SaintCyril (Stranger)
07-10-02 23:24
No 330965
      TFMPP and Browning of Direct Compaction Binders  Bookmark   

Does anyone have any experience with, or any ideas regarding the following problem: 
When a mixture of 1-3 triflouromethyphenyl piperazine, 1-benzylpiperazine, and one of the following binder/lubricant combinations the following results were found.

With a binder combination of Dextrose (DiPac), and appropriate amounts of Mg Sterate And Steric acid, after pressing the tablets they appeared in every way to be sound; however, after one week storage in an amber glass bottle the tablets became encrusted in a oily brown layer, the inside of the tablet remained sound.

The same results were obtained with a Lactose (SuperTab) binder mixed with appropriate amounts of the beforementioned lubricants.  The browning process seemed to take slightly longer.

Again the same actives and lubricants were mixed with a Microcrystalline cellulose Binder (ProSolv)the tablets upon compaction had a yellowed color to them, after 5 days storage, no browning has occured, but the yellowing has covereed most of the tablet.

The above binders were again tried with the exception of steric acid, the die faces stuck up with the mixture, as would be expected, but it was within tolerance.  The results of this test are 4 days along, and appear to be less brown, but that could jus be due to the differance in observation.

The above binders were again pressed into tablets; however in this case BZP was deleted from the mixture and the ratio of TFMPP increased.  In this case within 3 days the tablets with the sugar based binders were completely oily, brown, gross.  This tests unfortunately was not done with the MCC binder.

Hopefully someone can add some insight to this problem.  It would be much appreciated.

Thanks,
Saint Cyril 
 
 
 
 
    foxy2
(Distinctive Doe)
07-11-02 10:35
No 331216
      ummm  Bookmark   

Hope your not planning on selling those as E.

If you do....
What goes around comes around.

Those who give up essential liberties for temporary safety deserve neither liberty nor safety
 
 
 
 
    Nemo_Tenetur
(Hive Bee)
07-11-02 15:51
No 331264
      try commercially available tableting aid ...  Bookmark   

I've compressed a mixture of 40 mg TFMPP-HCl and 120 mg N-Benzylpiperazine-HCl with 100 mg lactose-monohydrate and 40 mg tableting aid (mainly microcrystalline cellulose) without any problems. They remain unchanged even after months of storage. Sorry, it is illegal to post sources, but there's in Germany a big well-known chemical/pharamaceutical company which sells two or three different types of tableting aid (ready-for-use, no additional lubricants required) in 20-kilo-boxes, no smaller quantities available. You should invest several hundred Euros and buy a box, it really worked well. You can find it in their lab chemical catalogue.
 
 
 
 
    Osmium
(Stoni's sexual toy)
07-11-02 15:58
No 331265
      I've read in a pharm book that amines and lactose ...  Bookmark   

I've read in a pharm book that amines and lactose etc. aren't compatible and always wondered why everyone (including me tongue) used that combination. Maybe they were talking about amine freebases?

I'm not fat just horizontally disproportionate.
 
 
 
 
    SaintCyril
(Newbee)
07-17-02 03:11
No 333409
      Ethyl Cellulose  Bookmark   

Thanks to everyone who reponded privately, I fould a cure, ethyl cellulose.  Ethocel, and this binder only requires 10% thats right 10% of the total weight.

Anyhow if you have a similar problem, this will solve it.

Cy

So you need a precursor to a pecursor, just to make a precursor thats what the people told me . . .
 
 
 
 
    JiB_BANDiT
(Newbee)
07-24-02 22:48
No 336664
      I am very curious to know what has caused this ...  Bookmark   

I am very curious to know what has caused this browning/yellowing of these tablets. Obviously some sort of non-spontaneous chemical reaction is occuring here. You say using ethyl cellulose works, that's great and I'm happy to hear you have a solution. However I would really like to figure out from a chemistry perspective what's going on here.

Could it be that the stearic acid is reacting with the piperazine dihydrochloride salt? Perhaps not completely but in some sort of equilibrium?

