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Few questions before I attempt my first extraction *updated with pics* help plz Options
 
skeetskeeter
#1 Posted : 9/13/2009 3:54:16 AM
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*SEE last post with pics of where I am right now and why im lost**

Hey, I am planning on trying my first extraction on MHRB. I’ve spent the last few weeks reading up different threads and extraction info. I’m pretty sure I know what to do but I had a few questions I want to get figured out before I start.
I am going to use 250 grams of shredded root bark, 260 grams of NaOH, and 3000 ml of water. I have read different things and I am not sure, should I mix the root bark and lye solution inside or outside? If I do it inside I can open windows and all but it will be around 70 degrees, if I do this outside it will be around 90 degrees. What do you guys recommend? I have read it is good to warm the naptha and I really don’t want to use the stove or anything inside. Would it be good to do it outside in 90 degree weather?
After I mash it/ let it sit for a few hours I am planning on pouring in 150 ml naptha and kind of swirling it with a spoon for 20 minutes or so.
I am kind of confused on the emulsion thing; will this happen if I mix too vigorously as in getting air bubbles, or can I put it in a big jar and shake it like crazy? Then I plan to pour the whole mixture into this tall glass vase I have, let it separate and siphon off the naptha layer with a plastic turkey baster (I can’t find a glass one anywhere lol).
This is where I get a bit confused, I put the naptha on a pyrex dish and put this into the fridge for an hour, and then move to the freezer. Wait a few hours and crystals should be in the pyrex dish. Then I am confused, I’m supposed to fish the crystals out of the naptha and put them out to dry, and then basically repeat the same process over again with the same naptha? After I’m done with the rootbark, throw it out, and then freeze precip. and evaporate the naptha and scrape up the pyrex dish?
Do you guys see me missing anything or doing anything wrong? Any help or tips would be awesome! Thanks Smile

EDIT: I tryed the extraction with 100g rootbark. I can't freeze precip anything out of my naptha..more details later in the thread ....I want crystals!!!! lol Smile
 

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GratefulDad
#2 Posted : 9/13/2009 8:43:42 AM

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Mixing the lye with water should be done first. This can be done inside with a sink full of cold water, the lye can be added to cold water, capped, and shaken, then pressure released, and recapped, then set into the cold water filled sink. This will allow the jug to cool. When shaken the jug will heat, and one can set it back into the cold sink to make sure it doesn't get too hot. HDPE jugs are good for this. When the lye is all mixed in and the jug no longer heats when shaken, the bark can be mixed in. This is then shaken again and left to sit for an hour or so. Again, though, I will refer you to the tek I posted, it has pictures of each step, including the optional polar wash and epsom salt dry for cleaning it up before freeze precipitating the crystals. Check it out: http://www.dmt-nexus.me/...=posts&m=78424#78424
 
SuperRad
#3 Posted : 9/13/2009 4:34:33 PM
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It's better to add lye to warm water, actually. If you add the lye to cold water it sinks to the bottom and takes a long time to mix, making temperature spikes more likely. Just add the lye SLOWLY with plenty of stirring. A cold water bath lets you add the lye more quickly, but I would feel safer simply mixing the lye in a controlled, cautious fashion. You don't want pH 13 water erupting at you Smile
 
GratefulDad
#4 Posted : 9/13/2009 8:56:34 PM

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Perhaps, warm water, extra slow, is safer, but SWIM never had a problem adding lye to cold water, it seems to dissolve just fine for him, and the jug heats much less rapidly. He can add half a lb of lye before the jug begins to get warm, and the cold water bath helps keep the jug cool enough to keep it from getting soft. He must admit, though, after doing the extraction many times, he tends to cut corners, which is probably not the best idea for someone new to the extraction.
 
SuperRad
#5 Posted : 9/13/2009 10:41:35 PM
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I didn't mean to imply that there's anything wrong with an ice water bath, it's a fantastic way to keep temperatures safe while freely adding lye. And always good to have on hand if temperature may become an issue.

I do stand by using warmed water initially, If you're gonna be pulling the jug out of the bath and shaking it then the water will heat up quickly anyhow, and that's what the cold bath is for. When I used cold water in a mason jar, I could clearly see a thick layer of lye form at the bottom. Then, as lye began to dissolve and heat the jar, much of the lye layer suddenly dissolved and the jar became VERY HOT, I believe I was very lucky the jar did not shatter. HDPE jugs have been known to get 'soft' when lye water gets too hot.

