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Quantum
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[*] posted on 11-12-2003 at 20:08
Ideas for first experiment?


I have my scale and my glassware. I have searched around for an idea but everything looks too hard or too exotic chemicals involved. Because I am just starting out I am looking for something to make that will:
Teach me about the chemistry involoved
Be easy to make with my equipment and chems
Fun
I have basic chemical knowlage(symbles,elements,reactions) but I can't seem to find something that is easy and sort of safe to do with household chems yet produces something cool. Also my parents will be happy if I prove I am learning something and not just fucking around. I was thinking something along the lines of a simple distalation or something but I don't know.

I have:
3 Flat bottem 500ml flasks
1 400ml beaker
stiring rods
thermometer(-10-110C)
100ml graduate
1 500ml erln. flask
achohal burner(its an alchohol lamp about 4" tall)
scale

I can get:
KNO3
S
Borric acid
NaOH
I have other stuff but its more common like rubbing alcohal and just random OTC stuff in my house

Any ideas about a simple synthisis or something along those lines? I have no ideas:(

[Edited on 12-12-2003 by Quantum]




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[*] posted on 11-12-2003 at 20:20
make simple esters


Try making ethyl and isopropyl esters, since both of those alcohols are readily available. Try making oxalic, citric, acetic, or tartaric esters, depending on what acids you can easily find. If you can afford to order other alcohols and acids, you can make a more interesting variety of esters. Simply heating the alcohol and acid together for a few hours with a bit of sulfuric acid as catalyst will enable you to prepare a variety of simple esters in moderate yield.
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Quantum
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[*] posted on 11-12-2003 at 20:54


I have heard that esters have interesting smells, is that true? Yes I have isopropyl alchohol and some citric and acetic. What is oxalic and where can you get it? I have no H2SO4:( Can I use vinager or some other weaker acid as a catalyst. I could try to concentrate the vinegar by boiling if the acetic acid has a higher boiling point than the water. What are some of the propertesy of these esters?



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Mumbles
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[*] posted on 12-12-2003 at 15:04


butyl acetate pear
octyl acetate orange
amyl acetate banana
ethyl butyrate pineapple
methyl butyrate apple
methyl salicylate wintergreen
ethyl propionate fruity
ethyl mercaptan(not an ester but it is the skunk smell)

Unfortunatly you are going to need either sulfuric, or HCl for this. The H<sup>+</sup> ion acts as a catalyst. I think it also has to come from a mineral acid. Vinegar, or acetic acid, is a carboxylic acid. These are what actually react with the alcohols.

The esters are quite fragrant. For the most part esters are flammable liquids. Most are fairly volitile. Some of the esters are poisonous, some arn't. You really just have to look it up.
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[*] posted on 12-12-2003 at 19:47


Hmm...my advice, just look around for something interesting to you, and then dive in and get your hands dirty. My first experiments were far from safe, and I had much less knowledge than you do. I just stumbled across something interesting and gave it a try. It wasn't always a pleasant experience-- especially getting an NaOH burn from a silly Anarchist Cookbook Pressure Bottle. But it was exciting, even if it was k3w|_ and far from novel.

I still work the same way. If some random thing catches my eye, I will go out to the garage and try it ( that flavor chemistry has now caught my attention too, btw ) or I make plans to try it and never get around to it :P .

If materials are your issue, don't worry about it. You will get chemicals over time. Buy them as you need them for a given reaction, and then save what you have left over. Over time, you'll gather many many chemicals, and soon think to yourself "Now what can I flush down the toilet to make room for this new chemical?"
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[*] posted on 12-12-2003 at 20:30


you may find this helpful, today i made methyl salicylate, and it was pretty damn cool IMO.

i took about 25ml of methanol and added 4 grams of crushed up asprin. i swirled it around and let it disolve then filtered it through a coffee filter to remove the white crap. i added a few ml of concentrated sulfuric acid to the filtrate and swirled it in. i covered the beaker with Al foil and set it on a hot plate and warmed it for about twenty minutes, then i took it off, let it cool, and smelt it. VERY wintergreeny!




