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quicksilver
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The sulfonozation of the benzene ring material in PA or related materials (styphnic acid) may produce poor yields due to oxidation of the precursor if
that portion of the lab is not monitored carefully. Generally, it is safer to allow for more time rather than higher temperature during this
preliminary (given that you are working with a fair quality H2SO4) - to the nitration. This had been the issue in the 19th century when wool, horn, or
Indigo had been substituted for materials such as phenol. Methylphenol (oil of wintergreen) or ASA are much more controllable except when
contaminated.
Those who did not attempt to clean up their ASA found this a constant problem.
A great deal of valuable material can be found in the thread dealing with oil of wintergreen as a starting point for PA as the sulfonization of that
material was a delicate balance between heat & time.
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Hennig Brand
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If one did have problems with oxidation would it be obvious at the end? Would there be just a mysterious loss of yield, or would it be very clear with
insoluble products. In reading posts on the subject I have seen many times people talk of red,dark yellow, maybe some almost black resinous material
which was very insoluble. I just wonder if maybe oxidation could acount for a loss or partial loss of yield and still maybe not be an obvious cause
visualy?
[Edited on 16-6-2009 by Hennig Brand]
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Rosco Bodine
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There may be a way to finesse the synthesis using
oil of wintergreen as a precursor, but from my own experience it was determined not to be nearly as good a precursor as ASA. ASA has no difficult
reaction management, contaminant byproduct, or end product purification issues. ASA is the way to go on this one,
and by closely following a pretty well tested general process model, the results are very predictably good.
It is usually counterproductive to vary the parameters
by very much, not to say that no refinements can be made upon a process that is general for further optimizing it.
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Hennig Brand
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These figures taken from Urbanski book 1
TABLE 109
SOLUBILITY OF PICRIC ACID IN WATER
Temperature°C Content of picric acid, g
in 100 g of the
solution in 100 g of the
solvent
0 0.67 0.68
10 0.80 0.81
20 1.10 1.11
30 1.38 1.40
40 1.75 1.78
50 2.15 2.19
60 2.77 2.81
70 3.35 3.47
80 4.22 4.41
90 5.44 5.72
100 6.75 7.24
Note: Picric Acid can be slow and reluctant to go into solution, don' t add heaps of water when dissolution is slow. Some time must be allowed in
between additions to effect solution. These tables will give a good idea of how much is needed approximatly anyway. It is obvious that with a small
yield one could easily(if not careful to be mindful of solubilities) to loose entire yield to solution.
The solubility of picric acid in sulphuric acid varies with the concentration
of the latter. It is highest for concentrated acid and lowest in 18-20% acid. This
can be seen from Table 110 [41b].
TABLE 110
SOLUBILITY OF PICRIC ACID IN H2SO4
H2SO4
CONCENTRATION
% PICRIC ACID CONTENT IN 100 G
OF THE SOLUTION
18°C 50°C 80°C
0 1.184 2.399 4.541
2.3 0.230 0.692 1.940
4.7 0.142 0.368 1.251
10.0 0.091 0.265 0.727
18.0 0.079 0.214 0.561
25.5 0.092 0.230 0.587
50.5 0.429 0.645 1.104
69.7 0.928 1.424 2.203
87.9 2.461 5.826 7.610
97.4 7.531 12.785 24.020
100.0 10.180 16.230 25.860
As can be seen easily at certain concentrations of acid the solubility of Picric Acid drops to almost nothing, which can be highly useful. Most
recipies try to drop the concentration to somewhere below 40% to extract the TNP from the nitrating mix.
Much prettier tables can be seen in Urbanki book 1 Chemistry and technology of explosives, as well as other tables and information.
Sorry I had this all neat and when I posted it it went all jumbled up again, erase if not useful if you wish or maybe tell me how to fix.
I must have been frigging with those tables for a while, Rosco got a post in(guess I should have looked)
I tried just about everything at one time or another by way of a Picric Acid precursor (at least the common ones). The only one I had real success
with the first time was Phenol.
