Biopowered - vegetable oil and biodiesel forum

Biodiesel => Chemistry and process => Topic started by: craig on July 22, 2013, 11:56:42 PM

Title: newbie needs help please
Post by: craig on July 22, 2013, 11:56:42 PM
OK what did i do wrong

i have made several test batches all turn out the same.

titration =6 ml + base 3.5=9.5g per liter
methanol=20%=200ml per liter
heated oil to 55 degree C
MIXED WELL
left over night.
then  3/4 of it is biodiesel floating. with a solid lump at the bottom.
done 3/75 test = good diesel

i then reduced the sodium hydroxide still the same but the 3/75 test showed a very little oil.
Title: Re: newbie needs help please
Post by: Tony on July 23, 2013, 12:01:54 AM
Hi Craig, welcome to the forum.

I take it you are using Sodium Hydroxide rather than Potassium Hydroxide?

6 is a high titration for oil, and 3.5g is old-skool base (most people use 5g/l base for Sodium these days).

But anyway, it appears you have made bio - the solid lump at the bottom is to be expected with Sodium - that's the Glycerol that should be drained off while it's still hot and runny!
Title: Re: newbie needs help please
Post by: Tony on July 23, 2013, 12:04:02 AM
Also 3/75 is not the usual ratio for conversion testing, usually it's 1 part in 10, IE 3/27, 5/45, 10/90.

That you reduced the catalyst and still got good conversion suggests your titration is out (too high).
Title: Re: newbie needs help please
Post by: craig on July 23, 2013, 12:36:17 AM
great thanks
still learning 3/27 is what i meant.
will attempt another small batch soon.i want to get it right before i make a processor.
 any other helpful tips would be great
THANKS
Title: Re: newbie needs help please
Post by: Rotary-Motion on July 23, 2013, 08:42:59 AM
good to meet you craig

Title: Re: newbie needs help please
Post by: Julian on July 23, 2013, 09:16:18 AM
Welcome to the forum ... keep playing, it's the best way to learn!

I started out by doing loads of Dr Peppers, collecting them up and then sticking them in the car.
Title: Re: newbie needs help please
Post by: Jamesrl on July 23, 2013, 10:13:12 AM
Welcome to the forum ... keep playing, it's the best way to learn!

I started out by doing loads of Dr Peppers, collecting them up and then sticking them in the car.

Did you have to shove the bottles down the filler neck with a stick?
Title: Re: newbie needs help please
Post by: Julian on July 23, 2013, 10:51:25 AM
Welcome to the forum ... keep playing, it's the best way to learn!

I started out by doing loads of Dr Peppers, collecting them up and then sticking them in the car.

Did you have to shove the bottles down the filler neck with a stick?

Stupid boy!

Of course I didn't.  If you warm them up they become quite pliable so no need for the stick.

Title: Re: newbie needs help please
Post by: Jamesrl on July 23, 2013, 06:41:02 PM
Welcome to the forum ... keep playing, it's the best way to learn!

I started out by doing loads of Dr Peppers, collecting them up and then sticking them in the car.

Did you have to shove the bottles down the filler neck with a stick?


Stupid boy!


Of course I didn't.  If you warm them up they become quite pliable so no need for the stick.

Mmmmmmmmmmmmmm, that's the trouble wiv bein' fik, l neva fort of that, 'ot bottles.

I bought a full bee hive once coz some one said me jam jar would run ok on bee pee.
Title: Re: newbie needs help please
Post by: craig on July 23, 2013, 07:26:09 PM
Glad I found this forum, seems like if i need some help a may get some answers.
like you say we all start somewhere.

I guess i took the long road - loads and loads of youtube vids and some American websites over the past 3 weeks.
hopefully i will get some good enough to run my motor.

also found that its not cost effective to use demijohns for test batches after a couple of inches of  Glycerol
sets in the bottom LOL.

 :) any chance i could steal some or most of the info on your website Julian for my own site.
I'm not near you so not a threat to your collections.

Title: Re: newbie needs help please
Post by: Julian on July 23, 2013, 07:36:44 PM
Welcome to the forum ... keep playing, it's the best way to learn!

I started out by doing loads of Dr Peppers, collecting them up and then sticking them in the car.

