hello everyone, complete and utter novice here!

[ozora]

i should really start by saying my first post on here is probably more a combined introduction and plea for help so i hope i'm using the correct section of the forum.
i've been reading quite avidly now as a guest for 3 weeks and despite being fascinated by the amount of knowledge on offer i have to confess i've probably fallen into the trap of information overload!

a short introduction...

i'm getting on a bit now, i made my debut with psychedelics some 30 years ago with the good old british liberty cap and have been a enthusiastic (although sporadic) traveller ever since, predominately i suppose with my good friend albert hofmann. i also went down the probably well worn path of party 'stimulants' during the late'80s/90s but grew bored with them a number of years ago. i've been aware of dmt for a long time but for whatever reason the opportunity to experience it alluded me, odd really considering my love of psychedelic trance festivals, maybe i've been wandering around with my eyes closed for years?!
all this however changed last month in hungary. i fell in love, not with any of the many beautiful women from all over the world at the festival but with changa. it literally blew my mind! i genuinely cant think of enough superlatives for the experience, i dont doubt though that you all know what i mean!
for the last month or so i've been on an almost obsessive quest for knowledge on the subject and despite being absolutely useless at chemistry at school (in my defence i had no interest in it whatsoever, i had to take a science subject to take metalwork!) i've decided i'm nearing the time to start experimenting again with renewed enthusiasm!

S.W.I.M. has been slowly gathering together the information and materials required to attempt a first extraction. his intention is to use the method highlighted in the DMT HANDBOOK (pdf download file), but is obviously short of experience and one or two ingredients. S.W.I.M. also would like to know if he has correctly sourced parts of suitable quality.

S.W.I.M. obtained 2.5L of 85% phosphoric acid which he assumes will probably last forever?
S.W.I.M. obtained 1kg of MHRB from here... http://www.mimosahostilis.co.uk/ .... is this a good supplier?
S.W.I.M. has got his hands on 1L of quality acetone.
S.W.I.M. has been completely unable to source any of the 'shellite' recommended in the DMT HANDBOOK in the U.K. and having read the forum is now totally confused as to what is a suitable naphtha? S.W.I.M. has so far been unable to source any coleman fuel in the U.K. and is now very worried having read conflicting reports on the suitability of various lighter fluids. which one is the best?
S.W.I.M. is wondering if this is prudent source for sodium hydroxide .... http://cgi.ebay.co.uk/Sodium-Hydrox...s_ET?hash=item35a2f9d164&_trksid=p3286.c0.m14 .... and whether or not it is of suitable quality? S.W.I.M. would be happy to learn of alternative suppliers.
S.W.I.M. is concerned about the seemingly vague description in the DMT HANDBOOK of waiting for a 15-20 minute period before starting the 'basify and extract' step and adding the caustic soda solution to the bark tea. if as stipulated 'temperaure is critical to efficient extraction' shouldn't the above description be more precise? should S.W.I.M. obtain a thermometre?
S.W.I.M. invested a massive £12 for an 11 litre stainless steel stockpan from ebay after reading alluminium was unsuitable due to oxidising. S.W.I.M. has since delved quite deeply into the properties of phosphoric acid and has learnt that it attacks stainless steel too. should S.W.I.M. have bought a better quality pan?

and finally (you can all draw some relieved breaths!)....

is S.W.I.M. being profoundly naive in thinking that despite the above concerns, the step by step guide in the DMT HANDBOOK makes it all sound relatively simple and that he'll soon have the freebase dmt needed to make the beautiful changa? is he therefore being nothing short of stupid in attempting to use 1kg of MHRB for his first extraction?


thank you all for taking the time to read this. i apologise profusely for the length of this post and appreciate you've probably all read something very similar to this before. fingers crossed though in eager anticipation for some answers to the above questions!

peace and love to each and every one of you.

 

[GratefulDad]

SWIM posted a simple 2 lb extraction, done with everyday household items, and no strong acids needed. Check it out here: SIMPLE STB PICTORIAL, with Step by Step pics. - FAQ - All your basic questions and answers - Welcome to the DMT-Nexus I am unsure of that supplier as I have never used them or heard of them. Try to find VM&P Naphtha which is Varnish Maker's & Painter's Naphtha. Hexane would work as well. Not sure of the solvents in your area, but if you can find any that have been suggested, then just do an evaporation test on some to make sure it leaves no smells or residues, and it's probably okay to use. SWIM gets lye from the local hardware store, and hasn't ever had to order it online, so he can't answer your question there, but it's used in making biodiesel and soap, among other things, so shouldn't be a big deal to order a kilo or two. SWIM has never found heat to be that necessary with an STB but with an a/b extraction heat can speed up the time that it takes to soak the DMT out of the bark. Multiple acid water soakings must be done with hot water to get out the majority of DMT, but with the STB tek I posted, it eliminates that step, and saves a lot of time and trouble.