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[*] posted on 12-12-2003 at 22:11


I too, tried the methyl salicylate synth today, following reactants from Madog. (Common note: 10 aspirins mass out to be around 4 grams) However, where he succeded, I failed. Mine was mostly thrown together, in much the same manner that Samosa experiments...
1. Something catches your eye
2. You do a mental rundown of the chems you have, and what you can do similar.
3. You clean some glassware and just go do it.

First, I didn't filter out the white junk left on the bottome. Second, I added more than likely far too little sulfuric, as in around 1ml. Third, I negated the heating process for extended time. The only heating I did was swirling the flask over a propane torch.
Madog obviously got good results, and it's a quick and cheap synth. On note of most of the other esters Mumbles mentioned: the acids and alcohols mentioned are more than likely non obtainable by the home chemist except for a few in far spread cases. We did a lab in chemistry last year dealing with most those esters...butyric acid, that stuff is horrible. There's a whimsy topic I made from that day while in school, and the butyric acid stench had drifted through the campus.

I'm definately going to get the oil of wintergreen working, as it's just in time for some festive holiday cheer.




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[*] posted on 13-12-2003 at 02:24
oh! butyric acid!


It certainly is nasty stuff, but I should mention that it can be obtained at home without difficulty. One time I deliberately made it from the hydrolysis of old butter (it was starting to show mold and I figured it wasn't good for much else!) Another time I accidentally obtained it experimenting with starch fermentation - what a stench!

Sadly, I'm not sure how you'd go about preparing the purified acid at home from a biologically-derived mixture.
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wink.gif posted on 13-12-2003 at 07:22


My first ester synth was the nitric ester of glycerine...
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[*] posted on 13-12-2003 at 08:27


Nice! polverone,I´m trying to do the same (but with fresh butter). So I´m glad to read that I´m on the right way! I´m at the saponification step (means: I boiled 100g butter with about 70g KOH in aqueous sln. My next steps would be:
-to acidify the sln. (to free the faty acids)
-warm the sln. only a bit (to get the higher faty acids melt)
-let cool the sln. and filtrate off the now solid faty acids.
-give some NaOH or KOH to the sln (until pH>7 and evaporate
-extract the remaining with EtOH or Acetone (I hope the butyrates are suluble!)
-evaporate again and destill with sulfuric acid to get the pure acid.

do you think this should work? I didn´t come to the idea to use old butter! F**k!! I think the output should be much higher since I read about (fresh) butter containing only about 2% of butyric acid!

Oh, by the way: maybe I have a gift for you polverone! since I´m a very lucky guy and had the chanc to buy three books of the Beilstein-collection (from1886!!!) (for about 330$) I could help you with getting butyric acid out of your fermentation. If you´re intrested tell me what you used I can give you informations about preparing butyric acid from 1)rice or starch 2)potatoe starch

Sorry to all! I´m not able to give you an electronic copy of this trerasure since I have no chance to use a scanner etc. But it should not be too difficult if someone has acces to a library of a university to get informations from newer versions of the Beilstein-encyclopedia!
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[*] posted on 13-12-2003 at 15:04


The library I regularly use has Beilstein and many other of the famous older German books of chemistry... But they were purchased in the 1950s and earlier, so they are the original German texts rather than English translations, and I studied French in school, not German!

In my fermentation experiment I used corn starch, ordinary bakers' yeast, a little sugar to get the yeast started, phosphoric acid, ammonium nitrate, and potassium carbonate to supply main nutrients, and a multi-vitamin pill to supply trace nutrients. It fermented for several days in a plastic jug in warm weather. The starch formed a viscous mass with a terrible stench like that of my butter hydrolysis experiment.

