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What Soap Levels Are You Seeing With Your Dry Wash Setup?
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Over on the equipment side Girl Mark has been discussing soap levels in finished product being run through dry wash systems.

The standard that Rachel over at Piedmont has come up with to get you into the ASTM spec for the Sodium/Potassium spec is as follows:

NaOH based Bio - 65 ppm
KOH based Bio - 44 ppm

So, what soap levels are you seeing in your own dry wash setup on the finished Biodiesel? (ie. what's your soap PPM level?)

If you're not sure how to test for soap, we carry a soap test kit produced by Arbor Biofuels Company.

More details are here: http://www.utahbiodieselsupply.com/soaptestkit.php

Also, we now have a nice video that shows how to measure soap levels using this kit.
Link To The Video

If you're not testing for soap ppm, what test are you using to ensure you're getting good, clean Bio?

I'd love to see how close folks are getting to the ASTM Standard with their setup...

Thanks,
Graydon

This message has been edited. Last edited by: Graydon Blair,




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Location: Utah | Registered: October 08, 2004Reply With QuoteReport This Post
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Chad & GCG from Arbor Biofuels Company noted the following...

Chads454
"The Demethed BD we sent through the eco2pure was 640ppm soap pre E2P and it went down to 60ppm after.."
http://biodiesel.infopop.cc/eve/forums/a/tpc/f/919605551/m/9931020482

Chads454
"We did do a soap test after running the BD through E2P(Eco2Pure)then through our Thermax Macro then finally through purolite.
We ended up at 50-60ppm, Started out with 640ppm."
http://biodiesel.infopop.cc/eve/forums/a/tpc/f/919605551/m/9931020482

GCG
"At Arbor Biofuels Company we consistently perform a methanol removal/recovery process combined with a 24 hour period of settling and have biodiesel that test between 450-900 ppm soap content prior to ion exchange resin purification. After passing through our columns the biodiesel is always <60 ppm (which amounts to .2 ml of 0.01N HCL with our soap test kit)."
http://biodiesel.infopop.cc/eve/forums/a/tpc/f/919605551/m/9931020482




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Location: Utah | Registered: October 08, 2004Reply With QuoteReport This Post
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-I ran another 75gls through the E2P today, But I didn't do any tests,We're up to 190-200gls of BD through the 10lbs of E2P,
-I'll run another 100gls tomorrow and do a soap test and report back.


Chad
2000 F350 SD 7.3PSD, 1996 F250 SD 7.3 PSD, 2005 Jeep liberty CRD, 2002 TC29D New Holland Tractor, 6K Diesel Generator, Heated Power Washer 'All Burnin Bio'

http://arborbiofuelscompany.com/ Selling Dry Wash Columns.

http://i88.photobucket.com/alb...icationGCresults.jpg
 
Location: S.E Michigan | Registered: May 12, 2007Reply With QuoteReport This Post
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Just finished another 100gls through the E2P(eco2pure)for an total of about 300gls,
and we are at 120ppm soap.

I'll be running more through and keep posting results.


Chad
2000 F350 SD 7.3PSD, 1996 F250 SD 7.3 PSD, 2005 Jeep liberty CRD, 2002 TC29D New Holland Tractor, 6K Diesel Generator, Heated Power Washer 'All Burnin Bio'

http://arborbiofuelscompany.com/ Selling Dry Wash Columns.

http://i88.photobucket.com/alb...icationGCresults.jpg
 
Location: S.E Michigan | Registered: May 12, 2007Reply With QuoteReport This Post
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what were the starting niumbers before that 120 ppm finish?
 
Location: Pittsboro, North Carolina | Registered: March 07, 2001Reply With QuoteReport This Post
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It was 640ppm,
I'll recheck it later.


Chad
2000 F350 SD 7.3PSD, 1996 F250 SD 7.3 PSD, 2005 Jeep liberty CRD, 2002 TC29D New Holland Tractor, 6K Diesel Generator, Heated Power Washer 'All Burnin Bio'

http://arborbiofuelscompany.com/ Selling Dry Wash Columns.

http://i88.photobucket.com/alb...icationGCresults.jpg
 
Location: S.E Michigan | Registered: May 12, 2007Reply With QuoteReport This Post



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Well the last 100gls or so was at 165ppm soap ,this batch has been settling for over a week now.
- We have run about 400gls through the E2P.

-We'll make another batch next week and run more through the E2P.


Chad
2000 F350 SD 7.3PSD, 1996 F250 SD 7.3 PSD, 2005 Jeep liberty CRD, 2002 TC29D New Holland Tractor, 6K Diesel Generator, Heated Power Washer 'All Burnin Bio'

http://arborbiofuelscompany.com/ Selling Dry Wash Columns.

http://i88.photobucket.com/alb...icationGCresults.jpg
 
Location: S.E Michigan | Registered: May 12, 2007Reply With QuoteReport This Post
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OK, I'm still not understanding why your soap levels are so low to begin with.

