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nannah
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[*] posted on 24-5-2014 at 22:30
Beginning chemistry.


Hi guys. I have been looking forward to this moment for a while now. I have been saving up, reading different lab books, like Lange´s handbook, and now i just got my basic chemistry glassware set i bought on ebay.

So now i want to try on a synthesis, and thought i would want to use something that you get from the hardware store, like steel wool, and muriatic acid. Run the reaction, recrystillize, and in the end you end up with a chemical that of reagent grade, or almost as good as.

I have read all the lab manuals, and i am quite sure it could be done if you have concentrated HCl.

I have to go, the kids are up. :)

/nannah

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[*] posted on 24-5-2014 at 23:27


You could make iron II sulphate from steel and sulphuric acid. This would need to be re-crystallized to remove carbon particles though.





I never asked for this.
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[*] posted on 25-5-2014 at 02:05


Don't use straight 30% HCl though - the vigorous exothermic reaction will cause much of the HCl to boil away. Either dilute it or add it slowly so as not to waste acid. I find it is easier to remove the carbon particles by filtering than recrystallisation.



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[*] posted on 25-5-2014 at 03:18


Congratulations nannah !

I'm very new to chemistry myself (a few months). It's great.

Here's some experiments i did with Copper Sulphate (sold as tree stump remover) which all worked well :-
In each case, start with a solution of Copper Sulphate

1. Add Table Salt.
The Green crystals are TetraCloroCuprate.

2. Add Bicarbonate of Soda
The Pale blue stuff you get is Copper Carbonate

3. Add Ammonia
The beautiful deep purple colour is TetraammineCopper(II)suphate complex.

4. Add Aluminium and a pinch of salt
If you're lucky, you get aluminium sulfate.
If not you get a dark grey mess

If you can get Muriatic acid, add some to wire wool to get Ferrous Chloride (Green) then either bubble air through it for days, or add some Hydrogen Peroxide to get Ferric Chloride (Yellow/Brown).

Enjoy !




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[*] posted on 25-5-2014 at 06:50


Well, reagent grade chemicals will require some form of purification. A lot of the suggestions made offer a simple solution to purification (recrystallization). Another simple synthesis could be sulfuric acid to steal wool (stinky do that one outside and it is pretty slow). keep in mind steel wool also contains carbon and often grease. So filtration of the 'digested' solution through a cotton ball can aid in the removal of the dark stuff. The steel wool can also be de-greased with a solvent such as acetone, but that is probably extraneous for a lot of basic experiments.

[Edited on 25-5-2014 by smaerd]




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[*] posted on 26-5-2014 at 18:22


Quote: Originally posted by Oscilllator  
Don't use straight 30% HCl though - the vigorous exothermic reaction will cause much of the HCl to boil away. Either dilute it or add it slowly so as not to waste acid. I find it is easier to remove the carbon particles by filtering than recrystallisation.


I saw somewhere you can purify muriatic acid into what he called, reagent grade HCI. He had one plastic box, with a lid. In the box he had two smaller tubs, one with distilled water, one with 30% HCl. 24 h later, he had reagent grade HCl.

Ever heard of it, of tried it? Sounds good.

Quote: Originally posted by plante1999  
You could make iron II sulphate from steel and sulphuric acid. This would need to be re-crystallized to remove carbon particles though.



That´s the kind of stuff i want to do. It feels like i have read every lab manual a dozen times each. I just don´t have access to a lab, so i haven´t developed any lab skills. But i am thinking aboutdoing this experiment, and i was thinking i was going to distill some water in order to get the practice.

Quote: Originally posted by smaerd  
Well, reagent grade chemicals will require some form of purification. A lot of the suggestions made offer a simple solution to purification (recrystallization). Another simple synthesis could be sulfuric acid to steal wool (stinky do that one outside and it is pretty slow). keep in mind steel wool also contains carbon and often grease. So filtration of the 'digested' solution through a cotton ball can aid in the removal of the dark stuff. The steel wool can also be de-greased with a solvent such as acetone, but that is probably extraneous for a lot of basic experiments.

[Edited on 25-5-2014 by smaerd]


Thanks everbody for taking your time. :) Have a great day.
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[*] posted on 26-5-2014 at 18:40


This is my favorite part of chemistry, just enjoying tthe reactions and the idea of produciing something, something usefull, even if only to you. I'm looking forward to this summer, I'm hoping I'll have more acess to reagents, as parents can be limiting at times... but I love 'em!
Anyways, enjoy your reactions! What glassware did you get?




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[*] posted on 27-5-2014 at 16:20


I got a chemistry distilling kit from Laboy. I have heard both good and bad things about them, but i think its good enough for me for now.