The Oil of wintergreen as I recall gave a very foamy reaction during nitration which threatened to boil over. I also got a much lower yield than I did
from aspirin, and the product seemed kinda damp and fluffy. I bet it does work as a precursor but I bet the procedure for it would look much different
than the one for ASA. I tried oil of wintergren 3-4 times, less success even than with aspirin at the time.
[Edited on 16-6-2009 by Hennig Brand]
[Edited on 16-6-2009 by Hennig Brand]
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Hennig Brand
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I would like to describe my last ASA experiment briefly that I did in parts over the last couple days.
I first made fresh HNO3 and was careful to end the distillation just as proceeding into the water zone. S.G. was 1.55, and I got 144mL of it, (awful
tempting to see if I could get close to100ml of N.G. out of it). Anyway this acid must be pretty close to pure (95-98%?), a little yellow but not to
bad.
First sulphonated at around 120C for 1 hour with 20g ASA and 100mL 0f 95% H2SO4.
Let cool to below 60C then started adding mixed acids(22mL of HNO3 S.G.1.55 and 28mL H2SO4 95%). I used a lot less acid this time because after doing
stoichiometry I realized that 20mL should be enough but I added an extra 2mL for losses due to distillation and maybe the inadequacy of my acid.
Temperature was kept around 70C during entire addition with very vigorous stirring from magnetic stirrer, after which temperature was brought up to
110C for 1 hour with some manual stirring .
Yield after 1 recrystalization was 17g of material that can be made to puck from a hammer blow on an anvil, though with a little difficulty. One more
recrystalization would make awsome material, and will probably leave me with approximately 14g very pure product if no effort is made to retrieve some
from the water of recrystalization.
I did not use the oven to dry this time as I think it was making a more fluffy product, though the differences in product could be more related to my
higher yeild this time than anything else.
I would have to say that keeping that water concentration down is key. I guess I allowed myself to down-play the water issue, it is off great
importance especialy when using aspirin I believe.
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Rosco Bodine
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Some presence of water within a certain limited range is actually favorable for highest yields in nitrations .
off topic but enjoy, all work and no play.... and all that
http://www.youtube.com/watch?v=3UYfa0jeL4k&fmt=18
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Hennig Brand
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Thanks man, I would like to watch now but alas I am way out in the country and technology hasn' t found it' s way here yet. My dial-up is even slow
for dial-up! Probably time to break for that satellite internet connection, it has come down in price a lot in the last few years. I will definately
check it out when at my girlfriends, as she lives in the city and has the benifit of high speed. Maybe just let it download when computer not in use.
Thanks and have a nice day 
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Hennig Brand
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I just watched the first minute or so of the video and I feel like I have reached the height of zen. Just joking, but seriously, very relaxing. I am
curious what you were thinking when you posted that. If you are catholic I meant no insult to the church in this post.
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Rosco Bodine
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The church is no enemy of science at all, but is generally its historical advocate. That definitely is a consciousness expanding video in my opinion.
The file is 21.7 MB and because these good videos have a track record of disappearing, I have saved the flv file on an alternate server.
http://www.mediafire.com/file/ztzdtzzfwyb/Mystico.flv
Here is a download link for a standalone freeware flv viewer which is good for playing saved flv files.
http://www.brothersoft.com/d.php?soft_id=59435&url=http%...
You might like this too. I've been on some of these climbs,
in my younger years.
http://www.youtube.com/watch?v=sVjYX4-LZx4&fmt=18
[Edited on 17-6-2009 by Rosco Bodine]
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quicksilver
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Quote: Originally posted by Hennig Brand  | If one did have problems with oxidation would it be obvious at the end? Would there be just a mysterious loss of yield, or would it be very clear with
insoluble products. In reading posts on the subject I have seen many times people talk of red,dark yellow, maybe some almost black resinous material
which was very insoluble. I just wonder if maybe oxidation could acount for a loss or partial loss of yield and still maybe not be an obvious cause
visualy?