 

[ozora]

thanks for your reply spIce-T. S.W.I.M. has read through the extraction method you've posted and will give it a go at a later date once he gets some more experience! S.W.I.M. thinks though for the first one at least he's going to stick with his original plan for the A/B method if for no other reason than he's read it so thoroughly and is psyched up for it now!

S.W.I.M. has also stumbled upon this ..... http://www.behlen.co.uk/Merchant2/m...OD&Product_Code=B650-0056&Category_Code=SOLVE this morning and is wondering if UK based forum users have used it before? is it the genuine stuff or just a convenient product name? S.W.I.M. has read through the product material safety data sheet but other than being slightly horrified at how nasty it can be is none the wiser as to its suitabilty!

S.W.I.M. is getting excited now, if he gets some favourable responses regarding the naphtha above he'll get some (albeit slightly annoyed at the £7.50 delivery charge!) and is ready to go!

 

[GratefulDad]

It seems to be the right stuff, judging from the MSDS. Just to be sure, do an evaporation test, though. And good luck with the a/b, SWIM has performed them many times, and they work great, although they take a lot more time and effort to complete, and sometimes don't yield quite as good without using excessive water that needs to be boiled down to a workable amount.

 

[ozora]

cheers again spIce-T, S.W.I.M. genuinely appreciates your help and hopes one day to be in a position whereby he can do the same for others!

 

[transitory]

Hi ozora

My friend recently contributed to this thread: New UK dude here!. Although the proposed extraction is a STB (Nomans Tek) there may be information there of relevance to you.


My friend has not performed the tek which your friend proposes but he can offer the following comments:

S.W.I.M. obtained 1kg of MHRB from here...mimosahostilis.co.uk

My friend used them and got great yields:wink: - others here have also recommended.​

in the U.K. and having read the forum is now totally confused as to what is a suitable naphtha? S.W.I.M. has so far been unable to source any coleman fuel in the U.K. and is now very worried having read conflicting reports on the suitability of various lighter fluids. which one is the best?​

My friend has succeeded with both Ronsonol & Zippo UK brands but upon evap. testing Swan brand left an oily residue

S.W.I.M. has also stumbled upon this ..... behlen.co.uk/...amp;Category_Code=SOLVE this morning and is wondering if UK based forum users have used it before? is it the genuine stuff or just a convenient product name? S.W.I.M. has read through the product material safety data sheet but other than being slightly horrified at how nasty it can be is none the wiser as to its suitability!​

My friend Hasn't used Behlen Naphtha but it looks like a great find! perhaps a chemist here can decipher the UK Behlen Naphtha MSDS for us. Regardless, as spIce-T says: "Just to be sure, do an evaporation test".

S.W.I.M. is wondering if this is prudent source for sodium hydroxide ... and whether or not it is of suitable quality? S.W.I.M. would be happy to learn of alternative suppliers.​

Sodium hydroxide is a watched chemical in the US (used in meth production). Not sure of its status here in UK. No need to leave an electronic paper trail by ordering online though when it's so easily obtainable over the counter here. Try Wilkinsons. Just ensure it says 100% sodium hydroxide on the container. Your friend doesn't want any other ingredients in there.

attempting to use 1kg of MHRB for his first extraction?​

Having not performed the tek before, my friend would first attempt 500g MHRB (scaling all other quantities accordingly). He also advises not disposing of anything until the desired result is obtained. Almost all problems are resolvable with a little help from your friends here- no matter how lost the situation may appear to be. Until its tipped down the drain that is:wink:.

S.W.I.M. genuinely appreciates your help and hopes one day to be in a position whereby he can do the same for others!​

Your friend already has!- If The Traveler continues graciously to maintain the Nexus then this topic will remain accessible via the search engine for years to come. Future UK psychonauts need not despair8)


Best of luck to your friend - I do hope he continues to update this thread with his progress!

PS: That Liberty Cap avatar is beyond cool:d

 

[ozora]

greetings transitory!

