Well I finally did a push/pull this weekend in my processor!
Here is a description for those interested:
I used 100L of mixed canola and sunflower WVO that titrated at 1.5 Naoh, I used 22% methanol. After passing the 3/27 I added 1.5 grams of phenolphthalein to the 3/27 sample and poured it into the processor which instantly changed the mix deep red. I arranged a trouble light behind the site tube for a better view of the colour change. I metered out 130ML of muriatic acid into a Pyrex graduated cylinder. I put the reactor under a 5Hg vacuum and started to suck the acid into the processor very slowly, a little less than 1/2 hour. Unfortunately my plan to feed the acid into the input of the pump didn't work out so I used a 1/4" poly line off of a 1/4" brass needle valve on the output of the pump to meter in the acid. I think I missed the colour change at around 70ML of acid so I kept going until about 125ML when I think I noticed another slight change in colour . I then reversed flow and heated to 160F while applying vacuum which recovered about twice the methanol that I normally recover from just the diesel but I have not measured it yet. I drained the very thick glycerin after about 10 minutes of settling.

Observations and questions:
I think I need to drive the heat up more as I did not observe the soap dropping out of the diesel like I usually do, However maybe this is because most of it settles out with glycerin?? I will know when I give it the shakem up test at the end of the week...
For anyone who has done this before how obvious was the colour change? The next time I am going to setup my tripod and video cam and catch the change on tape...
How can you tell when there has been a back reaction? I preformed a 3/27 after the meth recovery and it still instantly passed! Does this mean the fuel has not back reacted?
How much methanol should I be recovering on a 100L batch that utilized 22L of methanol?

Thanks for any help!
Jon

Good to hear your experience, Jon. Will be interested in hearing further news.

Jon,

Thanks for the update. I am glad that it worked out. I am very close to my first batch. This really nice guy named Jon Heron up in Ontario helped me figure out the wiring so I am on the home strettttttch.

OK I got another batch done!
I recovered about 8L of methanol total... does anybody know if this is about right? I am using 22L of methanol/100L batch.
I did not see the colour change this time either so I am wondering if I need more acid? I am using muriatic acid, I think it is 34%. Anyone know if when GL mentions he uses about 100ML/100L batch is he talking about pure HCL? I added about 130ML to this batch and I witnessed no colour change, other than when I first cracked the valve open a little too fast and let about 5ML in too quickly. I saw the colour change back to normal bio colour for less then 30 seconds. I am worried about adding too much acid but maybe this worry is unwarranted? What do you guys think? I would hate to ruin 100L of fuel!
After I drained the glycerin I brought the bio up to around 180F and tried to extract more methanol to see if any was left, I recovered less than a 1/2L so I think it was pretty much done. I get worried when I don't see any of the soap dropping out like I do when just recovering from the bio but it must be settling out with the glycerin?
I used up the last 100L batch before I could do a soap titration but hopefully I can get one done on this batch...
Has anyone else completed a push/pull or am I on my own here?

Thanks,
Jon

Jon,

at first i thought 1.5g of phenolphthalein..it must be cold that's not right...no I kept reading and yet you mean that much...ok..

if I remember right, biodiesel need about 12% methanol. this should leave 10l for recovery in your case. the fact that you got 8l out if fantastic!

-dkenny

Thanks dkenny!
Do you remember where you read about this statistic? I have done some searching without much joy.
When you say "fantastic" are you being sarcastic or is it normal to get about 80% out? I thought that the majority of the methanol is caught up in the glycerol. I normally get about 4L from just the biodiesel so I guess I expected to get more out of doing the whole enchilada...
The 1.5g of phenolphthalein is according to GL's instructions for titrating the whole batch for the catalyst neutralizing.

Jon

Update:
I contacted Graham via email about the concentration of HCL he based his 100ml per 100L batch on. Here is what his reply was in case it helps out the rest of you getting ready to try this:

quote:

I use 32% HCl now.
Dosing quantity does vary from batch to batch - if your oil is damp, you will need very little, because much of the NaOH ends up as soap, if it is dry you may need more.
Depends on your base amount of NaOH too - I use 5g @ titration which is typically +1 to +1.5g

Is your sight tube squished flat enough so you can see thru the biodiesl to gauge color change? I have about 1/8" 'thickness' of biodiesel to look thru, with a white plastic sheet behind it to make the biodiesel more visible.

Dose very slowly, and you will certainly see a definite colour change at one point, just stop there.

Do a 27/3 test before and after you neutralize , in the early days, just to develop confidence that you aren't back-reacting. You should have the same 23/7 results before and after.

So it looks like I may be overdosing on acid.
I have enough indicator for one more push/pull I hope to have a chance to run this weekend... I am going to relocate the acid feed to the inlet of the pump to see if that makes the difference...
Will update if I have any significant findings...
Jon

Ok, got 2 more batches done this weekend! Between getting a dumping of snow and fighting for access to my shed with an ornery skunk that finally fled the shed and is now currently in my fricken garage! Today it's going to die one way or the other!! Its been a long 2 days!!
I split the remaining 2g of phenolphthalein into 2 for the 2 batches. I moved the acid feed to the input of the pump and that seemed to make the difference.
On the first batch I did a glycerin pretreat on the WVO and recovered over 10L of methanol! After the pretreat it titrated at 2.5 NaOH. I witnessed the colour change at about 115ml of acid.
The second batch had no glycerin pretreat and titrated at 1.5 NaOH. I witnessed the colour change at 70ml of acid. And I recovered the now typical 8L of methanol.
Both batches passed the 3/27 with flying colours after the recovery so I believe all went well!
Does anyone have any theories on if I make soap from this glycerin if the phenolphthalein will make soap that stains your hands red?
Jon

EDIT: A note to others, if your recovered methanol looks cloudy it may still be of high purity. The 10L of methanol I recovered from the pretreated batch looked terrible, very cloudy with less than an inch of visibility but it tested at 99% pure according to an ethanol hydrometer.

Jon:

What are you mixing the phenolpthalein with in order to suck it into the tank. It is a powder you're using, isn't it?
I'm almost ready to try my first batch and still need to buy some phenolphthqlein. Do you have a source that you can recommend?

Thanks
Dave

Hi Hummerbk,
I am using powder and I have just been dumping it into the sample of bio I took for the 3/27 and swirling it around before dumping in. This works well.
I have not bought any phenolphthalein yet but it is available through VWR.
Jon