Where has Jules got to?,my process was basically following his first attempt but with a different acid,it wouldnt be fair for me to post it up before his
I think the only thing Methylate brings to the party is potentially less soap in the bio due to the lack of water produced.
NaOH or KOH would work just as well except that slightly more acid may be needed.
Sulphuric acid is so cheap and you need to little that I suspect it may work out cheaper than vinegar.
I have given some acid and Bromophenol blue to Bob (Photoman290 on VOD) for him to have a go with in his new processor.
Using this method really reduces the amount of kit needed.
No need for a separate bubbling/settling tank and no need for a consdenser as there is no methanol to recover (the small amount left in the bio after draining the second stage glyc goes out with the wash water).
If you use pre-pump injection of methoxide then there is no real need for a venturi and, if you get the oil to full process temperature before it goes into the processor (using a boiler, electric overnight heating etc) then you dont even need and inline or in processor heater.
I get my oil to 70C at the start of the day. Then glyc wash, then two stage process then in processor water was by this method.
Even after two cold water washes the bio is still at 35C to 40C at the end of the process with no extra heat added at any stage.
Has anyone tried titrating the finished bio?Mine tested at 7.5
If the acid turns the soaps to FFAs, are you sure they are all washed out during the washes or have you got acid bio?
Just a thought.
Can you measure the ph of Bio? I thought you could only measure the ph of water based liquids.Used a couple of indicators to get a rough idea,not very scientific admittedly
Am watching this with interest, as my processor will be built over the weekend.( Hopefully )Nice to see you on here Mark
I used to water wash (mist) about 4 the the volume of bio.
This sounds perfect.
Has anyone tried titrating the finished bio?
If the acid turns the soaps to FFAs, are you sure they are all washed out during the washes or have you got acid bio?
Just a thought.
Can you measure the ph of Bio? I thought you could only measure the ph of water based liquids.I don know,I used two different indicators to get to 7.5 and the other half took a sample to the sci dept on Mon and there ph tester also said 7.5
Good point, but a while back I wanted to find out about the 3/27 test. There was a post on the VOD stating that a cloudy result indicated MGs and DGs.
I'd not seen that before and spent a great deal of time looking for the earliest mention of the 3/27 test. I eventually found that Jan Warnqvist emailed it to Biofuel mailing list in Aug 2005., and there was no mention of MGs and DGs. When this was pointed out to the poster, he withdrew the comments.
this method sounds very interesting.where can i buy the acids needed to give this a got
thanks william
With this system you can use any acidic liquid you just need to do the titration with the same solution.
Paul
This is one for keith really. With such a short wash cycle ie 2 washes...does this completely deplete the amount of methanol within the biodiesel. Have you used your alcohol tester to check on the percentage of methanol left behind.I never gave that a thought Nigel,good thinking,i intend doing another batch tomorrow to double check my method so i will check the washes for methanol as well
Nige
I noticed the bottles i used said 5% acidity,not sure what that means?
Thats a better price than the sarsons i had to get.I noticed the bottles i used said 5% acidity,not sure what that means?
I think its simply the strength. As Mark says, not all vinegar is as potent / concentrated.
Asda does, i think 5 or 600 ml bottles of brown vinegar for about 8p a hit (or at least did when i wanted some last). I doubt it is that strong (i dont have a bottle to hand to check) but i used a whole load of them once for stripping some rust, and they worked for that.
Depending on how the titration quantities work, that may be a convenient source of less scary acid, for not loads of money.
Incidentally, my first and last water washing attempt ended in emulsion - i had some of these left over then, and they split the emulsion well - i dont recall having to use that many of them?
Jules, I always find strip down and rebuild time very scary.Nooooo thats the most enjoyable bit,i much prefer messing about with the processor as opposed to actually brewing a batch (unless theres something new to do) thats probably why im on No 4
It's that need to get brewing again before you have to visit the tax station that makes me cut corners,
or at least get it up and running before everything is just how I planed it,
my shed is still not finished and I just don't seem to find the time.