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I would refer you back to Rosco's experiments & his deductions on the subject. The "where, when" of oxidized product appears to shift. His
conclusions of ASA as superior may, in fact have more to do with the starting medium (liquid) & it's responses to temperature in a magnetic
stirrer (or without).
However it may also be a property of the oil of wintergreen itself & surrounding (additional) materials such as alcohol depending on where
obtained. Such a thing may exist with ASA. Large Boluses for cattle have minimal binder of a easily extractable nature. Adulterants will ruin an
experiment quicker than poor equipment. 
ASA may be obtained in a known purity level and as a solid, it may have more consistency when exposed to a given temperature (the oil of wintergreen
may separate out for a period during sulfonation).
I have seen successes vary with wool, horn, & indigo & the simple concept of their density may be a contributing factor in their usage (as a
precursor).
Obviously the horn must be ground fine, the wool must also be of a powdered property, & so on. Or the black sludge of oxidation will be apparent
sooner with higher temp than lower. But will exist more so than most any pure ASA. Frankly some of the finest light white-yellow TNP I have seen was
an ASA lab.
{.....Which "popped" consistently with impact at a multi-milligram level.}
The whole issue of an powdered alkali nitrate used to obtain nitrogen, etc is a separate bedevilment... Those that may add greater nitrogen my not be
the best for evolving a solution with H2SO4....
[Edited on 17-6-2009 by quicksilver]
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grndpndr
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Speaking of 'clean' ASA ive always seen cheap uncoated aspirin tablets slightly wetted to soften then dissolved in methanol or "HEET', a methanol
based gas additive,filtered and dried.The resulting ASA must have been relatively pure as the experiments were always very successful yielding a very
brightly colored light canary yellow before and after recrystalization using the very simple OTC H2SO4/NaNO3 method.However the vetrinary supply
route may be better as what Ive seen advertised is pure powdered ASA at approx $7 lb if your in a rural area its likely available at a farm /ranch
supply.Its claimed to be pure but the usual purification may be wise at its first trial use.I have always seen the lower temp range/more time for
sulfonation and nitration used.
although unfortunately no notes were kept.
[Edited on 18-6-2009 by grndpndr]
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Hennig Brand
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I wasn' t really trying to be critical of the video and to be truthful I have only seen the first bit. I have been under the impression, from
everything heard and read though that Christianity has many times been in direct opposition to scientific progression, or at least anytime when it
appeared to be threatening the power and influence of the church. The Catholic church was more than any other group responsible for the dark ages
wasn' t it. Although according to some sources the dark ages were not as stifling to all progress as is usually portrayed in the popular media. I
realy don' t know for sure. Weren' t many of the witches that were burned just people thinking a little differently than the church, some of them
scientists. The church has been very good in a lot of ways. In many parts of Europe until Christianity took hold there was little organization and
little progress in many ways(this is my understanding). I think the church has done horrible things in many ways that would definitely be deemed
drastic human rights violations today, to their own people and most definately to people of other countries and backrounds. Today judging by the state
of society many could use a little more religion though!
Does anyone know for sure that ASA is/or isn't more sensitive to oxidation during sulphonation than phenol, and if so by how much. I ask because the
reaction with phenol is much easier to find information on(for me anyway), therefor a comparison would simpify things.
I would think the phenol would be more delicate from my observations, at least than pure ASA. For sure it is during the nitration(maybe I am drawing a
false conclusion partly based on the nitration differences?)
As has just been said though the two or more starting materials may be very difficult to compare using similar techniques during the nitration
procedure. Results obtained would be relative to the procedure used. However there must be some way to find something conclusive about just the
sulphonation portion of the lab with different feedstocks. Someone, somewhere must have studied this(probably in one of those 30-40$ journals on
line). It doesn' t seem like the kind of thing I am prepared to tackle but I have seen procedures in texts to analize sulpho-phenol and
sulpho-salicylic acid after a sulphonation. It must have been done somewhere at least a few times. Isolating the problem would be ideal, but trial and
error does get good results usually, with a little work and record keeping.
