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How to find out whether your yellow unpurified PA substance is pure
Fire test: Purified (<80%) PA burns, unpurified PA (>60%) does not! I would imagine it would burn faster and more consistent the purer it is. I tried the fire test on all my batches of un-purified PA substance and none ignited, not even my best batch, even though I heated it until completely dry in the oven. I would therefore assume that you need a certain % of pureness for the substance to ignite - perhaps 50-60%+
Eye sight: I found this out myself by observation of substance and comparing to the yield achieved by the purification process. The more pure your PA substance is the more it will "sparkle". It is the pure PA crystals that make it sparkle. Needless to say; the more crystals, the more sparkles. Usually, an optimal produced batch of unpurified PA substance is pale yellow that "sparkles". It's worth noting though that one of my pale yellow batches had a very low yield so color isn't everything and 100g of pale yellow PA substance can in fact prove to yield less than 20% of pure PA crystals.
IMPORTANT: DO NOT assume that your unpurified PA substance is suitable as a high explosive booster! On my test blast I used 3g DDNP with 50g unpurified PA substance as a booster. At this point in time I believed it was potent but wanted to test for sure. Needless to say, the completely dry impure PA substance did not detonate and was just spread all over after the blast. I later (when I purified the rest of the same batch) found out the yield in that batch was a lousy 10%, so no wonder it didn't detonate.
Time required: 3-4 days for 1,5kg of unpurified PA substance.
Purification of the yellow unpurified PA substance is required as you need to be sure that the substance is potent. You will need approximately 40-50 liter of distilled water to purify 1kg of unpurified PA substance. You also need a 2L beaker for boiling/mixing and 20-40 other glass containers for chilling the liquid after the boiling/mixing. The chilling process will take up to 1-2 days so unless you have enough time, you should get A LOT of glass containers, to do everything in 1-2 batches.
Boil up 1,3 L of distilled water (70-80C) in a 2 L beaker. You don't need a hotplate-magnetic stirrer for this as a limited amount of stirring is needed. In fact a regular plate would go considerably faster since it heats up faster.
Start to dump in the unpurified yellow PA powder (powdered or clumps - around 50 g, exact weight isn't important). If the amount doesn't saturate the liquid you can put more in, until it is no longer soluble and bits of PA floats around. Just ensure everything dissolved before you go to the next step. Have a container of 500 ml additional water nearby and add it once you need to dissolve the insoluble PA. You can regulate the temperature somewhat with adding additional water to ensure the temp doesn't exceed 80C. I don't know for sure whether temps exceeding 80C will deteriorate the PA but I read from another source to keep temp between 70-80C so no harm following that advice. It said another place to remove the brown oil droplets. I tried this in the beginning with a plastic spoon but noticed that it impacted the yield of pure PA as I also removed some pure PA floating around with the droplets. I only noticed the brown droplets in my first batch which was very poorly made, but not in the other batches. There will hardly be any so just ignore this altogether.
1 L of liquid is saturated with 15 g of pure PA so this fact allows you to measure the yield of your yellow PA powder and the number of grams you can expect to purify. 50g of yellow PA powder in my case yielded from 10-50% of pure PA crystals. My poorest yield was my first batch. 300 g of PA powder was almost inert and yielded only 30 g of pure PA crystals. The other batches of PA powder was a better yield ranging from 15-50%.
When the liquid is saturated (you should have 1,8L of PA liquid), filter hot into glass containers. Filtering hot is not very important unless your PA powder is very unclean, like my batches (it was everything from bugs to other small impurities like pieces of plastic). I filtered 1,8 L into 4 x 500 ml beakers but since I only had 10 of these beakers I eventually started using all types of glassware. Since the crystals (when cooling slowly) "grow" slowly like bacteria I assumed using items which they use to boost bacteria growth would work in these cases as well. I experimented with various glass containers, different shapes and sizes. I used flat, long (long drink glasses), small, with everything from glass rods and plastic sucking straws in.
My findings were not 100% conclusive, in fact I'm still very uncertain, but I got the impression that certain shapes and sizes will allow for a greater yield. Smaller containers seemed better than large containers and adding plastic sucking straws so the crystals got more "surfaces" to grow from was a slight bonus. Beakers larger than 600ml yielded a lower result. I ended up buying 18 long drink glasses (each 300ml) which yielded an ok result. I was surprised to learn that the best yield was from a large circular glass bowl (5 liters) which I placed 1 liter of liquid in. It was an unclean bowl I had previously used to store my bananas in (in a plastic bag). In any case; the yield of pure PA crystals was 100-200% better than in other containers. I do not exactly know why; perhaps it was the dust particles in the bowl or possibly bacteria that promoted the increased growth. In any case; it indicates that the described purification method is flawed and the issue is worth investigating further. For obvious reasons, I don't have time for more research into this issue. Also keep in mind that larger glass containers uses considerably longer to cool (several extra hours).
Cool the two 600 ml beakers to room temp. For a 500 ml beaker this took 4,5 hours and a few hours extra for the 2L beakers. I notices, however, that when I let the beakers sit overnight (for a total of 12 hours) there was considerably more PA crystals generated. However, I do not know for sure if this will impact the total of crystals generated after you have further cooled it down in the fridge.
When the beakers and other glassware you might have used are at room temp (don't hesitate to let it stand for several extra hours, perhaps up to a day or two, after it has hit room temp) - then, put the beakers in the fridge. It said in another guide that I was to put it in the fridge for one hour but I'm pretty sure he meant that I chill the liquid down to 4C. Considering that I was purifying 1kg of unpurified PA powder and I had A LOT of beakers and other glass containers, it took 12 hours in the fridge for the beakers to reach 4C (since the room temped containers raised the refrigerator temperature from 4C to 12C within the first hour...:-) So, if you have a small fridge, like I did, consider chilling the containers in a "transit location", if possible, in order to shorten the "fridge time". I used the cellar floor which holds 8C. This saved me a total of 36 hours of "fridge time".
Filter once the liquid hits 4-5C (perhaps we can even increase generation rate if we let stand even longer. I am really not sure about this but it is worth investigating further.
The other guide said: scoop the crystals out of the filter. However, I like to save the crystals in the filter until I have a large enough batch to process as it maintains the moisture well and keeps it cool. I also like to process the filter papers all at once by using a 2m x 1m plastic board. I open the "seam" on the coffee filter papers and flatten it out like a pancake. Then I use a plastic/rubber spoon like object (the item used to smear cream on cakes) to get all of the content out.
When you have taken out all the crystals from the filters, put them in a plastic box and keep them with at least 20% water content (no problem if you take them out of the moist filters - newly moist filters = aprox 100% water content).
These should be used within 2-3 weeks or they may start to deteriorate and/or may increase sensitivity and thus become more dangerous to transport (according to another guide). If you store them saturated with alcohol in a sealed glass container, you can basically store them safely for 100 years +.put in oven for an hour.
Drying before use
Dry in oven for 30 mins to 4 hours based on water content between 50-80C before use. I dried the unpurified PA substance in the oven (no problem) but haven't yet confirmed with pure PA crystals. It should be safe because I dried DDNP in the oven the same way, which should be considerably more sensitive.
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