Then again if I had to add 200+ grams I would get impatient too...
 
skeetskeeter
#6 Posted : 9/13/2009 10:57:12 PM
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Alrite, so Im going to scrap my plan and follow what Spice T posted. I'm going to use 1/2 kilo (1.1 lb) bark. I'm going to the store to buy a water jug and one of those twisty Gatorade bottles. I'm planning to use 1 lb of lye, mix water in the way you guys describe. Then put in the rootbark, shake occasionally and let it sit for a few hours. Then pour in 400ml naptha, shake and let it sit for a half hour or so to seperate, pour off the naptha layer and use the gatorade (ghetto sep funnel) bottle to isolate the naptha, then put that on a pyrex dish and put in the fridge, then move to the freezer. And then repeat a few more times with new naptha and do the same thing over and over. After the naptha has been in the freezer for a few hours I pick the crystals out, dry them, and thats my spice. That sound good to you guys? I really dont want to screw this up because I only have enough for this one extraction and have been anticipating this for quite some time. I'm headed to the store, hopefully you guys give me the go ahead and I'll get this thang going when I get home. Thanks for all the help guys!! I'll keep you guys updated Smile
 
skeetskeeter
#7 Posted : 9/14/2009 4:36:00 AM
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So I decided to go with 100g root bark and give it a shot, I used 1500ml water, 115g of lye. First I mixed the lye and warm water until the lye was completltey dissolved, while the bottle was in the sink in ice cold water. Then I added the rootbark, and shook/ turned the bottle end over end for about a half hour. Then I added 160ml naptha, capped the milk jug and shook it/ turned it over and end, etc... for about a half hour, then I did my best to isolate just the naptha.
I have a few very small bubbles of lye/rb solution in the naptha that don't seem to seperate out, they are very small...like if you made a drop from an eyedroper, about 1/20th of a drop is about their size, so barely visible. I tried to add some sea salt to the mixture to get it to seperate better, still, no dice. Then I put the naptha with few impurities in the fridge for 30 mins, then moved to the freezer, and I have a bunch of white globs that form, when i scrape them they seem to be just frozen water becasue when I put them on a plate to dry out they just completley dissapear. Then I tried a second wash with the exact same results....
What am I doing wrong, how am I fucking up such a simple process. Im hella frustruated...time to smoke a bowl and go to sleep. I'll try to do a third run tomorrow...hopefully someone has some tips for me Smile Gnite every1!
 
skeetskeeter
#8 Posted : 9/14/2009 12:44:50 PM
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So I checked both of my naptha pulls and neither have any crystals, just white snow looking things that melt away when I scrape them from the bottom and put them out to dry. What am I doing wrong? Im headed to work now, I just mixed in 130ml naptha and am going to let it seperate for a few hours, come home on break and isolate the naptha and try the same thing, put it in the fridge then the freezer to precip. Please someone give me some advice, I feel like retard that I can't figure this thing out. Once again, thanks for your help guys, I dnt mean to be double and triple posting but no one has replied and I'd really like to get this figured out and get some spice Smile ...off 2 work...hava good day evry1!
 
GratefulDad
#9 Posted : 9/14/2009 2:46:51 PM

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In SWIM's tek, the polar wash and epsom salt dry are used to clean any sludge that was carried over after separation, and epsom salt dries the water left. This should eliminate ice crystals from forming in the solvent. Sometimes when the DMT is scraped up, and some solvent still remains, the warmth of the room can make the DMT redissolve into the tiny bit of residual solvent. Perhaps this is what's happening. If water has gotten into the crystallization, it could be that the DMT was ionized into the water, and this may keep it from forming nice crystals.

Perhaps collecting the solvent, and heating it in a heat bath a bit, before using baked epsom salt to dry it could clean out any moisture, and maybe the crystals will precipitate more easily. Also, since using less MHRB and more solvent, perhaps the naphtha isn't saturated enough for the crystals to precipitate. Have you done at least three pulls with the naphtha? If this is the case, evaporating the solvent until it becomes cloudy/milky, then placing in the freezer, one may have more success. Also, do not throw out anything until you have your DMT and I am sure we can help you get it out of there, if there was a mistake made in any part of the extraction.
 