The churches treatment of Galileo might be worth looking into for some as he was one of the primary founders of the scientific method and was treated
less than well by the church.
[Edited on 18-6-2009 by Hennig Brand]
[Edited on 18-6-2009 by Hennig Brand]
[Edited on 18-6-2009 by Hennig Brand]
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Hennig Brand
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Quicksilver after reading through your post again I can tell you have been "through it" with the Picric Acid in great detail. I would say a lot of you
here have more experience than me with this. In your post you stated that adulterants can ruin an experiment quicker than lack of proper equipment. I
used to, (before getting aspirin powder USP) purify aspirin with acetone and I always felt that something other than aspirin was still getting through
the purification that was easily oxidized(at least with my aspirin). I was very inexperienced at the time(more than now) and I tracked down some pure
ASA which seemed to put an end to a lot of my resinous oxidation products, though now that I know better what I am doing maybe I should give it
another go just to see? A lot of things where changing simultaniously at the time with my synthesis. Barring the impurities some kind of mechanical
stirring(magnetic seems to be the most convenient and effective at least for small scale) makes a horendous difference to nitration efficiency, and
speed and to reducing losses due to oxidation/localized heating, high concentrations of nitrate/HNO3 in spots. Hand/manual stirring can get the job
done but in my experience it is just tremendously tedious and laboursome and still does half the job of any good mechanical stirring device. I have
seen it stated in texts that in aromatic hydrocarbon nitrations(especialy TNP) that agitation is probably one of the most important parameters next to
temperature control. Then again if you use a feedstock with junk in it I guess all the care in the world to temp and agitation isn' t going to make up
for it(as you said), these things are still very important however. Using good ingredients is definately paramount though and to the inexperienced(me)
it can sometimes be difficult to tell.
Although maybe not absolutely necessary I find the magnetic stirrer to have greatly simplified the procedure, making it much quicker and easier, and
with a superior product(at least for me).
In my last few attemps, (which were more successful I think) I tried to get around some of those seperate bedevilments. One way was of course was by
using the known pure ASA, and the other was by avoiding the nitrate salts and using HNO3. I haven' t found NaNO3 only KNO3 so HNO3 greatly simplified
things in some ways compared to the K salt (I found anyway). When added as a mixed acid with H2SO4 it seems to be pretty straightforward and
convenient. I guess this all depends on one having the equipment to make the acid though, and as many have said not needing the acid(HNO3) is maybe
one of the main appeals of the other synthesis using nitrates, and even using this explosive at all.
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quicksilver
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Magnetic stirrers are a fine thing - that's for sure.
Occasionally, ammonium nitrate is just the thing for making a sold nitrate/mixed acid because it appears to "mix" well in your H2SO4 unlike sodium
nitrate, etc.
So lets say you only source is "cold packs" (that are expensive); you can still get a good mixed acid from such a thing.
IF you can only lay your hands on KNO3, use something to drop the particulate to a very fine level (600mesh or 40um). You'll get a much better mix
& a much better final product. This is where your $19.99 coffee grinder outshines the mortar & pestle. 
There ARE some threads on making a magnetic stirring device but must people find that a mechanical stirring device (non-magnetic) can be rigged up to
do the job as there are some stainless steel devices for mixing paint that, with a bit of fine tuning, will suffice. If you have a real one from a
lab; treat it like a baby. Replacements cost at least $100+.
Agitation with air is feasible: I have seen it done with an aquarium pump and a vortex design for the insertion tubing.
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1281371269
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Making one is very very easy if you have an old broken computer hard drive and fan lying around. A speed control can even be fitted with an
(apparently) simple piece of electronics. The issue is that the teflon bars aren't all that cheap. I tried making one with some screws and PTFE tape
but it wasn't really satisfactory.
