05-26-04 03:17
No 509622
Well SWIG has finally caved in to the LWR. He wants to reduce a small amount and needs a few tips before hes off to dreamland.
Tell SWIG if his ratios are right for a 48Hr LWR:
E-5.00G
MBRP-1.65G
I2(from tinc.)-6.00G
DH20-4ML
All precursors will bee as clean and dry as possible.
This is what SWIG has to work with:
Flask-500ML Flat Bottom
This will be connected to a 6'long 3/4" braided hose that has one looped in it and a punch ballon on the end.
Heat source-hotplate with a skillet filled with sand.
Now for questions:
1. In what order should SWIG add his precursors including the DH20?
2. Would it be safe for SWIG to leave the reaction for a long as 12 hours?
3. Does SWIG need to increase the temp. at any time during the reaction?
SWIGs main concern is having to leave the reaction for such a long period of time. SWIG plans on adding everything to the flask, placing it on the heat source, then maybe staying for a few minutes before he has to leave his hidey hole. The next time SWIG will have a chance to check up on how things is going will be around the 12 hour mark. Any feedback would be much help. Thanks.
(Deranged)
05-26-04 04:40
No 509643
add more rp, chances are your 1.6 is more like 0.8 in reality
ABM#5
.em evigrof doG yam neht emirc a si sdrawkcab gnitsop fI
(Hive Addict)
05-26-04 04:42
No 509644
Before starting...make sure the sandbath is calibrated properly so the flask will be sitting in 90-100°C for the complete rxn time.
This can be accomplished by using a flask with h2o and a thermometer extended down into the h2o.
Adjust the thermostat control until 95°C is constant.
Some times it doesn't hurt to UP the temp during the last two hours depending on visuals and smell to insure complete reduction but don't exceed 220°C. Any higher than 220C or any longer than 2hours runs the risk of SpaceDope Stash. Ibees gone safely at 220C for 4hours but it's pushing it.
Another area of concern is MBRP, Ibee would up the MBRP to at least 2.5G-3G
Since this is a smaller nano, if a smaller flask can be used, 500ml is pretty roomy and excessive.
Ibee's used little 40ml salt shakers on 5g LWR rxns successfully.
There is no violent eruptions of excessive Growth spurts that a 250ml wouldn't handle with ease unattended.
The rxn can be left unattended for the full 48 if all safety measures are in place.
The best way to insure proper safety measures are adequate enough is to run a sandbath with just h2o in a balloon capped flask for a long period. Sometimes it's the only safe way for unforeseen or unexpected events to be noted and corrected.
This is in lieu of having had successful runs to judge by.
One can never bee too careful when learning and Ibee likes to set up little experiments like this when venturing off into unknown territory. It's also good learning practice to devise little side mock experiment runs if one has the patience.
Now....we will have a series of preference based suggestions on the order in which is best on mixing the precursors.
Since it's not a fast take off rxn, the subtlty of mixing with ample h2o as a third ingredient will quench the alarms you'll likely hear about making HI first as the best way.
You can do it that way
Mix I2 and dh2o then add RP and heat til HI is produced then add E,
But Ibee still adds E to the Flask first, then adds I2 and mixes until liquid. This gives the I2 clumps a chance to break down some and intimately mix with the E. Then adds dh2o, mixes by gently swirling, then adds RP and stirs thoroughly before capping off and heating!
Sounds like everything is covered. If anything was missed I'm sure some other bees will chime in!
Good Luck, Bee confident, and above all bee patient!
Avoid looking for signs!
This rxn is the most forgiving compared to the Hot and fast and has a greater success rate than any Ibee's ever done.
And don't forget yer hat or the chant
a little less conversation, a little more reaction
(Of Counsel)
05-26-04 04:55
No 509646
You are using matchbook red phos, and using the molar amount of red phos. You are gambling here. You are gambling that the red phos is all red phos. It might not be. It might not be as clean as you think, and part of it might be glass. I suggest with first use lab grade red phos that a 1:0.4 ratio be used, E:rP. With mbrp, first use, I'd suggest you use a 1:0.75 ratio, and err on the safe side. I've done successful LWR's with mbrP as low as 1:0.5; I don't trust it well enough to drop it to 1:0.33.