S.W.I.M. thanks you very much for your in depth reply and is taking on board all the advice given with particular reference to the use of the lighter fluids and the purchase of sodium hydroxide.
S.W.I.M. is also relieved to hear that the source of his MHRB is good one and comes recommended. S.W.I.M. also acknowledges the wisdom in not setting his sights to high with regard to amount of MHRB he uses for his first extraction attempt!

S.W.I.M. has taken the plunge and purchased a tin of behlen naphtha (along with a felt tip mahogany scratch fill stick to take the order over the £11 minimum purchase price, he's sure this will come in very handy one day, should he ever posseess anything made of mahogany!)

S.W.I.M. has his fingers crossed that a chemist will look at the UK Behlen Naphtha MSDS sheet and throw some more light on to its suitable (or otherwise) properties.

oh and thank you very much for the kind words about the avatar. the result of some decidedly scary maneuvers with a husky chainsaw and a angle grinder with a sanding disc in it....

(apologies for going massively off-topic, if i've over stepped the mark, moderators please delete the image)

 

[DMTripper]

Hahaha this avatar is awesome! The Liberty Cap has taught me some extremely valuable lessons and I'd love one of those in my garden

Respect and good luck with your extractions

 

[Noman]

Wow! First glance at your avatar, I thought it was a Photoshop job, but damn that's nice work!
I'm not a chemist, but from what I can read of the MSDS, that naptha should do fine. Just make sure that it evaporates clean. I'm sure it will since it's intended as a thinner rather than fuel.
Your pot should be fine with the tiny amount of phosphoric you'll be using too.
Start small - 50 or 100g - before you run the kilo. You'll learn a lot right there about how you want to adapt the procedure for your operation. After that, I'd do half and then the other half for the same reason. Don't worry, that giant kettle won't go to waste, with it you can just extract over and over to pull out all of the goodies and then reduce everything down to a reasonable volume.
I think it's Alcolon 5 that advocates many many acid extractions and claims mad yields? I think he uses phosphoric too.
I'm glad you're starting out with an A/B - they're much more elegant than STB's, especially for large quantities where the lye quantities would just get ridiculous.
Just remember to write everything down, throw nothing away until it's really all over, and post your results.
And don't be shy about posting or PM-ing questions - that's why this forum is here.
Cheers.

 

[ozora]

ok, S.W.I.M. finally got round to doing his extraction. (it was temporarily abandoned due to S.W.I.M.'s freezer giving up the ghost!)

S.W.I.M. in what was probably a foolish act of bravado opted to attempt the whole kilo of mimosa using the A/B method as highlighted in the DMT handbook. S.W.I.M. reduced by half all ingredients (ie naphtha, sodium hydroxide etc) to support his 1 kilo extraction rather than 2 kilo.
S.W.I.M. was happy enough with the way things were going, he reduced his bark tea to one litre and basified the solution using approximately 1/3 litre of water to dissolve the sodium hydroxide. S.W.I.M. then added 150ml of naphtha and shook fairly rigorously for a minute before resting. he repeated this process 10 times and then syphoned off the basified tea bark. S.W.I.M. did 3 pulls like this all in all using 1/2 a litre of naphtha in total.
S.W.I.M. was unable to avoid some of the black oily stuff getting into his naphtha pulls, but at the end he decanted into a glass bowl and when the solution settled he removed the black oil using a pipette.
S.W.I.M. is concerned that instead of ending up with 'a milky solution' (as described in the DMT handbook) he has what can only be described as 'piss' coloured liquid. S.W.I.M. is also concerned that he doesn't have nearly the amount of liquid as the naphtha he added in the first place.
Regardless of this S.W.I.M. has put the liquid in the freezer and will report back in 3 days time as to the results.
S.W.I.M. is also concerned that having left the basified tea bark for a while it now has settled and there appears to be about 8mm of clear naphtha floating on the top. Should S.W.I.M. keep attempting pulls on this? S.W.I.M. is wondering if the reason it took so long for this naphtha to seperate is because the solution had lost all its heat?
S.W.I.M. has thrown nothing away (including the root bark) and would be very grateful for any advice as to how he should progress should he get a low or contiminated yield.
S.W.I.M. has included a photograph of both the solution he has put in the freezer and the basified tea bark he still has left.....

cheers in advance for some much needed help. S.W.I.M. desperately wants this to be a success!