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Rosco Bodine
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Please indulge this digression, to try to shed some
light on a consideration of ethics and science in a historical perspective.
Recommend you see all of it, then be the critic. Alice cannot describe wonderland before traversing the rabbit hole fulget crucis mysterium
| Quote: |
I have been under the impression, from everything heard and read though that Christianity has many times been in direct opposition to scientific
progression, or at least anytime when it appeared to be threatening the power and influence of the church. |
Better to ask a Christian than to trust the commentary of historians. There is a difference between the history of all Christendom in the entire
world, and what may have been the bad behavior of any ambitious sectarian interests, including any corrupt acts of a small minority of Catholics. I am
not a Catholic and I can recognize that. There is a very large population of the church and it is not all Catholic. Peter was one of twelve
disciples, so there are many more derivative branches than the Catholics. | Quote: | | The Catholic church was more than any other group responsible for the dark ages wasn' t it. |
Actually no,
the fall of Rome and the chaos which followed was probably most responsible for the early middle age decline of culture and learning, which the
scholars of the church preserved.
There is historical direct correlation in the declining use of Latin which was the language of the learned and cultured, the scholars, doctors,
teachers, ect. and the literature which sustained a higher standard of life, with the parallel decline
of society, in that early middle age period of decadence when
ignorance and darkness was prevailing.
| Quote: | | Although according to some sources the dark ages were not as stifling to all progress as is usually portrayed in the popular media.
|
Correct | Quote: | | I realy don' t know for sure. Weren' t many of the witches that were burned just people thinking a little differently than the church, some of them
scientists. |
Possibly, but that would seem unlikely. | Quote: | | The church has been very good in a lot of ways. In many parts of Europe until Christianity took hold there was little organization and little
progress in many ways(this is my understanding). |
Correct | Quote: | | I think the church has done horrible things in many ways that would definitely be deemed drastic human rights violations today, to their own people
and most definately to people of other countries and backrounds. Today judging by the state of society many could use a little more religion though!
|
No argument there, except that faith is better than religion, hope is good too,
and always love is still better than either.
http://www.youtube.com/watch?v=5nkZHidDGUk&fmt=18
Latin / English
O Lux beata trinita - O Blessed Threefold Light
Fulget crucis mysterium - The Mystery of the Cross Shines Out
Lucis creator optime - Most Wonderful Creator of The Light
Aeterna Lux caelestia - Everlasting Heavenly Light
Beata Lux - Blessed Light
| Quote: |
The churches treatment of Galileo might be worth looking into for some as he was one of the primary founders of the scientific method and was treated
less than well by the church. |
Galileo's astronomy wasn't what got him into trouble with the church, it was his trying to interpret scripture in the light of science which got him
in trouble. Wrong light for the job.
[Edited on 20-6-2009 by Rosco Bodine]
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Hennig Brand
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There are ways to make stir bars,procedures can be found in old lab texts. The one I have seen a couple times is to put something ferrous or magnetic
in a piece of glass tubing and seal the ends by melting process. The teflon is probably the best but a substitute can be improvised or so it says in
the books.
With regards to the stainless, I took one of those cocktail battery powered stirring devices(hand held), and replaced the cheap plastic stirring arms
with stainless steel welding rods(tig rods). The cromium I believe or something else made a huge mess and produced this big fluffy precipitate that
filled my beaker. And to make matters worse I couldn' t seem to get the beaker clean enough to keep the same thing happening even without the
stirrer(it looked clean but wasn' t). I eventualy did get it clean and never looked
back, now using only glass and teflon. It is good to point out though that there are many different types of stainless steel and some are probably
very suitable for nitrations(I believe industry uses stainless in a lot of these sorts of situation). I just don 't know enough about the different
metals, and was not sure that it would be cost effective, and would maybe raise some eyebrows if I order some exotic stainless. There may be some
common stainless that I overlooked though, that would be suitable) . I have since rounded up some large chunks of teflon in the form of runners for
snowmobiles(people do a lot of that around here) which could be cut/shapped into a paddle or something for the cocktail stirrrer. The batteries could
be replaced with a small cheap (wall wort) power supply of suitable voltage, and speed could be controlled simply by using variable resistance between
power supply and motor(remote control via cord). One of the main reasons I abandoned the regular motor stirrer, for the magnetic stirrer was abviously
because the stirring contraption had to be used with something large enough to except the stirring apparatus and still give space to work while doing
experiment. The rising acid vapors also were damaging to the stirrer(plastic, exposed metal, motor?), I could tell it would be an isue in the not to
distant future(probably destroy the stirrer), I am sure there are ways of doing it though, and protecting it from acid vapors. The cocktail stirrer
was only $5, so no big loss and it was a valuable learning experience. The magnetic stirrers seem much more versatile, useful and user friendly. And
in my limited experience easy to improvise a descent diy model.
