Sciencemadness Discussion Board - Picric acid: different instructions

The whole in the [center] was made with 40g of a gellitin dynamite, in a 3cm diameter pill bottle(plastic). Approx 15g NG, 0.6g homemade NC. Acetone was used to facilitate NC dissolution. Also 20g KNO3, 4g sugar(sucrose) ground fine together in coffee grinder before mixing in with gellitin. This mix is one of my favorites, although I normally use aluminum powder in place of the sugar, which does seem to make quite a difference in performance, or at least a lot better boom

The issue of whether aluminum (which would raise the temp of the detonation) has a substantial impact on the effectiveness of an energetic is an interesting subject in itself.

Generally, testing from Sandia Corp & Los Alamos indicated that the result [of the addition of powdered Al] was a higher temperature but slightly less speed. Yet the use of temperature enhancing materials such as Al is a common feature in both military and commercial materials.
One of the more interesting tests were the use of Al in the enhancements of "cool" explosives such as nitroguanadine. One of the performance theories is that due to a rise in heat, the blast-wave "spreads" quickly (as opposed to a lower temp wave front). This is pretty logical since heat generally lowers density.

Powdered Al had also often found it's way into modern (non-fulminate) detonators. It's principal use there was as a "lubricant" during the construction of the detonator, to facilitate packing with a lessening of friction. It apparently did it's job quite well as it's still illustrated in film clips about detonator construction.

edit:
- Pretty impressive pictures.
I was also quite lucky to snag some USP KNO3 and it's use in a variety of things has been great. It was really worth the hassle getting it.
If I ever break down & buy a digital camera I'm going to try find one with some level of macro capability. A strong close up of the metallic tears would have been very interesting.

[Edited on 25-7-2010 by quicksilver]

Hennig Brand - 25-7-2010 at 07:23

I always sort of wondered if putting Al powder in AN based explosives was kind of a waste because of the low heat of detonation. Maybe the ones with high concentrations of Nitric Esters or Nitrated Aromatics would get much more potential out of the Al powder.

Anyway here is a close(r) up picture of the hole the 2g of TNP made(2g TNP compound cap #1). Does anyone know if this seems like a reasonable amount of damage for 2g of TNP? It seems a little wimpy. Anyone with first hand experience, your opinion would be valued.

TNP blast hole.jpg - 173kB

[Edited on 26-7-2010 by Hennig Brand]

Hennig Brand - 25-7-2010 at 07:27

Here is a close(r) up picture of the hole the 1.5g of ETN made. Note that the ETN actually ripped the metal right out for the most part(I love this stuff).

ETN blast hole.jpg - 131kB

Hennig Brand - 25-7-2010 at 07:32

Here is a close(r) up picture of a section of the rather large hole the ~40g of KNO3 gelatin dynamite made. It made a huge hole, but the metal was mostly just all curled up. I could not uncurl the metal by hand.

Dynamite torn metal.jpg - 159kB

[Edited on 26-7-2010 by Hennig Brand]

pjig - 25-7-2010 at 09:47

I'd assume that you didn't get a full det out of the TNP.. It is quite insensitive and needs a lot of initiating power to get it to kick. The hole is probably from just the primary and a very small amount of TNP.. Try more primary or press a TNP base, then a 50/50 TNP/ primary , then your primary( kind of like a step prime)..

[Edited on 25-7-2010 by pjig]

Hennig Brand - 25-7-2010 at 14:41

You are on the right track, or at least my couple small tests would seem to indicate that.

I tried just the 0.4g of Lead azide in a cap to see what the effect would be on the barrel, and it hardly left a scratch.

I then made another cap with 2g of Picric Acid just as before, however this time I used 0.6g of Lead azide and 0.1-0.2g of Basic Lead Picrate as a flash igniter lightly pressed on top of the Lead Azide to ensure rapid and uniform ignition of the LA(I wanted to be sure).

Before even going to check the barrel, just by the sound I could tell I had a much better result. The hole is a lot bigger than before though a little smaller than what was made by the 1.5g of ETN, it did tear the metal right out in much the same way.

I guess I had a lower order detonation the first time. My Al tubing is pretty soft and thin, so the confinement is probably a little less than optimal. Also the LA from my last batch was kind of darker brown than normal, so maybe not up to normal standards (I don't know for sure, I guess I could test different samples to be sure). Anyway both TNP and LA were pressed untill the Al started to buckle. While 0.6g LA seems like a lot of primary to get TNP to really kick, when it does kick it kicks pretty darn well.

Here is a picture of the hole made by the second 2g of TNP(TNP compound cap #2), in the same barrel (I just rotated and exposed a fresh face).

TNP overdriven.jpg - 175kB

[Edited on 26-7-2010 by Hennig Brand]

quicksilver - 26-7-2010 at 05:19

Anyway here is a close(r) up picture of the hole the 2g of TNP made. Does anyone know if this seems like a reasonable amount of damage for 2g of TNP?

There are simply too many variables to be blunt & say: " 2 gr of TNP should look like this or that when detonated against 16ga sheet steel".
An appropriate illustration would have to take into account the direction of the cap, it's proximity to the barrel, the density of the TNP, the construction of the charge as a whole, & the phenomenon of ignition.

We know that TNP is generally a squeak stronger than TNT, so using that as a basis for comparison, the best agenda is to find TNT test results and see if you're in the ballpark.
I certainly think that IF the TNP were pure, you're on the money.

Does the TNP "pop" when struck on an anvil w/ a steel hammer? That's a cheap & easy way to know that you have little to no DNP in with it.
Make two caps with the TNP sample as a base charge. One with two gr and other with 4gr. If you see similar results and then a greater witness-plate hole; you know you are getting appropriate response from the TNP and not the det cap obscuring the results.

Hennig Brand - 26-7-2010 at 06:19

My last post shows much better results from 2g of the same TNP.

It is the TNP from the picture(my first picture of the coffee filter and 43g TNP, big crystals), made from ASA and NaNO3.

It does go snap with a firm wallop of a heavy hammer.

I should have said before, but when the Al starts to buckle I have pressed the TNP to ~1.4-1.5g/cc (in the ball park anyway, calculated using volume and mass).

There was no tamping, the compound cap was just laid on the barrel, and held in place with a bit of tape.

The first 2g TNP compound cap was definately a low order and/or partial detonation, but the last 2g TNP test(from the last picture and post) did much better(similar brisance it seemed to the ETN).

It seems that what I have read about TNP is true and it will tend to go low order unless overdriven quite a bit (most likely especially true in small quantities of TNP). I believe Rosco has discussed the need to overdrive TNP several times that I am aware as well.

Just realized that maybe I didn't differentiate very well in my posts the two different TNP tests. I labeled the two a little better now.

[Edited on 26-7-2010 by Hennig Brand]

Rosco Bodine - 26-7-2010 at 16:15

In the most precision and optimized cap I can make, I customarily overdrive a base charge by a minimum of 50% over the amount which is the minimum found will 10 out of 10 tests reliably produce a high order detonation. If it is a more improvised sort of configuration, then 100% or even more than the minimum ...
yepper double it ...and suffer no misfires as the reward for such "wastefulness".
When it comes to "economy" there is good economy and there is senseless economy. When it comes to explosives, and a few other things actually, it is better in my opinion to be sure you have "enough" by using a little "extra" than to come up short....it isn't like the "patient' is expected to survive the operation,
but generally is just the opposite idea, unless it some kind of anomalous "special application" scenario where surgical precision and selectivity is required....then blow the hell out of it, to make sure it is thoroughly well blown. Most of the time when you drop a light bulb onto a concrete floor it will shatter to pieces, but on rare occasion one will bounce instead of breaking. If the occasional anomalous uncertainty of a love tap is unbearable, a sledgehammer reliably removes all doubt.

In terms of velocity and brisance ETN would be expected to do better than PA. But there are other things that PA can do better, storage stability being one, and lower sensitivity being another. Really these are different types and class of explosives so it is apples and oranges beyond the fact that they are both energetic materials. ETN may be thought of as a generally similar explosive to nitroglycerin, a bit less stable, and in solid form. And PA is more of a TNT class material, so the parallel comparing ETN and PA is much like comparing NG and TNT.

[Edited on 27-7-2010 by Rosco Bodine]

Hennig Brand - 26-7-2010 at 17:47

Thanks for the input. My caps are definately not perfectly optimized, most likely from every perspective there is, but as you say they can be made to work.

So 0.6g LA doesn't necessarily seem all that excessive in my case then?

It is pretty impressive stuff(TNP) when it does detonate high order, love the sound, and the carnage

BTW, I have lately been experimenting with Basic Lead Picrate and found it to detonate very easily from flame and a bit of confinement, but mine seems very resistant to concussive ignition(wack with hammer). It it normal? I have always read the stories of it being supper sensitive, but then again many say that about pure TNP also.

quicksilver - 27-7-2010 at 06:28

As you've most likely read, well made lead azide can be brought down to an extremely light weight as an initiator to PETN; this is also likely toward more sensitive materials such as ETN. The level of initiator weight for picric acid may be similar to TNT and I would be fairly sure that your needs are much less than over half a gram.

Factors such as the level of density of your base explosive, the contact surface area, & the base explosive's physical structure all contribute to the efficiency of the cap.

In commercial production, special attention is often paid to the cap's housing. Anodized aluminum is often used and the type of aluminum is often not the soft, common Al tubing. What is produced by many firms are caps which use a type an extremely hard aluminum which does not "bulge" during the nano-seconds of a detonation, but shatters. This contained energy & violent release increases efficiency. The anodizing halts further oxidation.
The type of aluminum used is not easy to come by: but a source does exist. Aluminum arrows (used in archery) are made of the same tubing material and are unusually brittle. They are very strong in a linear fashion but shatter when used as a cap housing. They are very consistent & are generally the closest one can get to commercial cap bodies. When compared side by side with common 60x series aluminum tubing the simple substitution of this type of tubing appears to result in a much more profound detonation.

edit:
I have seen side by side comparisons that convince me of the above. Additionally I have no doubt that one tenth of a gram of lead azide is as much as would be needed in most instances as initiation has gone far, far below that.

[Edited on 27-7-2010 by quicksilver]

Hennig Brand - 27-7-2010 at 07:21

If everything was in fact perfectly optimized and cutting edge then you are probably right. Cutting edge is not where I am at, and I am more interested in more common practical things. I find Picric Acid to have a very nasty tendancy to go low order detonation, if not overdriven quite a bit. A bit different perhaps, but I was just lately reading an old popular science magazine article about Guncotton(from around 1900), and it said that the navy scientists found that dry compressed Guncotton could be initiated (if under perfectly optimized conditions) with a mere 2.7 grains(~0.175g) of Mercury Fulminate. In actually practice however they found it most practical, all things considered to use something like 35grains(~2.27g) Mercury Fulminate. This is without doubt a huge excess. It does seem to show that they were thinking along the same lines as Rosco though.

edit: BTW what is the diameter of these arrows, I don't think going smaller than 5/16" would be advisable with TNP. I actually prefer to use around 3/8", but I could be going overboard on the diameter. It (TNP) has a fairly large critical diameter, probably even larger in an improvized scenario.

[Edited on 27-7-2010 by Hennig Brand]

quicksilver - 27-7-2010 at 07:27

I find Picric Acid to have a very nasty tendancy to go low order detonation, if not overdriven quite a bit.

?
Now I've heard of NC doing this but not of Picric Acid. I am intrigued. What happen to show a low order det? Are you speaking of a cap det or a volume detonation?
Mercury fulminate is annoying to work with as it seems to demand high density to detonate with any real authority.
{OT}
I would really like to get a digital microscope camera. Some time back I was using a microscope to determine if any needles existed within lead azide samples (which IS a damn good idea from a safety standpoint). & I happen to check the classic and "optimized" clathrates at 400x - & at that magnification, you can see the lattice.

The nice thing about using arrow aluminum is that the sizes range significantly and actually available up to close to .5"
I was quite impressed with using that material. The level of quality is profoundly high. The interior in anodized as well as the exterior, it can be cut with little problem. The "shattering element" is no joke however. they splinter in such a manner that you really do not want to experiment without so genuine distance or shielding. But if two designs are placed one after the other, the "arrow aluminum" will show a performance that the softer material will not; with a variety of explosives.

[Edited on 27-7-2010 by quicksilver]

Hennig Brand - 27-7-2010 at 07:52

I have seen it a few times now with my own experiment, where I got a definate detonation but it did less than half the damage to the rock, or steel I had it placed on than it did with a bit more initiation. I have also seen it described a few times at least in old military/explosives books, IIRC it was one of the major criticisms of TNP shells, I think TNT also has this problem to some extent. From what I read the German shells (TNP) were particularly bad for going low order or underperforming, but it was a trade off between that and higher sensitivety(more primary, etc). Apparently when close to the critical amount needed(maybe not even all that close) it was often anyones guess whether it would go high order or low order. This is just from stuff I have read, I hope I am not just repeating someone elses bad opinions.

