Jan Warnqvist's Conversion Test- Outstanding! (3/27)
Jan Warnqvist's Conversion Test This is a quick Pass/Fail conversion test for your biodiesel and works because biodiesel will disolve into methanol while triglycerides do not disolve in methanol. It works with washed and dried, or unwashed biodiesel that is well settled.
1. Something to measure out 27 ml of methanol. 2. A small container in which to put the 27ml of methanol. I used a small glass jar about 11cm (4.5”) high and 5cm (2.5”) across 3. A 3ml syringe without the sharp. These cost me 15c each from my pharmacy and I used a new one for each test. 4. Biodiesel to be tested.
Procedure 1. Insure the jar is spotlessly clean and dry. 2. Put 27ml of room temperature (20- 22deg C) methanol into the jar. 3. Use the syringe to put exactly 3ml of the room temperature biodiesel under test into the methanol. 4. Put top on Jar. 5. Shake jar hard for 5 seconds.
If the biodiesel completely dissolves into the methanol and no oil settles out on the bottom of the container you have very high conversion biodiesel.
Further GC Testing by RickDaTech shows: "There have been a number of posts lately where people observed cloudiness even when they made high conversion fuel. In one case the sample failed for cloudiness, but passed GC testing for total glycerin. In addition I've found in my own testing that a number of variables combined influence the cloudiness.
Precipitation alone is enough of a test and it does raise the bar considerably. From my tests, it appears that if there is no precipitation, then the odds are in favor of the fuel meeting ASTM spec for bound glycerin. Also if there is precipitation, then you are highly unlikely to meet ASTM spec for bound glycerin."
Disclaimer The Warnqvest Conversion Test is not a substitute for the rigorous analytical testing needed to confirm B100 meets ATM 6751 specifications or any other specofication. Further, Jan Warnqvest or Tilly cannot be held responsible for misunderstandings of the test results that would lead anyone to use off-spec fuel in a diesel engine. ------------------------------------------------
This test of Jan's, while posted on the JTF site for quite a while, has been completely overlooked by most people. The thing that got me really interested about it is there is a fellow on the biodiesel Basics forum called Maurice who swears by it. He claims that if his biodiesel does not pass this test it will not work in his furnace. As no one has ever tested it, and no one put their hand up to test it when I suggested that it should be tested, it seemed to be a perfect project for a retired Mouse. So I teletyped my good friend Mickey and asked him to test it.
The results were unbelieveable! It actually works, and works well and quick. And it works on UNWASHED Biodiesel!
Immediatly below is the Test procedure as originally posted by Jan.
Below that are the tests Mickey performed to justify this post.
Jan Warnqvist original Conversion Test Posting
"Take exactly 25 ml of biodiesel and dissolve it in exactly 225 ml of methanol in a measuring glass.
"The biodiesel should be fully soluble in the methanol, forming a clear bright phase. If not, there is pollution in the biodiesel. Each ml of undissolved material corresponds to 4% by volume. Is there any undissolved material at the bottom of the measuring glass? If there is, your reaction is not complete and this is causing you trouble with the water test.
"This method does not cover every aspect of quality, but it gives a hint. It is valid only for biodiesel made from vegetable and animal oils. It is not valid for biodiesel made from oils with a very wide fatty acid pattern, such as fish oils."
This is the information exactly as teletyped to me a few hours ago by Mickey.
I must admit, I was sceptical; but a sceptic with an open mind.
The first test This test was performed with the quantities Jan suggests. I tested some of my standard 15% methanol production biodiesel. I put the 25ml biodiesel into the 225ml methanol, shook hard and watched. The methanol turned cloudy and over a few hours a large amount of biodiesel settled to the bottom.
The second test I have a number of samples of high conversion re-processed biodiesel sitting around from other tests, so I checked one of these. Again, using the quantities recommended by Jan, shook hard and watched the methanol turn cloudy. However, the cloud quickly cleared and NO biodiesel settled out. Could it be? Could there actually be something to this test procedure?
So I decided more tests were called for and, as I did not feel like using 225ml methanol per test, a bit of higher maths (using all 6 fingers and both thumbs) showed that 27ml methanol and 3ml biodiesel was in the correct ratio. At great expense I purchased 15 syringes so I could have a clean one to accurately measure out the biodiesel for each test. I found that biodiesel attacks these syringes very quickly, not sure whether it is the rubber or the plastic under attack.