Coffee grinders are awesome, I use them all the time and have several for different uses. The last two I bought were about $10 each and were simple
yet tough and practical. I always did powder my KNO3 for TNP nitration but a lot of the problems seemed to be in relations to the characteristics of
the chemical itself and its products during and dealing with them after nitration, rather than with the partical size of the chemical when adding. I
guess that could be a problem to, but I don' t know as I always powdered my nitrate as per Rosco' s instuction in his posts.
Note: when I was researching teflon I believe I found that it was at decomp temperature at about the same temp as melting, but that layers or pieces
could be made to fuse without decomp at a significantly lower temp. This might prove useful(I experimented a bit but didn' t put much in and didn' t
get great results). It is done however in industry routenly I think, whether or not teflon tape would work well I don' t know. Also there is much
thicker teflon tape that can be bought, one example is the stuff used for gas lines instead of regular plumming(it is much thicker, good around stills
too).
[Edited on 20-6-2009 by Hennig Brand]
[Edited on 20-6-2009 by Hennig Brand]
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Hennig Brand
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Interesting insites on religion and science Rosco. I only have the little knowledge I have on the subject because I have read some, but mostly I have
listened to those who have spent more time at trying to understand history(older family members usually). It seems like you know what you are talking
about and the things I posted where just my feelings mostly with out the benefit of a great deal of research. I maybe shouldn' t have said as much, as
these issues can be very emotionaly charged and personal for many(I don' t mean you personaly, its just that such discussions are not deemed
apropriate for polite discussion by many). I will check out your links soon and try to keep an open mind, I tend to develope tunnel vision when I get
into something to the exclusion of all else(it is my greatest weakness and also my greatest strength). Time could be well spend studying such things I
would say, for one interested in overall personal development and understanding. Some of what I wrote may have been distorded by my memory and
interpretation from the original source. I appreciate the links, and insite on the subject. I am not very religous, even though brought up more so,
yet I like to try to keep an open mind(more so as I get older).
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Rosco Bodine
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Something significant which many seem to forget is that the very origins of literacy and science are linked to religion of one sort or another since
ancient times as the means of recording and publishing and glorifying the
greatness of some royal personage of some variety, calendering and scheduling of rites, and seasonal events, constructing of monuments, composing
musical tributes, preparing medicines and so forth were
royal commissions which required patronage of the wealthy rulers and society in support of such arts.
Indeed for many thousands of years, the
greatest number of persons on earth who could even read and write only did so because that was essential to their commissioned occupation of
maintaining the records of royals, who also directed that religious and historical records, scientific, mathematical, literature,
and other art be preserved. So it was the "priests"
of whatever variety who then became the worlds museum keepers, chroniclers, historians, and librarians. Especially noteworthy in that regard were
Christian monks, some of whom were scientists as well as being priests at the same time. Roger Bacon outlined the general methods of logical
scientific experimentalism
which holds through little changed today, and he was a Franciscan friar affiliated with Oxford university. Orders of nuns have left their bodies to
science for post mortem studies of diseases of aging. The truth is that study and increasing of knowledge and reasoning is one of the principles of
Christianity from its originator, but there is the caveat that its purpose be ethical and serve the greater good. Not all scientific pursuit would be
reasonable or ethical simply by being scientific because
the same science which produces the cure for a disease like smallpox, could also kill many millions. And the same science which leads to the nuclear
power plant,
can also in a more perverse usage have apocalyptic effect. Therefore with scientific knowledge also comes a
moral responsibility. There are ethical oaths which doctors and engineers are supposed to follow in respect of that same moral responsibility to do
what helps rather than harms.
