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Second batch

Posted on Poppers Guide's Forum

Topic created by Charlie
on Wed, 27 Oct 2021 at 23:58

Charlie said on Wed, 27 Oct 2021 at 23:58...

This time I did the reaction in a chest freezer with everything but the peristaltic pump and a few inches of pumpís input and output tubes all inside the freezer.

The reaction vessel consisted of a 500ml Erlenmeyer narrow mouth flask surrounded by tap water in an 8C Pyrex frozen overnight. The reaction vessel had a temperature probe fitted inside to monitor the temp of the reaction. The flask was fitted with a drilled rubber stopper holding a 10mm borosilicate straw and the output tube from the peristaltic pump was suspended inside the straw. I used some modeling clay to seal the top of the straw so that the drops in theory would fall below the surface of the water. (The drops may have not been getting below the surface of the water because there was NO2 at points in the tube. See below.)

I set the pump to drop the acid/water mix (1.1 mol of HCL) over 92.5 minutes.

The peristaltic pump was predictably reliable. The freezer was blasting the entire time.

I stopped half-way and checked on everything inside the freezer. I had a puff of brown/orange NO2 when I lifted the tube out of the flask so obviously encountered an issue that needs to be addressed. Did my stir bar possibly stop rotating and I missed that - or were the drops maybe not getting below the surface of the water and the reaction was happening in the tube due to possible pressure issues since the reaction vessel was stoppered?

No white paste on the tube this time.

-The contents of the reaction vessel started out at -17C (probably could have gotten to -23C if I had waited longer or chilled overnight)
-After 15 minutes, it was -11C
-After 30 minutes, it was -10.2C
-After 46.25 minutes (half-way point), it was -9.7C
-After 60 minutes, it was -9.8C
-After 75 minutes, it was -9.2C
-At 92.5 minutes, it was -10C

I had some brown/orange NO2 at the end as well, maybe a little too much.

After letting the mix stir for an additional 15 min. outside of the ice bath, I had some waste phase settle on top of the yield again (maybe 1mm deep).

After I placed the solution in the separatory funnel and allowed it to settle for 10 minutes (not 20 min per the guide), there was still some waste phase on top of the yield. However, the waste phase did not effervesce as much in the separatory funnel like my first batch - much calmer. I was getting nervous after 10 minutes because the effervescing began to accelerate so I separated the waste and yield at that point.

The neutralization stage went much easier this time since everything was still cold and a new stirrer had no problem holding on to the bar. I poured off the yield (80 mL) and the wet baking soda stayed behind with no issue. The yield is drying on molecular sieves. The waste was fairly wet so I think I left behind some yield. What should the typical yield be for a 1 mol reaction?

At the end of this batch, I am left wondering why I had brown/orange NO2 at times. I will be tinkering with the apparatus moving forward and I have some ideas about how to improve it, especially moving back to a beaker to prevent pressure issues and prevent having any reaction take place in the dropping tube, if that is indeed what happened. It's speculation at this stage.

Charlie said on Thu, 28 Oct 2021 at 01:23...

I'm considering that any pressure built up in the reaction flask (because it was stoppered) could have been creating back-pressure in the dropping tube and prevented the acid from dropping below the water's surface. In hindsight, the apparatus that I created did allow any pressure that built up in the reaction vessel any method to escape. Need to fix this for the next try...

Charlie said on Thu, 28 Oct 2021 at 02:27...

Correction: In hindsight, the apparatus that I created DID NOT allow any pressure that built up in the reaction vessel any method to escape. Need to fix this for the next try...

Charlie said on Thu, 28 Oct 2021 at 03:08...

Another reason I would not want to use an Erlenmeyer flask again is that it is impossible to see what is happening in the reaction vessel at the cold temperatures. The glass is completely fogged and I really struggled to see if the spinbar was turning or what the heck was happening inside the flask. Trying to peer from above into the small flask opening was almost excruciatingly difficult, even with a flashlight. At least there is a little more surface area to tell what is going on with a beaker.