Are you doing acid-base biodiesel by chance?

everyone, when talking about soap levels, please list:

-starting titration of the oil itself before processing into biodiesel

-whether you used acid-base and/or 5% water prewash or glycerine pretreatment

-if you use 5% prewash, what do you do about the water left in the biodiesel?

-what is the soap level BEFORE any soap removal, such as 'dry wash' of any type

-what dry wash process you followed and what steps did it involve and for how long

-what soap level did you end up with
 
Location: Pittsboro, North Carolina | Registered: March 07, 2001Reply With QuoteReport This Post
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girl mark

I am going to post results in this thead,
But all the info your asking about came from this Thread

[Quote] GCG
Graydon and Girlmark,

Quick note to eliminate any misunderstandings:

1) Gross Methanol removal is recommended for biodiesel purification however resin function is facilitated by the presence of some methanol. Gel type resins require 1% or more to function properly where as we have found that our T45 BD Marcoporous works successfully at the 0.25% mark but our testing indicates that you probably shouldn't go lower than this. However at this level the bulk of soap and glycerin naturally seperate and then you go directly to purification.

2) At Arbor Biofuels Company we consistently perform a methanol removal/recovery process combined with a 24 hour period of settling and have biodiesel that test between 450-900 ppm soap content prior to ion exchange resin purification. After passing through our columns the biodiesel is always <60 ppm (which amounts to .2 ml of 0.01N HCL with our soap test kit).

3) As Chad said earlier our initial test with the Eco2Pure indicated similar results however at this point we have only processed 100 plus gallons through ~10 lbs of Eco2Pure.

4) Pressure build up or compaction in a column of Eco2Pure seems to be the challenge presently. As the material loads and compacts either due to contamination loading or simply as a matter of gravity and it being soaked with biodiesel and it settling harder and harder; produces process flow issues...

5) We have what we believe is a completely better design for the use of this product but haven't got it worked out yet. More in the future on this.

6) Our testing of water content is typically 0.02% however our initial water content is less than 0.25% and we use Sodium methylate which actually dehydrates during the biodiesel reaction. Then after gross glycerin removal, coalescence, demethylation and 24 hours of settle time - we just don't have any water issues.

Lastly there is the issue of FFA content or Total Acid Number - we sell a TAN test kit so people can quickly and accurately check there finished product to ensure the column isn't exhausting.

However due to the macroporouses additional capability of removing soaps through glycerin entrappment (later in column life) total ion exchange exhaustion isn't observed. Therefore it should only be exhausted due to dissolved glycerin adsorbtion and soap numbers in the final biodiesel shouldn't be the problem but instead dissolved/total glycerin numbers...

People who are having the biggest problems with ion exchange are running high methanol concentration and high contaminate concentrations using gel resins and this is resulting in high FFA or TAN's for the biodiesel end product.

Additionally gel-type resins are being advertised as a dessicant product (an end all solution) and although they can remove water and methanol they certainly are not efficient at it!
[Quote]
GCG


Chad
2000 F350 SD 7.3PSD, 1996 F250 SD 7.3 PSD, 2005 Jeep liberty CRD, 2002 TC29D New Holland Tractor, 6K Diesel Generator, Heated Power Washer 'All Burnin Bio'

http://arborbiofuelscompany.com/ Selling Dry Wash Columns.

http://i88.photobucket.com/alb...icationGCresults.jpg
 
Location: S.E Michigan | Registered: May 12, 2007Reply With QuoteReport This Post
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what was the starting FFA of the oil you used to tmake that biodiesel?

were you using acid-base processing?
 
Location: Pittsboro, North Carolina | Registered: March 07, 2001Reply With QuoteReport This Post
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Our Oil is Usually 1.0-1.5 FFA

No acid base,


Chad
2000 F350 SD 7.3PSD, 1996 F250 SD 7.3 PSD, 2005 Jeep liberty CRD, 2002 TC29D New Holland Tractor, 6K Diesel Generator, Heated Power Washer 'All Burnin Bio'

http://arborbiofuelscompany.com/ Selling Dry Wash Columns.

http://i88.photobucket.com/alb...icationGCresults.jpg
 
Location: S.E Michigan | Registered: May 12, 2007Reply With QuoteReport This Post
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Sorry, is that percent FFA or mls of KOH? What does it translate into for other homebrewers who use the 'homebrew titration'?
 