[Edited on 20-6-2009 by Rosco Bodine]
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Hennig Brand
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Very interesting indeed. Without really knowing, after reading your last post it all seems to hold true logicaly. I guess for whatever reason I was
unaware of the importance that the religious community played in laying the foundations of, and nurturing along the way of scientific progress and
achievement. They seemed to be the main players for a long time, especially early on, and still to a great extend right on up to modern time right?
I don' t know if you have had the same experience but in growing up my experiences when talking to priests or ministers was usually one that left me
feeling that religion and the church were in competition with science (or at least some of its theories). This is just the impression I got, not
necessarily reality. It may have been that I was tormenting these people a little by asking questions that may have conflicted with their belief
system(these people were also usually not science orientated to any great extent, or not at all), and I was being a little over enthusiastic and
threatening(unintentionaly), as I was young and lacked good people skills.
I wonder if western civilization could have made a lot of the accomplishments it has without its early start with, and influence of the christian
religion? I would guess not, but I don' t know exactly to what extent it is true.
Interesting stuff.
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Rosco Bodine
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If you think about the engineering and art which definitely involved science to an enormous extent and at great expense just for the construction of
churches then it becomes clear that by necessity the church is probably the single greatest patron of the arts and sciences. But the purpose of it all
being for the glorification on earth of a God who cannot be seen or measured with instruments but is a matter for the heart to discern, is a concept
which gives atheists indigestion, so they deride and ridicule the church. When surveying the worlds splendid monuments to whatever is considered
glorious by whatever religion, the architecture alone should make a statement. And institutions of higher learning, the colleges, particularly the
older ones were many of them
originally and principally seminaries whether that is the public perception or not. So it really comes down to it
that we can even read and write today is probably a heritage which is ours in the present age a gift from some ancient "holy men" of the past. They
were the worlds ultimate archivers and teachers of knowledge
at one time, and that time is one which may not necessarily be marked by a beginning or an end.
[Edited on 21-6-2009 by Rosco Bodine]
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hissingnoise
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| Quote: Originally posted by Rosco Bodine | But the purpose of it all being for the glorification on earth of a God who cannot be seen or measured with instruments, but is a matter for the
heart to discern, is a concept which gives atheists indigestion, so they deride and ridicule the church.
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Rosco, the thread is about is about synthetic routes to an energetic material; it has nothing whatsoever to do with a belief in an imaginary "Super
Being". . .
Your religious beliefs are your business and you're welcome to them but I am an atheist and I detest seeing organised superstition being
discussed on a science forum, of all places.
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Hennig Brand
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I agree we have derailed the thread a bit and will be more careful in the future about this. However I think it less than scientific to take a rigid
stance on some of these issues concerning science and religion(I do respect your right to your opinion though). I do feel however that without some
faith in something, or a belief in some way that "things will work out" life is more impoverised in many ways, life and death are usualy or can be
much more difficult for people with out a certain amount of hope for the future. For awhile I would have called myself a definate disbeliever and at
some level I still am for sure, but in looking around people with faith seem to generaly be healthier and have an easier time in life and death. It
definately gives hope to many. Sometimes entertaining the thought of a posibility of things we don' t understand can be healthy I think, and needn' t
take the place, or discredit hard science in my opinion.
Back to TNP and I am sorry to stray from the topic.