The Professor said on Thu, 28 Oct 2021 at 19:05...

if my math is right, n-Butyl nitrite molar mass = 103.12 g/mol and density = 0.882 g/mL. Molarity should be

molarity (mol/L) = [density(g/ml) X concentration(%) X 10] / molar mass(g/mol)

[0.882 X 100 X 10] / 103.12 = 8.55 mol/L

1 mole of that should be

X mole C4H9NO2 = X mole / molarity

= 1/8.55 = 117ml

The Professor said on Thu, 28 Oct 2021 at 19:12...

very nice looking temps, they stayed very low, which means that at the drop site, there wasn't enough energy to form butyric acid when the HCL drops; that's a very good thing both short term (more pleasant aroma) and long term (less chance of decomposition to aldehydes and nitrates).

A bit of NO2 is probably inevitable with so much oxygen floating around; I used to get trace amounts in the down tube also.

Yes, some method, perhaps another tube venting to atmosphere, would prevent pressurization of the Rx vessel.

your yield is a bit low, but that typically comes with practice and avoidance of generating NO2.

I think your apparatus and method has proven to be repeatable, and at this point, that's fantastic; one or two tweaks here and there

Charlie said on Thu, 28 Oct 2021 at 20:29...

TY Prof. Thank you for the math of the ideal yield. I also believe a few tweaks are necessary to improve the yield and reduce NO2 as much as possible. I do believe I left some yield behind during neutralization. I saw it floating with the baking soda after allowing to further settle.

I have been processing more what happened during the second batch. I believe I could have had 2 problems with the second batch: the tube dead-center in the vortex and pressurization of the reaction vessel. Next time, I will try with the dropping tube off-center again and see if the acid is carried away into the water thereby reducing NO2 in the dropping tube.

I plan to change the dropping tube setup and change back to a beaker next time.

Prof., can you make any inferences from the temperatures that I was seeing? I noticed that the temp immediately spiked in the first few minutes as to be expected. At the half-way point when I stopped dropping the acid, it cooled slightly. At the end, I noticed a detectable cooling of about 1-degree Celsius. Did that mean the reaction had consumed all the alcohol? I am asking, because I am curious, if detectable cooling would be a good indication of when to stop dropping the acid next time?

The Professor said on Thu, 28 Oct 2021 at 22:32...

There are many ideas about how to tell when the reaction is complete. Some way to monitor the waste phase pH for a sudden drop (excess acid builds up in the waste phase once the alcohol has been satisfied). Monitoring the temp is another idea.

I don't bother with any of that, since they both happen AFTER the fact; I don't really understand the desire to achieve perfection during dropping, when any excess (unless its extreme) will be taken care of during neutralization.

If you want to do something like that, a hydrogen probe will read activity in the nitrite phase even though it's anhydrous (pH strips won't give valid indications unless they are in an aqueous environment) .

I don't see that it would improve anything very much; the idea of a slight excess of NaNO2 and HCL gives very nice results, consumes ALL of the alcohol (the nitrite won't be dilute) and any overcorrection is compensated for during neutralization.

The Professor said on Thu, 28 Oct 2021 at 22:38...

just a thought; it might be desirable to measure your crude yield BEFORE you neutralize.

That way, your numbers won't include losses from neutralization, but that's probably a good thing. Doing it that way enables you to compare RAW yield between various preparation techniques. After choosing the optimum apparatus and procedure, you can then move on to minimizing losses during neutralization, which pretty much amounts to minimizing the dwell time (there's going to be losses from spinning yield and water together, but it's unavoidable (un-neutralized or partially neutralized yield is not healthy or fun to inhale))

Charlie said on Thu, 28 Oct 2021 at 23:27...

Thank you Prof. All makes sense and I will not "dwell" on trying to perfect the ratio of reagents for the reasons you mentioned, especially since I am neutralizing it as you said. More than anything, I was curious why I would see cooling at the end - and the possible reasons behind it. I expected to see the temp rise and rise, but then I saw it cooling and left me curious more than anything.

Will definitely measure crude yield next time - great suggestion. Will work on perfecting the apparatus ATM more than anything moving forward. Have some ideas I wish to try out...

I poured out my old batch onto some paper towels because I wanted to see what would happen. Wow, no joke that n-butyl evaporates quickly! Almost all gone within an hour or so.

