Microtek
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Posts: 205
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Registered: JAN 2001
posted 03-07-2001 06:45 AM
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First off, I would like to recommend Mannitol HexaNitrate as a base charge in caps; its performance is incredibly high, and stability exactly right for this use
( meaning much more stable than HMTD but less than picric acid ).
This stability means that you can compress it safely at much higher pressures than HMTD; my usual compression is at about 10000 psi for 3mm coloumns. These base charges are sensitive to 5mm HMTD ( that is, a coloumn of the same diameter and 5mm in length ), and have a better initiating performance than much greater amounts of HMTD.
My problem is this: I get very low yields with the method I use.
To begin with, I should say that I use MHN rather than RDX because it can be made without destilling the HNO3, so you can avoid that extra complication.
Anyway, the method I use is as follows:
Add 9.5 g AN to 6.5 mL 96% H2SO4 once all the AN has dissolved, cool the solution to
-5 C. Now add 1 g powdered mannitol in small amounts so the temperature stays below 0 C.
When the addition is complete, slowly add
5.5 mL 96% H2SO4 keeping the temp below 0 C.
Once this is done, I add the solution to about a litre of cold water with stirring.
After washing with water and some baking soda, I have about 0.5 g MHN. On Mega's site the yield is 2.3 g per gram mannitol ( with proper 100% HNO3 ).
So I was hoping someone could tell me whether this yield is normal for this method or if I'm doing something wrong.



nbk2000
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Posts: 1096
From: Guess
Registered: SEP 2000
posted 03-07-2001 09:56 AM
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It doesn't matter if you get low yields if you process is simple with dirt cheap materials.
No nitric distillation bullshit equals great to me.

------------------
"The knowledge that they fear is a weapon to be used against them"

Go here to download the NBK2000 website PDF.



Microtek
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posted 03-07-2001 10:08 AM
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I agree that it has revolutionized my cap manufacturing, as it is also much simpler than picric acid, but I have to order the mannitol from a pharmacy. The good thing about pharmacies where I am, is that they know next to nothing about chemistry so if you say glycerol instead of glycerine they won't get suspicious, but the downside is that these places are prohibitively expensive; I pay about 9$ for 100 g.
Oh, by the way, did I mention that the nitration gives off just about no fumes ?
It is quite safe to stand in the kitchen.




Mr Cool
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From: None of your bloody business!
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posted 03-07-2001 02:34 PM
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The only things I can think of are that the 4% water in the H2SO4, and any water in the "HNO3" mixture thingy are either stopping the reaction too soon or dissolving some of the product.
Is it a nitrate or a nitro compound? All nitrates are soluble to some degree IIRC, so maybe some is dissolving in the huge amount of water that you're dumping the acid/product mix into.


ezekiel
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posted 03-08-2001 03:42 PM
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perahps your chemicals are impure.
Perhaps you need to heat the mixture.
perhaps you are not retrieving all the product.
As for your caps...
It all depends on what you are doing with them...
Do they need shelf life?
Do they need to be weather resistant?
Do they need a booster?
Do they need to be electrically initiated?

Different components will achieve differnt ends.

------------------
Ezekiel

'Things bad begun make strong themselves by ill'



Microtek
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posted 03-09-2001 08:15 AM
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Ezekiel: I know what COULD be wrong, but as I have limited resources I do not wish to test all the possibilities myself, especially if someone knows, or at least has info that will narrow down the spectrum.
As for the caps, what are you talking about ?
Unlike secondary explosives, caps ( aka. detonators ) always need to be as powerful as possible, that is they need to have as high a DOV as possible in order to ensure reliable and complete detonation. Also, some secondary explosives, such as nitroglycerine, only achieve its full potential if it is initiated with sufficient force.
Homemade caps should generally not be stored longer than neccessary, but both nitromannite and HMTD keeps well, especially when compressed in an airtight tube. Of course you should coat the inside of the tube if it is metallic.
All caps should be weather-proof, and almost all good caps are made like that: You need a metal pipe which is certainly weather-proof. This pipe must be sealed in one end either seamlessly as I do it ( with a lathe; I mill the metal from a solid rod ), or with epoxy or solder. Either of these will give airtight seals. Sealing the other end until you need the cap is a simple matter of wax or a greased stopper.