If I come across some references I will get back to you.

In my own experience it definately needs to be overdriven, whereas something like ErTeN(ETN) always seems to work well I find(maybe I just always load it lots heavy, it is kind of sensitive).

A microsope camera would be very neat indeed. You could post some very interesting pictures for sure.

edit#2(revisit):The low order det may be more to do with caps and boosters, I don't know. The Germans did use alot of Picric Acid boosters, they often lacked "authority" quite often that is for sure, from what the old sources say. Maybe with a large volume of TNP it wouldn't be as much of a problem, and it would pick up to a high order, even if started out low order.

edit:The arrows sound really good actually, thanks for pointing that out

[Edited on 27-7-2010 by Hennig Brand]

[Edited on 27-7-2010 by Hennig Brand]

The WiZard is In - 27-7-2010 at 07:54

Just for fun, here is an old barrel I found and put to good use. I like to call this photo "Barrel Blasting".

You could cobble together a lead block for Trauzl's Lead Block
Test. I could make you one, however, and 8x8" cylinder of lead
me thinks would be expensive to ship.

http://tinyurl.com/2eto3cu

A Ballistic Pendulum perhaps.

"This apparatus consists of two essential parts, a cannon in which
the charge is fired and a pendulum which receives the impact of
the products of combustion and of the stemming. The pendulum is
a 12.2-inch United States mortar, weighing 31,600 pounds, which
is suspended by means of a stirrup from two cast-steel saddles
fitting over a steel supporting beam that rests on nickel-steel knife
edges on steel bearing-plates supported by concrete piers. The
swing of the mortar when the cannon is discharged into it is
measured by an automatic recording device and is taken as a
measure of the propulsive effect of the explosive."

http://tinyurl.com/3xhqkks pg. 47

djh
---
Men offer love in hope of getting
sex; women offer sex in hope of
getting love; both are cheated.
Richard J Heedham

Hennig Brand - 27-7-2010 at 08:26

Your Lead cylinder would weigh about 65lbs if I didn't mess up somewhere. A little heavy for shipping, you are correct.

Your ideas sound good, I kind of like the idea of the witness plates simplicity and cheapness, but I definately should rig something up much better than an old surface rusted barrel. Nevertheless the barrel did teach me a few things that I wouldn't have known otherwise.

I could maybe rig up some kind of mortar and ballistic pendulum, for making comparisons. I have made a couple of black powder cannons now (fairly crude though), so am used to working with metal a bit. A friend and I made a 3.5 inch(350 caliber?) black powder cannon just last year(large piece of heavy seamless pipe to start), finding good(cheap) projectiles was/is the hard part. Back on topic, I like the idea of the Ballistic Pendulum, sounds interesting.

[Edited on 27-7-2010 by Hennig Brand]

pjig - 27-7-2010 at 09:29

This is fine and dandy if you have large amounts of scrap material laying around. But if you want to see performance from a cheap stand point, use the sand test.

The WiZard is In - 27-7-2010 at 11:17

Quote: Originally posted by pjig

This is fine and dandy if you have large amounts of scrap material laying around. But if you want to see performance from a cheap stand point, use the sand test.

As dobe noted the sand test measures brisance [Please!
The word is French and not pronounced as spelled. Don't
look like an amateur by pronouncing it bris - ance.]

This from PATR 2700, Volume 1 XXI & ff, which see for drawing.

Sand Test or Sand Crushing Test (Sandprobe, in Ger) (Essai au sable, in Fr)
(Prueba de la arena, in Span).

This test, devised by W.O.Snelling in 1910 and studied extensively
by C.G.Storm & W.C.Cope (Ref 1), is considered to measure the
shattering (disruptive) power of an expl, called brisance.* This
characteristic is im¬portant because it determines the
effectiveness with which an expI can fragment a shell, bomb
casing, gren¬ade or warhead of a rocket

The sand test consists essentially in detg the amt of standard
sand (supplied by the Ottawa Silica Co, Ottawa, Ill), crushed by a
std wt (usually 0.400 g) of expl. The original sand passes through
No 20 mesh sieve(US Std) and contains no particles smaller than
No 30 mesh. The test in conducted in a cylindrical steel bomb, 3
1/2 " in diam, 8 1/2 " with cylindrical cavity 1 1/2" diarn and 6"
deep. Procedure: Transfer an accurately weighed 0.400 g portion
of test expl, of such granulation as to pass through a No 100 sieve,
to each of five empty No 6 commercial blasting cap shells (of Cu,
Al or gilding metal) held during transfer in loading block. Insert in
each shell a reinforcing cap provided with a small hole in the
center and by means of a plunger subject the charge(previously
placing it behind barricade) to a pressure of 3000 Psi for 3 mins.
With a pin, prick the powder train in one end of a piece miner's
black powder fuse 8-9" long and crimp to the pricked end one of
the above loaded No 6 caps, taking care that the fuse is held
firmly against the charge in the cap. Pour into the bomb 80.0 ±0.1
g of std sand and level it by striking the bomb with a hammer.
Lower the cap into the bomb so that the car is centered at the axis
of the bomb And just touches the sand. Pour 120 +/- 0.1 g of
sand being careful not to disturb the position of the cap. Pass the
upper end of the fuse through a tightly fitting rub¬ber tubing
which is then inserted in the hole of the bomb cover. Lower the
cover into position and fasten it securely by means of two bolts
with nuts. ignite the fuse and after expln of chge, remove the
cover. Transfer the contents of the bomb to a piece of glazed
paper, cleaning the bomb and cover thoroughly. After removing
pieces of cap and burnt fuse, transfer the sand to a No 30 sieve
fitted with a bottom pan and a cover and shake for 3 mins on a
mechanical shaker. Weigh to 0.1 g the sand which passed through
the sieve and record the average of all five values. This wt is the
sand test value or brisance value.

If the expl chge cannot be initiated by flame, it is pressed without
insertion of the reinforcing cap. Then a 0.300 g chge of LA is
placed on top of the expl, followed by the reinforcing cap and
another compression at 3000 psi. Then the fuse is inserted and the
chge initiated as above. After detg the amt of sand crushed by
these caps, subtract the wt of sand crushed by 0.300 g LA, when
loaded alone in No 6 caps

A modification of this test applicable to liquid expis is
described in Ref 9, pp 9 & 11. The sand test may also be applied
to detg the amt of LA and/or tetryl, that must be used as initiator
or booster to insure that the sample crushes the max net wt of
sand. This is designated as sensitivity to initiation test. (See also
Ini¬tiating Efficiency of Primary Explosives by Sand Test.) Refs:
I)US BurMinesTechPaper 125(1916) 2)US BurMines Rl 2558(1923)
2a)H.Kast & A.Haid, SS 18, 166(1924) DUS BurMines RI
3039(1930) 4)US BurMinesBull 346, (1930,109 13 5) L.V.Clark,
IEC 25, 664 & 1387(1933)6) OSRD Repts 803 & 804 (1942),24 7 7)
Davis(1943),422 3 8)Perez Ara (1945),124 9) PATR 1401,Rev
1(1950),7 12 9)TM 9 1910 (1955),60 10) PATR 1740,Rev 1(1958)

Send Test for Detonators. See initiating Efficiency of Detonators by
Miniature Cartridge Test and also under Initiating Efficiency of
Primary Explosives by Sand Test

*According to W.R.Tomlinson, Jr, formerly of PicArsD sand test
det "energy' I rather than brisance.

200 Gram Sand Test
TNT at 48 Grams = 100% you can do the math.
[Veltx No. 448 = 138% TNT]

[Ballistic Mortar and Trauzl TNT = 100%
Except PLX 95/5 where the Trauzl value uses
PA as 100%]

Amatol 80/20 ........................ 35.5 ...BM 130 Trauzl 123
.......60/40 .........................42.5 ...BM 128
.......50/50 .........................42.5 ...BM 124
Ammonal (AN 22 TNT 67 Al 11) .........47.8 ...BM 122
Ammonium nitrate ......................nil ...BM 56
Ammonium perchlorate ..................6.0
Baratol ..............................26.8
Baranol ..............................39.8 ...BM 96
Black powder ..........................8 .....BM 50 Trauzl 10
BTTN (liquid) ........................48.6
Composition A-3 ......................51.5 ...BM 135
............B ........................54.0 ...BM 133 Trauzl 130
............C ........................46.5 ...BM 120
............C2 .......................47.5 ...BM 126
............C3 .......................53.1 ...BM 126 Trauzl 117
............C4 .......................55.7 ...BM 130
Copper chlorotetrazole ...............27.4
Cyanuric tyriazide ...................32.2
Cyclonite (RDX) ......................60.2 ...BM 150 Trauzl 135
Cyclotol
.........75/25 .......................____
.........70/30 .......................56.6 ...BM 135 ...BM 135
.........65/35 .......................55.4... BM 134 ...BM 134
.........60/40 .......................54.6 ...BM 133 ...BM 133
Cyclotrimethylene trinitrosamine .....59.2 ...BM 130 ...BM 130
DBX .................................146 .....BM 146 ...BM 146
DATNB ............................... 46.6 ...BM 100 ...BM 100
Diazondinitrophenol ..................47.5 ...BM 97 ....BM 97
DEGN (liquid) ........................42.2 ...BM 90 Trauzl ... 77
DNPF
DNPS
DNPTB
DNT ..................................19.3 ...BM...71 Trauzl 64
DPEHN ................................57.4 ...BM.142 Trauzl 128
LVD (Mil Low Velocity Dynamite) ......40.5 ...BM ...92
MVD ..................................52.6 ...BM ...122
EC Blank fire (Smokless powder) ......46.8
Ednatol 55/45 ........................49.4 ...BM 119 Trauzl 120
GTNB
Explosive D ..........................39.5 ...BM 99
GLTN (Liquid) ........................13.1
GDN (Liquid)
H-6 ..................................49.5 ...BM 135
Haleite ..............................52.3 ...BM 139 Trauzl 122
HBX-1 ................................48.1 ...BM 133
HBX-3 ................................44.9 ...BM 111
HEX-24 ...............................12.5
HEX-48 ...............................23.7
HNO ..................................52.1
beta-HMX .............................60.4 ...BM 150 Trauzl 145
HTA-3 ................................61.3 ...BM 120
Lead azide ...........................19.0 ...BM ___ Trauzl 39
LDNR .................................20
LDNR Basic ...........................15
Lead Styphnate .......................24 ....BM ___ Trauzl 40
Mannitol Hexanitrate .................68.5 ...BM ___ Trauzl 172
Mercuy Fulminate .....................23.4 ...BM ___ Trauzl 51
MTN (Liquid) .........................43.7 ...BM 136 Trauzl 140
Minol-2 ..............................____ ...BM 143 Trauzl 165
MOX-1 ................................10.6
MOX-2B ...............................11.5
MOX-3B ...............................33.2
MOX-4B ...............................33.6
MOX-6B ...............................10.8
Nitrocellulose 12.6% N ...............45.0
...............14.14% N ..............52.3
Nitroglycerin (Liquid) ...............51.5 ...BM 140 Trauzl 181
Nitroguanidine .......................36.0 ...BM 104 Trauzl 101
NIBTN (Liquid) .......................28
NSX ..................................39.5
Octol 70/30 ..........................58.4 ...BM 115
......75/25 ..........................62.1 ...BM 116
PB-RDX
PETRIN
Pentolite 50/50 ......................55.6 ...BM 126 Trauzl 122
..........10/90 ......................49.5
PETN .................................62.7 ...BM 145 Trauzl 173
TNA ..................................48.1 ...BM 100 Trauzl 107
Picratol .............................45.0 ...BM 100
Picric Acid ..........................48.5 ...BM 112 Trauzl 101
PIPE .................................41.6
Plumatol .............................32.4
PLX (Liquid) ..........................8.1
........95/5 ........50.6 ...BM 134 Trauzl *PA* .............................................................127
KDNBF .................................44.8
PT.....................................54.8 ...BM 132
PTX-2 .................................56.9 ...BM 138
PVA-4 .................................58.5
PVN ...................................49.9
RIPE ..................................40.1 ...BM 118
Silver Azide ..........................18.9 ...BM ___ Trauzl 88
Tetracene .............................28.0 ...BM ___ Trauzl 61
TNC ...................................41.3
TNO ...................................16.3
Tetryl ................................54.2 ...BM 130 Trauzl 125
Tetrytol 80/20 ........................54.0
........75/25 .........................53.7 ...BM 122
........70/30 .........................53.2 ...BM 120
........65/35 .........................52.6
TNT ...................................48.0 ...BM 100 Trauzl 100
Torpex ................................59.5 ...BM 138 Trauzl 164
TATNB .................................42.9
TEGN (Liquid) .........................14.7
Trimonite .............................44.2
TNETB .................................____ ...BM 136
Trinnitro Triazidobenzene .............____ ...BM __ Trauzl 90
TPEON .................................58.9
Tritonal 80/20 ........................____ ...BM 124 Trauzl 125
Veltex No. 448 ........................66.4

quicksilver - 27-7-2010 at 12:21

Frankly, I once attempted making a friction Pendulum apparatus & .....it wasn't my best work.
The real problem is that as contact surface increases so does friction input; to make sure one's sample receives contact that area needs to be about a square centimeter. But build up that contact space and the results are thrown.
I saw a few picture of devices used by the USBoM, another from a private "powder company", etc. They simply don't get close enough to see how they solve that contact area problem.

