Has anyone performed the test on BD made from hydrogenated or partially hydrogenated oil?
A few hours ago I did my first test and the methanol immediately became a bit cloudy and then cleared up some after setting for a few minutes. It’s been about 4-5 hours and still no fall out. The methanol is somewhat clear but certainly not crystal clear.
Could the hydrogenated stock have a slight effect on the test?
I think your book is obsolete now.. Time to re-write it?
if by bd fails the test does that mean i cant use it? what do you do with it if it fails?
I would use it.
yep i just did the test and got a little bd in the bottom. why couldnt you use this in conjuction with the dr pepper test before you made a big batch?
No reason in the world, that I can see why not to do a test on your Dr Pepper test-batch before going to your main production batch--That way, you can 'trim' your catalyst/meth and fine-tune before committing to the main batch....
Sounds like a great idea, Another test in the quest for quality product definately cant hurt!
"As for testing, know now that----
only mechanisms built by bunglers require testing.---
Properly-built machines work properly." 'Doc' Smith.
How long should it take for the mixture to drop out any bio if it is going to?
2001 & 2002 F-250 PSD CC Superduty Running On Homebrew!
In my very limited experience, if it did not cloud it will not drop out biodiesel.
On the other hand, it does not take too long for the biodiesel to start dropping out if it was cloudy.
Well, I performed the test on both types of bio.. non-prewash and prewashed..
I used a couple babyfood jars.. 27ml meth and 3ml of bio..
My prewash sample clouded right up.. took about 5 minutes to clear and dropped out quite a few tiny tiny tiny dropplets at the bottom of the jar and one larger droplet..
My non-prewash dropped out almost 1/2 ml of bio at the bottom.. when it clouded up, it took 10 or 15 min to clear up..
I'm using a 3ml syringe to measure out the bio with and a 50ml cylinder to measure out the 27ml with.. I hope thats accurate enough..
For my next large batch, I'm going to add an extra 250 or 300 grams of KOH for the reaction.. I'm already using 22% meth so i'm not so sure more would help..
I forgot to add that I shook each sample for about 10 seconds..
A public Disclaimer
I have posted in this thread everything I know about this test. As to it's validity or otherwise is up to everyone here to sort out for themselves
A person has brought it to my attention off list that he has performed some tests with this procedure which shows that the amount of water in the methanol is a concern.
He also advises that he performed the test with the methanol at 5deg C on some biodiesel that he felt should have passed the test but did not.
He also advised that he performed the test on some unwashed biodiesel that he felt should pass the test but did not.
He also advises that there is something in the e-mail I posted from Jan which casts doubt on this test's ability to accuratly test biodiesel made from Rape oil.
My reply was: "I do not mind if you post this information on the forum, we are all in a steep learning curve with this and the more information out there the quicker we will sort this out."
His reply was much less complimentary.
If I have mis-led anyone into believing that Mickey has performed more tests than shown and I am withholding vital information, I assure you this is not the case.
I have invited Jan Warnqvist, the fellow who developed this procedure several years ago and Neutral to both come and give us their opinions.
I can do no more.
There are no warranties, written or implied
Being a newbie you can take this with a grain of salt but I have some grave concerns with the accuracy that seems to be required with very little tolerance for errors in measurement. I have tried it now several times on the same batch of bio while purposely using very small differences in meth volume with different results every time. Also it is important to immediately cover your receptacle because a very small amount of meth evaporation makes a large difference in the outcome.
Please give more info on your different results..
Then make more than 3 ml/27 ml proportions (for example there's nothing terribly difficult about the proportions that Jan W. recommendd originally)= if measurements quantity is a big factor, multiplying everything should make the results more repeatable, I would think?
First I tried it with close is good enough measurements, I had cloudy meth and about 1/2 ml of bio settled out, then I tried it paying much closer attention to my measurements and had clear meth with two or three almost microscopic drops of bio fallout, as it sat for a while a lot more bio dropped out but the meth was also evaporating away, so I did it and covered the jar immediately then I had clear meth and no drop out at all that was at least twelve hours ago and it is still the same.
Very good point, the original test was done using larger proportions, you are probably right, I'm gonna try it right now.
I just tried 25ml of methanol and 4ml of bd, it passed. It is just as clear as the methanol with nothing in it.
But both batches of the bd i have on hand with the prewash, cloud up and drop the whispy stuff, they will turn into very small droplets,maybe 8-10 of em about the size of a small pin hole.
The last prewash batch,and the NO prewash batch,were the same oil,and both titrated at 3.10g/l.
I used the same amt of oil, 22% methanol and the same amount of koh, the prewashed batch fails and the NO prewash batch passes.
I will fire up another batch tomorow if i can and test it right after it settles,and will not do the prewash.
Well heck,i just couldn't wait,i just got done puttng in the methoxide and will run it for 2 hours and drain the lower pipes and let it settle till tomorow.