ezekiel
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Registered: SEP 2000
posted 03-09-2001 11:33 AM
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microdeck:
Weather resistant does not neccesitate water resistance.
Did you know that some explosives are used in high temperature, high abrasion enviroments?
Some explosives are more prone to react to such conditions that others.
I don't need to be told about Vdet and caps (aka detonators).
oh and BTW you are wrong.
A high Vdet cap is not always a good cap.
Do you know why mercury fulminate and lead azide are excelent initiating exposives?
It is not becasue of their Vdet.
Transmission of shock wave is important; but that is not the same as Vdet.
And, yet again, I must point out that you do not need a massively powerful cap and booster for every explosive. In fact very few need it. If you need such power for initiation then I suggest your fillers are of inferiour quality.
I really can't just tell you what is wrong, because you ahvenot given and pictures, or detailed reference, or inference to your procedures.
So, none the less, i tried to show you where to start.
------------------
Ezekiel

'Things bad begun make strong themselves by ill'



Microtek
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From:
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posted 03-10-2001 08:01 AM
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Weather resistant may not neccesitate water resistance, but water resistance will give you weather resistance.
Are you telling me that there are secondary explosives that are less efficient if initiated by a stronger cap than is neccessary ? If this is the case then I would be quite interested to hear about them.
If not then please limit your hair-splitting to where there is a need for it, such as in precise formulae. Speaking of formulae, I fail to see what information my describtion lacks to someone who has information about this synthesis, so if YOU could specify YOUR request, I could give a better resume of what I did.


10fingers
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posted 03-10-2001 01:34 PM
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*
[This message has been edited by 10fingers (edited July 19, 2001).]



Microtek
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posted 03-11-2001 07:23 AM
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10fingers: Yes it would be nice to find a source of pure, cheap mannite. I tried looking for it on the net but the most plausible source I could find was in intravenous nutrient supplement in hospitals, but it was in solution with something else, I think.
My best yield so far was with 5 g mannitol which gave me 4 g MHN. With this batch I tried to use as little water as possible, pouring the acid/MHN mix into an equal amount of water and ice-cubes. I think crushed ice may be the way to go, as the addition of the acid to water generates quite a lot of heat.
You do need a minimum of water though, as there is a lot of ammonium sulfate that needs to be separated from the MHN. Fortunately it's easily soluble.
The only drawback with MHN other than the low yield is, as far as I can see, that it is incompatible with many solvents.
For instance NM and acetone; I had hoped to use the MHN with NM in a 85/15 ratio to give a very powerful explosive with optimal oxygen balance. The Berthelot approximation of this compound placed it at more than 180 percent relative effectiveness, and with the high brisance of MHN I think it could be close to RDX in performance. But when I tried adding MHN to NM, the MHN dissolved, and did not precipitate when the NM evaporated. The same thing happened with acetone, but ethanol will leave it intact.
I didn't experiment that much with it because I wanted to use what I had for caps.
Anyway, at the time I'm experimenting with making sheet explosive from MHN and silicon pastes and oils of different kinds. It looks promising.



10fingers
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From: USA
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posted 03-11-2001 10:40 AM
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[This message has been edited by 10fingers (edited July 19, 2001).]



Demolition
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Posts: 158
From: Australia
Registered: FEB 2001
posted 03-13-2001 11:08 PM
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Today I tried looking for Mannitol at several chemists.They said that they could order in IRC? Mannitol(Liquid Mannitol which you inject).Would it still work in the process for making MHN?
Demolition


10fingers
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From: USA
Registered: SEP 2000
posted 03-13-2001 11:48 PM
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I'm not sure but I would guess that it is a solution of mannitol in water. You would have to remove it from the water if that was the case.