Charlie said on Fri, 29 Oct 2021 at 05:16...

Hi Prof., do you have any opinion about smaller borosilicate Erlenmeyer flasks with ground stoppers being sold on eBay from China? Looks like about ~$8/ea. for 100-125mL.

I don't know if it's typical or because of this so-called commodity shortage/inflation, but everything here in the USA is exorbitant.

I was thinking that even if it's not the highest quality that it may be ok just for storage (no thermal shock)? I was pretty impressed with the quality of the dropping funnel - my fault for not ordering the right equipment! ty

The Professor said on Fri, 29 Oct 2021 at 16:54...

This prep doesn't put much stress on glassware; just about anything should be suitable

Charlie said on Sat, 30 Oct 2021 at 03:48...

Ty Prof.

Found these for storage:
https://www.amazon.com/gp/aw/d/B00551DZW4?

The Professor said on Sat, 30 Oct 2021 at 18:23...

they look very nice

Charlie said on Sat, 30 Oct 2021 at 23:07...

Ty Prof. I'll post how the amber reagent bottles work out.

Back to questions about storing NaNO2... ;-) Turns out the order of high quality molecular sieves never materialized. Need to start that search again!

In the meantime, I am wishing to store my NaNO2 in some vacuum sealed mason jars. I have a bunch of these moisture absorbing packets:
https://www.amazon.com/dp/B08SWBYVWS/

Do you see any harm in using those in the jars with the NaNO2 since I don't have good sieves on hand?

The Professor said on Sun, 31 Oct 2021 at 18:48...

I wouldn't expect any good results from silica gel. It is an aBsorbent, not an aDsorbant. If you want to try it, I suggest using a small amount. Silica will attract water, but it doesn't sequester it within its pores, like AA or MS

Charlie said on Sun, 31 Oct 2021 at 21:39...

TY Prof. I appreciate your advice and will wait to break the factory seals and rebottle the sodium nitrite in glass until I can held hold of some quality sieves. I'm glad I asked you first!

However, I actually have some activated alumina though. Do you think that could possibly work to keep the sodium nitrite dry?

Charlie said on Mon, 1 Nov 2021 at 02:46...

Professor, I've been wanting to ask you more about neutralization.

I've tried using both regular baking soda and anhydrous sodium bicarbonate on 2 batches now - both twice.

However, I do not think that I have ever seen any fizzing. I have reach an emulsion, but never a reaction that I was expecting. I have been expecting to see fizzing like a shaken can of soda or maybe even some effervescence. However, it's always just flat. Do you have any ideas about what could be going on?

The Professor said on Mon, 1 Nov 2021 at 21:24...

activated alumina will adsorb H2O very nicely

there should be quite vigorous effervescence; at least once; i've taken to sprinkling it in a bit at a time, and usually get at least one big puff of fizz, sometimes two or three.

Absolutely NO fizzing is strange;

On the plus side, if your reaction completed with a VERY slight hazy blue waste phase, and a VERY slight green tinge to the yield, then it's possible that you've landed at the perfect reaction speed and stoichiometry.

On the downside, if you used 1:1.05:1.10 ratios (alcohol to sodium nitrite to acid) then there is bound to be SOME excess acid in there, so I'm not understanding why there is no fizzing (is the baking soda still viable (check with a weak water/acid solution)?

Charlie said on Mon, 1 Nov 2021 at 22:44...

Ty Prof. I believe you hit on a very valid point...and I had just been thinking about this overnight. I believe the baking soda may be no good. Will just get some new. I was using a giant bag from Costco from who knows when! Probably bad decision.

Also, I was dumping all of the baking soda in quickly. Probably need to be more attentive to sprinkling slower and not overwhelming any fizzing.

I definitely believe there was acid left over after neutralization with this questionable baking soda because the final yield turned my dosing device (plastic test tube) a slight red color. The yield was smelling very acidic and unpleasant until I added some Kcarb and what a difference a day makes. I didn't quite understand why my first batch turned pungent so quickly, but now it makes sense that there was probably residual acid. This all leads me to believe the baking soda is no longer viable.