I still have 60 gallons of this same oil so if this batch passes, i will do another with the prewash.
I would be real interested if any body bought the new flip test, how it shakes out with the results from this test.....RICK
fabricator, you can leave the lid off, it will start to evaproate but i left a sample set on the bench all nite and it was still about 15ml left in the morining,along with the pin drops.
Thanks Jan Warnqvist for this test and Tilly for informing us on this test.
Works like a charm and its simple to do.
Keep up the great info coming.
One question to Tilly, if we use 27ml of Methanol and 3ml of biodiesel. After the biodiesel clears and there are minute droplets does this mean the conversion is poor or that most biodiesel will have some minute droplets?
My observations suggested that if the biodiesel did not clear withing a few seconds this was not a "Pass".
I received my pHlip test kit and have performed some comparison testing with the Warnqvist method.
My opinion is that: 1) the Warnqvist test is quick, inexpensive, works on washed and unwashed fuel, and definitely gives a quick indication of your conversion of oil to biodiesel during the reaction step of production; 2) the pHlip test is quick, easy to use, more expensive than Warnqvist, is intended to be used on finished (ie reacted, washed, dryed, ready to use) biodiesel, and is an outstanding indicator of the quality of the finished biodiesel.
If you are running a reaction and you want to know if it is complete, use Warnqvist. If you have finished biodiesel (or if you are buying ASTM quality fuel), then use pHlip.
I ran several samples per the Warnqvist method with varying results. Most of the results were predictable, and because the results were predictable I got a good, comfortable feeling that the test is good.
Three samples, out of the couple of dozen on which the Warnqvist test was performed, were selected for the pHlip test.
A little information about the three samples will help you understand why these three were selected.
The first was a sample of ASTM quality biodiesel. Selection of this sample was a no brainer. This sample is identified as ASTM.
The second sample was a washed and dried sample of finished biodiesel. The biodiesel was produced using a two step base/base reaction. It was washed, dryed and ready to go. I expected this sample, identified as Sample A to pass the tests.
The third sample, identified as Sample B, was prepared using Tilly’s Dr Pepper method. After it was produced, the biodiesel was left in a sealed container. It was not washed, the methanol had not been removed, and the glycerol layer was still present on the bottom of the container.
The results for Warnqvist are: ASTM = Pass; Sample A = Fail; Sample B = Pass. Sample A failed by the slimmest of margins, but it had a very small quantity of very, very, small droplets of oil accumulated. The accumulated oil could not be seen at the bottom of the container. When the container was agitated and held up to the light, the oil could be seen.
Elsewhere in this thread is a good right up by RickDaTech of how to interpret the pHlip results. It will not be repeated here. The following are the results of each item for each sample.
Clear and Bright: ASTM = Pass; Sample A = Pass; Sample B = Fail
Indicator Color is Cherry Red: ASTM = Pass (slightly darker); Sample A = Pass (slightly darker); Sample B = Fail
Indicator Turbidity: ASTM = Pass (none); A = Pass (none); B = Fail (cloudy)
Biodiesel Turbidity: ASTM = Pass (none); A = Pass (none); B = Fail (cloudy)
Mirror Surface on Interface: ASTM = Pass (looked clearer than pHlip reference standard); A = Fail ( very minute globules in center of “mirror”); B = Fail (This could have passed, but there was so much turbidity I couldn’t see a mirror through the cloudiness)
Orange and or Yellow color in indicator: All passed.
Based on the above results the following can be concluded: ASTM = good biodiesel (duh); Sample A = Well washed, dryed, and almost completely converted. Probably contains a very small amount of unconverted soybean oil, but darn good fuel. Sample B: probably contains mono- and di-glycerides along with glycerol, some soap is still in solution, there may be some catalyst in solution (not sure about this), probably got good conversion, but the fuel is not yet ready for use.
These results are consistent with expectations and meet the common sense aspect of the observations.
The following photographs were taken to help the explanation. I don’t know if these will post as part of this write-up. If not, then I will just follow up with 5 more posts each with one photo attached.
My opinion is the Warnqvist tests works well to determine the completeness of the reaction.
The pHlip test gives much, much more information about finished biodiesel. In fact I think using the Warnqvist test as a routine process operation, and using the pHlip on finished product will be a good strategy.
The pHlip test cost US$ 51.00 and comes with 1 reference vial and 9 sample vials. The effective cost of the pHlip is US$ 5.67.
Sample B on right with Warnqvist result to right. Note how clear and “good” Sample B looks.
pHlip reference on left. Sample A, ASTM, Sample B. All with Warnqvist results.
pHlip ref’ on left. Sample A with Warnqvist result – settled.
pHlip ref’ on left. Sample A on right, note Warnqvist result was swirled for photo.
pHlip on left. ASTM biodiesel on right.
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