’t tear it outright, you may not actually be filtering it.
I try to not go above the temp of a cup of coffee (180?)
Several of the problems you have run into, seem to me, to be the result of hurrying…the key is to be patient EVERY step of the way.
Agree on the patience. Doing all the drag out tasks over night so I am not in a rush. Working on 3rd batch now. I think second went real well, except for that initial whatman clog. Noted on the whatman heating. It seems to be holding well at 65F.
Speaking of whatmans, I tried a trick that was described elsewhere where the poster suggested backflushing the whatman. I backflushed with pure methanaol when filtering the binders out and it appeared to have damaged the whatman, as it never filtered well again. I have, however, lifted the needle out of the oil and pulled the remaining oil and air backwards through the whatman and noticed better performance and no reduced filtering. Just thought I’d throw that out there.
I’m not going to the trouble of whatman filtering the methanol/hormone mix again. Don’t think it is worth the trouble. I am just using a good coffee filter and being patient!
So If you think 5% might be a bit high, can you suggest Ba/BB/oil ratios? Do you go over 100mg/ml for prop? I am using Grapeseed BTW.
THX
[quote]K_D wrote:
Agree on the patience. Doing all the drag out tasks over night so I am not in a rush. Working on 3rd batch now. I think second went real well, except for that initial whatman clog. Noted on the whatman heating. It seems to be holding well at 65F.
Speaking of whatmans, I tried a trick that was described elsewhere where the poster suggested backflushing the whatman. I backflushed with pure methanaol when filtering the binders out and it appeared to have damaged the whatman, as it never filtered well again. I have, however, lifted the needle out of the oil and pulled the remaining oil and air backwards through the whatman and noticed better performance and no reduced filtering. Just thought I’d throw that out there.
I’m not going to the trouble of whatman filtering the methanol/hormone mix again. Don’t think it is worth the trouble. I am just using a good coffee filter and being patient!
So If you think 5% might be a bit high, can you suggest Ba/BB/oil ratios? Do you go over 100mg/ml for prop? I am using Grapeseed BTW.
THX[/quote]
Don’t backflush w/ methanol or by drawing back after lifting needle out of oil - both can damage the whatman, and the damage may not be visible, but you are no longer assured of filtering to the nominal value.
2%BA 18%BB 80%vegeatble oil of choice* has always worked well for me
*not olive oil though
Well, my yields are getting a little better now. >8g for five carts. I have a hunch that there is a bit to be gained in improving my crystal making process. I do not exactly know how fast and how big a drops they should be, and how much water to instantly add to get the process going. I do put it in the fridge and immediately see lots of growth, I filtered through coarse cloth and got 8g. Saw that the first rinse was cloudy and filtered it through a coffee filter and got maybe a 1/4g more. Where did the additional 1.75g go? I figure 1/4g lost in filter media at most. Can I ask what media you like to use?
I tried a cc of the latest 5%ba 100mg batch and got no significant pain. A touch of soreness the next day, no more than any needle. Can I raise the concentration to 150 or 200mg/ml? How much solvents? Do you have any experience in this area?
THX
I’ve spent countless hours researching the Syno Conversion process and am seriously tired of reading, comparing, and trying to develop a successful bottle of tesp prop. After completely blowing my first two batches I’m still not sure what I’m doing wrong or what method I should use next.
Seems like the steps would be much easier to follow if someone could post an updated method with pics. All the other methods with pics I’ve found were posted years ago and discussions on this board don’t even seem to follow any of the old methods.
I’m asking if an experienced homebrewer can post there method step by step with pics, this will aid the simple minded people like myself. Preferably a method that doesnt includ melting points of crystals, because that just seems way too technical for the average joe.
As a sympathy note I’ve posted the outcome of my last batch of useless crap bottle.
1 Like
You may not be that far off…
I’m not an experienced brewer, but like yourself have spent countless hours researching and asking questions. There are not many people that are willing to talk much about this.
I did put together a very detailed procedure for someone else. I’m not sure how to post it here, but will try tonight. Gotta go right now…
First off, there is nothing wrong with the instructions on basskillers website on making syno prop from dazed kit. All you have to do is either get a kit from finafast or others and apply exactly those instructions. Or…you can get your own stuff and skip the kit. I have had better luck myself. Use saturated naoh for the estrogen solubolizer. Adding it for 1 hour will yield mostly prop and remove the estrogen. 12-24 hours removes prop ester too. Here are my instructions:
5C Syno conversion
- Get a manual coffee maker. The part you really want is the filter funnel. It makes things so much easier than paper clips and beakers. One like this for $11 on ebay. The key search indicator is ?manual coffee maker?. This one uses a #6 filter. It is nice and big to make filtering easy.