Will be making another attempt shortly with a newly modified apparatus and new baking soda!!! I've invested a LOT of time and energy into improvements so I am anxious to share any success or challenges.

The Professor said on Mon, 1 Nov 2021 at 22:55...

time and energy are precious; you seem to be on a good path so far though, I'm looking forward to your next results.

Charlie said on Tue, 2 Nov 2021 at 00:32...

Ty Prof. This has been such an interesting journey and I have learned so much that I am forever thankful to you for all of your help. I would be so lost without you.

The Professor said on Tue, 2 Nov 2021 at 17:02...

The guide was started by popchef, is now curated by me, and includes contributions from several makers, including you (in the form of questions).

I'm trying to keep is useful; or doesn't contain anything mystical, magical or unknown, and is mostly existing data from various sources.

Chemistry doesn't have many corollaries in every day
Iife; a lot of people don't have much or any experience, particularly with terminology, and the guide aims to he a useful reference

Charlie said on Tue, 2 Nov 2021 at 18:47...

Thank you to you and everyone else that is involved. I just browsed the guide again and didn't realize the depth of your work to keep it a living document! Thank you for making it accessible and current. Honestly, it is this guide and your selfless help that has gotten me as far as I've gotten. I spent the first month trying to gather data from across the web and I was having a really hard time sorting fact from fiction...until your selfless help.

I tried the butyl nitrite last night during sex and wow, what an amazing ass relaxer. It is interesting because this second batch of homemade butyl nitrite, like the first, is not the psychological/euphoric high that I have experienced with some OTC nitrites, but the ass-relax was simply out of this world. Who knows what I was buying when I had those euphoric moments!

I am not someone who usually loves ass play, but the effect was incredible to say the least. Wow! I don't think I have felt something like that for a very long time from OTC nitrites, maybe going back 20 years to when I was buying plain brown bottles in the 90s in the Bay Area.

I am looking forward to making some blends when I have the process and apparatus sorted out better...still more work to do before moving on.

Reading through my notes, am I correct that n-amyl (pentyl) has some of the better euphoric effects of the alkyl nitrites?

Lastly for this post, how would you describe tert-butyl (and I assume you are combining it with other alcohols because of its solid state at room temp)?

Charlie said on Tue, 2 Nov 2021 at 20:49...

Love the brown reagent bottle from Amazon!

https://www.amazon.com/gp/product/B00551DZW4

Works very well. It's a little large for the small batch I ended up with in the end, but I love the glass stopper. I found them on Aliexpress for about half the price delivered from China.

The Professor said on Tue, 2 Nov 2021 at 21:35...

The active ingredient in alkyl nitrites, Nitric oxide, relaxes smooth muscle tissue (anus, vagina, sure, but also intestines, stomach lining, walls of blood vessels, etc.)

The vasodilation effects on areas of physical interest are self evident, but any phycological effects (psychoactive effects, bliss, euphoria) vary greatly as they are a function of how your brain is reacting to the changes in blood flow.

The alcohol involved in the making has a very minor role; the alkoxy fragment determines the volatility of the alkyl nitrite, and that's about it.

Ingesting fusel alcohols doesn't have the same effects that ingesting ethanol (any alcoholic beverage) does. The fusel alcohols are responsible for detrimental effects of cocktails in which they occur (as an unintended side effect of distilling ethanol).

All of the alcohols involved in making nitrites for street use aren't alcohols in the sense that ethanol is. Ethanol itself is poisonous, but at least its intoxication effects aren't deadly. Fusel oils have a much higher 'body load', and don't provide effects that are of value.

Luckily, once the NO is separated from the RO, the alkoxy radical is passed through the kidney; at only parts-per-million blood concentration, it is not responsible for any alkyl nitrite effects.

Taken together, it is my opinion that the primary difference between alkyl nitrites is their volatility. nothing more or less.

