Calling all chemists.... UJSSM iodoform test

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Calling all chemists.... UJSSM iodoform test

Postby hexokinase » Wed Apr 19, 2017 6:16 pm

Granted I am not a chemist by trade; I do however, have a good amount of chemistry under my belt including: 8 hrs general chemistry, 8 hrs organic chemistry, and 3 hrs biochemistry. I am a newb to this particular craft. I am working exclusively with UJSSM until I get a better handle on the art aspect of this. I am considering running the iodoform test on my output as I learn to make cuts by taste utilizing the spoon method. As this would give me a general idea about the concentration of aldehydes and methyl ketones present. Has anyone already performed this test to make cuts? If so what are the results of your tests. I'm considering 2-3 gtt (arbitrary number) nascent iodine (infowars x2 iodine) per 10 mL of approx 400 mL lots. I am also taking into consideration the sensory tests that I have read on this forum including exhaling into the distillate and testing if it burns the eyes. Bottom line is I would like to know the results of your tests on UJSSM as you progress through the distillation process. Also did you preform the test ante or post airing out the spirit for approx 24-48 hrs? How many gtt Iodine used and what type? My hypothesis is that the hearts will have the lowest concentration of these byproducts as would the heads... the tails may be another matter...
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Re: Calling all chemists.... UJSSM iodoform test

Postby HDNB » Wed Apr 19, 2017 7:31 pm

go hard brother. if you find something you can 'splain in english...i'm all fer learning. impressed with the amount of knowledge you picked up in 16hours of chemistry training. they tried to beat some into my numb skull for 3 years in high school, to no avail.
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Re: Calling all chemists.... UJSSM iodoform test

Postby hexokinase » Wed Apr 19, 2017 8:29 pm

HDNB my brother from another mother.... Ive read a lot of your posts about this skill set.... THANK YOU for contributing to what I know!!!!!! I pride myself on splainin in plain english... I love teaching bout the star stuff (the periodic table of the elements)... basically as you know the smell of nail polish remover predominates the first few bits comin out of the still... this is the result of dimehtylketone aka acetone aka nail polish remover.. as noted in my previous post the iodoform test would test positive for iodoform as dimethylkeytone is a methyl ketone... as the distillation process continues the concentration of furfural an aldehyde which is well within the tails will also increase. Iodine reacts with these types of byproducts (aldehydes and ketones) eventually forming a solid yellowish precipitate known as iodoform. Since I am using a pot still which I know will not give an accurate product separation as would a lab grad distillation apparatus there will be smearing across the distillate i.e. there will be some alcohol(ethanol) mixed with nail polish remover (dimethylketone) strongly at first and eventually disipating then coming to furfural (an aldehyde) as the temperature increases in the tails. So my hypothesis is that the concentration of iodoform will decrease (amount of yellow precipitate will decrease) as it reaches the hearts and will increase as it reaches the tails. So the lowest concentration of iodoform will be the hearts of the distillate... since i haven't performed the test i'm not sure how much of that particular type of iodine will be required... Note iodine will only react with aldehydes and methyl ketones not ehtanol making it an ideal test with easily sourced reagents (infowars x2 iodine)... I hope that splains my thought process brother! I recon if nobody has performed the tests I will have to and post the results... Either way I recon I'll have to get some more test tubes, racks and parafilm... that might upgrade me on some NSA list... lol... I've ordered so much lab equipment over the past couple years... lol... P.S. here's the secret I've learned about making chemistry interesting... at least for most men anyway.... general chemistry... things go boom.... organic chemistry... things make real big boom... biochemistry... haven't quite figured out how to make that go boom yet... I'll let you know..
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Re: Calling all chemists.... UJSSM iodoform test

Postby Oldvine Zin » Wed Apr 19, 2017 11:09 pm

hexokinase wrote:general chemistry... things go boom.... organic chemistry... things make real big boom... biochemistry... haven't quite figured out how to make that go boom yet... I'll let you know..
:lol:

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Re: Calling all chemists.... UJSSM iodoform test

Postby Oldvine Zin » Wed Apr 19, 2017 11:15 pm

HDNB wrote:go hard brother. if you find something you can 'splain in english...i'm all fer learning. impressed with the amount of knowledge you picked up in 16hours of chemistry training. they tried to beat some into my numb skull for 3 years in high school, to no avail.