Did you have to shove the bottles down the filler neck with a stick?


Stupid boy!


Of course I didn't.  If you warm them up they become quite pliable so no need for the stick.

Mmmmmmmmmmmmmm, that's the trouble wiv bein' fik, l neva fort of that, 'ot bottles.

I bought a full bee hive once coz some one said me jam jar would run ok on bee pee.

I'll have a pint of whatever your drinking.
Title: Re: newbie needs help please
Post by: julesandtash on July 23, 2013, 07:43:04 PM
I wonder if it is something Vince produced  :)
Title: Re: newbie needs help please
Post by: Julian on July 23, 2013, 07:46:56 PM
Glad I found this forum, seems like if i need some help a may get some answers.
like you say we all start somewhere.

I guess i took the long road - loads and loads of youtube vids and some American websites over the past 3 weeks.
hopefully i will get some good enough to run my motor.

also found that its not cost effective to use demijohns for test batches after a couple of inches of  Glycerol
sets in the bottom LOL.

 :) any chance i could steal some or most of the info on your website Julian for my own site.
I'm not near you so not a threat to your collections.

May be better to stick to the info on the wiki.  Many youtube videos offer information of dubious quality (witness Cragie in New Zeland!).  If stuff's not clear on the wiki, just ask on here.  It's good to get feed back from newcomers, having made bio for quite a while now we often take things for granted.

Re the website there are three Julians on here, but I assume you mean mine.  If so yes use what you like and thanks for asking ... many haven't.

The only thing I would ask is that it's not a carbon copy as Mr google won't like that and we'll both suffer.  Use the text but reword it a bit, change the layout and if you use any photos, give them different file names and Alt text etc.

Title: Re: newbie needs help please
Post by: craig on July 27, 2013, 12:06:49 AM
THANKS for the OK to steel parts of your website not started mine yet,
I will add a little about you (bit of extra SEO for you)

i still have problems with the washing=lot of soap and looks like orange juice
any good tips?
Title: Re: newbie needs help please
Post by: nathanrobo on July 27, 2013, 12:39:53 AM
THANKS for the OK to steel parts of your website not started mine yet,
I will add a little about you (bit of extra SEO for you)

i still have problems with the washing=lot of soap and looks like orange juice
any good tips?

Hi Craig... and welcome.

The orange juice is normal during washing, the longer you leave it to settle (also the more you wash it) the clearer it will get.  At the end of the process drying will give you perfectly clear fuel.

btw when you scale up consider dumping the titration (bit old school) and doing 2 stage no titration dosing - more accurate.  The titration of 6 was probably because you needed to blank your IPA.

Also there are a number of techniques for water washing - all well tested, one of them will suit your scaled up process and desired processing times.
Title: Re: newbie needs help please
Post by: craig on July 31, 2013, 09:27:58 PM
That's good to know, it nearly got binned ;D.
This might be a silly question but just learning.
OK i don't have a processor yet
the last tester i did was 25 liters in a plastic drum left it overnight and the bottom 2" set solid
leaving me with bio above this is what i have been washing and it seems to be OK 3/27 good.
is it OK to carry on doing it this way until i get a processor  :-\
yes i know it would be easier to drain the glycerin while liquid but as i cant see through the bucket
i don't know how long to leave it and how much to drain off.

and what is the 2 stage no titration
Title: Re: newbie needs help please
Post by: Head Womble on July 31, 2013, 10:57:00 PM
Two stage reaction, read this
http://www.biopowered.co.uk/wiki/Two_stage_process_with_no_titration

You can make bio in a bucket, but it's for safety reasons we build dedicated reactors.
Title: Re: newbie needs help please
Post by: craig on July 31, 2013, 11:29:54 PM
Two stage reaction, read this
http://www.biopowered.co.uk/wiki/Two_stage_process_with_no_titration

You can make bio in a bucket, but it's for safety reasons we build dedicated reactors.