I'm going to try the next batch with 85% phosphoric acid.I brought some Brick acid home today,9% Hydrochloric, so i will test that next,at that strength its a sort of happy medium and easy enough to obtain
There would be no real reason to do this as it is quite expensive (I got it at a bargain basement price and was still £2.50 a litre) but I have around 15 litres or so of it so I will give it a go
The processor is now in piece for a while so I can move it all and rebuild the bund for it in a better position.
Interestingly the bio/veg/glyc/water combination that had accumulated in the bund had seriously degraded the concrete blocks and mortar and was starting to leak out across the floor.
The new bund is going to be lined with 18mm OSB plywood then covered in fibreglass which seems to be immune to everything.
It's a good time to strip the processor back to the basic requirements needed for this method too.
It would take about 2 of the bottles (568 ml) to do a titrated wash on a 125 litre batch,how much do you think you used to split that emulsion roughly?
Jules, I always find strip down and rebuild time very scary.Nooooo thats the most enjoyable bit,i much prefer messing about with the processor as opposed to actually brewing a batch (unless theres something new to do) thats probably why im on No 4
It's that need to get brewing again before you have to visit the tax station that makes me cut corners,
or at least get it up and running before everything is just how I planed it,
my shed is still not finished and I just don't seem to find the time.
I know that Nigel took water samples from a few of us at last years BBB to test if the differing hardness affected 50/50,s which it did,i think that was one reason he came up with the soap test kits.
Im sat on limestone so our water is very hard
I know that Nigel took water samples from a few of us at last years BBB to test if the differing hardness affected 50/50,s which it did,i think that was one reason he came up with the soap test kits.
Im sat on limestone so our water is very hard
very interesting,
i have noticed that no one has mentioned blanking the ipa/methanol befoer adding the bio, would it not be a good idea to get an accurate result?
As we used universal indicator it proved our methanol to be neutral before we added bio
I'll bubble overnight.
Just a follow up, how do you test KH?Used universal indicator and it showed it not far off neutral,im not saying this method worked,just what result i got :)
Remember with this process you are only really looking to neutralise any excess base chemicals that could cause soap formation when adding water as the excess soap formed can lead to emulsion when water is added with too much agitation.
Hi all
Having spoken to Mark I think he's going to be ok as he did several water washes after over dosing so should have washed the acid out. As for different proforming vehicle's I think that by overdosing on hydrachloric by so much he may have broken the methyel ester bond leaving him with FFA's or depending on temp and agitation and how much free glycerine was in the bio at the time he could many have produced some mono's or diglycerides ( not sure about this but will be doing some tests soon along side testing a theory on hmpe's ).
If anyone get's hmpe's can you please save me them as I think I may be able to prevent them in the wbd system but need different sorts to get some proper results.
Cheers
Paul
right chaps, I've been trying too keep up on this thread even though I'm more than happy with my method and not thinking of changing, but as ever just trying to simplify/clarify things
But ifn we assume folks have done a reasonable conversion and haven't used to much catalyst you should be able to work out some rough guidelines for amounts of acid per litre to neutralise the soaps created from good oil thyrough to bad oil?
And assuming someone did use a little too much would that cause any major problems, except needing more water to remove?
EDIT: just read Nathans post it's where I'm leaning
I'd be very interested in that Chug.
I haven't tried to titrate bio and Glyc yet but I would assume that taking a sample while the batch is mixing then drawing 1 ml straight away and dissolving ipa should give close indication.
I'm going to try some test batches tomorrow if I can with some new oil .
Mark..the indicator in the soap kits is Bromophenol Blue not Bromothymol Blue
Nige, can you get me some bromothymol please? I can pop over when I'm back 4th or 5th, I'll have a bit of the sulphuric to to try out. Thanks.
Nige, can you get me some bromothymol please? I can pop over when I'm back 4th or 5th, I'll have a bit of the sulphuric to to try out. Thanks.
I've just emailed the company and am now awaiting a response regarding collection.
What's the thoughts on phosphoric?
I've got quite a few bottles of Bromophenol Blue, if you some anything urgently!
