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International Hazard
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I know, im such a chicken shit its not even funny.
I wanted to run it today but I started to have concerns that if there is to much air in the vessle I could risk fire even though I doubt it would
really be a major problem. Then I have fear of Phosphine generations on top of concerns about the vessle being able to hold up under the reaction
conditions because if it failed while full of Phosphorus vapors it would be bad. The one that was run using a stoked fire and covered with sand does
not have the same issues I have here because if the container fails in the fire its one thing where as if it fails in my case its going to drop molten
reactants everywhere while releasing White Phosphorus...
All in all I have decided that when I do run it I am going to cover the entire vessle in sand, which would aid in heating anyway, so that if things go
wrong atlest there is a little something to contain the reactants. I would then heat it as slowly as possible so that I don't get everything to hot to
quick incase things start to go wrong I could turn off the power and it would cool to a safe temperature quicker.
Now I really feel all thats left to do is grow big enough stones to set it up nice and stable and plug it in. Im afraid its going to be just like
Ketene where im sure I could pull it off, and I really really want to but lack the guts to start it in the first place. I always try to lean on the
side of caution which I guess is a good thing but sometimes there comes a point where you just have to go for it. I find myself all to often not
hitting that point even if I want to more then anything.
Knowledge is useless to useless people...
"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the
fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story
before."~Maynard James Keenan
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Melgar
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The air in the vessel will oxidize the carbon first, which just makes CO2 bubble out of the tube, and slowly at that. I wonder how hot you could get
it with a makeshift furnace fueled by bbq charcoal?
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Thing is there won't be any carbon around. The reaction im speaking of is Metaphosphate, Aluminum(or magnesium), and Silica. Details are laid forth on
the first page of this thread by polverone and many simple experiments have showed me Phosphorus vapors bursting out of the melt and igniting as well
as being able to trap a very small amount in order to watch it glow. I know it can be formed and it does so at a reasonable temperature of 550 degrees
C as stated in Polverones reference. I have not checked the exact temperature at which it starts producing Phosphous however but I can tell that it is
in no way the high temperatures normally associated with Phosphorus production. A dull red glow as noted a few post ago in this thread is all thats
really needed. I got to thinking that it might just be possible to do all this on top of a stove to be honest. Not something I would want to attempt
but I think they heat might just be high enough to get it going.
Even though this reaction does not call for carbon it may be a good idea to add a layer of it on top of the reactants just for the exclusion of air
from the mix. I cant see how it could really hurt at all by having it there so perhaps that would be a good way to go. I have seen Phosphorus forming
in the past by melting the metaphosphate and adding a little carbon so indeed all it would do is add some extra reducing agent to the mix while at the
same time scavenging avalible oxygen.
Knowledge is useless to useless people...
"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the
fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story
before."~Maynard James Keenan
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captaindrum
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Hi guys! I've been visiting this forum for a long time. I've read every single post of this topic and since I have some experience to share, thought
that it is time to register and contribute! Here goes my first post:
I ordered a kg of sodium hexametaphosphate for about $10. Nearly everything else was in my posession, so I had some really cheap experiments.
In both of my attempts, I used Na-HMP, powdered charcoal and SiO2 sand from a water-purifier (stochiometric amounts, about a total of 100 grams). I
found the purifier in the basement. Cleaned it up and bam! There was silica sand (about 1mm pellets), activated charchoal and here we have a reaction
vessel (as seen in the picture).
The heating took place in two different barbecue sets, respectively. First attempt included some stronger heating and better insulation, and the
reaction vessel was a column of the purifier. In the condenser, a lot of bubbles immediately formed which i believe was the expanding air. After about
half an hour, a colorful smoke came out from the condenser, and some whitish solids started to form.
Maybe because of the cooling of the condenser with a LOT of ice, the solids floated on the surface ( as seen in the picture). After the reaction(?)
was complete, I took some pictures and heated the water of the condenser. It melted at around 50C and after cooling the solids tend to sink.