Believe that those are credit hours - not real time.

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Re: Calling all chemists.... UJSSM iodoform test

Postby Saltbush Bill » Wed Apr 19, 2017 11:28 pm

I just have to ask, why complicate something so simple ??
You need some jars a nose and some taste buds to do the job.
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Re: Calling all chemists.... UJSSM iodoform test

Postby Kegg_jam » Thu Apr 20, 2017 2:11 am

I say go for it. Everybody's nose is different.

If you can come up with a method that works for you and can achieve repeatable results then that's cool too.
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Re: Calling all chemists.... UJSSM iodoform test

Postby yakattack » Thu Apr 20, 2017 3:37 am

Ok you have my attention. I have iodine here. I use it to test mash for starch conversion. I also have the results of my last vodka run. Which is refluxed.

So correct me if I'm wrong. In the heads I will form and iodoform and in the tails. But clean refluxed hearts should not form iodioform at all. Is that the general idea behind your hypothesis?

If so I can try a few tests tonight. See what happens. Should only need an ounce or two of alcohol from each section of the run for testing purposes.. heck if you have a process in mind post it up and I'll try it.
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Re: Calling all chemists.... UJSSM iodoform test

Postby HDNB » Thu Apr 20, 2017 4:56 am

Ok that makes a litttle more sense.
now i want to see some results.

and wtf is a credit hour? (becoming increasingly obvious that my formal education does not include any university)
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Re: Calling all chemists.... UJSSM iodoform test

Postby hexokinase » Thu Apr 20, 2017 5:48 am

Saltbush Bill wrote:I just have to ask, why complicate something so simple ??
You need some jars a nose and some taste buds to do the job.


The reason is that I smoke so it can be a bit difficult for me to detect smells that are not strong which leads to difficulty tasting it. So I thought if there was a way to visualize it, it may help me detect the end of the heads better. Since I had a wee drop of the creature when I wrote the last two posts I have to make a correction. This will not test for positive for furfural... the iodoform test only gives positive results for methyl groups directly attached to the carbonyl. furfural is a furan attached to the carbonyl. A test that could be used for all parts of the distillate would be the 2,4-Dinitrophenylhydrazine test.... that's not readily available to me... however, I do have what is required for the iodoform test that being iodine and sodium hydroxide (i make my own soap)

yakattack... yes the heads will form iodoform but the tails should not with this test unless it too contains something with a methylated carbonyl. So if you have produced pure ethanol with your reflux apparatus no iodoform will form. So my down and dirty test would go as follows: prepare a 6M sodium hydroxide solution (M means molarity which is defined as mols/liter... in this case if you were making a liter of solution add 240 grams of sodium hydroxide(NaOH) aka caustic soda aka lye to 1 liter of distilled water) if you don't have access to pure sodium hydroxide crystal Drano should work in a pinch... it's mostly NaOH... next set aside 5 mL of output to test and add enough iodine to colorize it then add enough NaOH solution to decolorize it.... you may need to shake or stir it... a positive test result will be yellow precipitate in the vessel... any cloudiness or the like would be negative... then pour out the test into a larger vessel and neutralize it with vinegar before rinsing it down the drain... the solution to pollution is dilution! Once I perform the test I will give a more accurate procedure..

as a safety note... if you have never made a NaOH solution... DO NOT add it all at once to the water the dissolution of NaOH is exothermic and could cause it to boil over splashing it everywhere and if it gets on your skin you could have a bad day... use nitrile gloves and keep a bottle of vinegar nearby in case you do spill some on you so you can quickly neutralize it...
Last edited by hexokinase on Thu Apr 20, 2017 7:56 am, edited 1 time in total.
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Re: Calling all chemists.... UJSSM iodoform test

Postby hexokinase » Thu Apr 20, 2017 7:31 am

So since my need to know things superseded my need to be lazy today I performed the iodoform test on spirits that were aired out for approximately 36 hrs. Also, I didn't feel like making a 6M NaOH solution and used some 1.04M I had on hand for acid titration. It worked well enough.. so here is the method

