10-01-03 15:48
No 462077
"Red phosphorus, is formed by exposing white phosphorus to sunlight or heating it under pressure to above 275C."
I read this, and i aslo remembered I read that it was the UV radiation in the sunlight that made the reaction go.
Is it possible to us an UV light to speed this reaction up?
Is it at all doable?
-jAmmin
(Hive Bee)
10-01-03 19:08
No 462099
Yea sure, if you have proper licensing and to handle white phosphorous which is a volitile and highly explosive material in the first place. If there is any way for YOU to get your hands and WP then getting RP should be a breeze.
--Word on the street is, You Reap What You Sow
(Stranger)
10-02-03 13:59
No 462264
Heh, point taken...
I read that many pyrotechs use RP as proppelant for their rockets perhaps one could start a pyrotech company to get it?
Anyone have any suggestions? I have used TFSE, but i have found no good suggestions.
The matchbook routine certanly is unusable for medium scale productions...
-jAmmin
(Hive Bee)
10-02-03 14:19
No 462265
Don't worry, the RP from matchbooks isn't all to difficult, I used to think it was useless to scrape 'em too until a fellow bee got a case and asked me to help him. We got a whole case (2500 MB's) it only took us a sleepless night full of geek and pot to get through them. After I was done, however I did have 3 blisters and a finger that stayed numb for a week but it was worth it cause I got some of the finished product. It was a little overgassed but I like to recrystallise anyway. That is what inspired SWIM to do his very own first batch. I wouldn't it even waste my breath trying to get industrial chemicals because there is so much widespread panic over the whole 9/11, anthrax, and weapons of mass destruction deal. I think anyone who claims to be getting lab grade anything either has to own there own business or be in some position of power. "Go" to your local conceited convenience store, they often have extra cases of matchbooks that they print their own lable on, after that it's all pluck, cut, acetone, and scrape.
--Word on the street is, You Reap What You Sow
(Hive Addict)
10-02-03 15:47
No 462273
If you burn a match strike pad in a beaker with a rb flask sitting on top full of cold water the condensate on the bottom of the flask will be white phosphorous. It will reignite over and over again until it is gone or it is submerged in water. Take it out of the water and in seconds it will reignite. Don't try this though because it will produce phosphine which is very poisonous. I did it outside along time ago and it will smoke really bad. I managed to get a little bit of the condensate on my arm and it burn like a mother######.
It wasn't Me!
(Hive Addict)
10-05-03 13:06
No 462708
WP is easily made with a modified arc furnace. The vapors condensed into water, and the WP heated to convert.
NA 1:7
(Stranger)
10-13-03 15:18
No 464398
Lucid_Dreamer: How much RP did you get from the 2500 boxes?
I did about 200 boxes, and got about 3 grams...
However I dont live in the US, and perhaps the RP content is different. But i wonder how i can test if the RP is clean?
I let it stand with HCl for two days, an then filtered it again, it looks like the pictures i've seen, but is there a good way to test it?
As said i dont live in the US, and cooking is something nobody does over here, so i doubt it would be to hard to get labgrade RP and I if you really put you mind to it...
However there is a ephedrine ban here and in the neighboring countries... anyone familiar with an "easy" EP synth, if there is such a thing?
I read the FAQ, but the patents mentioned are to advanced to me (yet
), somebody got a complete writeup?
-jAmmin
(Hive Bee)
10-13-03 19:41
No 464443
I usually get around 20-25 grams per case(2500 MBs). As long as you get all the glue and paper out of the RP it should be fine, the only other thing that should or could be in there is glass, metal, etc, and that stuff is not coming out. Did you use 200 BOXES or 200 MATCHBOOKS? 3 grams out of 200 matchbooks would be very good yeild but if you only got 3 grams from 200 boxes then you should probably PM me or describe your whole RP extraction or something, I have the strong feeling something went horribly wrong.
--Word on the street is, You Reap What You Sow
(Stranger)
10-14-03 10:59
No 464556
Heh, i did 200 matchbooks, and got about 3 grams...