Add the pseudo, water, red phos and swirl to mix. Then add the I2. Bring the temp up slowly, over twenty minutes or so, and only heat after the initial reaction between the I2 and the red Phos dies down. You should be wet enough to avoid any problems with byproduct formation. You shouldn't see any smoke to speak of. You don't need to.
The flask you use is too large for this size reaction. You are spreading this reaction out too thin, risking hot spots and uneven reduction. Better to use a smaller flask. I recommend a round bottom one.
I do not know how you plan to seal your hose. If you were using a condenser and an oil bath, I'd be a little happier telling you to go on and let it run. If you are new to this, I don't recommend that you walk off an leave it unattended. If you make the first hour to two hours with no seal problems, have consistent, even heat, and no increase or decrease in balloon size, you are likely good to leave it alone for the next few hours. No way to say for sure without knowing more about your setup or experience level.
After you get the flask contents up to about 100C, or just a little under it, you need not increase the heat again. Let it sit and simmer till done. I'd recommend 36 hours at least. Note that the sand bath will need to be hotter than this to have the flask contents reach the 95-97C temp.
After the first few hours you can up the temp, but I do not recommend going over 120C internal temp and do not consider the higher temp necessary to complete reduction. The biggest risk of by product formation is early in the reaction. I like to do the reaction without ever opening it up if I can, and while a lot can be said for making your HI then adding the E, I think you will find you are wet enough that you will have no problems.
mostly harmless
(Deranged)
05-26-04 05:36
No 509658
gee, you guys sure have alot of spare time on your hands
ABM#5
.em evigrof doG yam neht emirc a si sdrawkcab gnitsop fI
(Stranger)
05-26-04 05:38
No 509659
Thanks animal, ware and geez for the quick responses. Geez, SWIG thinks the MBRP will be ok to use in his upcoming dream. SWIG has already used it once in another dream which, in my humble opinion, make the MBRP cleaner (if properly cleaned afterwards).
SWIGs experience is limited to only hot-n-dry dreams. SWIG has done enough of them in his time and is happy with his results. SWIGs dreams are very consistent in regards to yeilds, potency, etc.
SWIGs is confident with his braided hose and punch ballon set up. SWIG plans on buying a new hose and connector before dreaming just to bee on the safe side. He figures if the set up can handle the stress from the high temp. of a hot-n-dry reaction then it should easy work on a LWR.
As for the 500ml flask, will it hurt the reaction to the point of failure? SWIG has had positive results using as little as 3g of psuedo with this flask. But SWIGs no pro so if it is imperative that SWIG uses a smaller flask then he will buy one.
(BEE-OTCH)
05-26-04 05:39
No 509660
IMO, it's never a good idea to let a reaction run unchecked for 12 hours.
On time is when I get there.
(Hive Addict)
05-26-04 06:02
No 509663
Okay...where is this course at? You know....The one that will teach me to type as concise as Geez!
I'd blame it on ADD but I'm aready using that excuse for my "need for speed" excuse
Animal...I hear ya!
Stoni: I fully respect your concern/opinion and agree that it's always best to air on the side of caution and safety.
Frankly...I found it hard to beelieve at first that the levels of anticipation would ever allow any bee to leave a trxn unattended for more that 4 hours.
Until the rxn got to be so boring, Ibee was one of those bees. After a few months, it got to bee rather routine doing this unattended and as I stated, Ibee had several failsafes developed and in place that he felt comfortable with and have yet to fail him yet.
Geez demonstrates his expressions perfectly and leaves me envious that I lack the ability that he displays with such ease when getting the facts on the board!
Anyone that can read can see I struggle, but hey....I'm thankful geez has learned the not so fine art of wareamiese.
Giver_hell: The reasons that geez pointed out on flask size are such because of the Hotspots that can develope over longer cook time and the refluxing that takes place and the reactant transference.
Follow his direction and I assure you, you won't be let down!
a little less conversation, a little more reaction
(Stranger)
05-26-04 06:21
No 509664
SWIG is feeling kinda stupid at the moment. At first SWIG couldn't see how hot spot would occur but if left still over such a long period of time then it becomes clear that it most definitely would. Since SWIG is a fast dreamer that seems to feel the need to swirl around the flask often, mixing and moving the reactants with every spin then one can see why SWIG didn't think about the hot spots.