Location: Pittsboro, North Carolina | Registered: March 07, 2001Reply With QuoteReport This Post



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Using our Total Acid Number test kit it has a TAN of 1.8-2.0 mg KOH/g which if you multiply by .55 yields a FFA% of 1-1.1.


Chad
2000 F350 SD 7.3PSD, 1996 F250 SD 7.3 PSD, 2005 Jeep liberty CRD, 2002 TC29D New Holland Tractor, 6K Diesel Generator, Heated Power Washer 'All Burnin Bio'

http://arborbiofuelscompany.com/ Selling Dry Wash Columns.

http://i88.photobucket.com/alb...icationGCresults.jpg
 
Location: S.E Michigan | Registered: May 12, 2007Reply With QuoteReport This Post
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This thread is more or less meant to compare what soap levels (and under what conditions) people are getting and what the reduction using non-water-wash technology is.

Please describe your titration using normal homebrew terms, which neither of those is because most people who are reading this forum don't talk %FFA. They don't talk 'industrial acid number' either, because while it's used in a finished fuel ASTM test as it's very sensitive, it's irrelevant to the 'starting' titration of oil where you're mostly trying to find out how much of your KOH is needed to titrate your oil (Neutral posted lots of things here about why the homebrew way of doing a titration is superior in this particular case- because KOH varies in purity and fatty acids vary in weight, so it isn't really useful to convert back and forth from %FFA if you're just talking about oil)

While you can guestimate wildly and convert back and forth from the crude 'homebrew' titration to %FFA, it's one step removed from a real-world titration and is unlikely to be accurate or necessary for people to talk about their oil (and no one is titrating oil in the mg/g acid value way that ASTM uses for finished fuel).

You can't really convert 'homebrew' titration to %FFA very accurately due to the impurities in KOH, I assume you guys are starting with a purchased known-molarity solution of KOH for your kits rather than making your own out of solid (the liquid is calibrated against a more stable acid when it's manufactured to ensure purity)
 
Location: Pittsboro, North Carolina | Registered: March 07, 2001Reply With QuoteReport This Post
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GM,

Being an avid reader of Neutral's and your post; I have read the particular thread your referencing. For those not familiar with this older thread - here it is

Neutral promotes doing good math and understanding what is actually going on chemically behind a particular formula. In the previously mentioned post he says that for all intents and purposes, the variance of FFA's is neglible:

"Oils are not made of only oleic acid hence this formula results in small errors, normally accepted. The range of molecular weights encountered in the used oil trade is from 270 for palm to 281 for canola."

He finishes with the calculation from homebrew titration to FFA%:

"For the homebrew titration the concentration of the solution is usually 1/4 of the above, 1g NaOH per litre. Sometimes it is 1g per litre of KOH. "

And then fortunately (for me in this conversation since I didn't know the conversion) he provides the conversion from Acid Number or Acid Value to homebrew titration:

"If you do a "homebrew" titration with 1g KOH per litre solution and use 1g oil you could directly find the AV:

AV = h / 5.61

where h = homebrew titration (ml)

If you use the more usual 1ml of oil you have to allow for its density, then:

AV = h / 5.16"

So given this formula and our Total Acid Numbers of 1.8-2.0 - this yields a Homebrew titration using 1 ml of oil and KOH:

2 = h / 5.16

or

h = 2 * 5.16 or 10.32

However this seems very high to me - is this how you interpet his formula?

GCG
 
Location: Michigan | Registered: May 08, 2007Reply With QuoteReport This Post
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The guys at the BioPro factory came up with a really simple conversion that I use on regular basis.

Granted, like GCG indicates, it's not "perfect", but it's close.

For KOH
Titration / 1.8

For NaOH
Titration / 1.2

ie. a Titration of say 9 using KOH = 5% FFA

It's not perfect, but for "ballpark purposes" it works great.

-Graydon




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Location: Utah | Registered: October 08, 2004Reply With QuoteReport This Post
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Sorry, I don't think it's close at all, due to the condition of the non-lab-grade KOH that most of us use for titration, something that's become more clear in the last few years- see 'why KOH gives weird results' thread (and I admit that this is a problem whether you're trying to talk about percent or whether you're trying to compare oil between users based on a homebrew titration- the homebrew titration is useful to tell you how much lye to use, not what amount of FFA is actually in there- because you don't ACTUALLY have a known concentration of KOH unless you've bought a standardized titration solution.

We all compare oils based on titration anyway, but I don't want to see people start to talk about percentage when yo'ure starting with an inaccurate titration AND doing a conversion to get an estimated percent. We're already one step removed from 'accurate'. Why make it worse with a rough guesstimate conversion?

For low titration oils all of this is kind of irrelevant.