I've read elsewhere that one can obtain butyric acid through microbial action by adding old cheese to a mixture of starch, water, and calcium carbonate. See http://en.wikipedia.org/wiki/Butyric_acid.
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[*] posted on 13-12-2003 at 16:03


Fine! I like Beilstein for it´s not only a source for further search of information but often a direct source of synthesizing-methods!

Hm,so i have this ´recipe´ for you:
(hey, and the first part sounds realy tasty;))
5kg rice (or starch) are boiled with 60l Water for some hours.After letting cool a mixture of 60g malt and 2l milk are added also 1kg meat (in fine pieces) and chalk.
This mixture stands some weeks at 25-30°C with stirring from time to time. when the gas-production had deceased the mixture is filtrated and boiled. Ca-butyrate precipiates (Ca-acetate and -capronate stay in solution)The Ca-salt is filtrated while boiling and decomposed with conc. HCl (or the Ca-salt is precipiated with Na-carbonate, filtrated, the sln. evaporated to dryness and decomposed with sulfuric acid (sorry, no concentration given) For purification the butyric acid is solved in water, the oily capronic acid is filtered off, the filtrate is neutralized with chalk and the sln. is evaporated. By this the Ca-salt precipiates and is separated. Finaly it is decomposed with HCl.

Though it sounds very strange I hope this could help you. But be careful! And always wear your lab-coat during this experiment!;););)
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[*] posted on 13-12-2003 at 16:09


If you produce something that stinks as bad as butyric acid as your first reaction, your parents might not want you to try a second.
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cool.gif posted on 15-12-2003 at 23:14
Methyl salicylate.


I too have just made this today with great success! the mixture turned purple and made a very powerful wintergreen smell.:D



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[*] posted on 18-12-2003 at 15:46


Well, five days later, my methyl salicylate is showing signs of mintiness. It has just been sitting on a shelf, and stirred occasionally and whenever I remembered it. The smell is there, but it isn't as strong as it could be, more than likely due to the fact that it isn't completely esterized. Yea, fun experient, cheap and simple, too.



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[*] posted on 13-1-2004 at 04:19


I believe there's been a mix-up in the list of ester scents, namely the iso-amyl acetate smells like pear, not banana. I have five bottles of this solvent so I noticed, but I didn't check the entire list. The included file is a short treatise on the subject, from Geoffrey Martin's "Industrial Chemistry" (1952).

The wintergreen synth is really a nice one, and it succeeds easily, esp. if more conc. H2SO4 is added to pull water created during esterification. But I have a question: what happens to the acetic acid bonded to the salicylic acid? One other thing to consider is that methanol is a highly toxic and yet very volatile substance so heating it in an poorly ventilated area can lead to poisoning. Even very small doses are poisonous to the optical nerve and produce visual impairment. So this is a great demo, but without a fume hood...

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biggrin.gif posted on 13-1-2004 at 19:32


Acetone peroxide and Nitroglycerin are both very easy and reguire only store bought materials. (They certainly are fun too)



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[*] posted on 13-1-2004 at 20:50


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IgnorantlyIntelligent, suggesting the synthesis of high explosives, and fairly sensitive ones at that, is not a good idea for someone who wants "beginner"-type experiments. Also, the original poster wanted something "sort of safe" that would prove he was learning and not "just fucking around."
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[*] posted on 15-1-2004 at 14:17


Was anyone elses methyl salicylaye an solid? I made some for a lab at school yesterday, and after heating the 10mL methanol and 3g SA for 10 min at 70 C then cooling, it precipated as a solid. the way that it has been mentioned in this thread made it sound like a liquid.
I also made ethyl ethanoate: liqid with a smell similar to acetone
and Ethyl salicylate: liquid with a minty smell.
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[*] posted on 15-1-2004 at 16:10


It is a liquid, viscous though. I think there is a 95% chance you didn't do it right. What sounds like to me is that you boiled off the CH3OH and the Salicylic acid crystalised. You have to add a Sulfuric Acid catalyst. I think it's the H<sup>+</sup> that catylises the reaction. It's either that, or in addition to that, the Sulfuric Acid soaks up water pushing the equilibrium to the right.
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[*] posted on 15-1-2004 at 18:02


I had added the sulfuric acid catalyst, this was a lab done at school with directions right out of the textbook(and followed corectly) and after I was finished I did get the wintergreen smell.
I believe everyone in the class got a solid too.
Mabey using aspirin instead of SA makes a slightly diffferent ester?