 

[ozora]

update...

this photo was taken several hours after S.W.I.M.s extraction finished...

it now has clearly seperated into three levels. the top level is about 10mm deep and S.W.I.M. is guessing this is naphtha. underneath this is a layer about 4mm in depth and is orangey brown in colour but as can be seen in the photo whiteish floaty bits have formed within it.

would S.W.I.M. be right in assuming he could reheat the contents of his jerry can by placing it in a sink of hot water for a while, shaking, allowing to settle and then do another pull with a syphon?
is there a time scale for doing this (or any other process for seperating these layers)?
would S.W.I.M. need to store his jerry can in any particular way until he can attempt a further seperation?

apologies for bombarding the forum and its members with so many questions!

 

[Macre]

S.W.I.M. obtained 1kg of MHRB from here... http://www.mimosahostilis.co.uk/ .... is this a good supplier?

I spoke to the guy who is this supplier, and he's very helpful. I'm not sure of quality, though I here from third parties it is good. He did tell me there's a backlog on orders at the minute, so orders may take some time to arrive. I too discovered Behlen naphtha, but hasn't heard of it being used yet. I'll be interested to see how everything turns out.

Macre.

 

[ozora]

oh S.W.I.M.'s god!!

S.W.I.M has just returned from the freezer and after draining the naphtha has this...

S.W.I.M. thinks he's very, very happy!

S.W.I.M has a little concern though. in the second of the above photos it can be clearly seen a brownish ring which has obviously been the level of the naphtha he had in the bowl in the freezer. now the liquid is drained of if the bowl is turned upside down this can be seen...

it's the same brownish stain that appears on the 2nd photo and S.W.I.M. assumes it's gonna be tainting the underside of his lovely white goodies. is this a bad thing once the naphtha has completely evoporated and he can scrape the goodies from his bowl??

and S.W.I.M has also one more query with regrd to his post on sunday....

his plastic jerry can has remained undisturbed since sunday and now looks like this...

there's what most certainly appears to be a level of about 15mm at the top of naphtha. could S.W.I.M. just siphon this off and stick it in the freezer and get more goodies despite the fact there's been no heat in the basified bark tea for several days or should he warm the whole lot up again in a sink of hot water before shaking, allowing to settle and then doing a 'pull'?

S.W.I.M. wishes to thank everybody who has helped him on his first exciting adventure. this is an ace place!!

 

[soulfood]

Nice going.

I usually get a yellow to brown ring at the top of my freeze precips. It's just where impurities float to the top and the bit at the bottom is a similar thing. If you want it clean as possible, then you can recrystalise it and it should all seem pretty clean, but I wouldn't worry about that for myself.

I don't use heat at all for my pulls. That naptha should be fairly loaded as is, if it has slowly seperated especially. Heated pulls seem to yield yellower spice. I usually do cold pulls until exhausted then switch to a stronger solvent.

Actually, I've just realised you have a fair bit of spice there. It may be worth recrystalising.

 

[Macre]

I must admit, I did get excited when I discovered Behlen Naphtha. But I didn't have an idea how it would perform, though my gut instinct was smiling.

I'm happy to see your extraction is going well, particularly as you have the same MHRB supplier as me. I thought everything would be A Okay, the dudes cool. I'm happy to see everything's going okay for you, and it relieves a few of my worries too, I must admit. But I'm genuinely happy for you, and I do mean that.

Anyway thanks for sharing, you've been a great help.

Enjoy the spice,

Macre.

 

[Aegle]

Ozora

Welcome, awesome avatar by the way. Good luck with your spice journey as i can see its underway.


Much Peace

 

[transitory]

Ozora

Thanks for updating. Congratulations on what would appear to be a very successful first extraction! 8)

As soulfood says, the remaining naphtha which has slowly separated from the base liquid will likely contain a significant quantity of DMT. It would certainly be worth trying to precipitate this. Reheating/shaking would IMHO do no harm. Reheating may pull more impurities along with DMT but these can be cleaned up later (sodium carbonate wash). It may be to your advantage to evaporate this final naphtha pull by 50% before freeze precipitation in order to ensure sufficient saturation of the solution.

The discolouration on the base of the bowl can be corrected with a recrystallization. I think that you would be pleased with the results.


I do hope that you continue to update this thread. The detailed account which you've so far provided will be helping others along the way.