Any info would definately be interesting!
 
 
 
 
    JiB_BANDiT
(Newbee)
07-24-02 22:50
No 336665
      Also, SaintCyril, I would be interested to know; ...  Bookmark   

Also, SaintCyril, I would be interested to know; are you using a home-made manual pill press or one of those big expensive professional automatic ones?
 
 
 
 
    JiB_BANDiT
(Hive Bee)
07-30-02 02:45
No 338711
      *BUMP*  Bookmark   

*BUMP*
 
 
 
 
    GOD
(Hive Addict)
07-30-02 02:59
No 338717
      utfse, or give the man a pm...  Bookmark   

utfse, or give the man a pm...

i FEEL funny.
 
 
 
 
    JiB_BANDiT
(Hive Bee)
07-31-02 04:38
No 339193
      I do not believe that this particular mystery has ...  Bookmark   

I do not believe that this particular mystery has even been encountered before, and therefore I do not believe that the answer exists in any sort of searchable database. UTFSE is getting to be used way too loosely around here in my opinion. If you simply don't give a fuck, then fine, don't read the thread and certainly don't waste everyone's time including yours writing out a useless response.

Anyhow, does anyone have a hypothesis or theory regarding what chemical reaction is occurring here?
 
 
 
 
    SaintCyril
(Hive Bee)
07-31-02 07:31
No 339251
      Apparently  Bookmark   

Apparently using a sudcrose or dextrose binder, with TFMPP, makes the sugar get somehow denatured into some sort of oily sibstance.  Seems to me like it MIGHT be some sort of oxidation because any piece of metal the mix touches: die tables, screens, even the brass inside the feeder shoe gets an oxidation effect.  By this I mean the steel turns into rust, and the brass turns green.  When Microcrystalline Cellulose is used alone it is necessary to use a press with higher pressure, 4t plus, a 2t just wont cut it. If ethyl cellulose is used then a lower pressure press can be used.  In storage now are samples which used a MCC/lactose mixture, after 2 weeks storage there appears to be no browning.  It should also be noted that once the MCC or ECC was used moisture from the air became a big problem in areas with humidity, and a lb of Drr-Rite was added into each 5gal bucket for 2 days, also a bad of Damp-Rid was placed into these rooms, and it seemed to correct the problem for the most part.

Cy

We are the people that your parents warned you about.
 
 
 
 
    java
(Newbee)
07-31-02 17:25
No 339400
      Ref.- Tableting problems  Bookmark   


http://www.bentham.org/ 

Currently there is s free access to the journal that  you need to check out  and othere for free at the above place and  a specific journal listed below , is also free to get whole article, I hope it helps

http://www.ingenta.com/isis/searching/ExpandSearch/ingenta?year_to=2002&year_from=1997&date_type=range&journal_type=words&title=tableting+&title_type=tka&database=1&newMatches=false&pageStart=1&index=9&WebLogicSession=PUfwnek10ABSBNchH5lk%7C-6755518938831412011/-1052814329/6/7051/7051/7052/7052/7051/-1
 
 
 
 
    JiB_BANDiT
(Hive Bee)
07-31-02 20:06
No 339444
      The steel parts rust because iron is a main ...  Bookmark   

The steel parts rust because iron is a main component of steel; the rust that you see formed is iron oxide. I do not know off hand what the metals are that are used to create the alloy brass, but from the green color you describe I would think copper. Anyhow, to prevent rust I would suggest using a sacrificial anode. A sacrificial anode is just a piece of metal that is more easily oxidized attached to the part that you want to spare from rust. The two best metals to use for this would be magnesium (the #1 choice) or aluminum which should also work. When I used to work as a dish washer at a crappy restaraunt the large metal sinks had chunks of magnesium bolted on underneath to prevent rust from occuring from the presence of water. The Mg(s) gets oxidized into MgO(s), and once the chunk of magnesium metal is all used up; about every ten years or so, it is replaced. I don't know if this would work for a solid compound which is causing an unwanted oxidation reaction to occurr, but I figured it was worth suggesting.
 