Hi Mark
I will be making a reactor tank when i know what I need.
I have started to make a wash tank that should work well :-\

As for 2 stage no titration Hm-mm maybe at a later date after more practice
Title: Re: newbie needs help please
Post by: Rotary-Motion on August 01, 2013, 07:53:14 AM
doesnt 2 stage take away the need to practice, makes life easy...
Title: Re: newbie needs help please
Post by: craig on August 01, 2013, 08:14:46 PM
It makes life easy when you know what your doing to start with.
Title: Re: newbie needs help please
Post by: Head Womble on August 02, 2013, 10:49:51 PM
It makes life easy when you know what your doing to start with.

It's easier and more relyable than titration, it just sounds confusing.
Title: Re: newbie needs help please
Post by: greasemonkey on August 02, 2013, 10:53:59 PM
Two stage no tit, is simpler, says the man who has only done one batch.
Titration sounds like a right fiddle to me, and requires more kit, and a greater understanding.
Understanding is all well and good, but getting bio out is what counts.
A no tit process is simple, just don't do a soap test at the same time as the conversion test.............
Title: Re: newbie needs help please
Post by: willbuild on August 03, 2013, 01:42:46 PM
circulated in the processor yesterday for about 4 hours and took a sample. was clear this morning with a dark brown drop out, so have circulate for 90 mins then put into settling tank.
now its just wait and see.
am going to make spray bar this afternoon, just in case!!!
Title: Re: newbie needs help please
Post by: craig on August 04, 2013, 10:20:56 PM
OK guys i need some more help :'(
just did a 50/50 water & bio shake test.
fully separated in 5 Min's
now i have 1/2 bio and 1/2 milkshake :(
how the _ _ _ _ do i get it clean.
Title: Re: newbie needs help please
Post by: craig on August 04, 2013, 10:27:25 PM
and what colour should it be?
a sample in a syringe it looks a golden colour
but in a demijohn it looks very dark.
Title: Re: newbie needs help please
Post by: Julian on August 04, 2013, 10:58:38 PM
In a 50/50 the bio will always pick up water, especially if there's even a tiny bit of soap around.  It will be a dirty orange juice colour and is quite normal.  It's typical of the colour you get when water washing.

With the 50/50 you are only interested in the colour and clarity of the water.  It should be clear, any white opaque tinge indicates that you've washed soap out of the bio.

If you leave it long enough, unlidded the bio will eventually dry and can be decanted off or added to the next batch on the wash cycle.

Is the demijohn the trial batch?  If so you only need to take a half jam jar sample for the 50/50 test.
Title: Re: newbie needs help please
Post by: craig on August 04, 2013, 11:21:53 PM
In a 50/50 the bio will always pick up water, especially if there's even a tiny bit of soap around.  It will be a dirty orange juice colour and is quite normal.  It's typical of the colour you get when water washing.

With the 50/50 you are only interested in the colour and clarity of the water.  It should be clear, any white opaque tinge indicates that you've washed soap out of the bio.

If you leave it long enough, unlidded the bio will eventually dry and can be decanted off or added to the next batch on the wash cycle.

Is the demijohn the trial batch?  If so you only need to take a half jam jar sample for the 50/50 test.



I thought it was washed well it cleared to a transparent golden colour not cloudy orange juice anymore.
so i decanted to a demijohn then took a 100ML sample bottle to 50/50 shake test.
i could immediately see it separating but the water is a white milky colour
if i start washing again will it eventually get rid of the white water

Its all new to me.
Title: Re: newbie needs help please
Post by: Julian on August 04, 2013, 11:32:31 PM
Have a read of this page ... http://www.biopowered.co.uk/wiki/Water_washing.

Regardless of the method of washing, the bio and water colours will be the same in each case.

If you have a milky 50/50 then you still have soap in the bio, despite it looking clear.  You can just leave it to settle for a week or two.  Over time you'll see a light, white/grayish gel type layer form at the bottom ... that's the soap.  Or you could try washing again.

Don't be in too much of a hurry to get results, time and gravity are often your best friends when making bio.
Title: Re: newbie needs help please
Post by: craig on August 04, 2013, 11:48:09 PM
Silly question Julian :-[
do I leave it to settle with water in it or do I drain it off
Title: Re: newbie needs help please
Post by: Julian on August 04, 2013, 11:56:23 PM
If you are going to let it settle there's probably not much point in draining the water now as you'll only get more water dropping out of the bio. 

You should see a layer of clear bio forming at the top which will get larger as it drys.