SWIG will not use the 500ml flask in the ever-so-close dream. Tell SWIG something, what other "ghetto" flasks could SWIG use? A 40ml salt shaker was mentioned. Any other ideas?
(Hive Addict)
05-26-04 08:42
No 509683
"IMO, it's never a good idea to let a reaction run unchecked for 12 hours."
No doubt! Swim is surprised that this wasn't mentioned earlier in the thread. Even with a push-pull unit Swim wouldn't even contemplate doing such a thing. Then again, with push-pulls there is an increased margin of safety.
At oilbath temps of 120-135C, what do you think might happen just from leaving a long wet reflux unattended for 30 minutes after a small pinhole leak in a 16" punch balloon?
A 5g rxn, probably not much but ya never know.
Do the rxn when you have more time to monitor its activity from start to finish.
Even if Swim decides to take a nap in an adjoining room he still makes sure there is someone available to check for smoke or balloon deflation every 15 minutes.
The two biggest reasons for drug lab raids are snitches and fires.
With meticulous security precautions, the rats can bee totally avoided, fires can happen to anyone and Swim would hope SWIY would want to bee around so the fire dept and CLRT don't necessarily have to earn their paycheck to do YOUR job for you.
Swim knows people that are doing more time in prison for consp to manufacture and child endangerment then others are doing for 3rd degree manslaughter!
Keep in mind, things have a tendency to escalate and 3rd degree murder usually is a gift after a long wait in jail (up to a yr) with many refused plea-bargains.
There is also possession of chemicals and eqpt with the intent to manufacture (which isnt much more leniant in terms of sentencing)
Lets not start any bad habits that could prove detrimental to your freedom.
Swim has dealt with rxn leaks, just looking out, absorb what is useful and reject the rest.
If you are going to do this, make sure it is an outdoors location with no trace to your identity or anyone you particularly care about.
Refuse/Resist
(Stranger)
05-26-04 13:38
No 509719
Well shit, SWIG is stumped on what to do. Choices, choices. To cook or not to cook? Hmm, here is the deal. SWIG has to sneak to his hidey hole when it get completely dark outside which happens around 9:00pm. After setting everything up and starting the reaction, SWIM would have to leave the spot and, as long as the fake family (SWIG named his new neighbors this cause SWIG thinks they really are undercover DEA spying on me hidey hole) isn't out with their binoculars, SWIG could check up maybe 3 times during the night. When sun comes up SWIG will have to wait until about noon before going on his visit so thats a 6hr wait. After that SWIG could check up as many times as needed for the entire day. Same goes for the next night and day. Soooooo, the longest time in between checkups will now be 6 hours. As far as fires are concerned SWIG will be placing the entire setup on a concrete floor that has plenty of space around and above it. So if a fire does occur then the only then that will burn will be the setup itself. Smoke is no concern really as the hidey hole is pretty airtight. So does everyone agree that SWIG should bee ok with the new 6hr in between checkups time?
(Hive Addict)
05-26-04 14:56
No 509729
Damn....SWIG wasn't kidding when he aptly named this thread "Caved In"
I'm not going to give any morality speeches here, but I liked it better when I felt like the instruction was beeing offered to an average ordinary bee and not CommandoChiliBee
The reason Ibee felt no large degree of concern by offering the suggestion that a 12hr rxn unattendance was okay, was because SWIG_H reported using sand instead of oil, although Ibee's done 3day oil cooks with 8hr interval checks without incident over 72hours, and SWIG_H pointed out the fact that a braided hose would be used. The Hose greatly reduces the risk of pinhole leaks compared to a balloon affixed directly to the flask.
One of the advantages of doing a LWR is that the HI stays in the liquid phase for the most part compared to HotAndFast which has a tendency to generate lots of HI gas and sometimes violent precursor spitting upward potentially depositing HI acid on the balloon which immediately chews a hole in the balloon.
The rxn can go uncondensored and uncapped with a balloon so Ibee sees no real concern.
There might be greater risk of discovery revisiting this set-up that Ibee reals feels uncomfortable condoning...
But Hey....Bees are gonna do what they want and I'm here to help offer suggestions to help minimize the dangers.
I can't control self made dangers.