Does someone know if I could purify or get the water out of my phenol? It is a hydrate?/bonded with water and made to fuse. On looking it up it
probably actualy has about 10% water in it even though before I said 8% from memory. Does anyone know off-hand how this is done? It would be a good
source of phenol as the little bottles come with about 100g in them and they are less than $10 and there is no hazard charge associated with their
purchase. It is still expensive I know but for experimenting it is fine(100g is quite a bit to play with)
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quicksilver
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My most productive advice on the subject would be this: Look to local Universities & attempt to "buy" their surplus chemical /lab equipment. YOU
WILL GET RESULTS if you appear in person are an adult & never offer to pay in cash (unless asked). I have gotten MANY goodies that way! Some
things of high value also! make absolutely sure that aside from rudimentary items - nothing you ask about may be used to make drugs - no List 1 stuff,
etc.
If you hit pay dirt, be very forthright about the fact that you love chemistry as a hobby and have some plausible reason for experimentation; such as
working on a new design stick fly-paper, but only when asked......No one REALLY cares about making a sub gram quantity of some designer primary or
whatever; even the ATF so long as the whole issue is quiet (no pun intended) & safe, but don't be irresponsible or you'll also get others in big
trouble. Remember they are thinking about that too! Seek and yea shall find.
Regarding the subject of religion, I am not a practicing Catholic but I remember the teasing about the Pope said there is no vacuum & things of
that nature but I still pray. I actually believe in something much greater than myself & I also shed a tear or two while doing so. I think that
ANY organized religion can be found to have made a mistake or several. but in the greater perspective of science & religion, it would be a damn
lonely place to be without some faith in something. But these are private matters that often change over time as had science.
If Albert Einstein (who was a practicing Jew) could believe, who am I to say such things are opium for the masses? I also remember his brilliance was
not recognized when he was young. That tells a great many things about perception of what is science & what is human nature.
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Hennig Brand
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I imagine everyone has seen these but I wanted to ask about it anyway.
http://www.jbc.org/cgi/reprint/82/1/1.pdf
There are other links (a couple I have found with procedures for Picric Acid purification), this one has a good procedure that can be used to produce
sodium picrate as the intermediate during purification or potassium picrate. I have tried these proceedures a few times a while back with some of my
yeilds from less than perfect nitrations of ASA with not great results. It did get rid of some material and made a better product I think but it was
still no where near what I have been getting lately from my more successful nitrations from ASA.
Even now when I do a nitration with ASA at the end during purification with water there is a small amount of much more insoluble material. It is not
resinous or anything, it is crystaline and some appears more boyant than the rest. I usualy scrap it of the surface with a spoon and decant to get rid
of the stuff on the bottom. I believe this material to be 5-nitro salicylic acid (+ other?),mostly which would be the result of incomplete nitration,
and early on I think I had much more of this(probably mixed with some resonous material). If you look up the solubility of this compound it is soluble
in more than 1000 parts of water, compaired to Picric Acid' s 78mL. And to make matters worse it forms salts with bases as do all the salicylic acids.
It would form a similar red/orange solution with sodium/potassium carbonate and is yellow before and after purification. I don' t know how much nitro
salicylic acid could be in the mix after nitration but when using the Picrate purification method it maybe works a little differently when going from
ASA than from phenol(different impurities, different situation?)
Interesting perpectives Quicksilver. People are very suggestible aren' t they, and perception is at least a distortion of reality, as well I believe.
I will take your advice and try to be tactful with the university lab people and see if I can get some results. The problem for me is(I think) once I
get talking to the educated in chemistry it becomes a little obvious what my interests may be. Maybe I am just perenoid. I also think that
universities can be as a matter of course not very friendly to the experimenter as a matter of course, with the justification being one of a liability
issue(which is at least partly true), but is used too often(in my opinion) to discourage any science outside of the
institutions(university,industry,goverment, etc). One has to learn to work with the system a bit out of necessity I guess.
[Edited on 21-6-2009 by Hennig Brand]
[Edited on 21-6-2009 by Hennig Brand]
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