My teacher let me keep the solid so Is there a certain test I can do to determine if it is SA or the ester?-would a simple neutralization work?

[Edited on 16-1-2004 by rogue chemist]
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[*] posted on 15-1-2004 at 18:48


Asprin would, by my knowledge, produce methyl acetate, or at least Acetic Acid, in addition to Methyl Salicyliate. I've tried the one with the asprin posted by Madog. I get an acetic smell. I got a green viscous liquid, that eventually solidified. I didn't purify the asprin at all.

Asprin breaks down in the presence of Sulfuric acid to Acetic Acid and Salicylic acid.

Now, since you actually did use a catalyst, I'm not sure what went wrong. Methyl Salicyliate is a liquid. http://physchem.ox.ac.uk/MSDS/ME/methyl_salicylate.html Perhaps a longer heating period is needed. One test I can think of is to dissolve it in water. Add a small amount of baking soda. The acid should be neutralised and give off CO2 at a decent rate. Methyl Salicylicate probably wont. There is the problem of Sulfuric remaining though.

Neither product are too soluble in water however.
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[*] posted on 15-1-2004 at 18:50
This is kinda cool!


MAKING A SOLID POLYMER
"SUPER BALL"
INTRODUCTION:


Two common liquids are mixed, and the reaction makes a solid that has the properties of rubber. This solid is a polymer. In this lab, you will produce a solid, silicate based polymer.
Wear safety goggles and plastic gloves.

MATERIALS:

Safety goggles
Plastic disposable gloves
Sodium silicate (water glass) solution, 20 mL
Ethyl alcohol, 5-10 mL
Small paper cup for each solution
Stirring stick
Paper towels

PROCEDURE:

1. Measure 20 mL of sodium silicate solution and pour it into a small paper cup.Avoid contact with your skin.

2. Place 5 mL of ethyl alcohol in another paper cup. Remember, alcohol is flammable.

3. Add the alcohol to the sodium silicate solution.

4. Using a circular motion, stir with the stick until the substance formed is solid.

5. Place the polymer in the palm of your hand and gently press with the palm of the other hand until a spherical ball that no longer crumbles is formed. Be patient. Moisten the ball occasionally by holding it in a small stream of water from the faucet.

6. Try bouncing your ball.

7. Store the ball in a small plastic bag. If it crumbles, it can be re-formed.

REACTION:


Silicon is a very interesting type of atom. Like carbon, silicon makes four chemical bonds and can branch out in 4 directions to make long chains. In sodium silicate, the silicon atom is fonded to four oxygen atoms and is not linked in any chains. The ethyl alcohol has just two carbon atoms. When sodium silicate and ethyl alcohol are put together, the silicate particles begin to link up with each other to form long chains as the ethyl groups ( sometimes shown as “R”;) replace oxygen atoms in the silicate ion. Some become cross-linked between chains. Water molecules are byproducts of the formation of the polymerization bond.
The large molecule is a solid. It is a type of silicone polymer:


R R
| |
O | O | O
/ \ | / \ | / \ /
Si Si Si
| | |
R R R

reprinted w/out permission from Labdad




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[*] posted on 15-1-2004 at 18:54
So is this!


CLEAR FLUID POLYMER
"SLIME"
INTRODUCTION:


A polymer is a very large molecule that is like a chain of smaller (often identical), molecules linked together. In this experiment, you will mix two clear solutions in a paper cup. You will produce a fluid polymer. If green food coloring is added, the product will be like the commercial polymer, slime.
SAFETY: Wear safety goggles and plastic gloves.

