When I mix 10ml of iso and 1ml of wvo w/o any water my digital ph meter says 9.5. With every drop of distilled water and lye it goes up..ie 10...10.5 etc. What am I doing wrong?

You're using a pH meter. Seriously, use an indicator such as phenolphthalein or turmeric. It is really easy and much better. PH meters are notoriously inaccurate for what we are trying to do. HTH

dont let my wife know that! told her i had to have this 80$ meter and have been cussing it under my breath for weeks. phenol? tried some in my iso and well after a ounce of distilled water addeed to my 10ml got a pink to purple deal. Have found that 3tsp of drain cleaner or 1 level teaspoon of white powder lye seems to work through whole process. thanks...but my ph of the final product is still 9.5-10.5 with my ph meter???

OK,
First, phenol red (the stuff you get at a pool store) is not the same thing as phenolphthalein. It works, but not very well. Phenolphthalein is the preferred indicator for titrating. Second, very accurate measurements are critical for doing titrations. You cannot measure the lye with a tablespoon. You need to accurately weigh out one gram of 100% NaOH (or the KOH you will be using in the process) and dissolve it into one liter of distilled water. This is your titrating solution. You also need to be quick about weighing it because NaOH absorbs water from the air affecting it's weight and purity. Here is the instructions I include in my titating kit. Saves me a lot of typing:
Titrating Directions

Needed equipment:
· Small clear glass or jar
· Isopropyl alcohol (IPA) 99% (Rubbing alcohol. Meijers or any good drug store $1.49/pint. Or Heet brand gas line antifreeze in the RED bottle)
· Two 3cc syringes (CVS or other drug stores)
· Indicating solution (phenolphthalein or turmeric) Phenol red works, but not well. It indicates at a different pH than what we want.
· Titrating solution (1% sodium hydroxide solution)
· Conversion chart (Supplied Excel chart)

Directions: Place 10 mL IPA in glass. The measurement doesn’t have to be precise. A tablespoon is about 15 mL- close enough. It’s just the solvent for the oil.
Put three or four drops of the indicator solution into IPA. This is just the indicator; it takes no part in the titration other than telling you when to stop. If the color change is not obvious enough for you, just add a couple more drops the next time.
Using one of the syringes, add one or two drops of the titrating solution to the IPA. This is called blanking the titration. Sometimes the IPA can be a little acidic. You want to begin the titration at the neutral (indicating) phase. One or two drops will usually be all it takes. You want it to just change color. Change goes from clear to pink for phenolphthalein, yellow to red for turmeric. Always use the same syringe for the titrating solution; you don’t want to contaminate it (or the bottle of titrating solution) with oil.
Use the other syringe to draw up 2 or 3 mL of oil. Point it up and get all the air out of the tip. Start at 3 (or 2 ½ or 2) mL and add one mL slowly to the blanked IPA. It is more accurate to go from 2 ½ down to 1 ½ than to try and go from 1 mL to the end of the syringe. This way you are assured of adding only one mL of oil. This measurement is critical.
Once you have the 1 mL of oil dissolved in the IPA, you can begin the titration. Using your titrating syringe, add the titrating solution a drop at time being careful to count the drops. Swirl the glass to insure good mixture. It’s OK if you need to fill the syringe again. When the acids are neutralized by the titrating solution, the indicator will change color. That is the point you want, when it just changes color.
Look at the chart for number of drops and it will tell you how many grams (of NaOH) per liter of oil you need. I also included grams per gallon on the chart. Multiply this number by the number of gallons you are using, and this is the number of grams of NaOH you need to dissolve in the methanol.
A little note about this chart: the excel calculations are adjusted for the syringes included in the kit. When you need to get new syringes, you need to make sure the number of drops per mL is the same as the old ones (30 drops/mL) or the calculations will be wrong. Things like tip size and shape affect the number of drops. It can vary by 10 drops or more. Any dropper will work, you just need to know how many drops per mL it delivers, and adjust the Excel calculations accordingly. This is the formula. =(A2)/30+5 The 30 is the number that needs to be changed. Also, cc’s and mL are the same thing.

Sorry you wasted 80 dollars on that meter. My kit is only 26 bucks. Graydon (Utah Biodiesel Supply) has a deluxe kit for 40.
Titration is very easy and quite accurate. It is also the most important step in making quality BD. HTH

If it helps to see a titration, I've posted a titration video on my site. It has a safety brief, runs through the titration three times and shows how to build a recipe. The video quality is a little rough around the edges, but hey it's a homebrew video.

