I wanted to first say thanks to Graham for coming up with this waterless, magnasol-less, way of washing/finishing fuel, for it has defiantly changed the way BD is made, at least for me.

I have attached what Magellan calls a PARTIAL REPORT, will be happy to post final report when received, but the sample submitted does meet the ASTM D6751 specifications. This fuel was made from WVO that titrated at 1.5, was made using NaOH, at a base of 6 + titration & 22% on the methanol. The 5% glycerin pre-wash was done, settled overnight. Once glycerin was drained, no water was used to wash or clean the fuel. Everything going forward was basically some version of what Graham has created, with the exception of the methanol recovery. This batch was made in a small 80 gallon processor, NOT a hot water heater type processor.

I post this so others can see the results of Graham's efforts and proof that his method really works. I was sure, the very first time I tried it, but at the end of the day, the lab is the only real way to have absolute results for some. This batch was also tested using the Jan Warnqvist test that was posted. Using the Jan Warnqvist test, there was very, very, very tiny pin head drops of something floating on the top of the methanol, but nothing that dropped to the bottom, and the methanol was a little hazy. So not sure about how the Jan Warnqvist test works, because every single batch always looks exactly the same when we do it. This batch was also Dr.Pepper tested, where you put the NaOH, Methanol, and BD, in a bottle, shake up, and it is suppose to turn to gel in 5 min, never turned to gel. Not taking any shoots at these tests, just stating that they were tried for comparison purposes, so others can gauge their results.

Thanks again Graham, keep up the good work! Your method does result in ASTM D6751 Fuel.

Well after writting this and trying to add the attachment I keep getting this message:

There was an FTP (file transfer) error. The detail is 'Upload to '/testdir/test.txt' failed. Detail: '552 Transfer aborted. Disk quota exceeded''.

Not sure what that means, but I will send the test report to someone else, and maybe they will be smarter than I, to post the report up so that it can be viewed.

Speedracer asked me to post these items.


and here's the link to the report:
http://www.utahbiodieselsupply.com/infopop/paul/Test_Report.pdf

Enjoy!
(Looks cool!)

Outstanding results, great report. Congratulations to you for the work and effort you have expending in reaching this level of achievement. Will be very interested in seeing both the preliminary and final lab results. Good work.

SpeedRacer

I reviewed your results. Again, great results.

In case anyone is interested, here are the applicable ASTM standards. Your test results are listed in parenthesis after the standard.

D 6584 Free and total Glycerin
Free glycerin: 0.020 mass % (0.010) [edit,standard is 0.020, originally entered as 0.010]
Total glycerin: 0.240 mass % (0.100)

D 93 Flash Point
130 min degree C (168)

D 2709 Water and Sediment
<0.05 max vol % (<0.05)

D 445 Kinematic Viscosity
range = 1.9 to 6.0 sq mm/s vol (4.809)

D 5453 total Sulfur
0.05 max wt % (500 ppm max, soon will be 15 ppm max) (2)

D 2500 Cloud Point
No spec'. Perform test and report results (-3.0C)

D 4530* Carbon Residue
<0.050 max wt % (<0.010)

D 664 Acid Number
0.80 max mg KOH/gr (0.11)

D 4951 Phosphorous by ICP
0.0010 wt % (<0.0005)

D 1160 Vacuum Distillation End Point
360C max at 90% distilled (357)

* My reference on Carbon residue refers to ASTM D4530. Your results based on D 524 are probably compatible.

I see two results of interest. I think the flash point is low for biodiesel. I am surprised to see sulfur as high as 2 ppm.

One more thing, if the lab still has sample left, you might ask them to run "D 874 Sulfated Ash". The result will show if all of the soap has been removed. No negatives in these comments, just observations stemming from respect.

Nicely done!

Just a thought experiment--if you did water wash, anyone have any idea which results might have been different? Is waterless washing advantageous for meeting any of the ASTM specs in particular?

one point in particular that I can see - and its only potentially problematic. That is with flash point. If the person who is using this method is not thorough enough with de-methanol'ing their biodiesel, then it could be possible to fail the flash point test. With water washing, I don't think that same potential exists.

Nice looking results!

A few comments:

1) The spec for free glycerin is 0.020 %mass (not 0.010 % mass) a typo?

2) A flash point of 168C is *not* low. We water wash our fuel 4 to 6 times and had a flash point of 165C in our latest Magellan test. (A flashpoint of 168C is 334F - diesel's minimum flashpoint is about 61C or 144F)

3) Sulfur of 3ppm is common in biodiesel made from WVO in our experience. I have seen this level of sulfur in Magellan tested biodiesel for about 6 samples over a three year period.