The Trauzl blocks I have seen appeared to be 1Kg as a 4"x4" cube with a 6mm hole. I hefted it and it seemed like 2lbs +. However I once saw a picture of one with a larger hole (it did appear 4x4 however). The lead should be pure; if it has tin or other elements the results will be thrown off & I don't know if it will expand without tearing or fragmenting. Making a mold for one would be pretty simple with 5 plates, some "C" clamps, and some "mold release" from hand swedging home-made bullets.

An impact test would be the easiest. A track for a weight (it's also been 1Kg TTBoMK) to slide down - could be rigged up pretty easily; the only challenge would be the actual impact surface....Too small or too spread out & you tweak the results. There would need to be one standardized contact surface area & I have not read what that is exactly. Pictures do not come close enough to the base area to make a determination.

edit:

Wizard - if you ever get any info on the above I would seriously appreciate it. I have not found contact surface area (size) for impact testing nor have I found contact design for friction (I have found that it was one cm however). I checked U.S. Bureau of Mines, Weaver, Federoff, Urbanski,etc (the usual).

[Edited on 27-7-2010 by quicksilver]

The WiZard is In - 27-7-2010 at 13:51

I A bit different perhaps, but I was just lately reading an old popular science magazine article about Guncotton(from around 1900), and it said that the navy scientists found that dry compressed Guncotton could be initiated (if under perfectly optimized conditions) with a mere 2.7 grains(~0.175g) of Mercury Fulminate. In actually practice however they found it most practical, all things considered to use something like 35grains(~2.27g) Mercury Fulminate. This is without doubt a huge excess. It does seem to show that they were thinking along the same lines as Rosco though.

"Wet gun cotton is not affected by percussion and can be
detonated only by the detonation of an amount of dry
guncotton bearing a certain ratio to the weight of wet
gun cotton employed. Its explosive effect is much greater
than that of dry gun cotton."

Compressed Gun Cotton for Military Use.
Translated from the German of Max von Föster
With An Introduction on Modern Gun Cotton
Its Manufacture, Properties and Analysis
By Lieut. John P. Wisser U.S.A.
New York: Van Nostrand, Publisher
1886

And I expect other refs. And Good-grief - another book I
own that is now available @ google.com/books!

Byda Them Brits used compressed gun cotton in WW II for demolition charges.

grndpndr - 27-7-2010 at 14:44

I always sort of wondered if putting Al powder in AN based explosives was kind of a waste because of the low heat of detonation. Maybe the ones with high concentrations of Nitric Esters or Nitrated Aromatics would get much more potential out of the Al powder.

Anyway here is a close(r) up picture of the hole the 2g of TNP made(2g TNP compound cap #1). Does anyone know if this seems like a reasonable amount of damage for 2g of TNP? It seems a little wimpy. Anyone with first hand experience, your opinion would be valued.

[Edited on 26-7-2010 by Hennig Brand]

If your cap was sitting with its end against the sheet metal it should have made a clean cut similar to a hole punch slightly larger in dia. than the det. Looks like the TNP failed to detonate.Pressing the primarys properly?

[Edited on 27-7-2010 by grndpndr]

[Edited on 27-7-2010 by grndpndr]

The WiZard is In - 27-7-2010 at 16:08

An impact test would be the easiest. A track for a weight (it's also been 1Kg TTBoMK) to slide down - could be rigged up pretty easily; the only challenge would be the actual impact surface....Too small or too spread out & you tweak the results. There would need to be one standardized contact surface area & I have not read what that is exactly. Pictures do not come close enough to the base area to make a determination.

Wizard - if you ever get any info on the above I would seriously appreciate it. I have not found contact surface area (size) for impact testing nor have I found contact design for friction (I have found that it was one cm however). I checked U.S. Bureau of Mines, Weaver, Federoff, Urbanski,etc (the usual).

Here is something to keep you busy while I compile some
better info.

Title: Evaluation of Test Methods for Pyrotechnic Hazard Classification.
Personal Author: Wilcox, Wayne R
Corporate Author: GENERAL ELECTRIC CO BAY SAINT LOUIS MS ENGINEERING AND SCIEN...
Source Code: 409145
Page Count: 160 page(s)
AD Number: ADB004208
Report Date: 01 MAR 1975
Distribution Code: 01 - APPROVED FOR PUBLIC RELEASE
Report Classification: U - Unclassified
Collection: Technical Reports

http://tinyurl.com/2b6t9dc

Hennig Brand - 27-7-2010 at 16:32

@Grndpndr
All caps where laid on their side on the barrel. Not a proper test probably, just for fun really. My endcaps are wood and epoxy so the end test wouldn't work right I don't think. The second comp cap with 2g TNP went high order for sure. It was a hell of alot of noise for only 2g of explosive, and the damage to the steel was not too far behind what the 1.5g of ErTeN did. I am pressing with a vice and dowel, just like you. I measured/estimated that I am getting compaction to ~1.5g/cc. I saw figures for Lead Azide and Mercury Fulminate and for best performance I think the densities were much higher. Honestly it is a little hard to tell exactly how densely the Lead Azide was pressed. I used about the same amount of pressure as I did for the TNP if that tells you anything. Both MF and LA are very dense materials anyway I guess, must be a lot easier to press I would think.

Oh yeah, I think I used "concussion" where I should have used "percussion" a few posts ago.

BTW, does anyone here have any personal experience with Basic Lead Picrate, in particular its sensitivity to percussion. Any experiences or info welcome. All I know is the stuff I made makes great firecrackers, but I don't know if I'd trust it to initiate dynamite.

[Edited on 28-7-2010 by Hennig Brand]

The WiZard is In - 27-7-2010 at 16:35

Wizard - if you ever get any info on the above I would seriously appreciate it. I have not found contact surface area (size) for impact testing nor have I found contact design for friction (I have found that it was one cm however). I checked U.S. Bureau of Mines, Weaver, Federoff, Urbanski,etc (the usual).

Muhamed Sudc'eska
Test Methods for Explosives
Springer 1995

Mentions and has a drawing of the BAM (FDR) apparatus.
You can read parts of the book @ google.books.com,
however, the drawing is missing (I own a hard copy).
La machine is made by Julius Peters KH, Berlin. Google
them.

He sez that the American US Bureau of Mines and ERL apparatus
are covered by MIL-STD-650, methods T 511.1 and T 505.1.
I have not been able to find this Military Standard in the usual
places. Google it.

The WiZard is In - 27-7-2010 at 16:51

Have stumbled upon the attached PDF

LLNL Small Scale Friction Sensitivity (BAM) Test

Hennig Brand - 27-7-2010 at 16:56

Wizard, thanks for pointing out that book, "Compressed Gun Cotton for Military use". I just downloaded it, going to give it a read. I have been playing with Guncotton a bit lately. Wrapped up tight in some tin foil it makes a pretty good bang on an anvil. A lot easier to set off this way than my TNP.

BTW just Google "Picric Acid and low order detonation" and lots of stuff comes up. Apparently even in large shells if not properly overdriven you will often get a low order detonation of the entire shell. Were you just messing with me a little bit Quicksilver? It must be nice to have a good memory though, one of these days I am going to forget how to get home(ok, not that bad maybe).

[Edited on 28-7-2010 by Hennig Brand]

quicksilver - 28-7-2010 at 05:13

Have stumbled upon the attached PDF

LLNL Small Scale Friction Sensitivity (BAM) Test

There was an attachment but (?) It didn't hook up.

However: thank you for checking into this. It's not easy to find this info. I usually can get a great deal of material but this has been a tough one.

Blasty - 28-7-2010 at 05:19

BTW, does anyone here have any personal experience with Basic Lead Picrate, in particular its sensitivity to percussion. Any experiences or info welcome. All I know is the stuff I made makes great firecrackers, but I don't know if I'd trust it to initiate dynamite.

By themselves picrates probably would not be reliable initiators of dynamites (mind you, apparently even black powder charges have been used successfully to detonate some types of dynamite, but not reliably.) However, mixtures of picrates with potassium chlorate and other chemicals have apparently been used to detonate dynamites reliably (according to the inventor's claims.) The earliest proposer of such a method seems to have been Prudencio Castellanos, who used such mixtures to detonate both commercial dynamites as well as those of his own invention:

http://www.google.com/patents?id=2C9tAAAAEBAJ&printsec=a...

This is an interesting topic for which there appears to be rather little information. As Castellanos points out, his preferred percussive mixture was that of Designoble & Casthelaz:

http://www.google.com/patents?id=oqoAAAAAEBAJ&printsec=a...

The problem facing anyone who wants to put Castellanos' claims to the test is that his patent (or that of Designoble and Casthelaz, for that matter) does not address the issue of how are these chemicals mixed without blowing up in your face. Mixing potassium chlorate and potassium ferrocyanide is already scary enough, needless to say adding a picrate to the mix. According to the Designoble & Casthelaz patent, these mixtures are made pretty much like black powder, but no further details are given. It goes without saying that the chemicals must have been worked wet, then granulated and allowed to dry.

[Edited on 28-7-2010 by Blasty]

quicksilver - 28-7-2010 at 05:21

BTW just Google "Picric Acid and low order detonation" and lots of stuff comes up. Apparently even in large shells if not properly overdriven you will often get a low order detonation of the entire shell. Were you just messing with me a little bit Quicksilver? It must be nice to have a good memory though, one of these days I am going to forget how to get home(ok, not that bad maybe).

[Edited on 28-7-2010 by Hennig Brand]

No: honestly I haven't googled it. Just from reading, I simply thought of NC (w/ low order det) and frankly was curious.

I was thinking back when or if I did use TNP and was confusing it with TATB & TNA. It was an error on my part of not searching (& maybe having a senior moment there).

The WiZard is In - 28-7-2010 at 06:27

Yes 3X.

Try this

http://www.osti.gov/bridge/purl.cover.jsp?purl=/273797-vzcRJ...

The most interesting thing in it is that when
diaminepropane diperchlorate was tested it broke the ceramic plate.

quicksilver - 28-7-2010 at 07:28

Excellent, Thank you.

"when diaminepropane diperchlorate was tested it broke the ceramic plate."

I think an "unknown" was: did this occur from a gradual weakening; a progressive deterioration or from the energy of the material itself?

edit:

Testing is such a detailed oriented aspect of science that (IMO) it takes a very detailed oriented mind to produce a paper with all bases covered. ...And then the reader is occasionally overwhelmed by the detail that unless acute organization is inherent within the design, some elements of the tests can be hidden from all but the most intricate search.

ps:
....need a paid subscription (of course...sigh) to snag MIL-STD-650. I once has access to the Library of Congress and didn't take advantage of it when I had it. That was a serious blunder I deeply regret. I could have gotten some of the most unique items imaginable & I took it for granted.....

[Edited on 28-7-2010 by quicksilver]

The WiZard is In - 28-7-2010 at 07:42

The Trauzl blocks I have seen appeared to be 1Kg as a 4"x4" cube with a 6mm hole. I hefted it and it seemed like 2lbs +. However I once saw a picture of one with a larger hole (it did appear 4x4 however). The lead should be pure; if it has tin or other elements the results will be thrown off & I don't know if it will expand without tearing or fragmenting. Making a mold for one would be pretty simple with 5 plates, some "C" clamps, and some "mold release" from hand swedging home-made bullets.

It could be any size, however, it dobe required that it is
large enough that the effect of the primer is not obvious.

The WiZard is In - 28-7-2010 at 11:20

I believe the last person to have any personal experience with
basic lead picrate was killed in an accidental explosion last week.

I do have a copy of Capt. E. de W. S. Colver's 1918, 830 page
opus High Explosives.

He notes —

Lead picrate. Lead picrate exist both as a neutral and basic salt.
Neutral lead picrate, [C6H2(NO2)3O]2 Pb.H2O is obtained by
double decomposition of an alkaline picrate with lead acetate
in dilute solution. Of all the picrates, this salt is the most
explosive and most sensitive to percussion.