The second vessel was a paint solvent can which had its cap drilled and had a tube of the purifier fit with a proper nut. A lot of effort was put on
in order to make the apparatus gastight; a roll of teflon tape used. I still haven't investigated the residue since I couldn't find the proper time
and space, but the second one did not have any smoke or a disturbing odor like the first one.
PS: Both of the heating procedures were performed with charcoal (several kgs of it in the first experiment). Both of the experiments took place in the
open air and safety measures had well been aware of.
PPS: I doubt the solids may also consist of paraffin as well, but I'm not sure of either...
Take care people,
Respect,
cpt. drum
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blogfast25
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Hi and welcome!
Glad to see someone else wanted to have a stab at this, this time trying to walk in the footsteps of the Bringer of Phosphorus, Hennig Brand,
himself… 
Can you provide some more info on your heating method?
Have you tested your goo? Is it phosphorus? Take a small blow torch to it and see if it burn brightly with white P2O5 smoke?
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captaindrum
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I was out of town for a convention/seminar, sorry for responding this late..
I heated the stuff, even tried burning it but it had so little difference than plain wax if any. I distilled wax guys. Sorry  (
In my previous post, there is a barbecue grill in the first picture. I used a deeper one for the heating. Used some sheet metal to cover the top for
insulation; and the thingie also had a good venting/exhaust system itself.. I could easily see a bright red color with a few pounds of charcoal. Spent
4 kgs for the experiments in total..
Thanks blogfast, your hospitality made me feel that I am in the right place; here in this site )
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blogfast25
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Ah well, if at first you don't succeed...
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The WiZard is In
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...disembarrassed of the charcoal...
I was hunting down refs on arsenic in wall paper and
hapend upon this.
Improved method of extracting- Phosphorus from Bones.—Le
Genie Industrial describes a process recently patented by II. Cari
Mantrand, of Paris, for extracting phosphorus from bones more
economically than by the processes heretofore employed. The
calcined bones, reduced to a fine powder, are mingled with a
sufficient quantity of pulverized charcoal to combine, as carbonic
oxide, with all the oxygen of the phosphate. The mixture is placed
in an earthenware cylinder varnished on the inside, filling the
cylinder to three-fourths of its capacity. The cylinder is then heated
red hot, and a current of hydrochloric acid gas is blown into it. The
phosphate of lime is immediately decomposed, forming chloride of
calcium and carbonic oxide, while the liberated phosphorus is
evaporated and driven through a copper tube, which leads into a
vessel of cold water, where the phosphorus is condensed. The
chloride of calcium, disembarrassed of the charcoal, in contact with
sulphuric acid, regenerates hydrochloric acid for a new operation.
The labour of pulverizing the bones may be saved by digesting
them with a solution of hydrochloric acid; using for this purpose the
water of the condenser from the preceding operation.
The Chemical news and journal of industrial science, Volumes 3-4
May 4 1861
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blogfast25
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Very... erm... disembarrasing, indeed!
Jokes aside, it shows considerable chemical ingenuity for its time...
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ScienceSquirrel
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Quote: Originally posted by The WiZard is In  | I was hunting down refs on arsenic in wall paper and
hapend upon this.
Improved method of extracting- Phosphorus from Bones.—Le
Genie Industrial describes a process recently patented by II. Cari
Mantrand, of Paris, for extracting phosphorus from bones more
economically than by the processes heretofore employed. The
calcined bones, reduced to a fine powder, are mingled with a
sufficient quantity of pulverized charcoal to combine, as carbonic
oxide, with all the oxygen of the phosphate. The mixture is placed
in an earthenware cylinder varnished on the inside, filling the
cylinder to three-fourths of its capacity. The cylinder is then heated
red hot, and a current of hydrochloric acid gas is blown into it. The
phosphate of lime is immediately decomposed, forming chloride of
calcium and carbonic oxide, while the liberated phosphorus is
evaporated and driven through a copper tube, which leads into a
vessel of cold water, where the phosphorus is condensed. The
chloride of calcium, disembarrassed of the charcoal, in contact with
sulphuric acid, regenerates hydrochloric acid for a new operation.
The labour of pulverizing the bones may be saved by digesting
them with a solution of hydrochloric acid; using for this purpose the
water of the condenser from the preceding operation.