If this is a good yeild, then i guess i should be happy? ;)
-jAmmin
(Hive Bee)
10-14-03 11:04
No 464558
LOL, don't worry pal you'll be scraping whole cases soon enough, If you aren't having problems finding the rest of the precursors here is a good synth for you to work on since you already have 3grams of RP ready.......
http://rhodium.ws/chemistry/meth.curbsho
--Word on the street is, You Reap What You Sow
(Stranger)
10-15-03 12:40
No 464769
Thanks a lot Lucid!
I just have some questions about the synth...
It says i need "small amount of peroxide (common household)"...
I have HydrogenPeroxide, i guess its that he means, but only in a 3% sollution.
Does he mean 100% pure?
I can distill it, but when it says "household", i can never imagine its 100%...
Where SWIM lives its just 3% at the pharmacies.
What kind of sollution should i use?
Also he mentiones "charcoal lighter fluid", what does this contain? I dont live in the US, so the brand names are all different...
Here lighter fluid is named "Rosignol" and it has butan as the "active" ingridient. What chemical does "charcoal lighter fluid" contain?
You've been a great help!
-jAmmin
(Hive Bee)
10-15-03 14:09
No 464781
You don't have to use peroxide, water will work fine
charcoal lighter fluid is non polar it's use in this synthesis is when your done with the rxn you base it and put the non polar in and the freebase meth goes into it when you acidify it makes the meth hcl (soluble in water and not in non-polar (charcoal lighter fluid, xylene,toluene,naptha,camping fuel etc..)
There is a thin line between genius and insane
(Hive Bee)
10-15-03 14:15
No 464782
jammin: lemme save ya a few flames...
Nix the Hydrogen Peroxide and use DH2O.
Nix the charcoal lighter fluid. Use warm Naptha or Xylene.
Consider adding more DH2O and refluxing.
Real Men Don't Preview Their Edits
(Stranger)
10-15-03 14:28
No 464788
I guess im ready for my first nano then!
Sorry for beeing such a New-Bee, but can some one post the reaction scheme?
I'd like to know what im doing before attempting it, so i dont accidentally kill myself....
I've started reading organic chemistry, but im not excatly a professor yet!
I can see we're removing the oxygen, but how?
C10H15NO + I + P + H2O -> C10H15N + ?
Also (dont flame a poor guy, please... simple yes or no will do
) by refluxing, you mean just boil with a condenser so the vapors go back into the liquid to
complete the reaction? I belive i got that correct, but for how long?
How do i know when its enough?
Sorry about the stupid question, but my english isn't that good, and science
terminology isn't even sligthy the same in our languages...
-jAmmin
(Hive Bee)
10-15-03 14:35
No 464790
Stick all that stuff in a test tube or cigar tube, put a ballon over the opening, suspend it in a frying pan with cooking oil, be careful when adding the RP to the iodine, it will create HI that you dont want to lose, so have your balloon ready. But before you do all that, learn how to do an A&B extraction....
Keep in mind this is busy work, the whole synth, it will get you half way prepared for the big one.
--Word on the street is, You Reap What You Sow
(Stranger)
10-15-03 15:05
No 464791
Thanks again for a swift reply.
I already know haw to do an AB extraction, but i wondered about the reflux,
how long shold it be performed. And also if i grasped the consept of refluxing right.
Also i wondered about a reaction formula, or what you call it in english...
So i could understand what was going on in the testtube...
-jAmmin
(Hive Bee)
10-15-03 15:34
No 464792
Don't worry about the RXN formula, the reactants are impure anyway, just reflux it for an hour or so, use the ballon as your condenser.
--Word on the street is, You Reap What You Sow
(Stranger)
10-15-03 15:43
No 464793
Thanks!
I'll proceed now, thanks to all your help!
-jAmmin
(Stoni's sexual toy)
10-15-03 16:35
No 464800
Don't use a fucking ballon, use enough water and reflux it overnight and you might even succeed.
Oh yeah, and UTFSE.
I'm not fat just horizontally disproportionate.
http://www.whatreallyhappened.com
(Hive Bee)
10-15-03 16:38
No 464802
Yea, well I guess he's right, hook up a condenser to friggin test tube!!!
--Word on the street is, You Reap What You Sow
(Hive Bee)
10-22-03 08:42
No 466082
In SWIMS understanding, it's easier to make hypophosphorous acid from WP than RP from WP. Besides, like mentioned above, unless you own your own carbon arc furnace and are reducing phosphorous salts to WP, than why can't you just get RP (as WP is so much harder to get)?