[C6H2(NO2)3O]2 Pb.H2O This yellow powder
explodes violently at 270o. This salt is, further, extremely
sensitive to friction and percussion in contradistinction to the
other picrates.

Captain Colver cites Will [Zeitschr. F. Schiess. U. Sprengst. 1906,
page 212] column 1. **
Urbanski column 2. Provide the following falling weight test values:

Picric acid 35 to 90 cm. ——-
Lead picrate 5 cm. 2 cm. 2 kg.
Fe III anhydrous —— 40 cm. 2 kg.
Iron 7 cm.
Copper 7 cm. 30 cm.
Zink 60 cm. no explosion
Sodium 80 cm.
anhydrous —- 19 cm.
Ammonium 80 cm.
Manganese —- 60 cm. 10 kg.
Chromium — 28 cm. 2 kg.
Nickel —- 40 cm. 10 kg.
Strontium — 17 cm. 2 kg.
Barium —- 2.5 cm. 2 kg.

Guttmann notes that the French ca. 1869 used potassium picrate and potassium
nitrate in powders for use in torpedoes, shells, as cannon and rifle powder.
“Designolle powders.” He notes (his book was published 1895) that “Designolle
powders have been abandoned.”

1894 VJ Feeny patented a mixture of:

ammonium chromate
potassium or sodium picrate &
ammonium picrate

As an explosive!!

There are a number of other picrates:
Aluminum
Cadmium
Cobalt
Lithium
Mercury
Potassium
Silver
Double salts

Esters of picric acid:
Trinitroanisol
Trinitrophenetol (ethyl picrate)
Phenyl picrate
Nitrophenyl picrate
Acetyl picrate

Other picrates/compounds of picric acid:
Guanidine picrate
Sodium peroxide derivative of picric acid
Benzene picrate
Napthalene picrate
Aniline picrate
Antracene picrate
Phenanthrene picrate
Phenol picrate
Acetophenone picrate
Picramic acid

Other than picric acid and ammonium picrate none of the others has found use.
Indeed even picric acid has been replaced by TNT &c. Ammonium picrate
“Explosive D” is used in armor piercing shells for ships gunnery. However, as
“guns” on ships are rapidly disappearing I would think the number of shells in
stock is adequate to meet demand.

** I own 3-volumes of this publication, however, not this year.
It dobe in German - bad. Script - terrible!

An Explosion Of An Appalling Character.

Report on the Circumstances attending a Fire and Explosion at
Messrs. Roberts, Dale & Co.'s Chemical Works, Cornbrook, Manchester,.
Gov. Rep. No. lxxxi.
Colonel V. D. Majendie, C.B.
In:—The Journal of the Society of Chemical Industry. Vol. VI. No. 12. December
31, 1887

THIS exhaustive report shows that the articles manufactured on the side of the
works where the explosion occurred, were picric acid, nitrate of lead, nitric acid,
hydrochloric acid (nitre cake and salt cake), tin crystals, tin solutions, nitrate of
iron, nitrate of copper, aurin, Manchester brown, Manchester yellow, lakes for
paper stainers and emerald green. Such raw materials as carbolic acid, sulphuric
acid and litharge, the litharge being used for making nitrate of lead, were all
present, the latter salt in very considerable quantity; some nitrate of strontium
was also present.

A fire commenced the catastrophe, this breaking out at or near the stove used
for drying the picric acid. The fire spread quickly, and in five or six minutes an
explosion followed, but not one of an alarming character. This explosion came
from the site of the picric acid stove as nearly as it can be located. It was
followed in something under a minute by a second explosion of an appalling
character, and attended with disastrous results in the shape of damage. One life
was lost.

There is little doubt that the fire was caused by the carelessness of a workman,
who was smoking. Several theories are advanced to explain the first and lesser
explosion, but the second, which was so disastrous, was in all probability due to
the blazing and molten picric acid coming in contact with the litharge placed in
close proximity and with the nitrate of lead and nitrate of strontium. It would at
once combine with these and form fearful explosives. Picric acid alone can
scarcely be called an explosive, but if it comes in contact even with plaster or
lime, it forms a picrate of high explosive character, and it is shown that picric acid
mixed with a little litharge in the cold, produces a mixture which explodes much
more readily than picric acid alone.

Finally, the precaution is urged, that in the manufacture of picric acid the
separation of the acid from all other substances or ingredients, contact with
which would be likely to produce under favorable conditions a picrate or
explosive mixture should be carefully seen to.

"At present picric acid and picrates appear to fall within the category of
'explosives,' and to be subject to the Explosives Act, 1875, only when they are '
used ' or manufactured with a view to produce a practical effect by explosion or
pyrotechnic effect. "

" In view of the present disaster," Colonel Majendie proceeds, "and of the results
of my experiments it will be a matter for careful consideration whether it is not
necessary in the interests of public safety to take advantage of the powers
conferred by the 104th section of the Explosives Act, 1875, and to extend the
definition of explosive to picric acid and all picrates, for whatever purposes
manufactured, and to apply the same provisions of the Act, subject to such
exceptions, limitations and restrictions as may appear reasonable. This point,
however, is one which, in the interests of the trade, as of the public, demands
the fullest and most careful consideration."

As to the storage together and in close proximity of the several substances which
resulted in the formation of such fearful explosives, Colonel Majendie stigmatises
it as the result of negligence.—W. S.

Curious —

By the action of ammonium sulphide on picric acid, salts of
picraminic acid are formed, and these are explosive if heated
rapidly. Lead picrate, one of the most dangerous salts of the
picrate series, is used in the silk industry; it renders the fabric
liable to spontaneous ignition.

[Weighted silk - the heaver silk was felt to be - the higher its
selling price. Though it may have been a dye.]

quicksilver - 28-7-2010 at 13:20

-={ Please excuse OT remarks}=-

Wizard:

Those were the size I actually saw and held. When I saw a picture in a technical paper it looked the same as well. But that's not a big deal....

What I did find was hard copy of frictional (& impact) studies from the US Bureau of Mines (if you have a source on the web please let me know because I have looked and looked and never found the real collection. I always had to send away for the paper copies.) The one that's pretty interesting is USBoM "Frictional Studies" Tech. Paper 234, 1919. In it there are studies on friction testing, chlorates/perchlorates, and sensitivities to copper. MANY of the tech papers in the 200's are interesting from an energetic materials perspective.
The copper stuff is very intriguing. There is also an attachment of the commercial production of Cuprous acetylide and Cupric acetylide! The latter being usable in electric dets; the former being a curiosity that just too sensitive to make more than about 100mg. Pointed was a supposed agenda of not being forced to use copper (I) salts (CuO2) but yet copper (II) salts (like copper sulfate. Therefore it would be damn simple to make with copper sulfate, ammonia, acetylene & normal caution.

The correct material will be a deep orange-red: the cuprous material will be a black sludge which is just too sensitive. They use both chlorate and the copper example to demonstrate sensitivity. Cupric (or copper acetylide) is the old fashion bridge-wire coating and the friction ignition, "pull wire" used in various pull ignitors. The cuprous acetylide is not a touch explosive but not predictable enough to have a great deal of use aside from "throw-down popper toys.
If I had a way to scan it I would have posted it. I really enjoy the "Mines" papers. It's worthy of trying to find the USBoM collection.
NOTE: I checked the US Dept. of the Interior and they DO have some USBoM material (they did a few years back) but none of the old stuff.

The WiZard is In - 28-7-2010 at 16:36

What I did find was hard copy of frictional (& impact) studies from the US Bureau of Mines (if you have a source on the web please let me know because I have looked and looked and never found the real collection. I always had to send away for the paper copies.) The one that's pretty interesting is USBoM "Frictional Studies" Tech. Paper 234, 1919. In it there are studies on friction testing, chlorates/perchlorates, and sensitivities to copper. MANY of the tech papers in the 200's are interesting from an energetic materials perspective.

I have a not very good photocopy I made years ago. If you are
in the US of A, Depository Libraries have copies of Bureau
of Mines and other publications supplied to them by the Gov.,
assuming they have not de-acquisitioned them!

Or ask the Inter-library Loan librarian at your library to obtain a copy for you.

I recommend Bureau of Mines publication Bulletin 346,
Physical Testing of Explosives. 1931 146 pages.

I have a photocopy. Try this

http://digital.library.unt.edu/ark:/67531/metadc12516/

You maybe able to DL it as PDF, my request is pending.

Hennig Brand - 28-7-2010 at 17:58

Thanks for all the info guys.

Didn't mean to give you a hard time Quicksilver, I am well aware that many of you guys know more than I, which is one of the reasons I really thought you were messing with me alittle(I was not upset by it though). You say you may of had a senior moment, I had you pegged as a smart younger adult, not a smart older adult(I assume you are implying that you are older with the senior moment thing). I'm not a kid, but I'm not old either, young adult I guess. As you can see I do have an adolescent enthusiasm for anything related to fire.

I made what I think is Basic Lead Picrate with the method in "the preparatory manual of explosives", I know it is not the best reference but it does have some interesting things in it. First put TNP in solution, use NaOH to convert to sodium picrate in basic solution, then add Pb(NO3)2 solution gradually+heat and stir, filter, wash, etc.(general summary I think) I wonder what I may have done wrong, mine is explosive as hell to a flame, but pretty damn insensitive to percussion. Maybe being the monohydrate makes it alot more insensitive? What would be the result if my TNP was alittle less than pure? I thought(not knowing for sure) that I might have been giving the impurities the slip when making the Picrate, but maybe not.

Blasty - 28-7-2010 at 21:38

I made what I think is Basic Lead Picrate with the method in "the preparatory manual of explosives", I know it is not the best reference but it does have some interesting things in it. First put TNP in solution, use NaOH to convert to sodium picrate in basic solution, then add Pb(NO3)2 solution gradually+heat and stir, filter, wash, etc.(general summary I think) I wonder what I may have done wrong, mine is explosive as hell to a flame, but pretty damn insensitive to percussion. Maybe being the monohydrate makes it alot more insensitive? What would be the result if my TNP was alittle less than pure? I thought(not knowing for sure) that I might have been giving the impurities the slip when making the Picrate, but maybe not.

At the bottom of that same page where the preparation of lead picrate is given, there's a section entitled "Lead picrate initiating mixture". It is similar in general composition to the ones used by Castellanos to detonate dynamites back in the 1870s (picrate + chlorate + other chemicals.) The procedure looks fairly simple: the materials are worked wet, packed into "pellets" and allowed to dry (however, Castellanos says that such mixtures work better in loose granules, not pressed.) Since you seem to be able to perform such "noisy" experiments without much trouble, have you thought about trying it? (in a smaller scale than stated in the book would be wise) The author of that book claims it can work with RDX (yes, we all know he's not always reliable, but maybe he actually tested this.)

quicksilver - 29-7-2010 at 05:32

I recommend Bureau of Mines publication Bulletin 346,
Physical Testing of Explosives. 1931 146 pages.

I have a photocopy. Try this

http://digital.library.unt.edu/ark:/67531/metadc12516/

You maybe able to DL it as PDF, my request is pending.

Yea: I'm in the US. And that was a good tip. (I snagged it as a PDF) - Thank you.
Usually universities are tough to access. I had a damn hard time with our "local" one.
When my wife was working on her degree I was able to get a library card & it was "kid in a candy store" time.
I would love to see a thread in "REFERENCES" on sources people use to find materials. Because some people come up with obscure sources that I would NEVER have thought of.

quicksilver - 29-7-2010 at 05:56

Thanks for all the info guys.

Didn't mean to give you a hard time Quicksilver, I am well aware that many of you guys know more than I, which is one of the reasons I really thought you were messing with me alittle(I was not upset by it though). You say you may of had a senior moment, I had you pegged as a smart younger adult, not a smart older adult(I assume you are implying that you are older with the senior moment thing). I'm not a kid, but I'm not old either, young adult I guess. As you can see I do have an adolescent enthusiasm for anything related to fire.

I made what I think is Basic Lead Picrate with the method in "the preparatory manual of explosives", I know it is not the best reference but it does have some interesting things in it. First put TNP in solution, use NaOH to convert to sodium picrate in basic solution, then add Pb(NO3)2 solution gradually+heat and stir, filter, wash, etc.(general summary I think) I wonder what I may have done wrong, mine is explosive as hell to a flame, but pretty damn insensitive to percussion. Maybe being the monohydrate makes it alot more insensitive? What would be the result if my TNP was alittle less than pure? I thought(not knowing for sure) that I might have been giving the impurities the slip when making the Picrate, but maybe not.

HA.....I'm on the deeper side of 50! - getting close to social security age (which God willing I will see a few dimes from). I have had a very eclectic career in diverse vocations. I also was one of those guys who "lived in school". And honestly, I wouldn't fuck with you; it's too serious a subject. I just made an honest boo-boo. When you get a bit older, the second thing that goes is the memory.....