Test 3 This test was with the new smaller amounts of methanol and biodiesel. This test was with another high conversion re-processed sample. This time instead of shaking hard I just swirled the test around with the liquids going no further than about 1/3 up the side of the jar. The biodiesel immediately completely dissolved into the methanol with NO cloudiness to the methanol. It remained this way for several days until I disposed of it.
Test 4 This test was performed the same as test 3, but the biodiesel tested was with some of my 15% production biodiesel. The methanol immediately clouded. Over an hour or two the cloud cleared and a substantial amount of biodiesel settled to the bottom of the jar.
Test 5 This was with Another re-processed high conversion batch and again the biodiesel immediately completely dissolved into the methanol with no cloudiness. No biodiesel settled out.
Test 6 I poured a small amount of the biodiesel from test 4 into about 30ml of biodiesel from test 5 and tested as per instructions. This produced cloudy methanol which cleared within an hour and a small amount of biodiesel settled out on the bottom of the jar.
Test 7 Yet another batch of 15% Production biodiesel which clouded and settled out biodiesel as it set.
I then re-processed a litre of this biodiesel with 1g NaOH in 50ml methanol. As expected more glycerine settled out. I then Washed the biodiesel and tested the reprocessed biodiesel
Test 8 This test was of the reprocessed biodiesel used in test 7. To my surprise, this test produced cloudy methanol! I was amazed. But over an hour or two a number of “Drops” of biodiesel settled out onto the bottom of the jar.
I then re-processed this oil a second time and a “Soft Gel” developed which indicated high conversion. However, I then re-shook the gelled biodiesel and it broke down into a liquid and cloudy phase and still remains like this 4 or 5 days later.
Test 9 I tested this unwashed re-reprocessed batch and it passed! No cloud, no biodiesel settling out. This test seems to be more “Discerning” than the World Famous Dr Pepper ASTM Reprocess Technique (Pat Pend) and apparently works on unwashed biodiesel!
Test 10 I made a litre of high conversion biodiesel from some WVO titrating at 0.4 I used 7.5g NaOH mixed into 300ml methanol. One hour after last shake I tested this biodiesel and the methanol remained clear and bright!
Test 11 I poured 20ml of this biodiesel into a container and added 2ml of my 15% production biodiesel and stirred thoroughly. I then tested this and the methanol clouded. After about 30 minutes the methanol cleared and there is clearly a small “Glob” of biodiesel on the bottom of the Jar.
Test 12 Re-tested this unwashed high conversion batch I made a few hours ago. Results- No cloud and biodiesel completely dissolved in the methanol.
What can I say? It seems to be a resounding success and conversion testing of biodiesel will never be the Same
Thank you Mickey, fortunately I do not receive many royalties on my now out of date conversion test. I wonder if it will end up in a biodiesel museum?This message has been edited. Last edited by: Tilly,
July 07, 2006, 09:26 AM
It is not valid for biodiesel made from oils with a very wide fatty acid pattern, such as fish oils
This statement from JTF leaves me highly concerned. What is "a very wide fatty acid pattern"? This is a subjective statement that does not define which oils work and which oils do not work. If there are some oils it works for and others it does not work for, then we need a good quantative definition of what oils work and what oils do not work or we will not be able to trust the results.
How many different oils have you tried it on? Did you try it using fish oil which the author reports does not work?
There are many things on the JTF site that concern me. Mickey said "Production Biodiesel" Having viewed Micky's procedure this includes Sunflower, canola, tallow, palm, cotton seed, and probably the occasional dead cat. Fish oil does not seem to be a common oil used in fryers and i know Mickey hates fishing so I doubt fish oil was included.
I have sent an e-mail to Jan telling about the tests performed and have invited him to join in the discussion.
July 07, 2006, 09:45 AM
I have 40 to 50 samples of biodiesel saved from past batches. I will perform this test on the samples this weekend. I am particularly interested in the results on the intermediate and second stage samples from my two stage base/base processes.
If all works well I may try adding some tumeric pH indicator and a few ml of water to the methanol and see what happens. Maybe this is what is in the pHlip test.