Demolition
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Posts: 158
From: Australia
Registered: FEB 2001
posted 05-03-2001 04:31 AM
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I was just wondering if anyone has had any luck with another method for making MHN using H2SO4,AN and Mannitol?
Demolition

I just wish to make all know that currently in my contry mannitol is OTC as a baby diuretic-laxative, sold in 10grams soap like agglomerates of powdered mannitol for 50cent each.
i tried to nitrate some using the xNO3 method but it looks like i got a very bad yeld.
not more than 3grams of MHN out of 10g M, but will be probably less after completely dry.

today the MHN is almost completely dry, i made two batches, one was neutralized and then washed and dried, a smaller one was dissolved in alcohol and reprecipitated.
The first one gave a white hard mass, very thin powder, the latter gave a much better product, the mass is soft and easy powders just by touch of my finger, the cristals are a bit bigger but flaky appearance, very easy to powderize, but high volume for a small weight. I tried bot with hammer and didn't see any difference in detonation, just the one reprecipitated from alcohol is orange since my alcohol is died red.
i will wait a day more to be sure that the mass is completely dry before crushing it, is more hard than DS, and not as crispy as AP, looks like very fine powder of CaCO₃ lumped together.
More tests to come.
The yeld is 3 grams, over 10g starting mannitol, VERY VERY bad. :mad:
i will try next thursday with HNO₃ instead of xNO₃

Nevermore, I can give some info as MHN is my favourite. It is underestimated here, Mega gives VoD for hand pressing, it can go to 8.25 km/s according to Kast/Stettbacher etc. ! Let me just copy some results:

MHN (Mannit Hexanitrate) yield improvement + tests

1. Warm neutralisation (bad yield)

65ml SA 96% + 65g AN mixed, cooled to -20C, 10g M added, put 1 day in the freezer, poured in 1 L water, filtered, cooked with 100 ml 2%-bicarb, washed, filtered, warm-dried at 80C. Melted at 80C and gave hand-mouldable plastic after cooling (partly denitrated to penta/tetranitrate making eutecticum?), but solidified after 5 minutes to a very hard block. If powdered properties are like MHN, 4cm/2kg impact and 50N friction sensitive. Yield was 8g.

2. Wrong solvent (1)

Made with standard method (50ml NA 98% + 10g M below zero, 50 ml SA 96% added, filtered, washed, neutralised, washed, filtered, dried. If re-crystallised with 96% ethanol stable for years. But when BBQ spirit used (denaturised with pyridine), most was destroyed, only 1/4 crystallised at cooling! According to Beilstein, pyridine in alcohol destroys MHN!

3. Wrong solvent (2)

When grabbing a bottle of thinner instead of ethanol, and evaporating it to get the MHN back at 80C, it turned into a very good plastique which stored well if airtight, and stayed mouldable for days later. When kneading 1/4g of HMTD into 3/4g to make a case-less cap, it detonated while mixing and punched a 1" hole in the table. Bad idea, but I am fine + the table was old!
I guess the non-neutral MHN gave off nitric while heating, this partly nitrated the toluene in the thinner, as the plastique was yellow and smelled like almonds. The nitric acid traces may also have further sensitised the HMTD.

4. Maximum yield (1)

I am still improving the method, but the best yield so far gave the synth described in (1.) with 70mL SA, 50g AN and 12g M. Neutralised at only 40C the yield was 12g. Fine powder with mp 100C. Must still contain some % of the lower nitrates, this is probably a feature of the SA/AN method. Pure product can be obtained by cooling a hot saturated solution in ethanol. Some percent pentanitrate are not bad, they hardly decrease VoD but give more energy due to better OB.

4. Maximum yield (2)

Same method with 80ml SA gave 14g yield after neutralising with bicarb at 40C. It seemed to be more before the neutralising step, so next time I will weigh it before and after and use cold bicarb solution.

4. Maximum yield (3) - warm up or not?

150ml SA 96% + 100g AN mixed, cooled to -20C, 35g M added, put 1 day in the freezer. To test if 'warming to room temp' before pouring into the water - as recommended by several people here - gives better yield, the mix was equally divided and one part processed while at -20C, the other allowed to warm up for two hours. First yield was 22g, second was 23g. Therefore it is not necessary to let it warm, the difference is minimal, and it can be more safely diluted while cold. But neutralising should be done at near room temperature, not warm! The yield is at least 10% higher and the suspension does not turn yellow.