There were some in depth discussions (back about '06) about Normal & Basic Lead Picrate & most people pretty much agree that unless certain steps are taken, it's not a quality initiator: but it could be workable.

Legard (Preparatory Manual of Explos) does have some interesting stuff, it's just his citations suck. And therein lies the problem. If something interests you; you're generally stuck because his damn patent numbers are often incorrect.

Remember that many materials have a place in commercial production. Primers for firearms need to produce a strong flame spit, fuse-caps need to have a flame sensitive contact material, stab detonators need to have a very friction sensitive primary, & on and on.... Too often we examine a primary from the standpoint of "will it drive an explosive train?" when in fact, it may have more utility than just that alone.
Both Lead Picrate & lead styphnate will initiate a secondary; they just need a bit more mass than an azide but they certainly have utility.
If I could have found that old thread, the contributors had a great deal to say about the flexibility of picrates. It's worth hunting for but it's way back there.

edit:

And thank you for the complement but remember, anyone can make a mistake - so it's always a good idea to check info from internet conversations for veracity, accuracy in detail, & any omission.
I remember long discussions on alt.engineering explosives (UseNet) and some of the truly professional folks there occasionally made a typo or forgot something; even those who were truly gifted professionals. This is much too dangerous a hobby not to take anything with a grain of salt. If the guy gives citations for his perspective or has a reprint of an article, you're on much stronger ground but he could still misinterpret the idiosyncrasies of the subject. Some of the people I most respect have made an occasional omission or honest mistake.
I have really studied Legard's 2nd & 3rd edition & as much as I get down his case about the material, he's certainly someone who put some work into his books. ...But I would always double check the lab prior to getting into anything. It could have been his editor or he could have basically made a mistake which went over the heads of his proof-readers. Either way, his stuff isn't worthless, it's just a potential minefield - IF you don't double check. Remember he had the "copper fulminate" entry which was totally incorrect (& which I have always wondered about).
I believe it's vital that we as a group care that the information be as accurate as possible and honestly care for the safety of the other contributors.

[Edited on 29-7-2010 by quicksilver]

Hennig Brand - 29-7-2010 at 09:43

Thanks for all the good advice, and information. I am going to try and track down some of the older picrate thread stuff.

Your still a young fellow yet, my Dad is getting close to 70.

Different peoples comprehension and interpretation of what they read or saw, even in a good reference, can vary greatly can't it. I'm always getting new, or expanded meaning from things I am reading again for more than the second time sometimes.

The WiZard is In - 29-7-2010 at 11:27

Quote: Originally posted by Blasty

The problem facing anyone who wants to put Castellanos' claims to the test is that his patent (or that of Designoble and Casthelaz, for that matter) does not address the issue of how are these chemicals mixed without blowing up in your face. Mixing potassium chlorate and potassium ferrocyanide is already scary enough, needless to say adding a picrate to the mix. According to the Designoble & Casthelaz patent, these mixtures are made pretty much like black powder, but no further details are given. It goes without saying that the chemicals must have been worked wet, then granulated and allowed to dry.

potassium chlorate and potassium ferrocyanide is already scary

Best mixed the same way porcupines make love....

Augrendre's White Powder [White Gunpowder]

K ferrocyanide - K chlorate - Sugar

...The respective quantities of the ingredients are then weighed
off, poured upon a sheet of paper, and intimately mixed with
the fingers or a feather......

Brannt-Wahl
Techno-Chemical Receipt Book
Henry Carey Baird & CO
Philadelphia 1917

{Maybe available from Google books.}

A Dictionary of Explosives
(Second Edition)
Lieut.-Col J. P. Cundill, R.A.
Entirely Re-arranged and Brought Up To Date
by Captain J. H. Thomson, R.A.
London HMSO 1895

I own an original it has been reprinted, or can be DL'd
from Google Books. Also Daniel's Dictionaire Des
Matières Explosives

9. IV2 Acme Powder, invented by Mr. Liardet, consists of a mixture of
picric acid, chlorate of potash, nitrate of potash, and tar. This explosive
proved fatal to its inventor. (Spec. No. 19,391, 23.10.1893)

[Mr. Liardet's powder is gon'a be a tough sell!]

Hennig Brand - 29-7-2010 at 12:37

Sorry for my sort of gratuitous use of pictures, but I think this is maybe more the picture Quicksilver was looking for when he asked for a picture of the metal tears. Shot taken down the end of the barrel with the top off(barrel stood up).

Blasty, thanks for pointing out the Lead Picrate composition stuff, and the Wizard for elaborating. Porcupines in coitus, that is funny to think about.

[Edited on 29-7-2010 by Hennig Brand]

Barrel blasting (interior shot).jpg - 169kB

Barrel blasting (interior shot).jpg - 169kB

Three Basic Igniters

Rosco Bodine - 30-7-2010 at 01:59

Igniters based on derivatives of lead picrate

US1478429 See example 1 for synthesis of basic lead picrate which is the parent compound for the two more advanced derivative compounds below. IIRC this compound is a brick red orange color and extremely fine granulation crystals.

US2175249 See example 2 for one of the best "first fire"
low order detonating flash igniters , a superbly useful
and easily made compound , lead nitrato-bis basic lead picrate. The color of this one is bright yellow a bit coarser crystals.

US3293091 See example 4 for a similarly useful different compound, basic lead picrate - lead nitrate - lead chlorate tertiary clathrate, bright yellow crystals. As an interesting further note, a 4/16 azo-clathrate derivative can be made from this parent compound, and is a more powerful azo-clathrate than the 4/12 non-chlorate variant already described. The 4/16 azo-clathrate is experimental but a sample appears stable after several years of adverse storage conditions.

All of these compounds are excellent flash igniters for use as "first fire" compositions as a loose powder priming for fuse or electric ignition and readily undergo DDT low order in sub tenth gram amounts. All these materials are free flowing dense fine mesh crystals, not hygroscopic, and appear to be perfectly storage stable even at moderately elevated temperatures.

Attachment: US1478429_US2175249_US3293091.pdf (1.4MB)
This file has been downloaded 1304 times

In my opinion Legards books are trash. Caveat emptor.

[Edited on 30-7-2010 by Rosco Bodine]

The WiZard is In - 30-7-2010 at 05:42

Wizard:

Those were the size I actually saw and held. When I saw a picture in a technical paper it looked the same as well. But that's not a big deal.....

Your memory works, they were Small Trauzel Lead Blocks.

These blocks are used for testing detonators and are cylindrical
100mm. in height, and 100mm, in diameter. A hole is bored
in the block the exact diameter of the detonator and of such
depth that the top of the detonator is flush with the top of
the block. The tests are reported on the same form as that
used for reporting Trauzel lead blocks.

Munroe and Tiffany
Physical Testing of Explosives at the Bureau of Mines Explosives
Experiment Station Bruceton, PA.
Bulletin 346
1931

quicksilver - 30-7-2010 at 05:55

The "flower-petal" tear in the metal has a certain significance re: the proximity. power, and speed of the det. I really have to find the information related to this as it's tucked away but aside from a forensics aspect, there is a variety of information that witness-plate punctures provide (the barrel's a damn big witness plate).

For those who do not have it, Roscoe posted the classic Dec 20 "Clathrate" patent, which may have enormous value to anyone who is seriously interested in primaries (US329091), It's this patent that is the basis of some great work & extremely interesting material.

US1478429 makes reference to nitrated cresol as a building block. Cresol is (IMO) much easier to nitrate than phenol but very difficult to obtain, which is a shame because there are quite a few things that employ it. The reagent-grade material is quite expensive & unnecessary, yet I have not found a source for anything but high-end cresol. I would really appreciate it if anyone who does know more about where to obtain same would post their experiences. {TNC is very close to TMP in a variety of tests.}

EDIT:
Re: those lead blocks, I wish I could post a picture because the one that I had looked like it fit a detonator. but I've read about ones that could be used for free materiel w/ tamping so the hole HAD to be bigger than 6mm.
I'm fairly sure a really accurate example could be home-made for just a few dollars.

[Edited on 30-7-2010 by quicksilver]

The WiZard is In - 30-7-2010 at 08:25

Re: those lead blocks, I wish I could post a picture because the one that I had looked like it fit a detonator. but I've read about ones that could be used for free materiel w/ tamping so the hole HAD to be bigger than 6mm.

I'm fairly sure a really accurate example could be home-made for just a few dollars.

[Edited on 30-7-2010 by quicksilver]

Sure, however, if one wanted to publish their results the lead
block would have to meet the current standard.

Occam would have approved of this :—

Drop and friction pendulum tests were designed to replace the old English Dupre tests. (Dr. August Dupre 1835-1908).

"A small quality of the explosive is spread on a large stone table and is struck a glancing blow
with a mallet; the explosive is thus subject to the combined effect of shock and friction. Use is made of two
sorts of mallets, one of rawhide and the other of beech wood, similar to those used by wood carvers. The
rawhide mallet weighs about 12 ounces and the wooden one about 11 1/2 ounces. The rawhide mallet is
more effective, especially with chlorate explosives. If the sample explodes in this test it is repeated using a
broomstick instead of the mallets. The broomstick is held on the stone at an angle of about 60o and a blow
is struck with its end, taking care that the movement of the stick is in the direction of its axis. If an
explosion is obtained in this way the test is repeated, the explosive being placed on a hard wooden table
instead of the stone one and, finally, if necessary, on a soft wooden table. If an explosive other than those
used for caps, detonators, etc., explodes even partly on softwood it is considered too sensitive for its use to
be authorized. Needless to say, the mallets, broomsticks, and tables must be clean." (Physical testing of
explosives. Bureau of Mines Bulletin 346. 1931)

See also :—

S. P Howell
Sensitiveness of Explosives to Frictional Impact
US Bureau of Mines Bulletin Technical Paper 234. 1919

http://tinyurl.com/27rh885

Hennig Brand - 30-7-2010 at 08:29

Rosco, what would be the consequence of not doing the addition slowly into the Lead Nitrate solution? I probably messed up the lab out of impatience and not fully understanding the process. I made the addition very quickly then heated for fifteen minutes or so to around 80C. Stirring was not what it should have been either. I didn't look at the product under a microscope but what I had looked more like a dense amorphous powder to the naked eye. It is very sensitive to flame(sort of flashes like Mercury Fulminate when lit in a tiny pile in the open). It is quite insensitive to percussion.

Here is a picture of about 12g of the material I made, I don't know if you can tell much by the picture.

Lead Picrate ~12g.jpg - 150kB

Trauzel on steroids

The WiZard is In - 30-7-2010 at 08:32

RELATIVE STRENGTH OF EXPLOSIVES

For finding the relative disruptive power of different explosives,
and thus enable the officers to apportion the amount of charge to
be used in testing, a modified form of the Trauzel lead-block
method was adopted Although this method has since been
superseded it will be of interest to briefly describe the process and
some of the experiments. The blocks in use at Woolwich were of
cylindrical shape 12 inches high bv 12 inches diameter, with an
axial hole drilled to a depth of 7 inches having a capacity of 5 fluid
ounces. In the early experiments the blocks were frequently
recast, but some results having brought suspicion upon the
accuracy of the tests it was decided to use only "virgin" lead blocks
for each test. When 1 ounce of No. 1 dynamite was fired in the
cavity, with stemming, the expansion of the cavity would be about
30 fluid ounces, as compared with an expansion of only 3 ounces
from the same weight of gunpowder, which made dynamite
appear ten times stronger than gunpowder. Experiments in other
directions having proved that the real proportion of power was
about 3 to 1, an examination of the block method led to the
adoption of placing a considerable weight over the charge to be
fired when gunpowder was being tested. Another of the lead
blocks, weighing 5 hundredweight, answered the purpose. This
placed over the orifice thoroughly confined the charge, and
brought out approximately fair results. With a high explosive the
effect would be brought out by the tamping of dry sand. In this
way were obtained the following figures, showing the relative
strength of different explosives by equal charges, and the weight
of equivalent charge required for the same amount of work done,
taking dynamite No. 1 at 100:

http://tinyurl.com/25wdp7m

The WiZard is In - 30-7-2010 at 08:42

RELATIVE STRENGTH OF EXPLOSIVES

http://tinyurl.com/25wdp7m

If'n you DL the 780 page PDF so you can print it out - this is PDF pages 340-356.

Has good photos (2) of the Bureau of Mines Friction Pendulum.

The WiZard is In - 30-7-2010 at 09:01

Re: those lead blocks, I wish I could post a picture because the one
that I had looked like it fit a detonator. but I've read about ones
that could be used for free materiel w/ tamping so the hole HAD to
be bigger than 6mm.

I'm fairly sure a really accurate example could be home-made for
just a few dollars.