 
 
 
    JiBTECH_WARRiOR
(Stranger)
08-13-02 01:07
No 344768
      Some tablets were made with BZP using a pill ...  Bookmark   

Some tablets were made with BZP using a pill binder extracted from Asprin tablets, because no other pill binder was available at the time. Without going into the process used to seperate the pill binders from the tablets; the result is a pill binder with trace amounts of Asprin. The tablets within a couple days went brown and soft! Would this result be from a reaction with the ASA, or with some of the pill binders, perhaps sugars?
 
 
 
 
    foxy2
(Distinctive Doe)
08-13-02 01:51
No 344797
      Ummmm  Bookmark   

Mind if I ask why you produced those tablets?

Those who give up essential liberties for temporary safety deserve neither liberty nor safety
 
 
 
 
    JiBTECH_WARRiOR
(Stranger)
08-13-02 02:08
No 344811
      Tablets are desired because it is more convenient ...  Bookmark   

Tablets are desired because it is more convenient than having a drug scale (illegal?) around always and weighing out each dose individually. Also, tablets are easier to carry than a bag of powder and a scale. It is for convienience and legal reasons. Don't worry foxy, I am not planning on selling these as E. Many people gave SaintCyril lots of unwarranted bullshit about what he's doing instead of awnswers. Can someone please just answer my questions based on scientific fact or empirical knowledge?!?
 
 
 
 
    SaintCyril
(Hive Bee)
08-13-02 02:34
No 344835
      The sugars  Bookmark   

All of the sugar binders used alone seem to brown:
Lactose
Sucrose
Dextrose

The non-sugar binders do not brown:
Microcrystalline cellulose
Ethocrytaline cellulose
Starch
Scilified MCC

Look at the back of the pills you are grinding up and see what binders they have, steric acid and magnesium sulphate should be in the ingredients, and th eingredient before that will be your binders.

Cy

We are the people that your parents warned you about.
 
 
 
 
    JiBTECH_WARRiOR
(Newbee)
08-15-02 20:16
No 345698
      Ok, so now we all realize that piperazines should ...  Bookmark   

Ok, so now we all realize that piperazines should not be used in conjunction with sugar-based binders. Previously in this thread, Osmium mentioned that he read that amines were incompatable with sugars, however amphetamine based compounds are pressed into pills all the time, I would think using sugar based binder which are very common. I am wondering, are there any other drugs besides piperazines that should not be used with sugar based binders?

Also, I am extremely curious as to what in the structure of the BZP/TMFPP molecule would react with the sugar molecule to cause this unwanted reaction.
 
 
 
 
    Osmium
(Stoni's sexual toy)
08-15-02 23:37
No 345761
      Piperazines contain two basic nitrogens.  Bookmark   

Piperazines contain two basic nitrogens. Assuming that only one of them is neutralised during salt formation the other amine can still react with the binder.


I'm not fat just horizontally disproportionate.
 
 
 
 
    JiBTECH_WARRiOR
(Newbee)
08-16-02 00:51
No 345787
      Fascinating. Thank you Os! :-) :-D ;-)  Bookmark   

Fascinating. Thank you Os!smilelaughwink
 
 
 
 
    Ritter
(Master Whacker)
08-16-02 02:23
No 345817
      acid reaction with sugars  Bookmark   

One thing that must be kept in mind is that if there is any free acid left in the amine salt, it will decompose some sugars to a brown tar-like mess.  Did you make the HCl salt of the psychoactives yourself or were they purchased in the salt form?  If you made the salt yourself and didn't use proper purification techniques, there is a very good chance that this is the culprit!
 
 
 
 
    JiBTECH_WARRiOR
(Newbee)
08-16-02 11:52
No 345948
      The dihydrochloride salt form was purchased.  Bookmark   

The dihydrochloride salt form was purchased.