Bon Voyage! :d

 

[ozora]

hello everyone!

been a little while now since S.W.I.M. last updated his thread but he feels the following information might be of use to those like himself who are taking their first tentative steps into the land of extractions!

armed with his notes from the DMT handbook S.W.I.M. set himself the probably ludicrous (for a complete and utter novice) target of emulating the author of the above tec and therefore achieving a respective yield of approximately 6.5gs from his 1kg of MHRB.

after the initial elation of discovering what appeared to be a large amount of spice (pictured above in his last post) following on from freeze precip S.W.I.M. was disappointed (perhaps puzzled might be a better expression?) to discover that after drying his extraction had infact yielded only 2.6gs of spice. so where could he have gone wrong?

two things stood out to S.W.I.M. where he had perhaps erred from the step by step guide...

a) on his first acid cook he thinks he might not have used sufficient water. on draining he acieved only about 1/3 litre of bark tea. it was a mistake he didn't repeat with the next two boils however and in total after 3 boils he ended up with approximately 2.5 litres of tea before reduction. doubts were lingering though that perhaps S.W.I.M. had messed up with the first boil and that maybe he hadn't exhausted his MHRB ?

b) after reducing his bark tea to 1 litre S.W.I.M. used 100gs of sodium hydroxide to basify, he wondered if it was possible that he'd used too much water to dissolve this in (a quantity isn't stipulated in the handbook) and therefore hadn't achieved the required ph14 ? he confesses he didn't check this at the time with litmus paper!

other than the above though S.W.I.M. is convinced he followed the subsequent steps ie 'shaking' 'resting' and 'pulling' 3 times very accurately. so where were his missing 4gs ?

following on from the kind advice given in this thread (and via p.m.) S.W.I.M. pulled again from the naphtha (pictured above in his last post) which had remained undisturbed in his jerry can for several days and stuck it in the freezer for 3 days.... result another 1.4gs of spice after drying.... excellent, but..... still someway short of the 6.5gs he outrageously thought he should get!

S.W.I.M. had kept the naphtha from his initial 2.6g pull and he combined it with the naphtha from his second attempt, poured it all back into the jerry can and shook it about like a mad man for several minutes and then let it rest for 24 hours. he siphoned the naphtha off, stuck it in the freezer and 3 days later.... a further 2.3gs of lovely goodies, S.W.I.M was ecstatic! a total now had been achieved of over 6g and it seemed apparent that the better yield in the 3rd go had been a result of the violent shaking the 2nd one hadn't recieved.

bouyed on by his success S.W.I.M. thought he had nothing to lose by again recycling his naphtha so once more he stuck it back in the jerry can, shook it about like lunatic and left it to settle etc and 2 days ago got a further 1.3g of white/yellowy spice! that's 7.6g now in total. where does this all end??!! this beyond S.W.I.M.s wildest expectations!

is it worth another go? it would certainly appear that despite the halfing in the yield between the 3rd and 4th freeze precips the quality of the spice 'looks' no different. could it be that 'looks' are decieving and that he is infact now getting an inferior product?? S.W.I.M. is of the opinion he has nothing to lose in going once more and that he can expect yields to lessen to the point whereby it's not worth the effort anymore. is that the case??

all in all S.W.I.M. is absolutely delighted with his venture. with his first 2.6gs of spice he made a changa (or enhanced leaf) mix at a ratio of 1:1.5 using blue lotus and calea and was absolutely blown away by the results! in the true spirit of dmt and this forum he has shared his spoils not only with seasoned travellers but also with adventures new. all of whom have been as delighted with S.W.I.M.s 'product' as he has!

S.W.I.M. has kept seperate the spice from each of his pulls and has a total of roughly 5g in three seperate little containers. his goal is now to decide in which way to use it. he will certainly try different changa combinations and is plucking up courage (remembering his very limited chemistry knowledge!) to attempt the next step of refining his product that little bit further.

the journey has just began!

peace and love to you all.

 

[acolon_5]

cheers again spIce-T, S.W.I.M. genuinely appreciates your help and hopes one day to be in a position whereby he can do the same for others!

FYI, you don't have to do the SWIM thing here. In fact it's kind of discouraged. If you really want a disclaimer it's best to put it in your signature.

Phosphoric acid is a good acid to use...I think it works a lot better than vinegar.

A couple of things to help you out on your extraction:

1) you can use as much water as needed. Personally, I fill up my crock up 1-2" above the mimosa level each and every cook. I also use less and less acid each cook. I usually will do a total of 4+ cooks, between 1-4 hours each, on low/medium. Your bark is 100% spent when it turns greyish and the water from the cooks turns yellow or very light red.