So you CAN get 1:1 yields or slightly better with a nitrate, but 99% nitric can give twice that. Try yourself!

P.S. Funny to be a newbie again after 20 years of ‘blasting around’….

Well
thank you for the very exaustive informations!
maybe i made some mistakes in my calculations since i used 40g AN + 60ml SA, both cooled to -15°C prior to addiction, then they warmed up when mixed to +25°C but addiction of mannitol was started only when the temp reached 8°C and never went up to 10°C.
The final dry yeld was a pooor 2g, part of it have been recristallized from denatured alcohol (here for denaturation is used tiofen, and denatonium benzoate in methiethilchetone).
the recristallizated one showed better appearance in flakes, more easy to crumble and very fluffy.
I will try 90ml SA and 40ml HNO₃ 55%, i hope i will have better result. after then i will try your maximum yeld 2, since AN and SA are cheap over here.
I neutralize always by stirring for a couple hours in saturated NaHCO₃ solution until no more bubbles are seen.
My product color is pink white in the one not recristallized from alcohol (my AN is lightly pink), and orange in the one from alcohol (my alcohol has a deep red dye).
One question, how long was your nitration time?
i let it nitrate for around half an hour.

Nevermore, I simply pre-cool the SA/AN mix in the freezer overnight (–25C at lowest setting), add the mannitol all at once and shake it for a minute. Then I put it back in the freezer, and over the rest of the day give it some more shakings. Next day it is poured into water (min. 10 times the volume, and ice cold), stirred, filtered, put into cold bicarb solution and left in there another day with occasional stirring (PH 9 is OK, not too strong). It is then washed with water a last time, and dried. It is stable for month if stored slightly ventilated (glass with cloth cover against dust), sealing accelerates decomposition once it has started. I only re-crystallise if it is used for caps and must store a year.

That’s all, if you have patience the whole process takes only 30 minutes (3 x 10 minutes) – the rest is time off! You will not loose much yield if you wait 3 hours between the steps, and dry it in warm air, in case you want to use it the same evening. But my method gives best yields and is most convenient IMO.

P.S. Funny to be a newbie again after 20 years of ‘blasting around’….

Hello
i usually never leave a nitration alone and absolutely not in the fridge where someone could disturb it or it could mess in case of runaway, anyway i suppose i got very bad yeld since i made wrong calculations of SA so i added too little, next time i will try with double amount.
I always neutralize by excess NaHCO₃ and never had any problem, but i advice anyone to recristallize since the product has much better appearance, while i was getting rocky cakes not recristallizating i get fluffy and easy to powderize ones when doing from hot alcohol..
definitely worth the time..
:D

At minus 25C there is no danger of a runaway. The mannitol dissolves very slowly and is nitrated as it dissolves, therefore you hardly have any temperature rise. Even when making NG you can add the glycerine in two portions, each in one big gulp. The thermal mass of the reagents (I use ½ litre) absorbs the heat. With the first addition temp jumps from –25C to +10C within seconds. After re-cooling to –20C you add the rest and it jumps to around +5C. Don’t try this with the NA method, it has less mass (no sulphate and surplus SA) and will heart up more. You will have to add it in at least four portions, or cool during a much slower addition with an ice bath.
BTW my MHN is a fine white powder already after washing, and it stores for month without a sign of decomposition. But you are right, for caps etc it should be re-crystallised.

And my fridge is MY fridge, I would not use Mom’s again! She once fed some spoonfuls of blasting agent to an old lady next door. This is no joke, she had mistaken it for corn flour and mixed it into the soup. Thank God it was just starch-ANFO with the diesel still missing…..I guess it solved her constipation anyway! :p

I tried both methods, the first one with 55% HNO3 and excess sulfuric, i used 40ml HNO3 and 90ml H2SO4 for 10 grams mannitol, i got nothing. Not even a gram, everything went dissolved...
after that failure i tried AN recipe, used 50g AN and 75ml H2SO4 96%, this time went better from 10g mannitol i got 5.2 grams of dried recristallized product.
All the nitrations have been performed at -10°C, for 3 hours.
I wish really to get the yelds you seem to get, but i've never been able to pass the 5g stop, not even by using very dry AN and 96% H2SO4...
i wonder if in the mannitol there is something else that is parasiting the reaction