Having said that; some people are of the opinion that lower nitrites such as n-Pentyl and isoPentyl (possibly n-Butyl) put a person in a headspace that's somewhat 'zoned out'.

not in a virtual coma, like the lethargy/narcotic/tranced out/dirty high that you can get from nitrates, but in a warm, safe place that doesn't remember to continue to take hits to sustain it.

that CAN happen, it did happen with us, and our nublu delta (our mildest blend) is fantastic for bottoming.

Also having said the above, some people are of the opinion that the higher nitrites (n-Butyl sec or tert butyl) put a person in a headspace that's more alert/energized.

Our nublu alpha is my personal favorite; it uses just a bit of tert, which to me has a 'fresh makjer' effect like biting into a peppermint patty. Not particularly MINTY at all, but the same type of sensation (brisk, alert)

That's my personal experience with varying alcohols in the nitrites.

I hope it was somewhat useful; I'm not the best at descriptors

Charlie said on Wed, 3 Nov 2021 at 05:51...

All of it makes complete sense though this unskilled mind needs some time to process all of it ;-) I deeply appreciate the explanation.

Nitritespecialist said on Thu, 4 Nov 2021 at 15:43...

@Charlie....what did your second brew smell like and did the odor change over time?

All the nitrites I have tried can have strong ass relax effects. It will be of interest to note any sudden or longer term side effects you may experience with your butyl.

The Professor said on Thu, 4 Nov 2021 at 19:00...

@Charlie,
the poster above is not who he says he his.

Ken's ideas were wrong enough, but the master is also out there.

I'm not saying DON'T respond to him, it's your call, but he'll only infect this topic with his proven false notions

Charlie said on Fri, 5 Nov 2021 at 00:59...

Life's gotten crazy and in the way, but will be back shortly once it settles a little and I have another batch to report (still waiting on new supplies).

The Professor said on Fri, 5 Nov 2021 at 22:25...

When you're ready again, I cobbled together a peristaltic dropping mechanism, so I'd be able to play along if you had obstacles.

It's a much more set and leave it alone endeavor now; a drain hole will prevent the ice bath from floating the reaction vessel (if you don't intend to use the measuring cup for actual cooking anymore).

I used 2.4 mm ID tubing, set the drip rate for no NOx evolution at the start (3 sec per drop). After an hour, I bumped the drip rate up to 1.74 seconds per drop and let it run to completion. Total reaction time was just over 3 hrs

It's much easier to gain reaction control with a peristaltic pump; no more babysitting the apparatus, no more toxic clouds of NOx. Changing the ice bath is also much easier; just stop the pump, dump and refill the salted ice, and turn the switch back on.

If it weren't for the extra expense of the pump, I'd be inclined to totally re-write the guide with a pump in use.

As it is, I will at least add it as a very viable alternative to the batch dropping method, as it is by a great deal easier to get repeatable drip rates.

The Professor said on Fri, 5 Nov 2021 at 23:05...

I used molar ratios 1:1.05:1.10 (alcohol to Sodium Nitrite to Acid), and got very close to perfection (Just turning green yield, JUST barely blue waste)

I had no foaming, no NOx gasses and no biphasic yield layer; also no pin and needle bubbles boiling out of the yield or big bubbles bupring out of the drop tube

Nitritespecialist said on Fri, 5 Nov 2021 at 23:22...

Wow...I thought Thomas had it ALL figured out to a perfect Tee ages ago.....and now he thinks just maybe he should mix it up...LOL

And just for the record...Thomas the Professor has ZERO idea what pure n-butyl nitrite, isobutyl nitrite, n-amyl nitrite or isoamyl nitrite should smell like...simply because he's ALWAYS mixed the alcohols, falsely thinking that even though they are all very similar, that mixing them will result in a much improved product. It won't!!! All the best traits can be found in n-amyl nitrite....great nondescript odor and potency that last a very long time without all the nasty harsh side effects of the other commonly made nitrites.

The Professor said on Fri, 5 Nov 2021 at 23:35...

you KNOW I've moved on to vapor phase prep, whether you are Ken or the master. Everything else you said is wrong or a lie.

You are destroying your own credibility, dude, saying things that are easily disproven; if you're trying to get a rise out of me, you have failed; watching someone purposefully self destruct can be quite entertaining

Charlie said on Sat, 6 Nov 2021 at 06:03...