The Chemical news and journal of industrial science, Volumes 3-4
May 4 1861
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I assume that you have tried this out and it works?
The process is only 150 years old.
An author claim to distill spiritus sanctus de la sange de l' agneau from donkey shit and you would publish it as truth. 
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The WiZard is In
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| Quote: Originally posted by ScienceSquirrel | | Quote: Originally posted by The WiZard is In | I was hunting down refs on arsenic in wall paper and
hapend upon this.
Improved method of extracting- Phosphorus from Bones.
The Chemical news and journal of industrial science, Volumes 3-4
May 4 1861
|
I assume that you have tried this out and it works?
The process is only 150 years old.
An author claim to distill spiritus sanctus de la sange de l' agneau from donkey shit and you would publish it as truth. |
If you want posts Kitchen tested you could do us the favor
and run this experiment through your lab.
Take your time and do a good job.
Cæsium.
AT the last meeting of the Chemical Society, Dr. Roscoe gave a
short account of Professors Kirchhoft and Bunsen's spectrum
researches, and mentioned that the new alkali metal which they
had discovered by that means had been named Cæsium, from the
Latin word casius, signifying grayish-blue, that being the tint of
the two spectral lines which it shows. By working with the residues
from twenty tons of the mineral waters of Kreuznach, Professor
Bunsen had succeeded in obtaining about 250 grains of the
platinum salt of the new metal. Cæsium is closely allied to
potassium in its chemical characters, the chief point of difference
being the solubility of its nitrate in alcohol. Its equivalent number is
117,—exactly three times that of potassium.
The New Alkaline Metal, Cæsium.
BUNSEN has discovered in the waters of several mineral springs, a
new alkaline metal, the existence of which was first detected by
the spectral method of qualitative analysis. The new alkali exists in
these waters, together with potassium, sodium, and lithium, and
its presence may be shown by the spectral analysis with the
greatest facility, although only a few milligrammes are contained in
several kilogrammes of the material. The author gives only a very
brief preliminary notice of the new metal, promising a more
extended investigation. The chloride may be distinguished from the
chlorides of sodium and lithium by the yellow precipitate which it
gives with chloride of platinum. It is distinguished from potassium
by the solubility of its nitrate in alcohol. The vapours of the
compounds of this metal, when heated so as to become luminous
, give an extremely characteristic spectrum, which at the same
time exhibits the remarkable simplicity of the spectra of the other
alkaline metals. Its spectrum consists of only two blue lines—a
weaker line, corresponding with the blue strontium line, and
another which lies only a little farther toward the blue end of the
spectrum, and which vies in intensity and sharpness of definition
with the red line of lithium.—Journal fur prakt. Chemie.
The Chemical News and Journal of Physical Science (With which is
incorporated the “Chemical Gazette”)
A Journal of Practical Chemistry In all its applications to Pharmacy,
Arts, and Manufactures.
Edited by William Crookes, F.C.S.
London 1861
djh
----
Good thing Herr. Bunsen invented his burner/clamp or
his name would have been lost to history.
Reminds me of — The Battle of Balaclava which most remember
only for 3 reasons.
A poem.
A quote of General Pierre Bosquet —
C'est magnifique, mais ce n'est pas la guerre.
And (sorry if I offend as it is not PC to mention this) a woman
who spent 20-years in bed.
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jgourlay
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All, I have wanted to contribute to this thread since it's inception. But, being as I'm more of a vinegar and baking soda volcano kind of chemist,
I've had nothing. But now I have something tiny to contribute.
At Lowes, in the paint section, I ran across "DAP TSP". MSDS says it's 30-60% Phosphate, tribasic and 10-30% Sodium Carbonate (so what's the rest, I
wonder?).
Point is...it's a source of TSP readily available. And, at $10 for 4lbs, it's cheap and you don't have to pay shipping.
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symboom
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| Quote: Originally posted by jgourlay | All, I have wanted to contribute to this thread since it's inception. But, being as I'm more of a vinegar and baking soda volcano kind of chemist,
I've had nothing. But now I have something tiny to contribute.