(Stranger)
10-27-03 14:15
No 466992
Hammer: what do you mean... Can i substitue RP for H3PO3?
an in that case how?
I can get labgrade I but not RP yet... :/
-jAmmin
(Stranger)
11-03-03 04:08
No 468426
How much rp do you need? By fabricating a simple carbon arc chamber (a chamber to sheild the arc and direct the phosphorus vapor) and dissolving bone ash in acid and then making a carbon/acid paste to dry into pellets, it is about 3 days work and you wind up with a kilo, 5 kilos, well as much RP as you care to produce and alot cheaper than the going rate of 70 bucks a pint for hypo. In other words, you make a fat brick of RP once, and you are done. The chamber need only be as low tech as a terra cotta flower pot (about a 2 gal size with a short short transfer tube connected to the bottom hole. Whatever is easiest, WP/RP is not rocket science, just an element that requires common sense in handeling just like any other.
uh, you know, stuff.
11-22-03 05:01
(Rated as: UTFSE!)
(Horrible Personality)
11-23-03 17:51
No 472663
is dangerous.
is very poisonous.
a lil´ on your hand will teach you this.
this hurts like not very much things else do, believe me.
But for a fact white phosphorous can be used instead of red phosphorus if done carefully.
But there are much better ways to HI - look for the H3PO4 route or for what I posted on tin lately (stannous and stannic salts....).
(Hive Addict)
11-24-03 08:36
No 472811
A chunk of white phosphorous(immersed in H2O) has been left in the sun for 3-4 weeks now and a fine layer of Rust Red powder has formed on the bottom of the Jar.
Stand by for further comments.
When "THE PEOPLE" start making the laws, I'll start respecting them.
(Horrible Personality)
11-24-03 19:01
No 472887
is some phosphorus you think to be red but still containing significantly amounts of white phosphorus - IMHO better use the white variation as is - it works - with the necessary care taken befor generating a white/red bastard mix which you may think to be red - till you learn the hard way it was enough white left to hurt you badly.
If you have white phosphorus - be EXTREMLY careful - dont fuck around with it in any way but use it. This stuff is not good for nothing except to get used up in a reaction ASAP.
I am not joking.
And I am not from the HIVE-dontdothisathomekids-police as everyone knows.
(Hive Addict)
11-24-03 22:34
No 472930
That white phosphorous can bee really nasty and don't forget it will self-ignite if you take it out of the water for more than a couple minutes if that long.
If you ever wondered why new rp either lg or mb seems to work better in a rxn than used rp its because there is a small amount of wp in the rp. It is listed as an impurity or contaminant. It won't bee present in used rp and therefore rxns don't seem to bee quite as strong as with new. So if that small amount makes such a difference then imagine what wp alone will do. Wish i had some.
It wasn't Me!
(Hive Addict)
11-26-03 02:28
No 473204
Good to see you back.
Who did you piss off to get that handle?
Thanks for the P4 advice. I am aware as to how dodgy this stuff is, and I made sure to speak with one of the big bees before I did anything.
The P4 (a chunk about the sizeof 2 cubes of billiard chalk) was stored under water in a jar and kept in a garden shed for over 2 years and no change was noted in appearance, however, after placing it outside for 3 weeks (no iodine crystal was placed in the jar). The chunk has converted to a layer of rust red material that has settled on the bottom of the jar as fine particle matter. It is going to be agitated with a spatula, under water in order to expose any unreacted material and left exposed to UV for another couiple of weeks.
Further reports to follow in 2 weeks. There is no hint of any white coloring.
When "THE PEOPLE" start making the laws, I'll start respecting them.
(Horrible Personality)
11-26-03 15:10
No 473278
there is no "white" visible any more.
Doesnt say it isnt present.
why dont use "as is"?
for my title:
whom not..... LOL
pssst!! ALL emperors are naked...... LOL
(Hive Addict)
11-27-03 02:39
No 473375
why dont use "as is"?
I am not much of a tweaker. I would rather see bees handle this stuff in it's safer form and as there is not much info here on the conversion of WP to RP, then I will go ahead and do it this way in order to supply info for other bees.