Prof., I'm so excited to hear about your peristaltic pump.

I'm just about to give it another go. Received my supplies to try my new apparatus and tinkered with it for a few hours. Currently everything is freezing overnight.

Your post had me thinking...maybe my drop time was too fast if I was getting NO bursting out even at the cold temps on the second batch. I have been shooting for 90 minutes, based on the guide, maybe in error and not knowing what I'm chasing and why. I'm clueless remember!!!

You noted a 3 hour drop time. If temps are kept cold indefinitely and keep a low temp indefinitely is not a concern, for example, what does the ideal drop time look like?

I want to give my next batch every fighting chance and I feel that timing is where I am iffy and doubting myself. Should I change to 3 hours? Ty

Charlie said on Sat, 6 Nov 2021 at 06:49...

Prof., also one more question while it's on my mind:

Is there any concern with the acid sliding down the inside of the glass dropping tube to the water/NaNO2? I've been trying to get perfection with the drops falling perfectly down the center of the drop tube, but that perfection is difficult without the peristaltic pump tube centered perfectly and close to the surface of the water. The higher that I suspend the peristaltic pump tube, the more that the drops want to slide down the inside of the drop tube.

The Professor said on Sat, 6 Nov 2021 at 15:44...

The batch I ran yesterday took about 3 hours, which is longer than my lab notes from when I was making that way.

I was intentionally on the conservative side with the drop rate, and believe that the run time can be reduced without damaging the yield very much.

The dropping funnel notes mention a drop every 4 seconds as a guide point, and that's a bit the best I could do with a dropping funnel. Even with practice, there will be bursts of liquid every now and then, as one tries to readjust the stopcock.

With the dropping funnel, reaction speed was still a bit too fast (pounds and needles evolving from the yield, larger bubbles evolving from the drop tube., Etc.

With a peristaltic pump, the temp stays lower since they're are no bursts of higher reaction speed. At the surface, and as far done as I could see the liquid look like a calm lake, no volcanic activity underneath.

Long and sorry of that.... It seems that a 90 minute drop time might not be a bit too fast for reaction speed. I was able to get up to 98% purity that way, but I bet the batch I made yesterday would test above that (probably not 3 9:s like vapor phase making, but still very very nice.

As the reaction progresses, the reactants are becoming more sparse. This means that a drop at the beginning generates more heat than a drop near the end. I started with a drop every 3 seconds as a guess, and it seemed appropriate (my molar tattoos were 1:1.05:1.10 with the HCL diluted with 20ml of distilled water). There was no gas, so I didn't slow it down any further. After the first hour, I bumped the speed up to A drop every 1.75 seconds, and still no NOx has or boiling yield. I let it finish, and the prep took about 3 hours.

You can probably improve on this reaction time. The initial phase of extreme sensitivity to reaction speed likely lasts 1/2 he to 45 minutes, so the reaction speed can be increased some, and possibly faster than my first run.

I mainly did this so I'd have visual cues to go by as you reported what was going on for you. It's a very worthwhile method, even though it does increase the cost of entry.

The Professor said on Sat, 6 Nov 2021 at 15:50...

I dropped by drilling a hole in the bottom of a soda blank (a thick walled PET plastic container that looks like a test tube (they are what those 2 liter soda bottles are made from), and flying the pump tubing into the bottom of the blank. I clamped the blank to the ring stand with the same clamp I had been using to mount the dropping funnel. So, my drops descend into a river that is about 3/4 inch thick, and never touch a side. That's not a problem at all with the peristaltic pump (reactant running asking the inside of the rubbing instead of falling straight down by gravity). Pumps can handle a bit of back pressure.

The Professor said on Sat, 6 Nov 2021 at 16:12...

I don't know that I directly answered your first q. The ideal drop time looks very uninteresting.

At the beginning, each drop will yield a burst of blue nitrous acid that dissipates very quickly (that's under the surface).

That nitrous is satisfied by adjacent alcohol, and the yield floats above the reactants.

The surface remains calm, with no worries of gasses, until it's complete.

By contrast, with a dropping funnel, there always seemed to be at least a bit of foaming, indicating the reaction speed is too fast.

