AH, What am I doing wrong!?!?

[Bio Popo Member Find all posts View Profile Close Bio Popo]

I am getting fed up....all the postings on the internet and forums make doing a 1L test-batch with new veg oil seem so easy, but I have made two now and they have both been unsucessful.
I am using the 'Dr. Pepper' method.
I am using new Canola oil and KOH.
I measure out 5.5g of KOH (90% purity) and add to 200mL of methanol in a HDPE old 2L milk container (cleaned and dried) and mix until all of the KOH is dissolved. I heat the oil to 55C and pour into another 2L HDPE juice container. I then add the methoxide to the oil and shake vigorously for a minute or so over a half hour period (the first batch) or just for 30 seconds (the second batch). I then leave to settle for 24 hours. After I get a clear seperation that appears good. BUT when I do the quality-test as posted on J2F (adding 150mL of water to 150mL of unwashed biodiesel, shake violently for 10 seconds, and watch for separation), I fail miserably. Both times after shaking it turned to a mayoinasse looking substance and failed to separate completely in under 30 minutes as it should. In fact, the only separation that occurs in 30 minutes is about a centimetre of yellow looking oil with white foamy floaties, sitting on a large layer of white creamy stuff.
So, yeah, I am dismayed.
The J2F website suggests 5 possible reasons:
1) better titration - I'm using new oil so no titration was done or needed
2) try more methanol - I don't see this as mattering too much bc some people say to use 200ml/L oil and some say 250ml/L oil.
3) Better agitation - I shake violently and appear to VERY thoroughly mix the liquids
4) longer processing time - the inventor of the Dr. Pepper method only says to shake for 10s, whereas J2F says to process for an hour. I have done both and neither works
5) better temperature control - I heat the oil to 55C and use it right away, I don't see this as being the issue either

One thing that I can think of, is that the inventor of the Dr. Pepper method mentioned that when mixing the oil and methoxide there should be no noticeable pressure produced, but mine has both times. Maybe I'm doing something really wrong?

I know this was a long post and if you read it all, thank you, I would really appreciate any advice as I am DYING to get on with it and make 15L batches!

Dave

[geewizztoo Senior Member Find all posts View Profile Close geewizztoo]

Re: AH, What am I doing wrong!?!?

Hi Dave, chin up, you're almost there,

Two things about your post get my attention. The first and most important is that I'm pretty sure the JTF quality test refers to fully washed BD not unwashed. If it doesn't then it should! The water test is to check if there's any residual soaps left after washing. When the BD is clean it will separate rapidly from the water and the water will be sparkling clear.

Vigorously shaking freshly made BD with water is almost certainly going to create an emulsion.

I suggest you try washing it first. Take your freshly made BD and carefully pour in the water down the insides of your juice bottle. Then GENTLY invert it 5 or 6 times, no more, let it stand for an hour or two and the water should be milky and the BD opaque like orange juice.
Drain the water and repeat this procedure 3 or 4 more times or until the water stays clear. Each successive wash you can be a bit more vigorous with the mixing. There might even be some white floaty bits at the water/BD interface, this is normal. You can use warm tap water to speed up the process.

Your clean BD will be wet at this stage, it will still be opaque and needs drying. Separate the BD from the water and leave it in an open conainer in the sun for a few days and it will clear. Alternatively heat it in the microwave to drive out the water or blow bubbles, from an aquarium pump, through it for a couple of days. At this point you can try the water shake test.

The second point is that the base amount of KOH should be 7g/L, (7.7g for 90% purity) to ensure maximum conversion, 200ml methanol/L oil is OK. Washing becomes more difficult if you have unreacted veg oil in the BD.

But for now, try the gentle washing first.

Also, when you've mastered this, read the thread on 'Water washing'

[Bio Popo Member Find all posts View Profile Close Bio Popo]

Re: AH, What am I doing wrong!?!?

Hey, Thanks geewitzo....
This watering method though, of pouring the water down the sides and inverting a few times, could I use that same method for a 15L batch? I've processed it in a 20L carboy and am looking to wash it now.
Thanks,
Dave
p.s. when you say 'invert', do you mean slowly turning the container upside down, and then upright again?

[geewizztoo Senior Member Find all posts View Profile Close geewizztoo]

Re: AH, What am I doing wrong!?!?

Hi Dave,

Yes, all I mean by saying pour it down the sides is add the water carefully, without excessive splashing or aggitation of the BD. When I was making small batches in a 20L pail, I added the water using a funnel with a short length of tube attached to the spout so I could direct the water to the bottom of the bucket. But I think I was being over cautious in the beginning.