July 07, 2006, 09:54 AM
Earlier this week I ordered the basic pHlip test kit. If the test vials arrive today I will have them available this weekend. Then, some side by side comparisons can be performed.
July 07, 2006, 09:55 AM
Tilly, Thank you for all your hard work in testing. Once again, you share your knowledge so the rest of us can benefit.
Now that the a$$ kissing part is over , the questions.
Is this new test valid for someone who mixes all their feedstocks into one tank? All my collections go into a holding tank.. No fish oil there but I have Canola, soy, Cotton seed, corn, peanut, etc etc all mixed into the same tank. Would the test be oil with this?
2nd. Part of your post says "mix 25ml" and part says "mix 27ml"... Which is it? did I mis-read something?
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July 07, 2006, 10:23 AM
I anxously await the results of your tests. The pHlip test clearly shows the biodiesel on top of the test solution so I am sure it is mostly water.
Mickey always mixes his feed stock. Every batch is guaranteed to have at least 4 different types of oil in it. Jan originally says to use 225ml methanol and 25ml biodiesel. Divide both numbers by 25 and multiply by 3 gives you 27ml methanol and 3ml biodiesel
July 07, 2006, 12:10 PM
This is very exciting!
I guess even JTF hits it lucky once in awhile.
I am struck once again at the difference between our site and his. We happily acknowlege good/useful science when we see it. Keith seems incapable of acknowledging anything useful that he didn't invent or perhaps "borrow".
July 07, 2006, 02:01 PM
High Compression II
Love this test! So quick, easy and repeatable!
Thanks Jan for coming up with it, and a big thanks to St Tilly for bringing it to this Forum!
Here are the tests I did...
My current batch, finished this morning and pumped into main storage-tank. It was a 'Two-Base', 50/50 reaction, with 12.5% meth each time, but with 6.5 grams plus titr, X 1.2, devided by 3, and times by 2 for the quantity of NaOH per litre for first stage.. 1000 litres oil, yielded 150 L glyc. by-product at first settlement.
Second Base, straight 5 grams again in 12.5 meth, this time 250 Litres glyc drained...
Washed dried as normal, and tested with this test....
Perfectly clear methanol, No cloudiness even when first mixed, and no settlement after an hour...
I have a litre sample of 78% Ester BioDiesel from a single-base reaction which was GC tested some time ago at OAS Oil Analysis Services here in the UK..(Maybe a couple of months old now...)
I tested this....Immediate clouds, almost opaque, and after 10 mins, settlement of orangish 'oil' at bottom, and the meth had not cleared...
I have a theory (Oh, No I hear you cry, Not another one!.....) The amount of 'oil' settled at the bottom, definately isnt 3mL...
Could it be around .6mL It certainly looks like around that amount. Cant measure this at the mo, as the sample is at work, and I only thought of this on the way home anyway....
IF its around .6 mL, This equates to around 20% of 3mL .....which is the deficiency of my 78% (78-100, = 22%) Ester-BioDiesel....
If so, and its a HUGE IF, then we have a simple and cheap test, that will determine the ester content of BioDiesel without a GC.....Something every Home-Brewer has been dreaming of!
Will measure this 'Oil' settlement fluid first thing Monday Morning!
Oh, and when I was testing it again, this time with the unwashed bio.. as I was stirring it, a yellowjacket flew right in my container. He lived about 10-15 seconds before giving a final gasp and then flipping on his back. I guess that methanol stuff really is poisonous
Left work for a while to run a couple of samples. The test produced results as expected from reading the above information.
About two weeks ago a series of five samples were prepared to optimize my catalyst. The samples,numbered 1,2,3,4,and 5, were dosed with catalyst at the rates of 1.25%, 2.46%, 3.71%, 4.95%, and 7.37%, respectively, all on a weight of catalyst per weight of oil basis. Each sample was prepared and left sealed in its own 500 ml, clear, HDPE bottle. Today the samples were all very clear and each looked like good biodiesel.
Samples 1 and 3 were tested by the current method. Even though both samples looked good (very good, in fact) I expected sample 1 to fail and sample 3 to pass. This expectation was based on past experience and the low % catalyst in 1 and the "optimum" (for me) % of catalyst in 3.