At Lowes, in the paint section, I ran across "DAP TSP". MSDS says it's 30-60% Phosphate, tribasic and 10-30% Sodium Carbonate (so what's the rest, I
wonder?).
Point is...it's a source of TSP readily available. And, at $10 for 4lbs, it's cheap and you don't have to pay shipping. |
ah neat another source of phosphorous by far one of the interesting source of element phosphorus i made was from bones from this great baby back rib i
had well did not want to be wasteful so i just used the bones to make phosphorous. First tried crushing it up with a sledge hammer found out i have to
heat it i guess the heat helps break it down ad it was a lot easier to crush. luckily i was sunny charcoalized some wood with my big ass Fresnel lens
then crush that up mix it with the bones put it in my reaction vessel (used up non refillable oxygen tank) drilled out cylinder put on some elbow pipe
that lead into water then point that lens and heat the crap out of it was more worrying about melting the container
because it started to glow red hot so i had to move back the focal point. Anyways that's my experience on that defendantly more involved than making
sodium from electrolyzing molten sodium hydroxide
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pip
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Is there a reason everyone still wants to try the "furnace" method over the "beaker" method? I have LiAlH4 and carbitol but can't find the
triphenylphosphine only triphenylphosphate.
Has anyone actually performed this synthesis as I am guessing no due to its lack of documentation here but if so was your triphenyphosphine purchased
or made?
edit: as soon as I say somthing I find it on ebay. I swear it wasnt there last time I checked.
[Edited on 18-5-2011 by pip]
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Rogeryermaw
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| Quote: Originally posted by pip | Is there a reason everyone still wants to try the "furnace" method over the "beaker" method? I have LiAlH4 and carbitol but can't find the
triphenylphosphine only triphenylphosphate.
Has anyone actually performed this synthesis as I am guessing no due to its lack of documentation here but if so was your triphenyphosphine purchased
or made?
edit: as soon as I say somthing I find it on ebay. I swear it wasnt there last time I checked.
[Edited on 18-5-2011 by pip] |
my guess would be that not everyone but many, still like the furnace idea because 1. there is much documentation about it here, 2. it is proven to
work, and 3. the reactants are super cheap, easy to source and, in their non-reacted form, they are pretty harmless.
also the videos of the process on my you boob page pretty much answer all the questions about how to carry the process out in detail. those with
ingenuity know that the furnace i use is a lot more than is really necessary for the task. a small desktop job made of refractory and powered by
propane and an airbed inflating pump can do the same job if you use a retort similar to the first one i had success with. it was constructed of E.M.T.
1" pipe about a foot long, hammered flat at one end and welded shut. to the other end weld a rigid steel nipple and then screw on a reducing 90 degree
fitting and from that a 4"-6" half inch nipple submerged in water about one half to three quarter inch.
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pip
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Cool, hopefully I get around to doing "the other way" and we'll have pics of both.
edit: turns out I have the phosphine but need the phosphate, thoughf it was the other way around but I checked and its the phosphate.
[Edited on 19-5-2011 by pip]
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Rogeryermaw
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anyone heard of this yet?
http://www.omicron.de/en/products/deco-/instrument-concept
looks and sounds quite interesting but where to get gallium phosphide...(GaP)
i wonder if this technology, or at least the concept may be adapted for use on a home scale?
[Edited on 22-5-2011 by Rogeryermaw]
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peach
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That's a Knudsen cell type furnace used for spraying molecular beams of dopant at semiconductors in ultra high vacuum chambers.
Definitely works but, as they're working at the 99.9999%+ purity end of the spectrum, the price will make your eyes water .
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ngoclan4ever
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Hello,
My first post:
Based on the article "Method for Preparation of Small Amounts of P4", I mixed: 35g NaPO3 + 15g Al + 10g SiO2 to get 60g mix.
After 3 runs of 20g each, I am now a proud owner some P.
However, They are not at the same color. Each one weight in at a whooping 0.2g (yes, 200 milligram). The article use 3g to obtain 0.5 g of P.
Why are they different in colors and why are the yields are terrible low?
Any thoughts?