When "THE PEOPLE" start making the laws, I'll start respecting them.
(Hive Bee)
11-27-03 02:42
No 473379
It's also usable to make hypo, but that is more dangerous, it produces phosphine gas I think, it is easy though and most patents suggest an inert gas atmosphere.
--Word on the street is, You Reap What You Sow
(Hive Addict)
11-27-03 04:36
No 473395
(Rated as: good read)
This report describes the chemical behaviour of red phosphorus in water and compares it to
the reactions of white phosphorus. Whereas white phosphorus consists of P4 molecules, spontaneously ignites near room temperature and is highly toxic, red phosphorus is an allo-tropic modification of elemental phosphorus which is mostly an amorphous polymer so that the physico-chemical properties of red phosphorus are very different from white phosphorus.
Red phosphorus ignites only above 260 °C, is of very low toxicity and moderate reactivity.
Even white phosphorus has a very low solubility in water of about 3 mg/L. Due to its polymeric nature, red phosphorus is practically insoluble in water. However, since elemental
phosphorus is thermodynamically unstable in the presence of water and oxygen, red phosphorus will very slowly react via intermediates such as hypophosphorous acid (H3 PO2 ),
phosphorous acid (H3 PO3 ), and phosphine (PH3 ) to phosphoric acid (H3 PO4 ). These reaction products dissolve in water and contribute to a concentration of total phosphorus compounds (calculated as phosphorus) of 1 mg/L after 24 hours starting from 100 mg/L. Even after 4 months and starting from 10 000 mg/L the concentration of phosphorus compounds reaches only 270 mg/L corresponding to a conversion rate of the red phosphorus of only 2.7 %. Since these disproportionating and hyrolysis reactions
proceed at a very slow rate, even critical products like phosphine (not readily soluble in wa-ter) will be finally converted to phosphoric acid in oxygen containing environments.
Experiments indicate that the traces of white phosphorus (< 200 mg/kg) present as a contaminant in red phosphorus cannot be readily extracted by water. As a consequence, the
new and so far unpublished experimental data in this report indicate that the content of white phosphorus in red phosphorus should not be used as a sole reference for extrapolating the toxic effects of red phosphorus to aquatic organisms.
Red Phosphorus is produced by thermal conversion of white phosphorus. The obtained red phosphorus still contains up to about 100 mg/kg of white phosphorus. The upper limit given in the product data sheets is 200 mg/kg white phosphorus. Red phosphorus is a red powder which can be handled easily compared to the safety precautions necessary when handling white phosphorus. Main applications are matches, aluminium phosphide and flame retardants.
The major distributor for red phosphorus for matches is located in Europe. Europe is also the principal market for red phosphorus due to the production of aluminium phosphide and the use as flame retardant in plastics. In Europe red phosphorus plays an important role as a flame retardant for plastics, especially for polyamides in electronics, polyurethanes and latex. Despite of its red colour it is used because in some cases it is the only material which meets the high safety requirements for the end products combined with the high technical requirements. In polyamides for electrical and electronic applications it is preferred because of its high stability which enables the use of such plastic materials up to high voltages.
Red phosphorus: short process description
Red phosphorus is one of the allotropic forms of elemental phosphorus. It is largely amorphous and is considered a polymeric version of white phosphorus. Commercial red phosphorus is normally produced by heating the white phosphorus at a temperature range of 250 –350 °C for 40 – 50 hours in a closed furnace (exclusion of oxygen) and at ambient pressure.
After the polymerisation, the product is milled in presence of water then treated with an alkaline solution in order to remove traces of white phosphorus and finally filtered, washed and dried. Although this special treatment is applied for removing white phosphorus in the production process, some mg/kg of white phosphorus still remain in the final product.
Specifications of commercial red phosphorus are presented in annex 1. The specifications state that the level of white phosphorus is < 200 mg/kg, but the present technology is able to reduce the white phosphorus content to < 100 mg/kg.
It wasn't Me!
(Hive Addict)
01-02-04 01:45
No 480153
Post 472811 (abolt: "P4 and Sunlight", Stimulants)
What looked like a "layer of dust" was in fact a hard plate of (mostly red) P4.