skeetskeeter
#10 Posted : 9/14/2009 9:38:30 PM
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Thanks for all the help, Ive done three pulls with no results. My stuff has seperated into 3 layers, a dark bottom layer, a lighter mid layer, and the a thin layer of naptha on top (small amount I couldn't get off). I have no clue where to even start, I have added sea salt to the mixture to try to get it to seperate better...no luck. I believe I should have gotten something between 3 pulls. What could I possibly be doing wrong? My first pull took about 30 mins, my last pull I let my naptha and aqueous solution mix for a few hours before decanting and seperating the naptha, so its not my timing, I have put the whole solution in warm water to help it seperate, etc... I am tempted to say fuck it and scrap the whole project, try once more with my 400g of bark I have left, and if that doesn't work just say fuck it. Anyone have any advice. This process should be very simple...I am using measured amounts of chemicals that have worked for others....what could possibly be going wrong? SOOO FRUSTRATED... I JUST WANT SOME DMT LOL

p.s....Here are pics...the white stuff is what has precipitated, the stuff on the razor is the white stuff that I scraped up (DMT?), And you can also see how there are 3 layers in my glass vase....so confused...what to do?
skeetskeeter attached the following image(s):
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Spock's Brain
#11 Posted : 9/15/2009 1:53:18 AM

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skeetskeeter wrote:
try once more with my 400g of bark I have left, and if that doesn't work just say fuck it. Anyone have any advice.?


Perform an A/B extraction with the 1/2 the (200g's) remaining product, have patience. take a few days to a week to perform; follow these steps:


1. Cut the bark up into small pieces with some scissors.

2. Prepare a solution of white vinegar and water to a PH of 3-4.

3. Put some of the bark and the solution in a tuff blender and blend, blend, blend.

(repeat step 3 multiple times as you can only run so much thru a blender at once without burning it up.)

End up with a reddish brown soup of vinigar acid water root bark puree.

4. Have it in a large glass jar like a pick jar and put it on the stove IN A DOUBLE BOILER CONFIGURATION... Heat it at a simmer for like 1/2 hour, remove from water several times and carefully agitate, use a few towels to hold & gently shake, don't break the glass it's not pyrex.

5. After it cools, strain it thru a tea shirt, napkin, or sock, into another awaiting glass jar. I use a combination of 100% cotton hankerchief and cotton balls thru a funnel.

6. Collect all the shredded root bark that you've seperated from as much fluid as possible, and take it back to step #3. Perform a total of 3 times.

(The idea is to cut up, immerse in acidified water, blend, and heat the purified root bark, for 3 total pulls from the bark and end up with a dark purple filtered water solution from each pull. On the first pull heat for 1/2 hr, and seperate. 2nd, pull heat again but let the puree sit for a few hours and continue to agitate, 3rd pull after heating let it sit for most of the day.) Heating speeds the reaction, agitating and having a thouroughly pureed product ensures the reaction touches every part of it, letting it sit (time) ensures it's complete.)

7. conclude acid solution step- At this point you've got one glass vessel with the combined liquid of 3 seperate pulls from the root bark, it's exhausted- toss it (the root bark NOT the liquid). Put the liquid back on the double boiler and reduce it by boiling to a managable volume. After that, put it in the fridge. When it's cold you'll have a sediment. Decant (pour off) from the sediment and filter again.

Now your ready to basify your solution-

8. make a solution of water and sodium hydroxide (pure lye.) by adding lye crystals slowly to warm water. You can basically guestimate and eyeball it (THRU SAFETY GOGGLES! - ALWAYS WEAR WHEN YOUR AT THIS STEP AND BEYOND!!!)... just keep slowly adding until the water reached close to saturation - and a bleach like consistency... PH of 14-15

9. Slowly drip the base solution into your acid solution described in step 7. When your acid solution turn from dark purple to JET BLACK your 75% there... check your PH and continue until you raise it to around PH 12.5.

Now your ready to do your first naptha pull.

10. Put your basified solution back onto the stove and heat it up to 140 F.

NEVER EXCEED 140 F ONCE YOUR SOLUTIONS ARE BASIC AS THAT IT APPROCHING THE BOLING POINT OF FREEBASE DMT...

11. Put a small amount of Naptha into another double boiler configuration and heat it up to 140 also.

12. Pour the naptha into the water solution, shake it up and set it back into the warm water and let it settle for a few minutes. You'll end up with a layer, it contains the DMT.

DO NOT EXCEED 140 F.!!!!!

14. Pour the solution into a sep funnel. Get a sep funnel, it's indespensible. let it seperate, drain of the purple-black water part back into it's original vessel for aditional prossess. let it seperate some more, and drain again. Now your sep funnel only has the naptha in it that's tainted yellow if you did everything right thus far. Drain the naptha into another jar or beaker.

Go back to step 10, but check your PH of your water solution again. If it's not 12.5+ go back to step 9.