Have a super day everyone.
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Strepta2
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@ngoclan4ever: describe your source materials and methodology in more detail. Did you use pyrotechnic Al? How well did you incorporate the
chemicals--ie, How fine were the chemicals prior to mixing? How did you mix them together? did you use a blender or coffee grinder? Did the resultant
mix ignite and self-sustain after heating? Did you use a glass tube as the reaction vessel? If so did you see the phosphorus migrate to the cooler
section of the tube.
I never ran a batch as large as you're describing, but I always obained yields in the 40-50% range.
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ngoclan4ever
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@Strepta2: Thank you very much for your comments. Your yields are what I'm trying to achieved.
For the source materials, I'm not sure about the Al since I brought it long time ago. It looks gray and is 35 µ, 425 mesh. The SiO2 is 200 mesh.
The NaPO3 is coarse so I use a blender to chop it into a fine powder. I then dried the 3 ingredents by baking them, sepereately, in a 275 degree F
oven for a few hours. I then mixed them together using same blender.
The mix then put into a 1" by 8" glass test tube, filled with CO2. When apply the heat using propane torch, I can see the resultant mix ignite to a
big red blob and self-sustant after heading. The phosphorus are condensing at the cooler section of the test tube (I wrapped the end of the tube with
2" paper towel with a tail and pump ice cold water to it. The tail drips the water back to the pump reservor).
Not sure which ingredient is the source of the problem. And, my materials are not lab grade. Do you think I should try to get the pyrotechnic Al? or
try with a smaller batch?
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Strepta2
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I would suggest the following: grind the SiO2 and the NaPO3 to be as fine as the Al. When thoroughly incorporated (intimately mixed), the resulting
mix should act much like a liquid—If you have a tt about 1/3 full and sharply rap it on a table top it should spurt up like a liquid.
I heated the tt in a horizontal (nearly level) position, with the charge spread along about one-third of the tt nearest the closed end and leaving at
least half of the volume of the tube above the charge free for expansion of the residue of combustion. I heated the mix along its length but more
intensely near the open end of the tube which caused ignition to begin there and progress toward the closed end. I continued heating the area of the
combustion after it ignited to ensure the any free P4 would be likely to migrate away from the reaction site. How long did you maintain heating the
tube after the reaction appeared complete? Also, you state you filled the tt with CO2—was this a continuous flow? You must have provided an exit
path as the internal pressure rises on ignition. Can you provide a photo or diagram of your tt and how you fixtured the protective atmosphere?
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ScienceHideout
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I know this is a bit off topic, but are there any methods using TSP?
hey, if you are reading this, I can't U2U, but you are always welcome to send me an email!
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ngoclan4ever
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@Strepta2: My set up consists of a tt with 2 holes stopper fitted with 2 tubes. The end of the first tube connected to a CO2 generator. The CO2
generator is a 16 oz bottle filled with some baking soda and has a side tube for the vinegar to drip-in. The end of the second tube immersed
partially in a flask filled with water to capture anything which may escape from the tt.
The CO2 is not a continuous flow. To start, I just tilted the tt about 45 degrees and generate the CO2. When enough bubbles escaped from the tt (as
seen from the flask), I stop the flow of the vinegar which in turn stops the flow of the CO2, put the tt in horizontal position then perform the
experiment. At the end of the reaction, I continue heat the tt at the bottom and at the side for about 2-3 minutes to drive any residual P to the
cool end of the tube.
I think www (what went wrong) is that most of the time I headed the tt from the bottom (the close end) and the material is not as fine as they should
be and I did not allow enough room for the expansion which might have prevented the P to escape.
I ran out of the big tt. So, naturally, I've ordered some. But I can't wait. I'll will try again this weekend using 15x150mm tt with your advice.
Please let me know if you have any additional comments/suggestions.
Thank you very much for your help!
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sternman318
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Does anyone else find it humorous that some dude a few hundred years ago cooked his piss with sand and carbon in an attempt to make 'the philosophers
stone' and made phosphorous, yet the modern home chemist is having much trouble making it themselves, despite having superior equipment, materials,
and knowledge? 
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