As a reference I also tested a sample of biodiesel that has been fully tested to ASTM specs. I acquired this sample several months ago and use it periodically for just this type of purpose.
Three (3) ml of each biodiesel sample was added to 27 ml of methanol.
Results: Sample A - the methanol turned very cloudy immediately upon introduction of the biodiesel. Within less than 10 seconds a mass of oil had settled to the bottom of the beaker. This sample was retained for about a minute. During this time the methanol never cleared. About 1 to 1.5 ml of oil had settled.
Sample B - the methanol remained clear and no oil settled to the bottom in the minute or so of observation time.
Sample C - the methanol remained clear and no oil settled to the bottom during the time of observation.
Conclusions: Sample 1 (A) was expected to fail and it did. I had hoped sample 3 (B) would pass, and it did pass by today's procedure. Sample C passed and it was expected to pass because I know it has met the ASTM test requirements.
Based on the above, very limited, but controlled tests it appears the Conversion Test works as described.
One other observation. My samples 1 and 3 have not been washed. I checked the flash point on the same samples and it was found to be 22 C for both (the temperature of the room where they are stored). So there was some methanol still in the biodiesel sample as collected and tested. The oil in Sample 1 (A) still turned the methanol cloudy and some dropped out of solution.
July 07, 2006, 04:20 PM
I love dead yellow jackets. Those buggers hurt!
July 07, 2006, 07:16 PM
High Compression II
Originally posted by clark_bailey: I love dead yellow jackets. Those buggers hurt!
Err, Forgive my ignorance, but what IS a 'Yellow-Jacket'--and in what way do they hurt!
"As for testing, know now that---- only mechanisms built by bunglers require testing.--- Properly-built machines work properly." 'Doc' Smith.
July 07, 2006, 07:23 PM
Yellow Jacket = Wasp
Similar to bees and hornets.
Their stingers pad a hell of a wallop. Glad to hear of one that got his final "buzz".
OK. Buzz = slang for drunk.
US and UK. Two great nations separated by a common language. (I think Churchill said this.)
July 07, 2006, 07:39 PM
Well, a fair bit has happened since I went to bed last night.
Hello Troy Yes, I think that is the most hilarious part of this whole thing. This test, which is probably one of the most useful bits of biodiesel information on the JTF site, has been posted there for a long time. Keith never even bothered to test it. Instead, Keith has been pushing that nonsensical "Shake-um up" test calling it "the most useful all-round test,..."
Hello HCII Good to see that you have performed some tests with this procedure and find that it seems to work as advertised. Yes, the biodiesel that drops out is definitely not the total amount that you put in. The amount that drops out varies with the conversion rate of the biodiesel under test. The answer may be as simple as methyl esters are slightly miscible in methanol and mono, di and tri glycerides are not. Jan makes a suggestion in his original post.
I have no doubt that someone with the proper equipment could develop a fairly simple method of measuring the amount of biodiesel that settles out and calculate the conversion % of the biodiesel under test.
Hello Producer So you couldn't wait for the end of the day to test this procedure. I hope your boss does not mind you slipping off to do a few tests. It is good to see that your test results seem to line up with all the rest. It would be great if this really turns out to be the Holy Grail of simple home conversion testing that can be performed immediately at the end of the reaction before the biodiesel is even removed from the reactor. We have been looking for it for a long time.
July 07, 2006, 08:54 PM
It seems that Jan is wasting his time at JtF, seeing as how no one has even bothered to try his discovery, and it turns out to be quite astounding.
It gets definitely cloudy. Look through the side of the jar. The cloudiness is somethig you will not miss. Also, if it is a fail, biodiesel precipitates out fairly quickly. A pass has no biodiesel precipitation.
No, I do not have a picture.
July 07, 2006, 09:29 PM
High Compression II
Originally posted by steved: hi tilly, thanks for telling us about this test. i tried it and all my stuff passed. how cloudy does it get ? do you have a picture ? i have been using 9 grams koh base. all of it i tested has been settling for 3 weeks or longer.
On the testing I did, the methanol went quite opaque, like a milk and water mixture, but with the 'oil' settling at the bottom.. Guess how bad the conversion is, will depend on how opaque it is when mixed up first...
My 'good' fuel remained perfectly 'sparking clear' even just after mixing