Bob in Berthoud

The Trouts,

Yes a typo. I looked at the results instead of the standard when I typed it.

I will go into the original post and change it for posterity. Thanks for the heads up.

Can I ask how much does Magellan charge to do a test? Ball park figure will do. Just curious because if its not to high I would like to have my BD tested as well. Thanks. John

The cost is $950 for the test. We are going to send another sample off next week out of our 250 gallon processor and get it tested at another lab that is $600 for the same test. Will let you know how the $600 lab works out. If the service is just as good, will be happy to pass along the info. Magellan was fine, but slow in my opinion. This new lab claims they will turn around results much faster, we shall see.

Hi Speedracer

Thanks for taking the time and expense in doing the test, I´m delighted to see it worked out well.

I hadnt seen your post before now, as Im in the mountains of the Czech Republic on vacation at present.

Thanks again

Hello Speedracer

Here in Australia I am required to regularly test by biodiesel and a full lab test here costs A$2,500.
If I can get my samples tested in the States for the prices you mentioned I would like to send them over your way. I would appreciate it if you could advise the contact details of the lab you use. Thanks



.

quote:

Originally posted by SpeedRacer:
The cost is $950 for the test. We are going to send another sample off next week out of our 250 gallon processor and get it tested at another lab that is $600 for the same test. Will let you know how the $600 lab works out. If the service is just as good, will be happy to pass along the info. Magellan was fine, but slow in my opinion. This new lab claims they will turn around results much faster, we shall see.

Hey Speedracer,
Would you mind describing the methanol removal method you used to achieve these results? I understand you did not recover, but how/when did you know you had removed enough methanol to meet flashpoint?

Not sure how much methanol in the BD will continue to keep soaps in suspension but ASTM requirement of around .2% seems pretty hard to check for using homebrew methods.

Just curious when folks out there using the "GL 1 day" method know when to stop demething.
No flow on the condenser does not seem reliable as many factors seem to be at play...temperture of recirc., introduction of headspace air, bubbling for increase evaporation surface area, etc,etc..

I'm using Graham's 1 day method too; I only wait a couple of hours after the 5% wash, then I boil off the methanol ( I cant be bothered to set up a condenser just yet, but I will do) and the results are great. After my last 20 gal batch I did a water shake test and it hardly had any milkiness at all. A lot of people owe Graham a big debt of gratitude.

PS - My processor is even based on his; I'll post pics of it whenever I have some time.

PPS - And thanks Speedracer and Graydon for posting these specs.

Yes, thanks to Graham, Speedracer and Graydon.

My question though is with "boiling off the methanol" (with or without a condenser).

How are people knowing what level of methanol reduction they are achieving?

As we have seen in many posts, the boiling point of a methanol/biodiesel solution goes up quite high as the methanol percentage is reduced. A batch that stops "boiling" at 200degF does not mean it is free of methanol or even within the range defined by the ASTM spec for flashpoint.

While much concern has been given to conversion and soaps, remaining methanol is a parameter that does not seem to be being addressed with any quantitative results.

I have the same question. The "does it bubble when I heat it test" seems a little inadequate for very low levels. I've been planning to run a test where I heat some bio up to 400F or so, cool, add 0.2% methanol and reheat to see if I can detect any bubbles.

The only quantitative test for methanol I know of is GC.

...or a correlation to flashpoints.

Which gets at the heart of the matter...is the ASTM spec for flashpoint actually looking for flashpoint for material handling issues, or is it really looking for methanol content for other concerns.

If the real reason the spec includes flashpoint is indeed for material handling/safety, why is is the spec for biodiesel 130degC while that for petro-diesel ranges from 52-95degC.

If the reason for the spec is to determine methanol content for other concerns, why not specify a GC test instead of a flashpoint test?
And what are those other concerns? Material compatibility?

I was thinking that this sensor could be used to determine how much methanol was left near the end of distillation:
http://www.futurlec.com/Alcohol_Sensor2.shtml

All we would need is a DC source (battery) a 3 volt regulator (cheap) and a volt meter (can get them from harbor frieght for 2.99 every so often).

Andy

This sensor appears to be able to detect methanol vapors, not methanol in solution. How would you use this to know how much methanol was left near the end of distillation?

Was any Rancimat testing ever done on that procedure? I don't know if there are other threads about this procedure, but I'd be interested in trying it. I have a 750 gallon reactor (I built a small commercial facility), but I've had oxidation stability issues (I don't even water wash). Any help would be greatly appreciated. Thanks