Try - http://tinyurl.com/3y9x52m

Rosco Bodine - 30-7-2010 at 09:02

Rosco, what would be the consequence of not doing the addition slowly into the Lead Nitrate solution? I probably messed up the lab out of impatience and not fully understanding the process. I made the addition very quickly then heated for fifteen minutes or so to around 80C. Stirring was not what it should have been either. I didn't look at the product under a microscope but what I had looked more like a dense amorphous powder to the naked eye. It is very sensitive to flame(sort of flashes like Mercury Fulminate when lit in a tiny pile in the open). It is quite insensitive to percussion.

Here is a picture of about 12g of the material I made, I don't know if you can tell much by the picture.

You may have made what Legard thinks is basic lead picrate but believe me that is not basic lead picrate, so then you may safely assume that order of addition, temperature, dilution, and reaction rate are important variables in real actual chemistry done by real actual chemists and not just fiction novels having some dreamt up reaction scenarios written by assholes who are pretenders. If you want to make basic lead picrate then go by the method of the Friederich patent. If you want crap, follow the Legard wetdream and mental masturbation guidebook for chemist wannabees. (caveat emptor - translation provided)

What the bright yellow material gotten from the reverse order of addition could possibly be is a hydrated intermediate and/or possibly contaminated double salt. It may be possible to accomplish its conversion by long stirring it in very hot almost boiling water. The use of very hot water is in part necessary for decomposition (dehydration) of a hydrated intermediate which leads to the end product.

All of these basic lead picrate derivatives are made by a dropwise very slow addition into an excess of dilute and hot (95C works well) and vigorously well stirred lead nitrate solution, an hour is good as a kind of rule of thumb for the addition. By vigorous stirring that is meant "suspension" of the solids, not islands of solids accumulating on the bottom, but everything circulating in a vortex of liquid. If it takes a magnetic stirbar on the bottom and a propellor stirrer above or a prop making an orbital sweep, then that's what it takes. It isn't just mix A+B any old way and get C, but is a precise process. The basic lead picrate is the parent compound, and that can be gotten first and then gradually redissolved and reacted subsequently to form daughter compounds. That is the variation which I prefer and is allowable as a process refinement, but is more of a long way around than any shortcut. Actually there probably is no shortcut process for such low solubility reactants where the reaction has to be pushed with heat and dilution and efficient stirring. It isn't complicated really, it is just that the reaction conditions are quite specific.

[Edited on 31-7-2010 by Rosco Bodine]

Hennig Brand - 30-7-2010 at 09:32

I'll give the (long way)/(proper way) a run through and see if that works better. It most likely will, I am just a little unsure as to why. One thing I did learn is you don't think very highly of Legard, and I guess I can see why. I think his Lead Picrate synthesis is not that far off though. I am sure I messed it up. I will do it properly and get back to you.

Oh, I found a little immersion heater. I can control this with a light dimmer and use with an oil bath, together with my magnetic stirrer, to heat and stir. Should work well when making TNP as well.

BTW thanks for the nice patents.

edit:
Thanks for elaborating in you last post, appreciate it.

[Edited on 30-7-2010 by Hennig Brand]

Rosco Bodine - 30-7-2010 at 09:41

No problem. You try it the other way around and let your eyes tell you that something different is occurring and something very different in appearance
is also being the end product. Chemistry can be a real bitch about specific
conditions. And how well do I know that a lot of folks would argue about details which they may think make no difference and are of no consequence, when
there are subtleties involved in the reaction that are simply not recognized.
But as they say, the proof is in the pudding, or crystals in our case. You'll see the difference. Go very slowly and watch for the color shift and the change thresholds and you will see that bright yellow shift to orange brown right before your eyes. I promise you can visually discern the transition as a distinct change in appearance and viscosity also. The needle like felt fiber like bright yellow initial precipitate will transition to a darker orange brown compact crystalline material having much denser and reflective appearance.
It will be more like a dense fine sparkling orange brown sand than a fluffy yellow amorphous garbage.

[Edited on 30-7-2010 by Rosco Bodine]

quicksilver - 30-7-2010 at 10:08

@ Wizard:

Excellent hits: Thanks. I honestly appreciate it when you find material correlated to questions (because generally that means I don't have the resource or it's too damn buried).
I have bought books from Albris ( the book seller in the link) and was really happy with what they had and the way they described condition. I an going to see what they have from Vannoy Hartrog Manning, etc. IF you're ever going to buy, I recommend Albris. They are not the cheapest but I always get high quality from them (bindings aren't shit, etc) and they had the PATR as individual volumes from various libraries. - NOT as one $1000 set.

To reiterate, there WAS a time when USBoM material was available for D/L. It was a long time back. I think you would go to the US Dept. of the Interior & do a search for US Bureau of Mines and they had a page that told the story and how it was defunct but had a "search" component that would lead you to another page of the papers in numerical order which you could access. Back then I don't think they were in PDF but you could get them by doing a "print page" and having some manner of PDF printing mechanism. The US Patent Office has a link to use a TIFF printing utility which is not that much of a hassle to put in to a PDF. The utility is called ALTERNATIFF.exe if you ever want to snag unique patents from the gov web page. It's a plug-in for a browser made to work with their web site to view print or save the patent as it was filed.
I am going to try the Bureau of Land Management; as they may have taken the documentation from the USDoI in so far as mining.
If I find the collection, I'll post the link - If you should ever find anything please let me know!

[Edited on 30-7-2010 by quicksilver]

Rosco Bodine - 30-7-2010 at 10:29

I am not a "professional chemist" neither am I a pilot but I can fly an airplane.

You don't have to be a carpenter to hit a nail on the head, you just need the right tool for the job and to pay attention to get it done correctly.

I have contempt for the Legard books because they are rife with error to the point of unacceptability and exposing of the fact that the author is no authority regarding the material which is collected research of others, neither understood nor confirmed by the author. Such literature is unenlightening.

[Edited on 30-7-2010 by Rosco Bodine]

Hennig Brand - 30-7-2010 at 10:35

I found with the Picric Acid synthesis, as long as I had excellent magnetic stirring, that alot of the other things were much less important. A lot of the "recipes" floating around don't even discuss the need for good stirring. I would say it is even more important than temperature control maybe(up to a point).
I have probably read too much fringe literature garbage, which is likely why I am always suspicious of synthesis details. Usually if I experiment with a particular supstance long enough I develop an understanding of why certain things are done or not done in a synthesis. My biggest fault most likely is always trying to find an easier way out

I am going to give it another shot, tommorrow maybe.

I deleted that last edit from my last post as you and Quicksilver had already posted, and it didn't seem to fit anymore. Yeah, I guess one needn't be a proffessional to be good at something.

Here is the deleted edit, don't know if it adds anything, but hey.
One thing I would like to add. Now I am not a proffessional Chemist or anything, but it seems to me that sometimes there are very elaborate procedures that are designed to get maximum efficiency/yeild, when a much simpler approach would have gotten you 95% of the way there(which most times is good enough for me). Other times(and this is starting to look like one of those times), cutting corners can really cost you. I believe Einsten was often noted along with quite a few other famous scientists for saying that the established academia quite often made things much more complicated than what really need be, and many folks would be able to understand much more if it were not for this(or at least it would be easier). On the other hand, we can't dumb everything down to the level of every scienctifically challenged individual. We are seeing the consequences of that now in many schools and society. This is all just my opinion, not being critical of advice given at all.

[Edited on 30-7-2010 by Hennig Brand]

Rosco Bodine - 30-7-2010 at 10:46

Objection your honor, counsel for the stirrer is arguing facts not in evidence and contradicted by the thermal realities applicable to the reaction conditions

Stirring is important for keeping the reaction temperature evenly distributed along with the reactants in the mixture, however heating is generally required in aromatic nitrations where higher nitrations are being accomplished, and the reaction rate is greatly slowed or incomplete absent that heating. In large reaction masses conservation of the heat of reaction itself may be sufficient, but for smaller scale batches where radiational cooling causes the reaction to be deficient in temperature to maintain the reaction to endpoint, then supplemental heating is required. You got to work with the thermodynamic that is applicable, whether it involves supplemental heating or cooling and that varies with batch size.

[Edited on 30-7-2010 by Rosco Bodine]

The WiZard is In - 30-7-2010 at 10:49

I have bought books from Albris ( the book seller in the link) and was really happy with what they had and the way they described condition. I an going to see what they have from Vannoy Hartrog Manning, etc. IF you're ever going to buy, I recommend Albris. They are not the cheapest but I always get high quality from them (bindings aren't shit, etc) and they had the PATR as individual volumes from various libraries. - NOT as one $1000 set.

I never recommend Alibris anymore, I mentioned it on the
Venom mailing list several years ago, and someone with
a lot larger excheque then mine apparently bought up everything
including a $600 book in Latin.

You can DL PATR 2700 in theory from dtic.mil, there are a number
of PDF copies for sale on the cheap, however, both are image
copies and are not searchable.

I am finding more Bureau of Mines stuff @ google.com/books
and have just found Bichel's historical New Methods of Testing
Explosives, 1905.

The WiZard is In - 30-7-2010 at 14:57

The US Patent Office has a link to use a TIFF printing utility which is not that much of a hassle to put in to a PDF. T

Google.com/patents are already in PDF format.

The WiZard is In - 30-7-2010 at 15:21

US1478429 makes reference to nitrated cresol as a building block. Cresol is (IMO) much easier to nitrate than phenol but very difficult to obtain, which is a shame because there are quite a few things that employ it. The reagent-grade material is quite expensive & unnecessary, yet I have not found a source for anything but high-end cresol. I would really appreciate it if anyone who does know more about where to obtain same would post their experiences. {TNC is very close to TMP in a variety of tests.

You have a chemical engineering problem. Cpt. Colver notes that
when you nitrate crude cresol ... as soon as the the dinitro
stage has been passed the dinitro products of o- and p-cresol
are oxidized, and at the conclusion of the process only trinito
meta-crysol remains.....

.... commercial cresol gives only a yield of 90-100% in comparison
with the theoretical value of 220%, pure meta-cresol gives a
yield of 150% on trinitometacrysol.

Me thinks you will find buying a tank car load of the commerical
product vs a pound or two. Try the Chemical Week Buyers Guide.
Though getting someone to sell it to you........!

Hennig Brand - 30-7-2010 at 17:52

Well you certainly have a way with words Rosco. I have to be more careful with mine when I am around you, I can see that

Certain temperatures are very important as it controls what will or will not happen in an aromatic nitration, but isn't the stirring more responsible for how fast it happens? I just recently realized by not having mechanical stirring for the last stage of TNP nitration that I was not getting nearly as complete a nitration in the time taken(meaning I wasn't getting as good a nitration practically speaking, in effect). In small scale unless using reflux the HNO3 can be being distilled away mighty fast as well. Does this seem more or less right, not really contradicting you I think.

Just did first year general Chemistry for Engineers this year. I did alright, but to tell the truth untill I get my hands dirty a little bit the theory only goes so far. Its one thing to regurgitate some theory and pass a test(well there is some understanding), but another to really apply things in a real situation. I always figured some of the career science types lived in the abstract better than I did. My personal view is you need both to do things right. Sorry for the rant.

Just did the Basic Lead Picrate synthesis again, couldn't wait until tommorrow.
The only thing I did a little different from the basic method in the patent 1478429 for Basic Lead Picrate was keep the temperature around 40-50C(because it was inconvenient to do otherwise tonight). I also did the addition in about an hour as you suggested, instead of the 1/2 hour the patent suggested.
To tell the truth I was a little disapointed at first. It still looks orange even after 2-3hours in the oven, not red. The crystal structure is very fine, but that is what the patent said would happen with reduced temperature. I next tried a small burn test, less than a tenth of a gram for sure. It was much more energetic, lit in the open it made quite a loud pop(sort of like lighting a little pile of HMTD only much louder, a whump I guess). I don't know what the difference is but you seemed to know what your were talking about. Things had to happen gradually and in sequence I guess. The before picture must be a mix of something, with LP in it.

One question, how necessary is using a perfectly pure sample of Picric Acid? Maybe a silly question, but this could never be considered a sort of purification of sorts(going form TNP to Picrate)?

[Edited on 31-7-2010 by Hennig Brand]

Rosco Bodine - 30-7-2010 at 18:43

Near boiling temperature is your friend here, believe me. Hydrates are unstable in the hot water so what you get is going to be the lowest hydrate or anhydrous product if you precipitate it from a hot solution. On some reactions a cycling of temperature from lower to higher is necessary because the hydrated expanded matrix is an essential precursor for the thermally induced destabilization and collapse and dehydration to the crystalline form, so it may have to go in a two stage process for some materials.
Just for grinning curiosity try increasing the temperature to just below bp and increase the dilution by 50% for the Friederich patent process and see what you get. Orange would be more like it on the color too, definitely not yellow.
The crystals should be non caking free flowing like hourglass sand. They should pour right off the filter paper when dry
with almost no fines or dust. I just checked my old lab notes on the Friederich patent process and found the product described as reddish orange brown in color. Yield by Friederich method 8.5 grams, 94% of theory.