You then need a second container like a coffee pot or pitcher. A margarita pitcher at Wal-Mart for $10 like this one:
The coffee filter funnel fits nicely over this rim as well and it holds a lot of fluid. It also has an exaggerated pouring spout that helps with the crystals.
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Start by pouring 12 oz of Heet (normal sized container) (make sure it is methanol, not the isopropyl type) into the coffee pot and 5 carts of Syno. Let it set over night with Syran wrap over the top, occasionally swishing around to help dissolve before you call it a night. You will be left with white stuff at the bottom, but no pellets left, just white residue. Let it settle on the bottom and don?t shake it up the next morning.
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Use a 60cc syringe and an 18ga needle to suck up the clear methanol/hormone fluid without the white powder. At this stage, you can use a coffee filter. Just squirt the syringe contents into the bottom of the filter. It should drain relatively quickly because you are trying not to pick up the filter clogging binders with the syringe. When you get all the easy clear stuff, then you can finally pick up the coffee pot with the last bit of liquid, swish it around to get everything moving and pour it in with one stroke into the filter. Find something else to do while this gradually filters down. When this is done, discard the filter with binders. You should have relatively clear (slightly cloudy) methanol/hormone mixture in the pot. Pour this into the larger (margarita pitcher) pot so you will have plenty of room for all the water you are going to add.
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Now you have to make some saturated NAOH. Here is a handy calculator:
http://www.handymath.com/cgi-bin/naoh5a.cgi
Take a look at the examples to see how to use it. You will need a scale like this one I found on ebay for $18 with the search terms ?cd scale?.
The gist is this: put 10ml-distilled water in a vial. Place the vial in a bath of ice water. Measure out 10 grams of lye crystals and add and agitate. I do it with an old 100cc vial and a small plastic funnel and small sugar spoon. A beaker and glass stirring rod should work too. After I add the lye, I put the stopper on and shake under cold running water to keep it cool. It will take a bit of agitation to get it all to dissolve. This will very nearly be a saturated NAOH solution. You will draw out 2.5ml of this with a syringe and 18ga needle and shoot it into the pot with your methanol/hormone solution and swish it around. Keep the rest for your next conversion.
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Put some plastic food wrap over the top of the pot to keep the methanol fumes down while you wait 1 hour. It should have a yellowish hue and be somewhat cloudy. Prepare 500ml of COLD distilled water in a measuring cup. I add about 150ml of it directly to the Heet solution after the hour has passed. I then set up a cottage cheese type container to sit on top of the pot with a couple holes punctured in the bottom with an 18ga needle. Add the rest of the cold water to this and put the whole thing in the fridge while it drips the water in. Within 10 minutes or so you should see crystals forming. When all of the water has dripped in, there should be a semi-clear, slightly yellow, loaf of fluffy crystal mass in the pot.
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Take the filter funnel and use a circle of somewhat coarse material for a filter. I used something like the material of a coarse pillowcase, or see-through window covering. This is taking place of the infamous painter?s cap that is non-existent these days. Push the material in the funnel all the way and make sure it is big enough to reach over the sides a little. You will pour the pitcher full of Heet/crystals into the filter while it is over your second pot. Do it slowly, as the mass of crystals will tend to slosh and slap into the filter as they go over the pour spout. If you use coarse material instead of a coffee filter at this point, you might see that the solution going through the filter is still cloudy. This is test powder as opposed to crystals. If you poured the whole first batch into a coffee filter, it would take forever to rinse. I have seen somewhere between .25 and 1 gram of test powder in the pot when I have gone to the trouble of recovering it. First time, you should probably ignore it to keep things simple and just harvest crystals. You can capture this first rinse and later run it through a coffee filter to try to save it when you become proficient at this process.
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You will empty the pot under the filter when needed and continue to rinse with cold, distilled water, using at least another gallon or more. I use a lab wash bottle like this 500ml one off of ebay for $4:
It can be used to penetrate and thoroughly wash the load of crystals (don?t forget the folds of the filter material) in the filter, and at the end, you can use it to wash and direct the load to the center of the filter media, so it is not so spread out before you lift it out to dry. When done, the test crystals should be white, not yellow, and the rinse water should no longer have the sweet smell of methanol. If not, keep rinsing.
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When that is done, you will lift the material out of the funnel of the manual coffee maker and lay it into a clean baking pan with many paper towels underneath. I used to bake at low temp for several hours, but now just air dry for several days. I remove the wet paper towels underneath within the first hour or so and lightly put a paper towel over it and store in a safe, dry place for a few days. You risk melting the hormone in the oven, as the minimum temp of most ovens is very near the hormone melting point. Just be patient.