This "plate" was turned over (whilst still immersed) and was found to have white speckles still through it.
P4 will be treated to sunlight for a while longer until conversion is deemed finished.
http://www.afsc.org/iraq/relief/default.
(Hive Addict)
01-02-04 09:13
No 480192
Red phosphorous will contain white phosphorous. Apparently it is very difficult if not impossible to remove all of it. It is listed as a contaminant in the documentation.
So you might bee waiting quite a while if your expecting a full conversion.
It wasn't Me!
(Wizard Master)
01-03-04 03:55
No 480222
Carbon Disulphide, CS2, will disslove WP; leaving RP. Only trace amounts of RP is soluble in Carbon Disulphide. Some literature saids RP is insoluble in Carbon Disulphide.
(Hive Addict)
01-03-04 08:12
No 480231
(Rated as: good read)
Content of white phosphorus in red phosphorus
Even with state of the art technology it cannot be prevented that red phosphorus contains
traces of white phosphorus. This amount of white phosphorus is determined by extraction
with carbondisulfide and subsequent measuring by phosphorus-NMR spectroscopy in com-parison
with a standard sample of white phosphorus in toluene. The average content of
white phosphorus in commercial red phosphorus is normally about 50 – 100 mg/kg, even if
the upper limit given in the specifications is 200 mg/kg.
| white phosphorus | red phosphorus | |||
| CAS-number | 12185-10-3 | 7723-14-0 | ||
| structure | contains discrete P4 molecules | highly polymeric Pn | ||
| appearance | crystalline, waxy, translucent | amorphous or crystalline, | opaque | |
| melting point | 44 °C | 585 – 610 °C | ||
| vapour pressure | high | very low | ||
| density | 1.83 g/cc | 2.0 ... 2.4 g/cc | ||
| solubility: | ||||
| in organic solvents: | yes | no | ||
| in water: | only ~3 mg / L | no (very slow hydrolysis) | ||
| toxicity | highly toxic | very low toxicity | ||
| heat of sublimation | 13.4 k cal/mol | 30.0 k cal/mol | ||
| chemiluminescence | yes | no | ||
| ignitability | spontaneous ignition in air at | - ignites only above 260°C | ||
| room temperature | heat necessary for ignition in | |||
| spontaneously ignites in chlorine | chlorine | |||
| smell | characteristic | no smell | ||
| reaction with aqueous | produces phosphine | none | ||
| alkali |
It wasn't Me!
(Hive Bee)
01-03-04 17:11
No 480248
adolt perhaps you could react it to something useful other than RP, easily?
Make a vile of the WP/RP for a souveneire?
Maybee you could try adding only enough WP solvent for a supersaturated solution, with WP then still being exposed to the UV rays and precipitating to the aqueous phase as it converts to RP?
It sounds almost unbelievable that traces of WP can't be removed. maybee they mean that it isn't purified by the industrial process only?
(Hive Addict)
01-03-04 22:35
No 480294
Red phosphorus: short process description
Red phosphorus is one of the allotropic forms of elemental phosphorus. It is largely amorphous and is considered a polymeric version of white phosphorus.
Commercial red phosphorus is normally produced by heating the white phosphorus at a temperature range of 250–350 °C for 40–50 hours in a closed furnace (exclusion of oxygen) and at ambient pressure.
After the polymerisation, the product is milled in presence of water then treated with an alkaline solution in order to remove traces of white phosphorus and finally filtered, washed and dried.
Although this special treatment is applied for removing white phosphorus in the production process, some mg/kg of white phosphorus still remain in the final product.
Specifications of commercial red phosphorus are presented in annex 1. The specifications state that the level of white phosphorus is < 200 mg/kg, but the present technology is able to reduce the white phosphorus content to < 100 mg/kg.
The term red phosphorus is used for describing a variety of different amorphous forms of the elemental phosphorus showing a range of colours from the orange to dark-violet. Such differences in colour can be explained by differences in:
• particle size of the powder,
• molecular weight,
• impurities normally present on the red phosphorus surface
Although the red phosphorus is largely amorphous, X-ray diffraction, optical microscopy and differential thermal analysis (DTA) have established the existence of several crystalline red varieties of pure elemental P in addition to the amorphous form. Normally the commercial red phosphorus is amorphous and the crystalline form is present only to a limited extent (< 10 % w) which is due to the ordered framework of different degrees of polymerisation.