The gist:
dropping by funnel requires skill and at least periodic monitoring, and is capable of 98% purity.

Dropping by pump is plug sand play, very repeatable without monitoring and I'm betting high 98 to low 99% purity.

The run time is likely less than 3 hrs, but one would have to decide for themselves if the slight increase in purity is worth the extra processing time.

A rule of thumb is that a human can detect differences of about 10% in a process.

Charlie said on Sat, 6 Nov 2021 at 17:49...

Prof., thank you so much for all of this glorious information. The timing could not have been better. I am going to make adjustments and draw out the drop rate and watch it closely to better understand what I am seeing.

I am using my very limited time at the moment to process everything you wrote and will try to apply it to my next batch. I'll take my time with my next response with a post-batch review/assessment. Thank you again. Again, the timing and info were absolutely perfect.

The Professor said on Sat, 6 Nov 2021 at 18:02...

Glad to be of help

Charlie said on Sun, 7 Nov 2021 at 00:45...

Been testing out the Kamoer peristaltic pump to drop the 111 mL HCl and water over 3 hours and I think I got it set. I am using 1/16"x3/16" Tygon Chemical tube - beautiful tubing. I believe for the third batch that I am NOT going to adjust the drop rate part way.

I was able to slow the pump down so that it drops about .61 mL per minute. And the pump is only operating at about 2.5 of 7 on the dial, which means it can go even much slower - slower than the specs show. It's an analog dial which controls the speed electronically - very interesting. I'm pretty happy for $100 and in a neat little package ready to go. A quality dropping funnel isn't cheap so $100 + tubing is worth it to me.

Nitritespecialist said on Sun, 7 Nov 2021 at 16:10...

@Charlie...I might suggest you perform the Italian study's method of making a small amount of alkyl nitrite to use a reference standard for all your large brews. The Professor shared the link with everyone which is how I discovered it. If you don't know the target, its precise odor and effects, how can you possibly know when you are close to making a proper popper????

The Professor claims the Italian method results in a highly pure nitrite, good enough for a reference standard, the highest purity possible. To start with large brews without knowing your target well and having no gas analyzer to test for purity seems illogical to me.

Charlie said on Sun, 7 Nov 2021 at 17:03...

@Nitrite, I saw that thread recently. Very interesting. Had me thinking that maybe my idea of using a freezer is not a bad idea (darkness)! I think it's probably too complicated for my meager skills at this point and that I have some apparatus work still to iron out with the method in the guide.

I hope that once I have an apparatus and yield that I am happy with that I could get it tested so I know where I'm at. But that's down the road... I completely understand the desire to know I purity because I'm wondering myself!

The Professor said on Sun, 7 Nov 2021 at 17:47...

You're on a good path Charlie. The first batch I sent on for analysis was about 6 months after my initial runs. The first few runs were focused on finding the ideal environment and stoichiometry for the apparatus and method I chose.

Comparing the runs with my notes, the nitrite obviously wanted to be made slower and colder. (I was initially running at OC). The run I sent was scoring (in my arbitrary rating of 1-10) an 8, and was undertaken at -6C for about 90 minutes. that got me to 95% purity.

A few more runs, and then testing again. (After the first certified test, you now know how you're personal rating relates to an actual purity percentage. After the second test, you'll know if the changes you noted scored higher or lower, so you'll know what changes to look for going forward.

I ended up at -12C, 90 minutes and 98.3% purity. I'm being that the peristaltic pump method scores even higher than that, although absolute perfection is likely to be past the optimum point, considering time.

This procedure isn't what Bruno thinks it is. It is NOT a 'my way is best' or whatever else he claims that I claim (so he can rationalize his rudeness on his mind). The procedure shows you how to determine and improve on, and perhaps eventually reach a preferred embodiment for yourself.

The Professor said on Sun, 7 Nov 2021 at 17:56...

Re light exposure. Looking at the graphs I posted, photolysis does happen, but the rate isn't of any concern (to me). For a reference standard, sure, but there's a point of limited returns.