Materials:
Infowars X2 Nascent Iodine (aq)
1.04M NaOH (aq)
5 mL each distillate test lot
test beakers

Procedure:

Take approx 5 mL of sample and to this add approx 1 mL of iodine. Swirl the test beaker until the sample is uniformly colored. Add 4 drops of 1.04 M NaOH solution and swirl until decolorized. If your sample is to test positive an extremely tiny amount of yellow precipitate will form in the bottom of the vessel. What you will notice before you can see the precipitate is the smell of iodoform. Every third lot of output was tested including the foreshots (I save it for solvent/lighter fluid)

Observations:
I knew prior to doing this test I am quite sensitive to the smell of iodoform so this test is ideal. There was a noticeable difference in the smell to me between jars 1 and 4 prior to performing the test. However, there was no noticeable difference between jars 4 and 7. After performing the iodoform test I could smell a very noticeable difference between jars 4 and 7. Jar 7's test had a faint scent of iodoform jar 10 was barely noticeable and there was no iodoform smell on subsequent tests.

Conclusion:
This has shown me that for this batch my hearts cut begins around jar 7. I can smell the fuels decently so until I devise another test... perhaps the 2,4-DNPH test if I can get ahold of the reagent... I will have to rely on scent and taste...

Here are the links to the images of the test:
step 1
https://drive.google.com/file/d/14_HgoC ... sp=sharing
step 2
https://drive.google.com/file/d/1Eya8cj ... sp=sharing
step 3
https://drive.google.com/file/d/1p8I9n4 ... sp=sharing
step 4
https://drive.google.com/file/d/1WGm6c0 ... sp=sharing
step 5
https://drive.google.com/file/d/1m3mnle ... sp=sharing
Iodoform
https://drive.google.com/file/d/1c76ggb ... sp=sharing
All tests completed
https://drive.google.com/file/d/12D6RZu ... sp=sharing
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Re: Calling all chemists.... UJSSM iodoform test

Postby hexokinase » Thu Apr 20, 2017 7:47 am

HDNB a credit hour is supposed to translate into hours of class time per week per semester... although with the sciences those labs can last much longer than an hour... So in my case for chemistry anyway that says about 285 hours of class time... I would say that lab time is actually closer to 3 hrs per week so it's more like over 400 hrs plus my own endeavors in chemistry... last summer I had a problem with roaches getting into my man cave and I couldn't get hold of boric acid to kill them.... I didn't like the idea of fogging up my man cave... so I synthesized it out of borax and muriatic acid... recrystallized it... put it in a sauce bottle with some glass marbles to keep it from clumping and bobs your uncle no more roaches...there's no defense against dehydration!! I know I've managed to get on some NSA list somewhere.... there for a while amazon was recommending precursors to black powder to me...
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Re: Calling all chemists.... UJSSM iodoform test

Postby Jes2xu » Thu Apr 20, 2017 2:23 pm

This is pretty exciting for me!

I guess I fall into the category of people that think objective testing is a great way to understand why/how/when something affects sensory tests/experience.

So anytime I see people exploring this sort of thing I sit up and take notice! Will be watching this thread closely ;)
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Re: Calling all chemists.... UJSSM iodoform test

Postby hexokinase » Thu Apr 20, 2017 4:07 pm

After some consideration today, I think I need to make a reagent grade iodine solution. I have no way of knowing what the actual concentration of the infowars X2 iodine. I think I will make a Lugals solution.... reducing my variables and all. I actually expected more precipitate than what I observed... I suspect all the methylated carbonyl's didn't react as there wasn't enough iodine in the test... I'll repeat the test when I get the reagents squared away.
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Re: Calling all chemists.... UJSSM iodoform test

Postby contrahead » Fri Apr 21, 2017 8:16 am

@ hexokinase
I notice that your pictures are hosted on Google drive. Nothing wrong with that but this site can host pictures as well and it's an easier process. The limitations are: image size restraints of 800 x 800 or less (neither height or width may exceed 800 pixels) and a maximum of 6 images per comment.