Red phosphorus has been described as a complex three-dimensional polymer in which each P atom has a pyramidal arrangement of three bonds linking it to neighbouring P atoms.
It seems likely that all forms of red phosphorus are built from the pyramidal white phosphorus structure and that the polymer growth is terminated by the occluded impurities
such as halogen, oxygen or hydroxyl groups.
In conclusion, the amorphous red phosphorus probably consists of entirely random networks of P atoms terminated by oxygen or hydroxyl groups. This assumption is confirmed by NMR spectra of the solid red phosphorus material. Due to the fact that red phosphorus is a polymer, it is not a surprise that physico-chemical characteristics, the reactivity and the stability are far different from white phosphorus: the white phosphorus is crystalline, contains discrete P4 molecules, has a melting point of about 44°C, is very soluble in organic solvents like CS2 and benzene, is very unstable and spontaneously ignites in presence of air. Whereas white phosphorus is a very toxic product, the red phosphorus is not toxic (LD 50 oral rat is > 2000mg/kg) as expected on the basis of the polymeric structure.
Red phosphorus shows a totally different chemical behaviour than white phosphorus. Red phosphorus is a polymeric allotropic modification of phosphorus. White phosphorus consists of reactive P4 – tetrahedra (molecular weight: 124 g/mol) whereas red phosphorus has a polymeric structure of Pn . Consequently, the reactivity of red phosphorus is much lower than of white phosphorus. Yellow phosphorus has to be handled under water otherwise it will start to burn spontaneously. White phosphorus has a wax like appearance whereas red phosphorus is a red to violet coloured powder which can be handled in air. The vapour pressure of white phosphorus at 25 °C is 0.05 mbar whereas red phosphorus has no detectable vapour pressure at this temperature.
Due to these differences the reaction velocity of red phosphorus with water is much slower compared to white phosphorus, but the main reaction products are also phosphorus-containing acids. If the total amount of white phosphorus contained in commercial red phosphorus (upper limit 200 mg/kg) were to dissolve in water, the following
concentrations given in Table 2 would be achieved. One has to bear in mind that white phosphorus also reacts with water so that these calculated amounts of white phosphorus
can only be achieved theoretically. Laboratory experiments revealed that the yellow phosphorus contained in red phosphorus is not readily extractable with water.
If traces of white phosphorus are released from the red phosphorus, they probably quickly react to phosphorus containing acids – the same products that the red phosphorus itself liberates. The source of these phosphorus containing acids be it white or red phosphorus cannot be distinguished by chemical analysis, because the products themselves are identical and red phosphorus as a starting material is present in immense excess.
The concentration of obtained hydrolysis products from red phosphorus steadily increases with the amount of dispersed red phosphorus in water. However, the reaction of red phosphorus with water is extremely slow. The average amount of reaction products from 100 mg/L after 24 h calculated as phosphorus is about 0.7 %. This fraction rises very slowly up to a maximum of 3.7% of the nominal concentration of solid red phosphorus in water after 700 hours. In another experiment the soluble reaction compounds increased only up to 2.7% after 2 880 hours (4 months). These data show that red phosphorus does not dissolve as such in water which renders the concept of a maximum solubility unapplicable. Instead, a continuous but slow series of reaction occurs leading to phosphorus containing acids. The amount of products formed increases with the available amount of red phosphorus and time.
It wasn't Me!
(Newbee)
02-27-04 16:06
No 491421
----------------------------------------
jammin: lemme save ya a few flames...
Nix the Hydrogen Peroxide and use DH2O.
Nix the charcoal lighter fluid. Use warm Naptha or Xylene.
Consider adding more DH2O and refluxing.
----------------------------------------
ok peroxied nixed, dh20 used.
can i use toulene istead of naphta, xylene?
i got a OTC solvent that states 30-60% xylene, but my thermometer can go further than 120c. And if i recall right xylene boils @ 140 or so. So i cant distillit properly.
But i recon i can distill the toulene since it has a lower BP....
-jAmmin