I've got quite a few bottles of Bromophenol Blue, if you some anything urgently!
I too have a ready supply of Bromophenol Blue Nathan....however, my post to Richard was about Bromothymol Blue.
I've got quite a few bottles of Bromophenol Blue, if you some anything urgently!
I too have a ready supply of Bromophenol Blue Nathan....however, my post to Richard was about Bromothymol Blue.
Realise that you have a supply, implied by the soap test kits and earlier posts on this thread. I was saying that I have a number of bottles of this that I won't be using.
If you are using vinegar then the easy way is to add maybe 1/2 L and mix then do a 50/50 water test . If the water is cloudy then add another 1/2L , do this until the settled water is clear (ish ) then you know your ready to go onto the water wash.
With vinegar I think it would be hard to overdose , the excess will be washed out with the water wash
Paul
If you are using vinegar then the easy way is to add maybe 1/2 L and mix then do a 50/50 water test . If the water is cloudy then add another 1/2L , do this until the settled water is clear (ish ) then you know your ready to go onto the water wash.
With vinegar I think it would be hard to overdose , the excess will be washed out with the water wash
Paul
Thanks. So I add the vineagar to the bio without adding water, then when 50/50 clearish I can start to add water?
Can this be done at ambient temp. or do I need to heat?
Dawson
If you are using vinegar then the easy way is to add maybe 1/2 L and mix then do a 50/50 water test . If the water is cloudy then add another 1/2L , do this until the settled water is clear (ish ) then you know your ready to go onto the water wash.
With vinegar I think it would be hard to overdose , the excess will be washed out with the water wash
Paul
Thanks. So I add the vineagar to the bio without adding water, then when 50/50 clearish I can start to add water?
Can this be done at ambient temp. or do I need to heat?
Dawson
I've been using this method, so have others and it works very well! The last batch was pump washed to a crystal clear 50/50 (very aggressive shakeup) using just three bucket of water. It seems less fiddly than doing a soap test.
Ok guys, I've added 1.5 ltrs vinegar and a 50/50 looks good. Just one more question..
Do I let the vinegar settle then drain, THEN add the water
or
Just add the water straight away?
Sorry for basic questions but i want to do it right.
dawson
Can't wait to try the ASM - I hate Koh!!
Dawson
Thanks Nige!
Quick update.. I'm on my 10th wash is this normal? The sample still shows cloudy water. Guess I'll just keep going.
(http://i1023.photobucket.com/albums/af359/DawsonBullock/Image128.jpg)
I'm on my 6th wash now. I'm adding 10 L water at a time to 75L bio. I knew this batch would be soapy due to running out of sodium and wanting to use up the potassium I still have. I used a whopping 1Kg to convert this batch (usually only around 400g)!!
Can't wait to try the ASM - I hate Koh!!
Dawson
I'm on my 6th wash now. I'm adding 10 L water at a time to 75L bio. I knew this batch would be soapy due to running out of sodium and wanting to use up the potassium I still have. I used a whopping 1Kg to convert this batch (usually only around 400g)!!Did you do a 10/90?
Can't wait to try the ASM - I hate Koh!!
Dawson
I've got to be quick
I think you meth is duff or your oil was very wet .
This is why you needed so much base chems
Leave it to settle over night . Drop the water put more vinegar in
This batch could take some time
Very emulsified to me, too much base I think this is why I think it was wet oil/meth this is what held back the reaction.
The problem is that the stage fails so you add more base when realy it just needs dry meth, this means that when you get final completion it's massively over dosed with base
Hi Dawson
How long are you leaving the water to settle and how long are you mixing the water
It's my guess that had Dawson not used the acid wash method that he would most likely of had a massive emulsion on his hands.
Don't give up on it. Some water washing sceptics have now been converted using the titrated wash method. That carries an awful lot of weight in my book.
Nige
If i was short on meth on first stage would this be the reason i used so much caustic? I did dry the oil before use via condenser until no drips.
Don't give up on it. Some water washing sceptics have now been converted using the titrated wash method. That carries an awful lot of weight in my book.