Since I hate peroxides, I started to make MHN.
I added 50g of AN to 70ml of cooled SA, This mixture was subsequently cooled to -23 degr. C, and then the mannitol was added in small amounts.
I let this for a day in the freezer, but the problem I get is that not everthing gets dissolved. A tough layer is on top of the acid, it's a bit like chewy ice on water.
An other strange thing is that I get 2 kinds of products after filtering.
One very fine white powder, like wet CaCO3, and the other is more 'rough' and a little brown. There was also some foam on top of the water where I dissolved the acid in.
I couldn't detonate both with a ferm slam of a hammer.

Anyone knows what occured? I made the AN out of fertilizer, 70%AN 30% MgO, can any impurity have coused this?

thanks!

Well, probably some of your mannitol has been dehidrated to carbon, i suppose your AN was no pure enough so it caused strange products to form, the white powder could be Mg nitrate, you should try again using pure AN and maybe increasing the amount of SA in order to trap all the water.

The foaming is normal, you have some fine powder in the foam that will mostly sink down when you stir. The rest will be caught in the filter later.

The reason for the bad yield is probably that you "left" it in the fridge for a day. At these low temps the mannitol dissolves over hours, and is nitrated as it dissolves. The precipitated nitrate is insoluble in the acid mix and will prevent fresh acid from reaching the un-reacted stuff. Therefore you have to shake/stir like hell several times during the first 3 hours, and a few more times over the rest of the 1-2 days.

Your ratios are about right, a little more SA would be good though. There are a few more things to remember:

- The mannitol should be as fine as flour, and as dry as possible (desiccator).

- The acid must be 96-98%, not 90% drain cleaner. This can be boiled down, it is ready at 330C, NOT as soon as it starts to fume.

- The AN must be pure and dry. Fertiliser has to be re-crystallized, i.e. dissolved, MgO/CaO filtered out, solution evaporated, the crystals dried sharply at 110-130C (do not melt them) in a pan for 1 hour.

- The mix must be dumped into LOTS of cold water, not 1:1 or 1:2 like PA. Otherwise the spent acid re-dissolved and decomposes part of the yield (same for ETN, PETN, NG etc.).

With this method I get a 45-55% yield, i.e. 11-14g MHN from 50g AN, 75ml SA, 10g mannitol, reliably every time.

If you want 90%, you have to use distilled NA, e.g. 50g NA + 50ml SA give 22ml NA (stop when the dropping rate has halved). Dissolve 12g mannitol in this, and add 25ml SA, all below 0C. Will give you 27g of MHN = 90% yield (theory is 29.8g). For 95% yield you need MUCH more acid, so I think this ratios are most price-efficient.

Thanks Boomer!

My mannitol was comletely dry and very fine powdered, I got it from a pharmacy store. My SA was 96%.

It dissolved in hot EtOH, and if I re-cristalyse it I get very fine crystals.
I can still kneed it after I dryed it, need it to be more dry, or am I kneeding it to death this way?
What is a safe method of testing? A blow with a hammer didn't work, and I still don't have my EBW working fine.
Would a epoxied tube with some flash powder and at one side 0,5gr. MHN packed work?
This is the first time I make a HE, so that's why I ask so much...

Thanks!

COB

----------------

There's no need to sign your posts as your username is standing next to each of them.

Rhadon

Ok, I tried MHN the first time today and expected poor yields as a lot of people hear posted. Luckily that yield was better than I thought.

A short summery of my notes:
200ml 96% H2SO4 and 120ml 69% HNO3 are prechilled to 0°C
40g mannitol are added in 2-5g amounts
the temperature is hold below 10°C, stir occasionally
I would recommend a magnetic stirrer anyway, as larger mannitol clumps are floating on the top and creating hot spots ! (visible yellow points)
after all the mannitol is added the mixture is allowed to stand for 90minutes
there should be no visible clumps left on the top
the finished MHN gets filtered and washed with water
final yield 40-50g MHN (I´ll weight it again when its dry)

/edit
ok, I recrystalized it now in 200ml alcohol
I let the alcohol evaporate

there should be no visible clumps left on the top
the finished MHN gets filtered and washed with water
final yield 40-50g MHN (I´ll weight it again when its dry)

That is an excellent yield for that method, however, I would suggest that scaling down is a good idea, a runaway with 320ml of reaction mixture is no fun at all...
I've never got any yield with mixed acids, but I might give it a go...