With virgin oil and the correct catalyst/methanol ratio, your BD should be quite tolerant of water being poured gently on top.

And yes, inverting means gently turning the container over a few times. Should work for any sealed container as long as you can pick it up. Why not just buy yourself a $10 aquarium pump and blow bubbles through it, and you can use this for drying too. Make sure you regulate the bubbles to a small & steady stream using a $1 tap from the same pet shop.

[Bio Popo Member Find all posts View Profile Close Bio Popo]

Re: AH, What am I doing wrong!?!?

Ok, well, today I tried washing. It went horrible. I don't know how but I wound up with about 30% conversion!! I started with 15L of oil and ended up with what looks like maybe 5L of biodiesel! The whole thing was just SO much trouble....I think I'm just going to switch over to doing a 5% pre-wash.

[Terry Syd Senior Member Find all posts View Profile Close Terry Syd]

Re: AH, What am I doing wrong!?!?

If you do not have problems with the disposal of the glycerin, then you could increase the pre-wash to 10% of the oil. You will get a pretty good pre-wash at that level, but it will also create about another 50% of byproduct for you to dispose of.

[dillyman Senior Member Find all posts View Profile Close dillyman]

Re: AH, What am I doing wrong!?!?

Hi Guys,

Looking at your postings with interest. Geewizztoo, I thought that JtoF quality testing was checking for quality of processing before the wash. I did that with a 150 ml and got a dense cloudy water in rapid seperation, with crystal clear bd. Are you saying this does not indicate anything? This is my first 100 litre batch. I will post digi's of the test sample after 2 hour mixing and 500ml sample post process (I split in two) the second sample I gave it a pre-wash (messed up though and put more like 15% water instead of 5%(Mea Culpa!) leaving both samples to settle till I was able to drain the glycerin. I did this after 20 hours (the settling was from Tery Syd's suggestion of a good settling period without draing the glycerin. Boy! I could not believe the difference in the samples 2 samples. If this reaction happens after pre-wash boy is that for me. Will post pics later today, the pre-wash looks fantastic - more Glycerin than BD. Will post later

[tillyfromparadise Senior Member Find all posts View Profile Close tillyfromparadise]

Re: AH, What am I doing wrong!?!?

Hello dillyman
The "Shake-um up" test on the JTF Crapolla mis-information site is not a meaningful check for much of anything.
It is a pretty good test for spotting unwashed biodiesel.
It is a meaningless test for conversion of your oil.

You said: "I did that with a 150 ml and got a dense cloudy water in rapid seperation, with crystal clear bd."
Can you be more specific,I have never seen water and biodiesel which is violently mixed seperate to cloudy water and crystal clear biodiesel.
Every time I have done it the biodiesel is cloudy as well.

Tilly

[dillyman Senior Member Find all posts View Profile Close dillyman]

Re: AH, What am I doing wrong!?!?

Hi Tilly,

Thank you for your response. I tried to post pics earlier, camera battery gone flat. I will post soonest. I feel a bit like Bo, Most of my info was from J to F. Been devouring the stuff for weeks ready to go. Luckily I asked for advice from Joe at Brissy, otherwise, my titration would have been off also. I will await battery charging (2 hours) then post. It will give me time to contemplate the 100 litres in my wash tank and the other 100 I processed yesterday late afternoon. I will then try and pick myself up off the floor. It looks as though I could have St----- U big time.

Cheers Tilly,

Dillyman

[joe Moderator Find all posts View Profile Close joe]

Re: AH, What am I doing wrong!?!?

Hi all,

boy has this thread been a mash up of basic and advanced tips and tricks.

I'd be urging the newbies here to forget about the shake 'em up test, washing, prewashes and all of that other "advanced" doodad for the moment. It can all be a bit daunting.

The original problem was that 'bio pop' flew past successfully producing a batch of biodiesel (of what ever grade) and instead of drinking to that milestone Dave went on to mar his success by going on to produce some mayonnaise.

Bio you appear to have made biodiesel. Well done.... If you continue doing what your doing for that phase of production you will probably never look back. So hold up your glass and look forward to what you'll be doing next.

I'm not going to advocate "washing" or "not washing" at this time but I would suggest if your not sure which way you wish to progress that you take the time to read all of the information available about the whole washing discussion. Washing involves water (and quite a lot of it if your not recycling it) other specialised equipment that can be readily obtained, power in some shape or form and drying (more energy). Not washing involves time and gravity and loads of storage space.