(the idea is to do 3 pulls with warm naptha from your basified water solution. each pull get's less and less, but it's for completeness.) Now you've got an exhausted solution, and another container with the naptha in it and also some emulsion. Don't worry about the emulsion. RAISING YOUR PH WILL BREAK UP ANY TROUBLE EMULSION THO...)

You can save your "exhausted" solution and do additional pulls with WARM HEPTANE (rubber cement thinner) it'll pull remainders that naptha won't. Or you could do a combination. (first pull naptha, 2nd 1/2-1/2, 3rd 100% heptane.)

Now, FREEZE PRECIPITATE as follows:

15. Pour your thinners (naptha&heptane) off any remaing emulsions. into a glass baking plate. put a fan over it and reduce it by evaporation as you carefully watch. The idea is to reduce the volume until it's SATURATED.... It should turn white in color if you view it from the side, and you may see spiraling confluences of soluables beginning to coalesce... PREPARE FOR OUTER SPACE....

16. Cover the plate with the now milky colored solvents with foil and put in the freezer for like 3-5 hrs. Take it out.

17. The bottom of the plate will be covered with snow globes... remove the foil and pour the solution off the snow crystals into another glass plate. Let the plate sit and dry for at least a few hours... until completely dry. Scrape up with a razor blade.

Figure out what to do next....

***Never perform any of the above described actions****










"Infinite Diversity, in Infinite Combinations."
 
skeetskeeter
#12 Posted : 9/15/2009 3:46:32 AM
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Really, I'd rather do a STB tek, they seem much easier and I don't want to spend another dime on materials. So what do you guys recconmend i do....heat up the whole jug, pour all the naptha back in from the freeze precip dishes and evaporate until is very little solvent and then try to freeze precip all 3 runs in one? How do I get it to seperate into 2 distibct layers instead of 4 layers? WTF should I do,,,im done for the night...should i reusue my old naptha and let it sit with the lye solution over night or what should i do..p.s..i smoked all the stuff pictured on ther razor blade in 1 hit out of my roor and did not feel anything. Very disapointed....There should be a foolproof method for this...can someone please help me out...i have 100g of rootbark sitting in lye that idk what to do with and 400grams of unused bark that I dont want to waste.
Whaty should I do so i dont waste any and accually get the dmt...ive tried warm water baths and salt and tapping...what do you do when nothing works? please help....am i just getting unluckly? Its a very simple process i dont see what I could be meessing up.....let me know ....thnx
 
Spock's Brain
#13 Posted : 9/15/2009 6:27:26 AM

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Recheck your PH and make sure it's plenty high.... mix everything together, and agitatate it repeatedly over several hours... high PH... 14-15, did you check your PH? It's all about PH... put everthing on the stove in a double boiler and heat it up so it's about 140F?. put everything thru a filtration medium until you end up with just liquids. Agitate it some more. Seperate the naptha layer off and put it in a glass dish and see what you've got after complete evaporation, forget about freeze precip initially, go back and re-crystalize later. If you succeed, and when you see time seem to completely freeze as you blast out of your body, you'll understand why it's pointless to hurry the proccess...
"Infinite Diversity, in Infinite Combinations."
 
GratefulDad
#14 Posted : 9/15/2009 5:12:21 PM

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skeetskeeter wrote:
So I decided to go with 100g root bark and give it a shot, I used 1500ml water, 115g of lye. First I mixed the lye and warm water until the lye was completltey dissolved, while the bottle was in the sink in ice cold water. Then I added the rootbark, and shook/ turned the bottle end over end for about a half hour.


The jug should be left to sit for at least an hour after mixing well. this allows for the DMT to be loosened from any of the larger bark particles.

skeetskeeter wrote:
Then I added 160ml naptha, capped the milk jug and shook it/ turned it over and end, etc... for about a half hour, then I did my best to isolate just the naptha.

Trying to separate 160 mls of naphtha from the jug has to be extremely hard, so adding enough naphtha, probably 250 mls will make that easier, and at the end, the naphtha can be evaporated a bit before freezing, to be sure it's concentrated enough for precipitation.

skeetskeeter wrote:
I have a few very small bubbles of lye/rb solution in the naptha that don't seem to seperate out, they are very small...like if you made a drop from an eyedroper, about 1/20th of a drop is about their size, so barely visible.