MATERIALS:

Safety goggles
Plastic disposable gloves
Polyvinal alcohol, 4% solution
Sodium borate, 4% solution
Small paper cups and stir stick
Food color (preferably green)

PROCEDURE:

1. Place 20 mL of polyvinyl alcohol solution in a paper cup.

2. Optional: Add food coloring to the desired color, and stir to mix completely.

3. Add 3 mL of sodium borate solution

4. Using a circular motion, stir vigorously with a stir stick

5. As the solution begins to solidify, continue to stir.

6. When a gel has formed, remove it and continue to shape it with your hands.

7. Investigate the different ways your polymer will act.
Does it flow? Can it be flattened? Does it fracture(crack)? Does it get hot or cold when it flows? Will it bounce?

REACTIONS:


When the sodium borate, Na2[B4O5(OH)4] * 8H2O , is added to the polyvinal alcohol, [CH2CHOH]x , a cross-linked polymer is formed. The new polymer is composed of strands of polyvinal alcohol held together side-by-side (cross-linked) by the borate particles.
--- polyvinal alcohol ----- polyvinal alcohol ----- polyvinal alcohol ---
|
| |
| |
|
borate borate borate
|
| |
| |
|
--- polyvinal alcohol ----- polyvinal alcohol ----- polyvinal alcohol ---

reprinted w/out permission from Labdad




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[*] posted on 15-1-2004 at 18:58
How about something useful?


SAPONIFICATION
PREPARATION OF SOAP

INTRODUCTION:

The preparation of soap from fat and lye has been, historically, a household task. Only in the last century has the making of soap become a commercial undertaking. Our ancestors made soap by boiling animal fats with the lye obtained from leaching wood ashes. In this experiment, we will make soap by the same process, called saponification, but will use modern ingredients.

In the process of making soap, animal fat, which is a triglyceride, is hydrolyzed by the action of a strong base, such as sodium hydroxide, and heat. The resulting products are soap and glycerol:
CAUTION: Safety goggles must be warn throughout this experiment. This lab is intended to be done in a school lab, with adult supervision. Sodium hydroxide is very caustic, and can cause severe burns to the skin, especially when hot.


This is an investigative lab of the SAPONIFICATION process. If you wish to make soap in volume, search the web for a web page dealing with the making of soap as a craft.
MATERIALS NEEDED:

*80 ml of 6 Molar NaOH solution
15 grams of lard
75 ml of distilled water
**300 ml hot sodium chloride solution
100-ml graduated cylinder
Wire screen
Ring stand
Ring
Wire gauze
Burner
Tongs
Stirring rod
400-ml beaker
250-ml beaker

* To make 6 molar sodium hydroxide, dissolve 19.2 grams of NaOH in enough water to make a total volume of 80 ml.
** This is just a saturated solution of NaCl.

PROCEDURE:

1. Obtain 80 ml of 6 molar NaOH and 15 grams of lard, and place 40 ml of the NaOH solution and the lard in a 400-ml beaker.

2. Heat to boiling, on a standard ring stand set-up, then continue boiling the mixture over the lowest flame that will sustain the boiling process. Stir the mixture constantly to avoid spattering. If Spattering occurs, remove the flame and continue stirring the mixture. Replace the flame and continue heating after the spattering stops.

3. Continue boiling and stirring for about 20 minutes, or until it appears that most of the water has been evaporated. Then carefully add the remaining 40 ml of NaOH solution and continue boiling for an additional 20 minutes, or until most of the water has boiled off. DO NOT LET IT BOIL DRY.

4. As the crude soap cools, a waxy solid should form. Add to it about 25 ml of distilled water and about 100 ml of hot, saturated sodium chloride solution. Stir the mixture, breaking up lumps with your stirring rod. Decant the wash solution by pouring it through a wire screen, which will trap small soap particles.

5. Repeat the wash process twice. After the final washing, press the soap between two sheets of paper towlling to expel as much water as possible.

YOU HAVE MADE LYE SOAP.

reprinted w/out permission from Labdad




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