I've laboured over what I wanted to say in all of this, but the good advice in this thread seemed to be getting lost. I thought that the more experienced crew in here should take a step back, recognise each milestone and treat each step as its own chapter.

Bio, also 90% purity for the KOH; I'd be desperate to find out what the other 10% is.


Joe

[tillyfromparadise Senior Member Find all posts View Profile Close tillyfromparadise]

Re: AH, What am I doing wrong!?!?

Hello Joe,
This exact discussion is also occuring at infopop where I have answered Bio Popo's questions.
http://biodiesel.infopop.cc/groupee/...1/m/3071079931

As I have answered his questions there I did not bother to also answer them here.

Making biodiesel is so easy it should be illegal!

Tilly

[Dodge Senior Member Find all posts View Profile Close Dodge]

Koh

Tilly why 7.8g koh i thought for 90% pure koh it was 5.44 grams.

[dillyman Senior Member Find all posts View Profile Close dillyman]

Re: AH, What am I doing wrong!?!?

Hi Joe,

Reading your postings this morning, brings to mind some comments you made way back. If I remember correctly you were about to do something with recipe, but, decided it had been done to death, so would leave it alone. For me, I think it is a great idea to have our own setup. I can remember a few days ago, I asked for some quick advice from you. Thankfully I did - things moved on from then for me. 2 X 100 litre processes, the first one I ended up almost like Bio Pop, certainly not far off. Have cleared most of it with reuse of the glycerin, some hot water settling and further washes, (heck of a lot of time). Water was reasonable clear with .2 of PH higher than tap water. I though well one more wash, so I used a 50mm piece of wood as a paddle (as my stirrer is a problem) and gently mixed it very slowly until I had a mix. awaiting the results this morning (after a cuppa), tongue in cheek as it seems any amount of stirring causes the dreaded big E I really believe that if J to F is so poor on guidance, how about we as a forum do something about it ourselves as you previously suggested. I read and re read J to F almost like a bible for weeks. Now I hear it is not so crash hot. I also will check this morning another 100 Ltr batch I drained off the Glycerin yesterday. I will be posting pics in reply to comments from Tilly, have to reduce resolution to fit in with posting first but will be done today. I feel tempted at this stage to to do pre was and settle for 5 days.( Not finding any solutions like that though) At present feel quite desperate. "Will not give in".

Rgds

Dillyman

[dillyman Senior Member Find all posts View Profile Close dillyman]

Re: AH, What am I doing wrong!?!?

Hi Everybody,

I have just checked my wash tank. The last thing I did yesterday to try and move PH from 7.8 to to PH 7.6 (as is the town supply.) I added 20 Lt's of cold water and siphoned it below the surface as to not over agitate. Slow stirred with a flat 50mm stick and this morning, a drum full of lovely emulsion, (granted it is a bit thinner in viscosity, but this time its the whole tank) Stirring with the stick, I felt like a slow movie of Charlie Chaplan in slow motion.
Yesterdays 2 - 1lt trials have settled and the first - my standard, processed and settled. This morning at 6am was cloudy now at 9 am it has cleared to about 25 mm heavy glycerin the rest is almost perfectly clear - light honey colour - can see fingers through it, not pristine like the pre wash settled out at first but very clear. (pre wash clouded overnight anyway)
I feel perhaps I will go back to some 1 Lt trials and use different methoxide mix. The mix I was using was 20 Litres Methanol + 900gms of KOH (99.9%)This is a base of 7gms for wvo + titration which was 2gms per litre for 100 litre batch. Although the Processing seems to go exactly as expected. Thats were it ends? I am not sure what to do with the 100 litre batch I drained off the glycerin from yesterday. It will come to no harm I suppose for the moment. So have dumped yesterdays batch of Glycerin in the wash tank.
Baffled for the moment I saw the post by tilly when I came back, will check it out first with a couple of cups of tea! Boy do I feel stupid! If others learn from my stupidity then its not for nothing.

Rgds

Dillyman

[dillyman Senior Member Find all posts View Profile Close dillyman]

Re: AH, What am I doing wrong!?!?

Hi Folks,

My 2 x 1 lt test batches yesterday are washing easily and beatifully. I am doing it quickly so will now slow down and finish it off. The obvious fact for me means that gentle means super gentle for me. I shall question all methods of fluid introduction also. I hope this lesson was the problem.

Rgds

Dillyman