By transferring the clean naphtha to a new dish, the little drops will usually stick to the bottom of the original container, and can be separated, leaving one with just naphtha.

skeetskeeter wrote:
I tried to add some sea salt to the mixture to get it to seperate better, still, no dice. Then I put the naptha with few impurities in the fridge for 30 mins, then moved to the freezer, and I have a bunch of white globs that form, when i scrape them they seem to be just frozen water becasue when I put them on a plate to dry out they just completley dissapear. Then I tried a second wash with the exact same results....

Are you covering the crystallization dish so no moisture or ice gets in? The water could turn the DMT to an oil that will not smoke and it will not allow the DMT freebase to crystallize properly. It's best to do all the pulls and combine them, wash them if desired, and even if not washing, the cooked epsom salt dry, will be sure to soak up any possible moisture in the solvent.

skeetskeeter wrote:
What am I doing wrong, how am I fucking up such a simple process. Im hella frustruated...time to smoke a bowl and go to sleep. I'll try to do a third run tomorrow...hopefully someone has some tips for me Smile Gnite every1!
Don't toss anything, I am sure if it's in there, we can find it.

The photos are kind of blurry and a few I am not sure what i am looking at, but SWIM says that it looks like ice in a filter in the first pic, and not sure what one is doing there, but it's definitely not part of the tek. SWIM uses a coffee filter only for filtering the epsom salts out of the dried solvent. It seems from all the pics, that no dish used has been covered when stuck in the freezer or fridge, which will definitely cause moisture and condensation to form in the solvent, and it will impede crystallization and will possibly form an unsmokeable oil from the water.

SWIM would suggest mixing the solvent with the MHRB/lye/.water solution, then placing it all in a heat bath, and shaking it enough to mix the layers, but not too hard. Let this sit in the heat bath until it's warm and has separated. If it separates very fast, then it could be shaken a bit more. When it has been warmed and separated, then remove the solvent.

Not sure if all 3 pulls have been done, but if it's not an easily visible layer when poured into the MHRB juice, then add enough so that separation will be easier. If 3-4 pulls with solvent have been done, split the solvent into 3 pulls again and repeat them with the used solvent, then collect them all together. If all 3-4 pulls have not been done, then use the first pull as I explained, then do 2-3 more pulls with fresh solvent, and combine them.

Once you have combined the solvent from 3-4 pulls, skip the polar wash, just be sure that the solvent has been poured into a fresh container that contains none of the MHRB/lye/water solution. Then, use a bit of baked epsom salts to be sure that all traces of water have been removed and filter them out through a coffee filter. Filter the solvent into a clean dry baking dish, and place a fan to blow on it.

Check the dish periodically, and when the solvent is cloudy, either cover the dish (sealed), or pour it into a dish that can be sealed (glass canning jar could be used, but is hard to scrape the crystals from. However, jug may be too large for such a small crystallization, so a half-pint wide-mouth jar would be ideal, but we'll worry about getting them out of the jar later if a larger one must be used). Place this sealed container in the freezer for at least 12-24 hours, and report back what you see. Save everything else, and we'll see how it turns out.

Good Luck!
 
skeetskeeter
#15 Posted : 9/17/2009 5:20:42 AM
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Hey, thanks for the comments everyone I really appreciate it. I tried to do another pull today with 200ml naptha, and did it in the garage in 80-90 degree weather. I can't get the layers to seperate, they are very cloudy...is it possible I messed up to the point of no return? I don't really want to put too much effort into this batch that doesn't seem to be working. I think I am going to try again with the rest of my rootbark, what should I do different this time to make sure I dont' have problems? Thanks again everyone...especially spice T, btw, in the pics thats not a coffee filter, thats just frost that got on the dish from being in the freezer. I think that was why I didn't get crystals, becasue there was too much moisture since I didnt cover the container.
 
turtleman29
#16 Posted : 9/17/2009 5:48:40 AM

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It sounds like you have alot of spice that is still in your naptha,I would take all your pulls combine them, evap that down and try and freeze precipitate from that. It could also be that your freezer is not cold enough, that looked like a fridge in the picture, definitely try something colder; the teks state that it should be -40 celsius which is -40 farenheit as well.

Best of luck
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skeetskeeter
#17 Posted : 9/17/2009 12:46:20 PM
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My freezer makes icecream hard to scoop, I thought thats as cold as it needed to be? If I make my freezer cooler all my food is going to get freezer burn and I'm not really feeling that lol. What should I do about this new dilemma? I still can't get the layers to seperate and I let it sit overnight in a warm garage, any advice or is this batch messed up beyond fixing? How many ml should I evaporate the naptha into before I freeze precip?
Sorry about all the questions...thanks for being so patient and helpful everyone!
 
 
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