When there is a simple reaction mixture where everything is in solution, it is a different reaction system where the entirety of the reactants are in contact and the behavior of such reactions tends to be linear and predictable.

Stirring can increase the reaction rate for suspensions by exposing the particles to fresh reactants and sweeping away spent reactants and products in the reaction zone matrix. When you have a suspension of materials which are reacting in a zone between the particles or on the surfaces of the particles, then algebra has arrived, because you actually have a layered reaction system where there are different but interactive processes occurring simultaneously in the larger reaction mixture
which is a system, but which is the sum of subsystem reaction processes in the zones between and/or on the surfaces of the particles. The chemical and thermal dynamics can become complex especially with increasing scale, but you can develop an ability to "read" a reaction and interpret the general dynamic involved after observing and analyzing your experiments. Keep notes and take readings and note them and then your process logs and end results give you answers or clues that can move things in that direction. There really is some art involved in fine tuning of chemical processes. The precision is very exacting for some reactions, and it can be tedious sometimes to duplicate the exacting conditions even for ones own experiments, unless careful and complete notes are kept. A digital recorder can help if you need to dictate notes which will talk yourself through the same steps later.

Regarding the purity of reagents, it is not something I have really evaluated for significance in these reactions. I use what is probably 99.9% or better, reasonably pure materials generally, just to eliminate variables, but it may not be necessary.

[Edited on 31-7-2010 by Rosco Bodine]

Hennig Brand - 31-7-2010 at 07:11

Thanks for the good descriptions of the process.
On leaving the freshly made Basic Lead Picrate out over night, I find that this morning it has less vigor. It was hot and very dry from the oven, it was very snappy stuff right from the oven. I used the exact same quantities of reactants as in the patent, 4.6g TNP to start, and my yeild was~6.8g of Basic Lead Picrate. It does have a crystaline structure but a microscope at 40X(lowest magnification) was needed to clearly see it. I did notice that when dry this time it broke up to a powder very easily, the last time it stuck together badly. I guess I need to try and make bigger crystals.
BTW still very insensitive to percussion, and mine looks close to a mustard yellow(a darker more orange mustard though).

My TNP purity may be the problem, I have been saving my best stuff for compound caps.
Lead Nitrate was made with waste acid from RDX synthesis(takes a while with only 20-30%HNO3, but waste not want not). Heat helps a lot.

Here is a picture of my yeild

Lead Picrate batch #2.jpg - 167kB

[Edited on 31-7-2010 by Hennig Brand]

Hennig Brand - 31-7-2010 at 07:17

Here is a couple of improvised microscope pictures. It is crap quality, but maybe you can see the crystals sort-of. Regular microscope just held the camera up to it. Also 40X seems to be the lowest power.

Lead Picrate microscope pic 001.jpg - 112kB

Lead Picrate microscope pic 001.jpg - 112kB

[Edited on 31-7-2010 by Hennig Brand]

quicksilver - 31-7-2010 at 08:38

Basic Lead Picrate (crude picture using cellphone).

Although out of focus, note color in relationship to yellow legal pad paper.

Material is highly reactive, responding to heat & impact with substantial energy. Microscopic examination @ 100x revels rough crystalline elements of undetermined shape coloration is rich throughout the crystal.

basic_LP-3.jpg - 162kB

[Edited on 31-7-2010 by quicksilver]

Rosco Bodine - 31-7-2010 at 09:32

@quicksilver That rust like color is more like it

@Hennig Brand You got something different from the expected result.

Something I don't understand is the drying in an oven you describe.
The product should be absolutely non hygroscopic and dry completely crisp
right on the filter, fold the filter and pour it off like sand. A few hours air drying
and it is done if you have sure enough, honest injun, bona fide genuine,
basic lead picrate.

Hennig Brand - 31-7-2010 at 14:39

Nice looking stuff Quicksilver, wish mine looked like that.
I finally broke down and used some of my TNP that was saved for detonators. Using impure TNP is not a plan I would judge now. I also kept the temperature up to around 75-80C through the whole addition. I did get a darker product but not nearly as dark as yours Quicksilver, I will attach a picture. Also got an increased yield(~7.5g). It does glisten nice now in the light, but still small crystals. The last thing I could be doing wrong(that I know of) and its a little stupid really, when I made my Pb(NO3)2, I heated untill it was almost completely dry, but not quite. There is likely a bit of residual HNO3 in that liquid. Is neutral Lead Picrate a lighter color than Basic Lead Picrate? Could one of you tell me a better way to deal with my Lead Nitrate? Thanks for you patience.

BTW, this stuff is much,much easier to set of with a hammer blow.

edit:
Just read from another thread, seems I should have redissolved my Pb(NO3)2 in water, and boiled to dryness again to get rid of most of the remaining acid. The acid can't be helping much.
Come to think of it I did see a little bright yellow flash of color right when a drop of Sodium Picrate solution hit the (extra)acidic Pb(NO3)2 solution. Sodium Picrate solution at least partially turning to TNP solution perhaps.

Lead Picrate batch #3 001.jpg - 150kB

[Edited on 31-7-2010 by Hennig Brand]

Rosco Bodine - 31-7-2010 at 15:31

Neutral lead picrate is bright yellow transparent crystals. The monohydrate and the anhydrous form look identical.

Basic lead picrate is opaque rust colored crystals, much finer mesh microcrystalline form, a dense microcrystalline powder.

What the scrambled egg colored stuff is I don't know, maybe a mixture of lower nitrophenolate derivatives is a contaminate....who knows ? Could be a mixture of the normal hydrate and the basic salt.

The yield is off too, so something is definitely haywire, precursors, process or both.

I noticed above you are talking about recrystalizing lead nitrate with boiling to dryness, do not do it that way as you will hydrolyze some of the lead nitrate. Just cool down a hot saturated solution and harvest some crystals and air dry them. You need good accuracy on your weights and good purity on your precursors, and good parameters on your process and then it will work. The process is pH sensitive so if you are not precise then the result will tell about it.

[Edited on 31-7-2010 by Rosco Bodine]

Hennig Brand - 31-7-2010 at 15:49

I won't bother you with my messed up Picrate lab anymore for now.
My yield being off could easily be caused by my having to estimate a dry weight of Pb(NO3)2 from a damp weight. I'll get back to you when I have done something better with my Lead Nitrate. Dryer and less acidic would be good.
I was not boiling to dryness originally as I was worried about damaging the Lead Nitrate, good to know. I guess redissolving in water would be ok, heat, then air dry the last moisture away. Its kinda damp in this part of the world alot of the time, making air drying difficult.

I guess even the simple Picrate stuff can be messed up pretty bad, if your not carefull.

[Edited on 1-8-2010 by Hennig Brand]

Rosco Bodine - 31-7-2010 at 15:57

Don't be discouraged. I measure using a centigram quad beam for accuracy to milligrams on these. The Friederich method can actually be fine tuned to a quantitative yield if it is done carefully with stronger solutions at near boiling. Higher temperature would help. I typically do these reactions at 95-98C.

For air drying stuff a crock pot set on a lowest heat and left open, or a sheet of styrofoam or stack of newspapers with a heating pad and a glass casserole tray works fine. Even the low heat from a reading lamp over a dish will do the job.

[Edited on 1-8-2010 by Rosco Bodine]

Hennig Brand - 31-7-2010 at 16:10

Thanks alot for the help. I am going to clean up some Lead Nitrate tommorrow maybe. I'll get back with results, of what I hope will be a Picrate that looks like Quicksilver's.

Rosco, if I am getting a fairly high yeild from a TNP from ASA synth, and recrystallizing, it would have to be quite pure, wouldn't it?

[Edited on 1-8-2010 by Hennig Brand]

Rosco Bodine - 31-7-2010 at 16:54

That is a good question. A lot of folks who think they have a good handle on picric acid may not have exactly what they think they have. It isn't totally foolproof, so some attention to detail is important there. The color of the product is telling for the purity of picric acid. If you go back to page six of this thread and look at the photo documentary that ordenblitz did, you can see how light colored
the still very acidic crude picric acid is on the first dilution, it is actually virtually white or very nearly white coming out of the first diluted nitration mixture, and that is a very good sign of purity, and so is the absence of "red goo" when doing a subsequent concentration by boiling down the residual solution from the first recrystallization for a second or even third crop of crystals. If you have a good clean high yield synthesis and clean crystallizations from that, then you are at close to 100% purity by color, melting point, titration, and other tests. If you have something less pure then it may be okay and it may not be okay depending on how demanding is the use, and I'm not sure what the range of tolerance is there, for syntheses or other uses. For synthesis it is probably a lesson you are getting that purity matters, and other variables too. But you are on the right track to be looking at the components with suspicion when a reaction that should work doesn't work for some reason. It isn't just jinxed for bad luck, but there is a real physical or chemical parameter that is out of spec, that is preventing the expected result.

[Edited on 1-8-2010 by Rosco Bodine]

quicksilver - 1-8-2010 at 06:41

For what it's worth I have learned a few lessons regarding successful synthesis in general - the variables that I needed to pay attention to:
I learned to "tighten up" on the addition of weights and their timing of addition, the temperature of the synthesis, the ph (where appropriate), I bought various stir-bars because on occasion the density of the materials changes and a heavier stir-bar allowed the continual mixing & exposure to continue without being "bogged down" by increased density or other factors to maintain exposure to my nitration acid (or other situations where the mixing was an influence).

I used a wrist-watch and simple volumetric devices to do my best to not let additions range out of control. If a sep-funnel was used: I tested it first: not while I was actively nitrating, if a dry powdered product was used I did my best to be consistent in those additions or adjust as necessary, striving for consistency in those additions. A digital thermometer (or quality glass one) was situated so that I knew what my temp was with the best accuracy I could maintain. If combinations or a pre-mix of chemicals needed to be available, I'd set up those in clearly labeled beakers or flasks away from the main activity - so I was not mixing and watching temp, etc at the same moment.

If I had to use an out-door setup (because of fumes) I kept as much UV away from my work as I could. A poorly working fume hood is worse than no hood, because if you KNOW you don't have fume safety you can take safety measure. But if the hood doesn't work well, heavy fumes WILL bite you. Some synthesis are "fume volume heavy" & it's important to account for that!
Before I would begin a lab, I took a moment & thought through what was going to take place and assembled my goodies, so that I would not be searching for an item or leaving my work area. I keep safety stuff on hand but also had both a notebook and the pre-defined synthesis printed out so that I didn't have to guess & I could record an anomaly. Occasionally the notes became very import to repeating a synthesis successfully as I would find a significant variable that had to be accounted for.

The bottom line, was that I made sure I was in control of the procedure: taking myself from "imitating a recipe" to understanding the chemistry & preforming a synthesis. The formula itself began to not only make sense but became a larger scale map of the activity. The greater my control of the procedure I had, the greater I could define the formula.

Hennig Brand - 1-8-2010 at 10:48

Thanks for all the good advice.
No real joy again though in my case. My yeild is up to 8g (actually 4, as I did a half scale batch). I think I fixed my Lead Nitrate problem though. I made a hot saturated solution of Lead Nitrate, cooled, then strained out the large crystals, and dried them well with very low heat over 2 hours. I used a scale that was accurate to 0.01g, and was very careful with my weighing of the reactants. I have a fairly good yeild of very energetic material, but it is still dark orangey yellow, not the rust colored stuff Quicksilver had.

Even though my yeild of TNP last time was very close proportionately to what Ordenblitz got back on page 6 of this thread, I still think I have lower nitro phenols or other contaminants in considerable quantity in my TNP.
I think I need to be a little more careful to get complete nitration in the final stage with heating. Mechanical stirring and longer final stage nitration at 110C+ would probably help.

To me it is starting to look like Basic Lead Picrate might be a good way to test purity of TNP. Of course there could still be something I am missing, that is wrong.

I will spare you another picture. It is just a little darker orange than last time.

[Edited on 1-8-2010 by Hennig Brand]

Rosco Bodine - 1-8-2010 at 11:30

Because it is a powerful dye even at 1 ppm, and some of the potential impurities are also strong dyes, it wouldn't take much impurity at all to cause a color shift.
Really it is the yield being off that is the bigger indicator of a possible problem, when that is taken together with a color shift it is more conclusive with two parameters raising suspicion then being doubly suspicious, as one is bad enough.

It is much easier for the neutralization on something like this to make up a larger sample of a standard solution of NaOH using a density chart and confirm by titration and an indicator if you want to make twice sure of the molar strength,
and then to measure out the volume needed using a buret or a syringe, or weighing the needed amount of verified strength of solution. With a hygrosocopic solid like NaOH and working with small quantities, it is about impossible to be accurate by weighing out a small amount of solid having a moisture content growing by the second as you are trying to weigh it.