E. G. You might gain a few hundredths of a percent in purity (which matters greatly if it's a reference standard you are making), but meaningless in use (those gains would be swamped after the first X (X is how long it took to make) hours of exposure to light.

From personal experience (and you'll arrive at your own number)I can tell the difference between 90% pure and 95% pure, but not between 95% , 98% or 99.92% purity.

Charlie said on Sun, 7 Nov 2021 at 22:19...

Thank you Prof. I will definitely reach out to you for some tips when I'm ready to get a yield analyzed...way down the road. I haven't even done a third batch and I am already considering ways to improve the apparatus. Is this one of those things that is ALWAYS a work in progress!!!? I started this endeavor thinking I would achieve a product I would be satisfied with, but now I am beginning to think it may be a situation where I will always be tinkering with something!!!

The Professor said on Sun, 7 Nov 2021 at 23:54...

;-)

Most of the makers I've worked with on our forum achieve reaction control after much more effort, so your experience is already above par.
If/when you'll be satisfied with your creation probably has more to do with your personal interest level than anything else.

This batch method dropping procedure is capable of preparing very high quality nitrite. Personally, I moved on to the vapor phase, and get consistent three nines purity out of it.

That's a lot of expense, and more dangerous, compared to the batch liquid process, in which I was consistently getting 98% purity (two nines if I am extremely attentive).

A more haphazard approach can still give at least 95% purity.

I didn't proceed to vapor phase because I wasn't satisfied with liquid batch; rather because I enjoy chemistry, and a challenge.

You'll notice your own personal threshold after a while; you don't HAVE to chase trailing zeros. myself, i could tell the difference between 90 and 95% purity, but not between 95% and anything above

Charlie said on Mon, 8 Nov 2021 at 01:24...

Prof., do you happen to know the appx inside diameter of the "soda blank" you used?

For the third batch, I'm using a 11mm (0.43";-) ID glass tube and I'm finding that the drops sometimes slide down the inside of the tube (I believe my apparatus is not perfectly plumb and level and the diamater of the tube is still quite small).

I am starting to consider that I would like the drops to fall neatly into the solution - even though I know you mentioned that it is not problematic if they slide down the inside of the tube. I found that the drops can "bunch up" if they are sliding and not as consistent and perfect drops from the center.

Consequently, I am considering ordering a larger 24mm (0.94";-) ID or 21mm (0.83";-) ID tube. Any thoughts on either of those considering the size of the soda blank you are using, or should i go even larger? I.e 26mm ID. BTW, when I Google "soda blank," a plain can of soda is what shows up. I cannot picture what you're using. Ty

The Professor said on Mon, 8 Nov 2021 at 18:06...

My setup is makeshift right now, just wanted to be able to follow along if you had a specific issue.

I got the term wrong, they are called preforms

https://www.teachersource.com/product/preforms-and-caps?gclid=Cj0KCQiAsqOMBhDFARIsAFBTN3eeTSy2X-2NX1yt7oCYdzz9znZCvdv5eCrYEYWH4D2z-KLRyA8QIRYaAq7TEALw_wcB

The Professor said on Mon, 8 Nov 2021 at 19:32...

PET will eventually turn yellow from exposure, btw

Charlie said on Mon, 8 Nov 2021 at 19:32...

Thank you Prof.

I found a description of the image for those soda bottle preforms that describes them at 1" OD.

Maybe then my idea of a 24mm ID glass tube would work - and is not so wild after all... Sure would fit in the burrette clamp nicer than the 11mm ID tube, and maybe get those drops to fall nicely into the solution. Suppose that I will have to try it!

Charlie said on Mon, 8 Nov 2021 at 19:34...

Prof., one more question regarding drop tubes:

The choices are quartz or borosilicate. Quartz is the cheaper option, interestingly. Which would you choose?

The Professor said on Mon, 8 Nov 2021 at 19:52...

glass tubing will be better, and 24mm should be enough diameter so you don't have to use a level to get the drops down the bore.

If given a choice, I always go for boro simple because I only have one reliably working hand, and am, clumsy on top of that. Borosilicate glass survives me better

Charlie said on Mon, 8 Nov 2021 at 19:54...

TY Prof.

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