* one problem with the 'Post Reply' screen is that these buttons can often be out of sight - and therefore one must scroll down to see them.
[Post Reply] > [Upload attachment] > [choose file] > [add the file] >[place in line]
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Re: Calling all chemists.... UJSSM iodoform test

Postby patrick10ghost » Fri Apr 21, 2017 11:36 am

The only problem I see with doing all these tests is the idea of building your drinks flavor profile. I collect everything from first drop out till 196° or I taste char. If I left out my heads it would drastically change my flavor. Tests are great but you are missing the point of learning to taste and build your skill to detect the flavors you want.

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Re: Calling all chemists.... UJSSM iodoform test

Postby yakattack » Fri Apr 21, 2017 2:13 pm

patrick10ghost wrote:The only problem I see with doing all these tests is the idea of building your drinks flavor profile. I collect everything from first drop out till 196° or I taste char. If I left out my heads it would drastically change my flavor. Tests are great but you are missing the point of learning to taste and build your skill to detect the flavors you want.

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1. Stop using tap talk. . Or if you are going to remove that dam add for tap talk.

Second learn to do cuts properly. The op isn't asking about this to negate cuts but rather to understand the biochemical relationship between cuts that he is looking for based on taste and smell.

If you are indeed keeping everything the you are only robing yourself of the best drink you can make. Anyways. Carry on
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Re: Calling all chemists.... UJSSM iodoform test

Postby hexokinase » Fri Apr 21, 2017 5:08 pm

@patrick10ghost
I collect and save everything too but no way in hell would I drink everything... The first bits that come off are highly concentrated with acetone(dimethylketone, 2-propanone, nail polish remover or whatever you want to call it) consuming large concentrations of acetone can lead to hepatic damage as well as renal damage... I don't want to risk hemodialysis, renal transplant, cirrhosis, azotemia, hyperbilirubenemia etc for a drink... I hope you dont drink all of that! I understand that some of the heads can be desirable but for me thus far I like a rather tight cut between the heads and the tails... some do make it into my final product but not much... where I make my first cut everything before that gets recycled into the next run... where I make my tails cut charges my thumper and the excess is also pitched into the boiler... the test doesn't take much longer than the spoons method... the iodoform test gives me another way to objectify what I'm learning to do and that is making proper cuts... also it adds to the sensory based tests if I cant see the precipitate... If I get better results with precipitation when I synthesize the reagent grade iodine i can then recrystalize it, weigh it, and get an idea about the concentration of those products. For me it's about exploring the science behind this hobby while getting a tasty beverage to boot. Once I obtain a level of mastery about making cuts that I'm satisfied with I think it would be interesting to perform an experiment where one final product is prepared by sensory based testing alone and the other by objective chemical tests alone and see how they compare
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Re: Calling all chemists.... UJSSM iodoform test

Postby Yummyrum » Fri Apr 21, 2017 8:05 pm

Hi hexokinase

Thanks for sharing this , its always good to learn of new tricks .
I was wondering what the " nascent iodine (infowars x2 iodine)" was .Is it a brand name ?
I'm a Labby these days and make up Lugals solution at work from Iodine solid and Potassium Iodide as a starch indicator .I have no real understanding of Chemistry but I am kinda interested to see if that works .

I am surprised that you are concerned about Acetone . I understood there is bugger all Acetone in our distilled product . However you often hear distillers talk about the finger polish remover smell . I believe this is actually Ethyl acetate which is the major component of heads.
At a recent Distillers get-together we got the opportunity to smell various samples of lab grade Acetone , Methanol , Ethyl Acetate , Propanols 1 and 2 , Butanols etc and it was quite obvious that what we thought was Acetone was in fact Ethyl Acetate .

Any Acetone that's present would surely be boiled off fairly early in the piece as it is very volatile with a BP of 65 degC . As we all dump the first jar or two as Foreshots , and then even cut out the heads , I think there would be no chance of any damaging quantity of it ending up in our drinks ......Liver damage from ethanol is likely to be a bigger concern .

