Workable Preparation....

Posted on Poppers Guide's Forum

Topic created by Nitritespecialist
on Sun, 31 Jan 2021 at 00:52

Nitritespecialist said on Sun, 31 Jan 2021 at 00:52...

10 grams Duda SN into 30mls DW
11-12 mls One pentanol into above mixture
FREEZE above mixture

15 mls muriatic Sunnyside brand
FREEZE

on moderate to high speed, using ice bath and done outside or with fume hood(over stove), slowly drip in acid

should see bubbling green top layer indicating full saturation of alcohol

siphon or drain off

wash 2x in cold water
rinse 3-4x in saturated brine/baking soda

dry on small clumps of anhydrous mag sulfate and potassium carbonate, 20 mins.

Pour onto fresh anhydrous Kcarb. shake....wait 24 hours and then pour
off onto fresh Kcarb. Should smell clean and fresh....with no acid or bitter undertones.

Nitritespecialist said on Sun, 31 Jan 2021 at 03:26...

The ratios here represent an excess of SN and acid. This should help the reaction proceed to completion whereby all the alcohol is saturated with nitrogen.

Any excess acid contaminating the crude yield can be easily washed out with water and then brine/soda.

Anhydrous Potassium Carbonate powder sucks up water and neutralizes acids. A popper must be kept dry and free from acid. HiMedia sells Kcarb on Amazon.

Jacko said on Sun, 31 Jan 2021 at 08:29...

Thanks Nitritespecialist, this is fairly close to my own n-butyl recipe.

I’ve found that if you introduce the frozen acid (or acid-alcohol mix) to the mag-stirred nitrite solution below the surface, this seems to yield a better quality product. 3ml disposable pipettes are ideal for this, as it also means the reagents are mixed a little at a time.

I’ve previously used dry baking soda to neutralise but will give the saturated rinse method a go, it sounds more effective.

Nitritespecialist said on Sun, 31 Jan 2021 at 15:53...

@Jacko...I have been aware of the "below the surface" addition of the acid or alcohol/acid mixture, but my brews are so small, it's difficult to do. I have wondered if it made a difference to the quality. Thanks for the input. I'll see if I can do it.

What I have found is that using a closely balanced recipe...using close to one mole SN to one mole alcohol to one mole HCl, is that I can't get a consistently good product. When it's bad, it smells bad and won't preserve. And effects can vary greatly.

I wonder what odor you are getting with your n-butyl nitrite. I have found that when it smells very sweet, almost candy like, it has the best effects. But often it has a bitter alcohol odor.....perhaps due to not using excess SN and acid.

Jacko said on Sun, 31 Jan 2021 at 22:01...

@Nitritespecialist, I usually do a larger volume recipe, targeting ~25ml (nightstand bottle) product yield. This gives me enough working volume to add the acid-alcohol mix below the surface, even with magnetic stirring. I have always taken this approach rather than neat acid addition, but will give direct acid a go to see if there’s any difference.

I have personally found that batches where red nitrogen dioxide fumes form are more irritating on the lungs and less potent. This happens either because of too fast an addition rate (ie me being impatient!), adding the acid-alcohol mix above rather than below the surface, or the overall reagent mix getting too warm. My ice bath setup is not ideal, so have to go slowly with intermittent cooling between additions.

The n-butyl is sweet and a bit like 7-Up soda when fresh. Bitterness only happens if it’s an old batch, towards the end of the bottle. Vigorous cold water washing seems to help.

I’m not sure about molar, but on a mass basis I use 10g SN, 8g water, 10g n-butyl alcohol, 12.5g HCl as the base recipe and usually double this for a big bottle yield. Note that the acid i use is only 25% HCl rather than 31% or 34%, so this means a little more water in the overall mix.

Nitritespecialist said on Mon, 1 Feb 2021 at 16:33...

@jacko....thanks for the info.

You are using 10 g SN per 12.35 mls of n-butyl alcohol. 10 grams of butanol, at .81 grams/ml...should equal 12.35 mls. That is similar to the 10 grams SN per 11-12 mls amyl I am using.

However, I am using quite a bit more water. I am using 30 mls instead of 8mls that you are.

I have tried many different variations. It's been difficult to find a definite pattern or tell tale sign that the reaction has been successful. With that in mind, and assuming that I still might discover something later, I have not found a definite link between the amount of nitrogen dioxide gas I see emitted and the quality of the product after being washed, quality as measured by a good odor, good effects and longevity of at least several days with use. If I use less water with excess SN and acid, I am likely to see more nitrogen dioxide gas, more vigorous foaming/bubbling, and likely higher temps. I haven't seen a drop in yield from using more water, more SN, more acid, but keeping the alcohol lower.

One mole of SN = 69 grams One mole of amyl alcohol is 88 grams or 114 mls. One mole of butyl alcohol is 81 grams or 124 mls. So a molar balanced equation would call for 6.9 grams SN per 11.4 mls amyl or 12.4 mls butyl. So 10 grams is quite a bit more than roughly 7 grams of SN.

Nitritespecialist said on Tue, 2 Feb 2021 at 14:59...

Of particular interest is that I'm finding that days 3 and 4 post bottling are the best for effects.

This is with daily testing/opening...and with Kcarb and sieves and at least one pour off at 24 hours.

Jacko said on Fri, 19 Feb 2021 at 22:53...

Hi @Nitritespecialist

I tried out the direct acid addition method on my latest batch of NBN and noted the following differences vs the alcohol+acid addition method I normally use. This was for a 20g SN + 20g NBA + 25g HCl 25% + 16g water batch.

- acid-only seems much more reactive, the brine layer underneath the nitrite goes deep indigo immediately.
- it’s nearly impossible to avoid NO2 formation, the mix fizzes with each addition and some fume evolves.
- the yield seems to be a bit higher, I get the impression the reaction is pushed closer to completion than with the alcohol-acid method. I did leave it stirring a bit longer than usual, though.
- the product seems clearer with direct acid addition. With alcohol-acid, the product looks more opaque or “fattier” initially, but clarifies after washing and neutralising.

Overall, the final product seems to work just as well made by either method on the day it’s made. We both tested it, and it was heady stuff! Will try again in a couple of days to see if there’s any change.

I expect with large/commercial batch production, direct acid is the way to go as smaller additions (relative to total reactor volume) can be made without dropping total reaction pH too rapidly, which seems to drive NO2 formation.

I suspect I am sacrificing some yield using the acid+alcohol method, but I may be able to address this by agitating for a bit longer.

Your comment about no apparent downside to having more water present makes sense, as this will both dilute the acid (reducing aggression of the reaction) and also buffer temperature against rapid exothermic spikes. I have avoided this to date because I’m using more dilute acid to start with.

Cheers,

Jacko