Nige
I was one of those sceptics, I started my bio life using demeth and settle,
I then started mist washing like Nige, but suffered emulsions (probably due to pore convertions).
Now after a few years of going back to demeth and settle I've again gone to water washing, but this time it's the titrated acid pump wash method.
So as you can see I've tried a few different ways to remove the soaps, and I'm now completely sold on washing.
1. Are you still doing it?
2. Have you changed your process at all?
1. Are you still doing it?
2. Have you changed your process at all?
I. Tried it but found it to be an unnecessary additional stage.
2. As the "dead man walking" above, returned to the post reaction 5/7% water wash.
Dead Womble walking, please get it right.
;D ;D ;D ;D ;D ;D ;D ;D ;D ;D ;D
Dead Womble walking, please get it right.
Feel free to use either phrase, the result will be the same.
Just another wooden cross in the corner of a distant field.
Sorry to disappoint, but if I loose my setup I'll not be attending the BBB,
how can I turn up with diesel in the tank, that's a hanging offence as it is.
Sorry to disappoint, but if I loose my setup I'll not be attending the BBB,
how can I turn up with diesel in the tank, that's a hanging offence as it is.
Just turning up is a hanging offence in your case and I know where you live, there's no escape.
So does that mean after 17 pages singing it's praises no-one now does it and it's not worth doing?
Im still doing it, cuts my wash time down considerably
So does that mean after 17 pages singing it's praises no-one now does it and it's not worth doing?
I use Sulphuric (From Nigel ) now and do 3 pump washes in the processor, then its transferred to the non overflowing mist wash tank where i just send 25 litres of water through to give it a final washIm still doing it, cuts my wash time down considerably
Could I ask what routine you have settled into with it and how it cuts the time compared to what you did before?
Thanks
So does that mean after 17 pages singing it's praises no-one now does it and it's not worth doing?
Wow. Your brave, asking a question like that.
I hope you get better answers than when I asked the same people on vod, "what are the advantages of acid washing" someone not only spat his dummy at me but chucked his toys as well. Lol.
What more can you ask for? the seal of approval from the soap king
I will stick a more interesting one on thereWhat more can you ask for? the seal of approval from the soap king
Praise indeed from the only scatologist on the forum.
Please don't.Too late
No.
We've tested it, It's been proved to work, some are still using it.
It's all about what each brewer finds works for him,
with so many ways of finishing our fuel there should be something for everyone.
Wow. Your brave, asking a question like that.
Not ALWAYS. The PC is usually on if I'm at home and I'll check the forum when I pass the PC!
I've been looking at exactly the same thing this evening. I did a 7% water wash with the glycerine (won't need glogs for a few months hopefully) and tried a shake up test afterwards ... results don't look promising, so I'll probably have to go back to titration for soap and add acid. Strange when I keep reducing the ASM.
After 7 previous batches with varying degrees of minor problems (but ultimate success), I just tried my first batch using this titrated water wash, and I failed :-(
I'm using universal indicator and mixed it with meth as per the wiki, it turned a little yellow so I added a drop of KOH reference solution which turned it nicely green, no probs.
Then when I added my bio it stayed green, and no amount of shaking or threatening it made any difference. I repeated the process with the same result. Just to make sure I didn't have a dud indicator I added a few more drops of KOH reference and it duly turned blue.
I should say that I processed using 4 stages, with each 10/90 returning less unprocessed oil until I got a pass. I deliberately do this as it's not a lot of extra effort and I know it should minimise soap production, but I wasn't expecting ph neutral!
Any suggestions? I've emptied it into my settling tank as I have to do another batch, but does this mean I could have washed it in the processor (as if I'd added acid) without fear of forming an emulsion?
Any insights gratefully received!
Mike
I've been playing with gradual additions until I get colour and viscosity changes coupled with a temperature rise.
It's detailed on another thread, I'll try and find it.
I assume it's the exothermic reaction taking place.
Last few batches I've only had to use minimal acid as I'm gradually cutting down on the catalist I use.