Anyways , that's my 2 cents and I look forward to your results .
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Re: Calling all chemists.... UJSSM iodoform test

Postby patrick10ghost » Fri Apr 21, 2017 10:32 pm

hexokinase wrote:@patrick10ghost
I collect and save everything too but no way in hell would I drink everything... The first bits that come off are highly concentrated with acetone(dimethylketone, 2-propanone, nail polish remover or whatever you want to call it) consuming large concentrations of acetone can lead to hepatic damage as well as renal damage... I don't want to risk hemodialysis, renal transplant, cirrhosis, azotemia, hyperbilirubenemia etc for a drink... I hope you dont drink all of that! I understand that some of the heads can be desirable but for me thus far I like a rather tight cut between the heads and the tails... some do make it into my final product but not much... where I make my first cut everything before that gets recycled into the next run... where I make my tails cut charges my thumper and the excess is also pitched into the boiler... the test doesn't take much longer than the spoons method... the iodoform test gives me another way to objectify what I'm learning to do and that is making proper cuts... also it adds to the sensory based tests if I cant see the precipitate... If I get better results with precipitation when I synthesize the reagent grade iodine i can then recrystalize it, weigh it, and get an idea about the concentration of those products. For me it's about exploring the science behind this hobby while getting a tasty beverage to boot. Once I obtain a level of mastery about making cuts that I'm satisfied with I think it would be interesting to perform an experiment where one final product is prepared by sensory based testing alone and the other by objective chemical tests alone and see how they compare

So my issue with this statement is you don't pitch your fore shots yet you recycle them into the next batch. It would seem You are concentrating the acetone and other chemicals by adding it back. I run 2 150 gallon runs and collect a total of 5-9 gallons of product from each one with 20 gallons of recycle made of tails only. I have never had an issue with harmful build up or hell even detection. I take careful watch and once I collect my insignificant levels of nail polish they are rubbed out by the aging process. But like I said if you are recycling those foreshore you are not allowing the harmful chemicals to leave the stilling cycle. Do be careful because with 10 or so runs you might start getting a distinctive amount showing up in your foreshot collection.

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Re: Calling all chemists.... UJSSM iodoform test

Postby hexokinase » Sat Apr 22, 2017 4:47 pm

@patrick10ghost
Sorry, I wasn't clear about what I do with the foreshots... I do save them for use as an organic solvent to clean my glassware and as lighter fluid but they are not recycled into the next batch... from the way it read in your post since you say that you have saved everything from the first drop I was concerned that you were using the foreshots in your product...

@yummyrum
Yes. the infowars x2 iodine is a brand name product... it is an iodine supplement. Its what I had on hand. I have no real way of knowing how much iodine is in the solution... I would much rather synthesize Lugals solution because my reagents would have a purity assay attached to them. I could probably titrate it to get an idea but that stuff is expensive. The haloform reaction that we are performing with the iodoform test will form iodoform with many methylated carbonyl which includes acetone and ethyl acetate. I would recommend doing the test with 5% I2 and 10% KI. This should give more than enough free I-. I also suspect that the 1.04 M NaOH would be insufficient to decolorize the test so I would shoot in the neighborhood of 3-6 M NaOH. The concern I was voicing about acetone was related to a post where I thought all of the distillate was being used in the final product. Like many things in life toxicity is all about concentration. I will need to reevaluate those scents... i'll see if i can find lab grade ethyl acetate.. I agree that since the forehshots are set aside and ethanol and ethyl acetate have very similar boiling points the majority of what were are testing is the presence of ethyl acetate. Since you are working in a lab surely there's some NaOH around somewhere so mixup a batch of 3M. I would go 2-3 mL of that Lugal's 5% I2 and add the NaOH (aq) drop wise then swirl, drop wise swirl until clear observing precipitate and scent.
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Re: Calling all chemists.... UJSSM iodoform test

Postby Oldvine Zin » Sat Apr 22, 2017 6:38 pm

patrick10ghost wrote: I run 2 150 gallon runs and collect a total of 5-9 gallons of product from each one with 20 gallons of recycle made of tails only.


That's a little too big for around these parts

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Re: Calling all chemists.... UJSSM iodoform test

Postby Bagasso » Sat Apr 22, 2017 9:29 pm

Sorry, jumped the gun.

I was thinking it was just for methanol but I see i missed the mention of ketones and aldehydes.
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