Furthermore is stirring indeed very, very important, clumps should be get rid of.

I don't know or if you did, you didn't write it, but you should first drown the nitration mixture into water, then filter, not the other way around. Though MHN is not very soluble in H2SO4 (that's why you have to add so much, to pull the equilibrium to the right) pouring it in (lots of) cold water may give a better yield and is easier than filtering the almost pure acids.

Of course I did, just didnt mention it.
I like larger batches as I hate it to work with little amounts.

Here´s the final, still wet, product.

/edit
ehm guys, whats wrong with the picture upload ?
it tells me its done, but it doesnt appear in my post

Make an account at photobucket.com, you can dump your pics there and link to here.
With HE's I feel more comfortable with small amounts, but that's me...

Ok, MHN is harder to neutralise than I thought...
I just washed it with a lot of water and recrystalized it.
Bad idea...

I´ll give it another try on saturday.

What went wrong? Did the solution turn yellow? I've had that problem before, the trick is to heat the EtOH (Take care that it isn't the stuff they use in hospitals, that contains pyridine, which destroys MHN) to boiling and thén add the MHN bit by bit. What it is all dissolved, add a pich of bicarb, and recristallise it.

Hm, I contained a white product of small (fluffy ?) crystals.
I wondered why it won´t dry, so I took a look at its ph and noticed that it was still a lot acidic.

It seems its hard to neutralise.

Are there any impurities in bicarb with can cause a yellow solution too ?
I gave MHN another try today, but as I added bicarb the solution turned yellow. (--> maybe NaHSO4 ???)

There was only about 20g MHN left at the end that time. (same amounts were used as the first time)

I´m a bit pissed of now...
The third synth that went down the toilett.


/edit
Is recrystalizing really necessary ?
Wouldn´t it be eough just to wash it with water and bicarb solutions ?

In my experience, recristalising is best. After some days, even after washing it very, very good it starts smelling to NO2. Wich such an instable nitro ester I wouldn't take the risk. Boomer however did sometime do something like adding MHN in loads of water + bicarb and put it in a blender, which seems to work.

What is the problem with recristalisation, I alway just heated the alcohol in a hot water bath, added (half wet) MHN untill no more would dissolve, I added a bit bicarb afterwards, and let the beaker cool down. The next day you filter out the MHN and there you go. The problem in getting pure nitro esters is that you can have some with 4, some with 5, and some with 6 nitro groups, and you need to separate them carefully...

What kind of EtOh do you use? Be sure there is no pyridine in, that will destroy for sure the MHN!!
Besides, there is no reason to flush 20 grams of MHN through the toilet, that amount is still good for 20 caps!

The alcohol doesnt contain pyridine !
But some sulphat was formed wich turned the solution yellow. (NaHSO4, ethylsulphat ?, ?)

As I dont know how MHN react with them I flushed it down the toilett.
You know, saftey first.
You don´t have to mention everything 2 times, I can read. ;)


I guess the problem is, that I thought recrystalizing neutralize it anyway, wich is just wrong. I never washed it with bicarb solution before, just with a lot of water. Not that bad at all, mannitol is about 12€ the kg here.

While checking the Patents regarding Mannitole Hexanitrate I found differing results wheter MHN can be ignited with a bridgewire or heat in general or if another primary charge for setting off the MHN base charge is needed.

Did anyone succeed in reliably setting off MHN directly with an electric fuse?

While it has been nearly 3 years since anyone posted in this thread, replying to old threads is OK if you actually had something salient to say.

The last two posters in this thread - Child-of-Bodom (Last Activity: April 16th, 2006) and Vinci (Last Activity: January 23rd, 2008), have not been around in a long time. Asking questions of and talking to people who are no longer here is the basic definition of necromancy.