For high titration oils it matters very much and probably explains a bit of why some esterification formulas don't seem to give totally predictable results- too many variables that can be 'slightly' off, two of them in the titration and one of them in the water content.

I think the variation in what you'll see with non-standardized KOH used for titration solution, and converting to percentage, is probably at least 15%, and since the solution itself carbonates as it ages, it can vary significantly more than that in some cases.

While this is all totally also true of the case when multiple users discuss oil in terms of homebrew titration numbers, talking about it as a percentage gives a false impression that you're being really accurate. There's a big difference between a 5% and an 8% oil for instance and I think it's important to be accurate.
 
Location: Pittsboro, North Carolina | Registered: March 07, 2001Reply With QuoteReport This Post
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True. I'd agree with that. Especially with KOH based titrations....

Man, I wish there was some magical INEXPENSIVE method that'd give repeatable results for truly accurate FFA% numbers (beyond getting super accurate solutions and doing it "the scientific way"), but, I guess it's what we have at the moment...

-Graydon




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Location: Utah | Registered: October 08, 2004Reply With QuoteReport This Post



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Hi Mark,

quote:
I think the variation in what you'll see with non-standardized KOH used for titration solution, and converting to percentage, is probably at least 15%, and since the solution itself carbonates as it ages, it can vary significantly more than that in some cases.


I don't mean to be disagreeable, but I wonder if you have any test data to base this 15% # on?

When you say "non-standardized KOH" are you referring to the same stuff I get at Pacific Coast Chemicals, across the street from Oasis? I asked them about it and they gave me an independant lab cert matching the batch # they sold me showing the stuff to be just over 90%.

I agree that once people start handling the KOH it degrades. And, much faster if they handle it incorrectly. But, I don't think the KOH from manufactures that are claiming the KOH to be 90% are going to be only 75%.

Also, it is not that hard, or expensive, to test the strength of a given KOH solution against a standard acid solution. Of course most people don't have standard solutions around. However they can be purchased.


Andrew

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Location: Northern California | Registered: February 27, 2006Reply With QuoteReport This Post
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I think they're starting with a 90% and it degrades at least another 5% percent, judging by the common experience of needing at least that much more than you'd theoretically expect to need.

there's an easy way around all of this if someone's already selling titration kits with chemicals- sell a 1N KOH solution that's standardized, and have the user dilute it to .25 or whatever is desired. I think that for titrating finished fuel for FFA, that's what you'd need to do.

For anyone buying HCl for soap titration, you should be getting it as a standardized solution anyway (I buy mine from Carolina Biological or Nasco or someplace like that). It's a good 'starting point' if you for some reason need to test your KOH purity as well. One or the other chemical really needs to be standardized in order to know what you're really working with, in this situation.

The situations where I think it matters are:
-HCl solution for soap titrations needs to be standardized. I keep asking where the Arbor Biofuels guys get theirs, because they're the only ones currently selling a kit with chemicals, I think. Graydon and Norm should probably sell standardized 1N HCl and KOH solutions, it's only something like $5/bottle and it lasts a long time.


-standardized known purity KOH solution for testing %FFA in finished fuel. I may be wrong, but I think this is important to test for because some ion exchange media create FFA which isnt trapped in the media, and one sign of a media going bad might be higher FFA numbers. I might be wrong on this, I don't think people are generally seeing a lot of that but I'm not sure how many of them are testing FFA in finished fuel.


-standardized KOH solution for those working with high-FFA oils, where these small differences actually matter, such as acid esterification processes that are based on %FFA (unlike DKenny's method).

-standardized KOH solution would be great to have (but obviously not always going to happen) for anyone doing experimentation who need to report what they're finding to others.


Again, people, standardized solutions of these two chemicals are CHEAP. They're easily available. I think the formula we use for homebrew titration is .25N, most of the standard solutions are sold as 1N, so you'd just dilute yourself a working solution as needed. A bottle of 1N cost me something like $5 recently.


I think it's not a step upwards at all in accuracy/good practice for people who start out with homebrew titration to start describing their oil in %FFA on the forum, since almost no homebrewers test it that way and it's a derived, guess-prone method in the first place- I know it's easier to say '5% FFA' than it is to say 'KOH homebrew titration of 9' but most people on this forum already do that pretty automatically.

Introducing more 'rough' conversions will just introduce less accuracy into the discussion (for instance I always do the conversion from homebrew titration to FFA% in my head and speak a 'guesstimated' rough estimate) GCG's post about having his numbers sound 'way off' is a good example of why introducing this habit of roughly converting to %FFA just introduces errors.
 
Location: Pittsboro, North Carolina | Registered: March 07, 2001Reply With QuoteReport This Post
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