Ultimately SWIG_H will make the choice based on the info provided and if Ibee hasn't safely conducted that which he speaks of from experience, it wouldn't be written or offered as a way of doing it.
Safety factors for anybee might not bee the best set-up for the next bee. Use your common sense. And Above all make a checklist of the safety factors and potential mishaps. Do a mock run if you have to. After all there should be no real hurry here and if external things are rushing you, I'd suggest you wait until you are better prepared to see this thng through to where you can gaurantee a taste of the fruits from all this labor!
So choose wisely and Giver Hell!
a little less conversation, a little more reaction
(Of Counsel)
05-26-04 16:51
No 509741
(Rated as: good read)
Leaving a reaction to tend itself involves inherent risk. Accept that. since I started doing LWR's I have lost one reaction to a failed seal, which I could have avoided with a little more patience setting it up or by monitoring it more closely. I have done LWR's which tended themselves from hour two to hour forty eight. I did not do this because I wanted to ignore the reaction. I did it because I have to go to work, I live somewhere other than where the reaction is done, and I can't be in two places at once. I would never run a reaction in a residence or occupied structure without it being checked on a regular basis. I have and do run refluxes in an unoccupied building without the reaction being monitored, and have done so many, many times.
This is not to say I just slapped the stuff on a stove and left. Far from it. I use an oil bath that has a thermal limit switch. I use a pump with a continuous duty rating to circulate water through a condenser. I use a thick balloon atop a condenser adequate for the job. I have a vent to the outside with a small fan which pulls air off the ceiling and I have fan running over the top of the reaction. The entire operation is so rural that even a major fire will not bring a firetruck to the scene, or bring the police. I know. I've had a major fire at the location without any emergency response. The fire had nothing to do with a long wet reflux.
I use a power source that controls the pump and the heat source and will cut off if either shorts out. It does not, admittedly, kill the heat source should the pump fail. I've had the pump fail. I did not lose the reaction. I might have had I not checked on it at about the twenty four hour mark. Hard to say. I think having a small fan blowing across the condenser kept the glass cool enough during the pump's down time to let the condenser work at the rather gentle temperatures I run the reaction. I changed types of pumps after that failure, by the way.
Does anyone recommend you do a reflux without checking on it? Of course not. Does anyone do it? Certainly. Reality sometimes conflicts with total safety. You take the precautions you must make to avoid failure and loss, and do what you have to do to let the reaction reflux unattended. You do as much failure avoidance as you can before you leave it unattended.
I would be far less comfortable with a hose and balloon set up than I would with a condenser; I would be less comfortable with a hot plate than I would with a thermally limited, cool-touch oil bath as a heat source. I would not be comfortable with either if I was cooking at home, and would check on the reaction frequently. That said, with adequate planning, precaution and foresight, you can set a LWR to run by itself without constant supervision. Do it as a last resort, and do it only if it is truly necessary. Do not, however, conclude that you must be there 24/7. You don't. You will learn the capabilities and the limits of the equipment you use, and learn to run your reaction within those limits. The discussion about whether you should do a reaction unattended is one that addresses questions different than the discussion about whether you can do one bascially unattended. The answer to the first is most likely "no." The answer to the second is most likely "If you have to."
But be very careful out there.
mostly harmless
(Stranger)
05-26-04 19:24
No 509755
SWIG applauds both ware and geez for taking the time to write such long and in-depth, comprehensive replys to SWIGs ramblings. You both seem to thoroughly take the time to explain things in a unique manner that helps SWIG, and many others, better understand things. Your efforts are well appreciated. Well SWIG is going through with his dream after he finds a suitable flask for the small reduction that planned. Again, much thanks for the replys. Ware, LMAF after reading your post....CommandoChiliBee, SWIG likes it.
(Hive Addict)
05-27-04 01:18
No 509803
I often leave my rxns going for up to 8 hours unattended however, i don't use an oilbath, just a hotplate. I also use a condenser with a balloon on top that only inflates a little if any.
It seems that everyone beat me to the post so i guess ill have to edit mine. I just want to add that my lab has a ceramic tiled floor with concrete underneath that, the walls and ceiling are concrete and constant ventilation from fans blowing air from one open window to another on the opposite wall.