Different people use different measuring devices to measure out the various fluids. It does not matter what you use to measure as long as you measure the 1 ml of oil and the titrating solution accuratly. The video shows various ways to measure fluids.

ok purchased some tumeric and used 7ml to turn iso pink/red. going to try and do some soy..already posted a question in the how it works or small batch forum. thanks again man this stuff is black

7mL!?!?!! Just for the IPA?! Or is that for the oil as well? Blanking the IPA should only take one or two drops of titrating solution. If it is taking 7mL to titrate the oil, look for another source- that's really bad stuff. And don't eat at that establishment either!

I wouldn't let 7ml scare me; you use what you can get. My last 2 batches were 8ml and 8.3ml. I use KOH and GL1day waterless washing. This minimizes the 2 major issues with "soapy" biodiesel. I (and you) just have to contend myself with lower yield (80% or so on those batches).

The BEST oil I've ever gotten was still 3.5ml KOH, and that was only 10 gallons from a 4th of July Funnel Cake stand. But it was enough to mix with some 9ml stuff and run a batch at the 5-7ml range I am used to.

Ryan, WOW, you're using 16-17 grams of KOH per liter of oil? I try and stay away from the stuff that titrates at 9 grams NaOH! Yeah, KOH does help reduce washing problems. Do you do the pre-wash?

Yeah...I was pretty desperate to get some lubrication to go with all the ULSD I've had to run the last few months (no brewing in the winter, no heated shop, my stored oil was all bricks!).

I didn't even titrate it first, just loaded the processor and said, "Whatever it is, that what I'm doing!" Of course, I knew the sources were typically 5-8ml KOH, so it wasn't a huge risk

Which pre-wash? There so many now...

5% water pre-wash: yes (and sometimes 6% just for extra soap capacity).

Glycerine pre-wash of oil: I have before, but have found the results very sporatic, so don't do it regularly.

Dry, clean glycerine pre-wash of product: haven't tried it.

And I've just started ordering my KOH from ChemistryStore.com by the 50lb bag, that cut those costs in half!

Ryan

Have you considered running acid-base? It's not so difficult and yield is much better.

Shane (processing 13.5g NaOH black stuff!)

got jelly with 12 grams of naoh granular
titration, 10ml of iso dash oftumeric, turned yellow, drops for ever and finally got it to turn pink and stay at around 3ml but since i started with 10ml of .01% then 7 ml in , hence 7+5=12
titration uuuugggghhhhh!!!Q! anybody want 40 gallons of soy?

Parker,
I am a little unclear on what you are doing. Are you blanking the 10 mL of iso before adding the 1 mL of oil? Then adding the titrating solution until the color change, right? I see you are using the 5 gram base, that's good. How are you making your titrating solution?

quote:

Ryan

Have you considered running acid-base? It's not so difficult and yield is much better.

I've considered it. Usually I can mix my sources to keep my overall titration in the 5ml area. Its just that right now, the lower titrating source happens to also be partially hydrogenated, so I can't use it because its solid. So I'm sucking off the liquid portions on the tops of my drums, which happens to all be the higher FFA source's oil.

yes using a method i found on here, believe from tilly, 100ml of distilled water then 10 grams of lye then 900ml of distilled water then shake then draw off 100ml or something like that?

I must be really lucky - my oil titrates between 0.5 and 0.8mls and always looks very clean; I did have a source which always black looking and had a terrific amount of sludge in the drums, but I chucked it without using it, it looked so bad - I bet it titrated very high.

more confusion. i get the titration to work out to 3.5 ml of NOH. my question is, how much NOH to use for the base or "neat" part of the oil. some say 4.8 grams NOH and some say 7 grams for neat oil. any help would be appreciated, and sorry if this is off topic.

5g/l base amount applies to NaOH catalyst.

7g/l base amount applies to KOH catalyst.

This same issue makes talking titration numbers a little weird too. The same oil that titrates at 3.5ml with NaOH will titrate at 4.9ml KOH. So if somebody says, "My oil titrates at 5ml", that would be pretty usable oil for a KOH measurement, boarderline crappy for NaOH.

thanx for the info.
just for the record. some articles say 3g/l for NaOH and 4.8g/l for KOH. and others agree with your 5g/l for NaOH and 7g/l for KOH. I have been using 7.7g/l of 90% pure KOH. plus the exact amount the titration calls for, ie 3ml for a total of 10.7g/l for this batch. am i close or out in left field?

anybody want to buy a ph meter? lol