2) You don't need to add much lye. when the color changes from red to BLACK (not grey) you are pretty much there. This depends on how much acid was used in the initial cook. But 100g sounds like a bit too much. This won't mess up your yield though, just a bit wasteful.

3) Naphtha (solvent) pulls. The easiest way to do this is as follows:

right after basifying your jugs, add 100mL naphtha
Shake gently, or better yet just swirll it around alot, agitate it as much as possible without forming too many emulsions. IF emulsions form add table salt (it works) and heat the jug.

After 5-10 minutes pull out the 100mL naphtha and stick it in a mason jar

Add a fresh 100mL into the jug, repeat agitation
remove 100mL from jug and combine with prior pull (should have 200mL naphtha in a mason jar). Stick this mason jar into the freezer.

While the jar is in the freezer add yet another 100mL to the jar. Agitate and leave for a few hours. The jar in the freezer should be clear and you should have a mass of xtals at the bottom.

Decant the naphtha into another jar (make sure you get ALL the naphtha out, turn it upside down for 2-3 minutes, don't worry the spice won't fall out).

Remove 100ml from your mimosa jug, put into mason jar and stick in the freezer
Add 200mL from your first 2 naphtha pulls back into the mimosa jug.

Now you have 100ml naphtha in a jar in the freezer and 200mL in the mimosa jug.

Swap naphtha over and over, collecting spice as you go. This method will have naphtha in the freezer and the jug at the same time, the entire time during your solvent pulls.

Stop when you are not getting any more spice falling out in the freezer.

This is an excellent way to exhaust your mimosa jug in the least amount of time...no evaporating of naphtha, no waiting, no liter of solvent used per kilo of bark.....and this has produced the best yields for me. I've done many, many, MANY spice extractions and the method I just described took many different failure to get to.

Your yield is really low, but I'm glad you did have success on your first try.

Give my suggestions a try and see what kind of yield you get next time.

Also, if you haven't figured out an easy way to seperate the solvent from the basified mimosa here is a little tip. use a milk jug that has a tapered top. Get a nasal aspirator (aka ear syringe). When it's time to remove the solvent squeeze the milk jug gently until the solvent is all the way at the top, suction off with the nasal aspirator (don't worry naphtha doesn't eat this type of plastic, so no plstic contamination). You should be able to get most of the naphtha off very quickly using this method. Leaving a bit of naphtha behind is not a problem, it will get picked up the next go around. By the end the naphtha left in the jug will contain almost no spice, so you are not wasting anything.

best of luck!

 

[ozora]

FYI, you don't have to do the SWIM thing here. In fact it's kind of discouraged. If you really want a disclaimer it's best to put it in your signature.

cheers for that. to be honest as very much a newcomer to the forum and having read only a fraction of it, it seemed the use of 'S.W.I.M.' was split about 50/50. as someone who very rarely uses capitals when typing as the norm it'll come as a great relief in future to find that i don't have to retype half my bloody post again because i've forgotten to re-hit the cap-lock button off after 's.w.i.m.' and a high percentage of the post had been 'shouted', i had no idea it was slightly frowned upon!

Your yield is really low

crikey.

i was basing the percentage spice from mhrb target to aim for using the dmt handbook as a guide. in that it stipulates a yield of 13.4g from 2kg which it states is a 'very high 0.67%' and that 'the average is 0.4 to 0.5%'

as i'd got 7.6g from 1kg (or 0.76%) i was feeling rather chuffed with myself albeit being an admitedly stretched and drawn out affair! what percentage should i be aiming for?

i really appreciate your reply and take on aboard all of its content. not least with reference to when the mhrb is exhausted. i've not thrown it away yet (as i said above i was a bit concerned it might not have been spent) and can confirm it certainly isn't grey in colour, nor had the water turned yellow. in fact a quick check just now has revealed the powder which has been stored in sealable plastic bags is dark brown/purpleish in colour. (the darkness maybe in part due to it still being damp although there is no evidence at all of any mould)
i'd most certainly considered further cooks with the phosphoric acid anyway, your reply has prompted this as a certainty in the very near future, infact prbably this weekend!

i'm here as a willing learner and also a one who appreciates he has much to learn. all help is gratefully recieved. if in turn my continuation of this thread benefits others than all the better!

take it easy sir.