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After a couple days, I go in with a couple of razor blades and cut it up into a finer powder from it?s dried lump form. I then carefully scrape it out onto a clean sheet of paper with a pre-creased fold down the middle. After I am all done working the last bit of crystals out of the filter material and gently scraping it together into one place on the paper near the crease and an edge, I empty this into a protein scoop. I pre-weigh the scoop and write this empty weight on the scoop. I use a small funnel in the scoop, but if you are careful, bending the crease in the paper and using it as a scoop/funnel itself, you probably do not need the funnel. The funnel just traps more powder on it that you meticulously have to try to remove with a toothpick. It will take a little time to get all the crystals off the paper and the razor blades and into the protein scoop. When all done, weigh it. I cover the scoop with a small piece of paper towel using masking tape to hold it securely over and store again for a few more days, allowing it to give up any more moisture it has. I write the total weight on the side of the paper towel. I check this number again a couple days later and it usually has not changed. That signals that it is dry.
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Order your own BA, BB and Oil from an online supplier, like Lemlange. I used grape seed oil and bought 16 oz of each. It is said that you can use any vegetable oil, but I have not tried it. I use a clean 100ml vial with stopper removed to do the mixing. I get the crystals in the vial with a small funnel and something like a toothpick to get it through and cleaned out. I would think you could use a small beaker and a mixing stick instead. I then add 5% BA and 15% BB to the crystals and note that they dissolve. I then add the oil.
Example: Let?s say we got 7.5 grams yield from a 5-cart conversion. To get to 100mg/ml concentration, we would ultimately want 75ml of finished solution.
You start by adding 5% of 75ml = 3.75ml BA to the dry prop crystals
Add 15% of 75ml = 11.25ml BB
Add 7.25ml oil per gram of Prop = 54.375ml oil
This will finish with 75ml of solution. -
I put this in a small pan of lightly boiling water for a while (15 minutes) to get everything into solution and hot. Put the rubber stopper in and stab it with a 25ga needle to let the pressure out as it is heated, no need if you are using a beaker. I find this to be very important to enable reasonable filtering later. You will want to look closely at the solution and make sure you do not see any trace of crystals left. When this is done, the solution should be very clear with only the tint of the oil and the misc. dog hairs that have made it through the process. When I have rushed this and thought it was done, I clogged the whatman with the first syringe full. Let the bottle in water continue to slow boil while you start the next step.
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Attach a new whatman 0.45u filter to a new 18ga needle and stick it into the stopper of a new, sterile 100cc vial. Also stick a new 25ga needle in the stopper to vet the vial as you add oil. Using something like a 20cc syringe and 18ga needle, withdraw your solution through the stopper, holding the vial with a towel (hot). Return vial or beaker to boiling water between filterings. As long as you are careful, the stopper should have no problem staying in place. Midway through the withdrawal, I usually move the needle around to let a stream of bubbles into the vial to equalize the pressure. You cannot do this by traditionally pushing air in first, as there is nothing to keep the stopper on, under pressure. Alternatively, you could put a 25ga needle in the stopper as well to vent, as it should not drip with its size. Withdraw the needle, put the cap on, pull the plunger back a little to get the oil out of the needle and remove needle and set aside. Carefully twist loaded syringe onto whatman and start pushing solution through the filter. When you get to the end, you can actually pull back on plunger and pull air backwards through filter and put several CCs worth into syringe. Then push the residual oil through the whatman until it spits air through the needle in the vial and you see air in the filter. Wait just a second and twist syringe off whatman. This is all to keep the whatman from burping precious solution back out after you have removed the syringe. Repeat until you have it all filtered into the sterile vial. Remove needles from stopper, clean up your mess and you are done!
I do not know how to attach the pics that go along with this, but I don’t think they are that important to get a handle on it.
As Testolius suggested, you might lower the BA/BB ratio to 2:18 or so. I have not found this to be too painful, but many have suggested the lowering, so I will try it on my next batch.
When I tried a FF kit, I could not get it to keep from crashing until I added a little Ba/BB to it. That is why I suggest doing it yourself. It will be way cheaper in the long run, and you actually know what is going into it.
It might also be said that Testolius has pointed out that in step 11, he does not think that the hot (212F) solution should go through the whatman. He says that it can compromise the filtering ability. You could let it cool some before the filtering.
Wow, that clears it up for me. I think what I was doing wrong is not weighing my prop crystals to make sure they are dry, and to make sure the proper oil/ba/bb mix is added.
I already ordered my whatman filter and accidently got the size smaller than .45u, it’s .20u! Will it still filter with a .20u?
The answer in general to that sort of problem is yes, just slower. But I have not tried this specific case (with regard to the material being filtered: have tried 20 micron vs 40 in other situations.)
Wow, awesome thread revival. I see RJ posted in this thread long before Ragnarok. A time when the hammer god, reigned peacefully over his once loved forum.