You can do the stoichiometry and get the actual required amounts a bit closer
to theoretical than is given by the stated proportions of the Friederich patent.
It may be that you are simply not allowing enough time / temperature / agitation for the material to transition forms, to "develop" .....and it indeed does go through a gradual transition, so you may be picking your plum before it is ripe, robbing the cradle, ect.

[Edited on 1-8-2010 by Rosco Bodine]

Hennig Brand - 1-8-2010 at 13:12

I shouldn't maybe be admitting to this, but I think it does illustrate something(maybe). The first couple of times I made(tried) Basic LP I literally made the two solutions and slowly poured them together with stirring. I next brought the resultant mess/(solution +precipitate) to a boil for 15-20min. I found the color was quite similar(a little lighter I guess) to what I have made with the hour long process with very vigorous magnetic stirring at ~80C. The crystals were of course tiny though.

You are right about the NaOH I think. I can actually see the little NaOH prills glistening right up with moisture, and that in 5-10seconds on the scale boat. I must admit, I have been adding an extra 0.1-0.2g to compensate. Yeah, I really ought to do something better in this respect.

I am making more NaNO3 right now, for a good TNP nitration. I have the capability of doing magnetic stirring through the whole nitration now. I have always felt my TNP was just a little too insensitive. Also, the Picric Acid solution seems a bit orangey, even before adding the NaOH. I don't know about the other lower nitro compounds, but Dinitrophenol makes reddish colored solutions doesn't it? Red plus yellow= orange?

Thanks for the advice, I will try and do something better with the NaOH. Maybe if I dried it well in the oven then weighed it quickly? Your idea would be much more accurate though.

[Edited on 1-8-2010 by Hennig Brand]

Rosco Bodine - 1-8-2010 at 13:57

You could use bicarbonate of soda for your neutralization finishing and watch for the end of effervescence of sprinkled crystals on contact as a visual endpoint. And you don't need the picric acid in solution, a suspension in hot water is fine there, as the heat and concentration with some bright light and close visual inspection will show you the endpoint pretty close when using bicarbonate to neutralize.
Sodium picrate is a lot more soluble than picric acid so the suspension will quickly convert to a solution as the picric acid is neutralized.

Maybe weigh out 90% of your neutralization equivalent of solid NaOH and just heap that in, and weigh out maybe the remaining projected amount needed to neutralize as bicarbonate, with maybe an additional 5%. Then just go with the finishing by small additions watching for the endpoint. Of course when it ceases to effervesce on contact, cease the additions of sprinkles of a few crystals at a time and call that close enough.

[Edited on 1-8-2010 by Rosco Bodine]

Hoveland - 1-8-2010 at 23:14

Phenol can be nitrated with 70% nitric acid, if gently heated.
http://www.google.com/imgres?imgurl=http://www.chemistry-blo...

Phenol can also be nitrated with Cu(NO3)2 in acetic anhydride
"with copper(II) nitrate in acetic anhydride or nitric acid/acetic acid mixtures gives high yields of the corresponding mononitro compounds"
ci.nii.ac.jp/naid/110003651630

That more concentrated HNO3 is not required should not be surprising, given that even 50% HNO3 solution can slowly burn through plastic over the period of a year.
The more dilute HNO3 is, the less NO2+ ions are favored in equilibrium.

Another reaction that was seen was
3Fe(NO3)2 --> Fe2O3 + Fe(NO3)3 + 4NO2 + NO

Fe(II) nitrate can be made by dissolving iron with very dilute nitric acid, or using HCl on Fe to make FeCl2, then adding sodium bicarbonate to precipitate out Fe(CO3)2, then either heating the FeCO3 with ammonium nitrate, or simply adding very dilute nitric acid. Ammonium nitrate can be made from a mixture of sodium nitrate and ammonium sulfate, the sodium sulfate being less soluble when the solution is cold (4.7 g per 100 mL at 0degC), leaving NH4NO3 in solution.

The action of nitric oxide in the presence of oxygen can oxidize substances that oxygen alone cannot. One would wonder whether
a little nitric oxide in excess oxygen and sulfur dioxide would not create some sulfur trioxide (which would likely further react to form nitrosyl sulfate).It would be important to have the gases free of any trace of water.
NO + O2 --> ONOO
2ONOO --> 2NO2 + O2 These two reactions are just guesses as to what the radical chemistry actually is.
"This conversion has been speculated as occurring via the ONOONO intermediate."(wiki)

quicksilver - 2-8-2010 at 04:51

I shouldn't maybe be admitting to this, but I think it does illustrate something(maybe). The first couple of times I made(tried) Basic LP I literally..........

Please don't ever feel uptight about examining an action that later on you may feel was unproductive. No one learns anything by always doing things correctly. If we all did things in a manner that yielded what we were after.....where is the learning process?

Even when a synthesis is successful, there are things that can be gleaned from the experience; you can trust me on that!

[Edited on 2-8-2010 by quicksilver]

Hennig Brand - 2-8-2010 at 09:51

@Rosco
That sound like a good way to handle the TNP neutralization. I think I'll try that next time.

@Quicksilver
I like to try different things, quite often by trying to take a short cut. Often times though I end up eventually doing more or less what the synthesis suggested. I usually find (eventually) that most processes in a synthesis were for good reasons, that I just wasn't aware of previously. I think you are right though, when doing things differently (or improperly even) one can learn a lot. Probably alot of things that wouldn't have been learned had everything gone smoothly.

I am going to see if I can do little better with my TNP and Picrate syntheses. I have a week or so work trip shortly, so it may be after that. I will post results, when I figure a couple things out. Thanks for the help.

quicksilver - 2-8-2010 at 15:07

By the way, using a microscope is a very sharp idea when working with lead azide. Taking a totally random tiny sample & examining it for any needle crystals can save you from a serious tragedy. It's a standard in industry. Needle crystals as you know are totally unacceptable in lead azide & @ 100x you should be able to see 'em.

"Different instructions" Try this...

The WiZard is In - 2-8-2010 at 15:15

Conversion of Morphine into Picric Acid. P. Chastaing. (Comptes
Rendus, xciv., 44.) The phenolic character of morphine recently
pointed out by the author, and also by E. Grimanx (YearBook of
Pharmacy, 1881, 22), receives farther confirmation from a very
interesting observation recorded in his present paper. By the action
of nitric acid on morphine, an acid product of the formula C10H9NO9
is obtained, which, when heated with water at 100° under pressure,
yields trinitrophenol or picric acid.

Year Book of Pharmacy 1894 [Google.com/books]

Other ref. suggest treating the product obtained w/ fuming NA.

Hennig Brand - 3-8-2010 at 04:27

When adding the ASA to the H2SO4, I find if I stir vigorously the ASA will dissolve quickly a spoonful at a time. If I let the ASA crystals sit on the top of the H2SO4(even for a relatively short time), it clumps together and is very hard to make dissolve. Has the ASA become degraded in some way, by not dissolving it quickly? Just curious if some of my TNP contamination problems could be originating from the Sulfonation. I bet Rosco knows if a person could botch a Sulfonation. Quite often I have made a bit of this insoluble material and it takes forever to dissolve it.

BTW after Googling it seems that Picric Acid solutions in water are only yellow when fairly dilute, so orange is normal. I guess I knew that already, trying to find a problem that isn't there I guess.

[Edited on 3-8-2010 by Hennig Brand]

grndpndr - 3-8-2010 at 16:12

Ive seen the exact same thing with dissolving the ASA in H2SO4 so to releive any muscle strain and improve mixing w/o any clumping at all I imp. a stir stick for a hand drill by heating and bending broken std glass stir rod.Made very short work of the ASA mixing portion of the synthesis and vigourous prolonged stirring was devoted to other time sensitive tasks. allowed Better organization besides the superior mixing as I dont have a magnetic stirrer or my IMP overhead stirrer completed.

Now that it seems most of the interested parties are present I have a question and observation concerning what if any major differences
are ther in performance between LA,MF,PB picrate,even PB styphnate a material I had thought most ofetn encountered in NC primers.If I were to just peruse the lists of VODs densitys etc. I would have to come to the conclusion they are all relatively closely matched.Even if I take into consideration the different methodologys in testing,circumstances etc.
All of the sources rate these 3 as roughly similar as far as I can tell.
I readilly admit i have not experienced PB azide,on paper,they all seem quite similar in density, vod and relative brisance in fact PB picrate is most often listed with ahigher RB than the other 2 ,LA often listed as having the least RB compared to TNT.I wont list all relavent
info Ive seen butI have LA listed at a density of 4.6 gr cm3 5300mps.
HG fulminate isnt far behind at maybe 5200 @ 4.2/IIRC RB was listed in the neighborhood of 37/47% LA,HG fulminate at the higher end and plain PB azide @ 4400 MPS .67 RB/2.8 gr cm3?And the painPB picrate/HG Fulminate can be improved upon with the addition of K chlorate and /or AL powder. I expect some discrepancy in measurements but...Subjectively PB picrate made with an excess of PA(2/1.2 pts PA/PB monoxide( with a dirty yellow orange coloration while still wet w/methanol is a darker orange when dry and has a gritty feel.What can i say about the fulminate,not purified simply washed still a grey
colored powder but fully capable of det comp caps w/PA.They seemed
subjectively, to have similar power,a small paper matchead size of loose picrate material in al foil heated to det on a stove produced a smart,sharp crack
on det.Very similar to HG fulminate.What am I missing?Respectfully Pndr.

Perhaps further testing using a test plate of sheet metal to either measure the dent depth /width or better, penetration when the cap placed on end and detonated leaving a hole punch effect.My main concern however is a plain PB picrate, maybe a composition with a chlorate/AL powder would detonate reliably a comp cap with PA as the base charge.

Finally Im likely going to have to visit an archery shop for some hopefully inexpensive scraps of carbon fiber shaft material to stiffen a forend in comb w/epoxy.I havent seen a carbon fiber arrow shaft would your opinions be AL arrow shaft material or possibly carbon fiber?I havent a clue as to inside diameters either or bursting strenghth.I dont think I want excessive burst strenghth.However the description of anodized hardened al shaft material sounds superior to soft mallebale AL tubing.

[Edited on 4-8-2010 by grndpndr]

[Edited on 4-8-2010 by grndpndr]

[Edited on 4-8-2010 by grndpndr]

quicksilver - 3-8-2010 at 16:33

I would imagine that letting the ASA sit upon the acid would form a layer of oxidized material = problems. Sulfonation technique is critical to many nitro phenols.

***Addressing the "Arrow question": I would add that I am very familiar with carbon fiber arrows and they take a quality saw to cut. They will splinter like crazy if anything but a fine scroll saw blade at high speed is used to cut them.
IMO they are fantastic for target archery. But for alternative uses, quality Easton aluminum is the way to go. I wouldn't steer you wrong there. - They (CF arrows) even leave splinters in meat on occasion and many folks won't hunt with them what-so-ever.
-=Easton Aluminum XX75 at 2215 should come close to 6mm cap body=-

[Edited on 4-8-2010 by quicksilver]

[Edited on 4-8-2010 by quicksilver]

grndpndr - 3-8-2010 at 17:06

I have them in mind to reinforce a somewhat flexible older generation GI fiberglass Item. Ill keep the splintering in mind perhaps best for the shop to do any cutting.The AL tubing sounds better
for ITS intended use..

Any thoughts as to the seeming similaritys in the heavy metals based primarys specs?

[Edited on 4-8-2010 by grndpndr]

The WiZard is In - 3-8-2010 at 17:48

Legard publishes one of the most questionable of any I have ever read wherein he uses one liter of 98% H2SO4 to 50gr of phloroglucinol. The actual nitration was 124ml 98% H2SO4 / 76ml HNO3 70% {yes: going back & forth between volume and weight measurements.}

----
Try US Patent 4 434 304 issued to the US Navy 1984 which uses
1 L of H2SO4 &c.

quicksilver - 4-8-2010 at 05:16

----
Try US Patent 4 434 304 issued to the US Navy 1984 which uses
1 L of H2SO4 &c.

(0616)
Jeez...I grabbed that right away & you were right on the money. I am seriously impressed. I really DID look quite a bit.
I had become numb trying to find his patents or applications.
-=Follow-up=- (0633)
I edited the previous post as I was wrong: it existed (as seemingly wasteful as it was; but that's another issue). I snagged the actual patent as I really wanted to understand why such a lop-sided level of materials were used & perhaps the notations would help more than any abstract.

QUOTE:
"Any thoughts as to the seeming similaritys in the heavy metals based primarys specs?

"

In what regard? In reference to BLP?

[Edited on 4-8-2010 by quicksilver]

The WiZard is In - 4-8-2010 at 05:38