At the risk of being rated as dangerous, i am more concerned about my water heater exploding or a leak in my natural gas stove than i am of a lwr. I haven't checked on my water heater since i had it installed. I guess i should though since that was about 2 years ago.
It wasn't Me!
(Hive Bee)
05-27-04 11:15
No 509894
That say you maybe felt asleep and your waterpump broke. Your LWR setup was placed in the basement in a empty room with a window, which was opened a little. The setup was running without watercooling in, that say 8 hours, what is the worst that would happened? Is the HI-gas explosive?
(Hive Bee)
05-27-04 16:27
No 509926
There is some good advice above with respect to safety when leaving reactions alone. Although never advised, it sometimes is inevitable that one has to leave a reaction unattended. The only times I've supervised an entire 36-hour reflux is when I've been overusing the product of the previous reaction.
To avoid worrying about hose connections and water leakages with your condenser, I would recommend using a more efficient model, which you can use as an air condenser. I've used a double surface (Davies) condenser for a mild 36-hour reflux with no water running through it. The high boiling point of concentated HI means the condenser is efficient enough to act in this way; the surface of the condenser is cool less than halfway up. There is no sign (visible or otherwise) of reactants escaping - and that's without a balloon attached...
(Of Counsel)
05-27-04 21:08
No 509960
Worst case scenario is that the condenser doesn't contain the gasses, which escape, the reaction goes dry, and you burn up the feedstock. Expect the place to smell like a meth cook. HI has escaped into the room. (Rust never sleeps.)
I had a seal fail while I was elsewhere, and the reaction went dry before I returned. I had to air the place out for about twenty minutes, but other than that, there were no signs that anything unusual had happened. I did not have smoke, only odor. The temperature of the oil bath was about 125C; that wasn't hot enough to cause the dry flask contents to catch fire or smoke significantly. The time I had a water pump fail, I had no smoke or odor problem, but would have had an odor problem had I not checked in on the reaction when I did.
I m sure at some temperature a dry rP reaction will billow smoke out of the flask as the rP combusts. I don't know what temperature is needed to make such a thing happen. I know it doesn't happen in the temperature range of the LWR as I do it, which will not be over 120C.
The smart way to increase safety and decrease risk is to buy a flow-controlled kill switch that will shut all power to the reaction if the water flow from the pump stops for any reason.
mostly harmless
(Hive Addict)
05-27-04 23:46
No 509968
Expect the place to smell like a meth cook.
Hey now...I resemble that remark!
A funny thing happened at the lab the other day I felt that some might find interesting...
Really not worthy of it's own thread so I hope ya'll don't mind it being inserted here among other newbee concerns.
About three years ago the outside of the door to the lab was painted white.
Well over time it was noticed that outside around the edges of the door were starting to yellow some where the weather stripping failed and was never fixed. After AWE....it's only a lab right?
Never paid it much mind until Ibee decided to do some spring cleaning.
It had gone from yellow to brown since it was first noticed.
Well Ibee's lab in the building was the only one that looked like that even though other tenants do industrial type work and their doors are all greasy and kinda in need of painting too.
Ibee had the bright idea to use bleach in a spray bottle to spray the outside of the door to loosen up the brown.....
He started thinking...."The doors closed and haven't done any tinc extracting in while"
WARE THE HELL IS THAT I2 smell coming from?
You guessed it! Shhhhheeeeesh!
Let this be a lesson....don't cook alot in the same lab....or paint often!
Wonder how much I2 can be extracted from the walls?
a little less conversation, a little more reaction
(Of Counsel)
05-28-04 20:07
No 510077
Hey Ware... I recommend Kilz before painting if the walls are Iodine stained.
mostly harmless
(goat)
06-03-04 15:30
No 511216
here's a possible ghetto safety tip that has worked for swim:
after putting the 4 ingrediants together in the flask, out-side, allow a few seconds for the homongenous mix to liquify and generate a tiny amount of gas to drive out the air in the flask. then cap the flask w/ condensor/ and or balloon. there will bee less O2 and less pressure for the long slow ride that follows.
actually, the entire dream can bee done with negative pressure.
quite nicely.
implosion beecomes the new concern, which, imho, is far less likely with round glass than explosion. the curves in the glass ware have compressive strength in spades; tensile strength is nominal.