Author Topic: Warning over the use of Phosphoric acid in titrated acid water wash  (Read 1626 times)

Offline julesandtash

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Having used up my stock of Sulphuric Acid I decided to start on my stock on 85% Phosphoric acid.

I have had repeated successes with the titrated acid wash using Sulphuric acid and like to think I have the process pretty much under control.

However, at the start of the week I did a batch using Phosphoric. Perfect 27/3 using Sodium Methylate - absolutely no haze in the 10/90 test and instant clarity. All glycerol drained and then acid washed using 20 litres of water and one litre of 85% Phosphoric (which is what the titration gave me for a 300 litre batch).

That is when problems started - real problems in settling.

Eventually I got the water to settle out (which came out crystal clear) and went on to water washes. No matter what I did I could not get clear separation although the water which did drop out was crystal clear (and a little acidic).

It took about 250 litres of water, including two mist washes to get clean bio which I then dried to sparkling clear.

Although confused for a while, some googling showed that Sodium Phoshate (which is the salt produced when using Phosphoric acid) is a  detergent that was, until quite recently, commonly used. It is also water soluble.

Having a load of water soluble detergent in a mixture of water and biodiesel is, in general, a really bad thing.

I have rescued about 280 litres of the batch but it took a lot of work (and water - thankfully I am not on a meter). I have passed my experience to Paul (Carrington) for him to have a look at when he has time in order to try to identify what has really gone on but, in the meantime, I would seriously advice against the use of Phosphoric acid.
7+ years of making bio.
1997 RangeRover P38A 2.5DSE and 2001 Audi Allroad 2.5 V6 Tdi all on B100
Home heating and hot water system on Palm based B100 and Aarrow 7KW wood burner on glycerol logs

Offline nigelb

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Re: Warning over the use of Phosphoric acid in titrated acid water wash
« Reply #1 on: March 02, 2013, 06:55:24 AM »
Jules...are you absolutly sure you have your titration spot on? 1.0lt of H3PO4 sounds an awful lot!

Congratulations on rescueing the bio....it must have been extremely frustrating.  A 20lt loss can be seen as a real result.

Nige

Offline julesandtash

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Re: Warning over the use of Phosphoric acid in titrated acid water wash
« Reply #2 on: March 02, 2013, 07:25:51 PM »
Well, guess what, you were right Nige

I made new titration fluid today and titrated the batch of 100% palm bio I was making

Titration showed I needed 90ml of H3PO4 which sounds far more realistic

Somehow, and I dont know why, I was a factor of 10 out last time - no wonder I had problems. Glad my processor is stainless  :)
7+ years of making bio.
1997 RangeRover P38A 2.5DSE and 2001 Audi Allroad 2.5 V6 Tdi all on B100
Home heating and hot water system on Palm based B100 and Aarrow 7KW wood burner on glycerol logs

Offline Head Womble

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Re: Warning over the use of Phosphoric acid in titrated acid water wash
« Reply #3 on: March 02, 2013, 10:11:00 PM »
Jules, have you done a 10/90 on that first batch, to see if you've had any kind of reverse reaction.
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