So i hope to soon get some free time to try out the kit.

What distillations, besides water can i try? I haven´t even done simple distillation, so i guess it´s there i start.

I want to try to purify, OTC chems, and solvents.

I have a water aspirator that i plan to use when i do vacuum distillations, but i´m not sure if its got enough pull. I am saving up to get a two stage pump at some time.

Thanks again. :)
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[*] posted on 27-5-2014 at 16:57


Water aspirators work like a charm! :D Just make sure the connections are well sealed.

I wouldn't recommend distilling volatile/flammable solvents if you don't have some experience already. Distilling water is a good practice.

Making crystals of copper(II) salts is nice and harmless! If you let them time enough you can get some pretty nice ones.

If you're into organic chemistry and something more rewarding than precipitating salts (and feel confident to use small amounts of conc. H2SO4), you could try methyl salicylate! It gives the wonderful mint odor of some products. You can modify the procedure to make it from aspirin.
http://www.sciencemadness.org/member_publications/methyl_sal...

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[*] posted on 27-5-2014 at 17:30


Start maybe with the classic ethanol distillation. Not too much hazard there. Definitely read up on the techniques and hazards of distillation, but there's not too much too it. Be careful with ether's and things that form peroxides.

Water aspirator might be sufficient for some distillations but, keep in mind how much water will be wasted. Nothing wrong with Laboy, had a distillation set up and a few pieces of joint-ware from them for 4 or so years now, no issues. Even after some abuse. I prefer to buy American or second-hand glass, especially while Dr. Bob is around giving out amazing deals.




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[*] posted on 27-5-2014 at 23:57


Alcohol vapours and an open flame can, of course, explode !

For a very first distillation, why not measure a quantity of salt, dissolve it in a known volume of water, distill that solution, then weigh how much salt is left over, and whether the distillate is salty.

Also measure and record the Vapour Temperature as you do the distillation.

Boiling Water is not really safe either, but at least it won't explode.




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[*] posted on 28-5-2014 at 04:47


Quote:

I saw somewhere you can purify muriatic acid into what he called, reagent grade HCI. He had one plastic box, with a lid. In the box he had two smaller tubs, one with distilled water, one with 30% HCl. 24 h later, he had reagent grade HCl.

Ever heard of it, of tried it? Sounds good.




This relies on the fact that hydrogen chloride is volatile and most contaminants(iron mostly) are not volatile, due to this some of the hydrogen chloride leaves the initial mixture, becomes a gas, and dissolves in the distilled water. Some gas then leaves that water and travels back to the muriatic acid and this occurs until the system is in equilibrium. The clean acid is probably definable as reagent grade(If no chemicals from the plastics were leached), but has a concentration of slightly less than 15%.
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[*] posted on 28-5-2014 at 05:15


Do you have an old PC power supply? I have beautiful crystals of CuSO4 that I made following the electrochemical method here by NurdRage. My equipment consisted of a power supply, scraps of wire and a skinny flower vase. My "reagent" was old acid poured out of a car battery.

I got my local library to get me a copy of "Illustrated Guide to Home Chemistry Experiments", this book. I recommend it highly.
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[*] posted on 28-5-2014 at 09:39


Quote: Originally posted by aga  
Alcohol vapours and an open flame can, of course, explode !

For a very first distillation, why not measure a quantity of salt, dissolve it in a known volume of water, distill that solution, then weigh how much salt is left over, and whether the distillate is salty.

Also measure and record the Vapour Temperature as you do the distillation.

Boiling Water is not really safe either, but at least it won't explode.


Yeah, maybe i try that. It can be good practice. :)

Quote: Originally posted by smaerd  
Start maybe with the classic ethanol distillation. Not too much hazard there. Definitely read up on the techniques and hazards of distillation, but there's not too much too it. Be careful with ether's and things that form peroxides.

Water aspirator might be sufficient for some distillations but, keep in mind how much water will be wasted. Nothing wrong with Laboy, had a distillation set up and a few pieces of joint-ware from them for 4 or so years now, no issues. Even after some abuse. I prefer to buy American or second-hand glass, especially while Dr. Bob is around giving out amazing deals.


Yeah i have seen those circulating aspirators and they seem could be pretty easy constucting. I don´t know, but i as soon as i have enough cash i will get a pump instead.

Quote: Originally posted by NexusDNA  


Making crystals of copper(II) salts is nice and harmless! If you let them time enough you can get some pretty nice ones.



Yeah, thats what im talking about. I can´t wait. :)

Ps. I have been on the look for glacial Acetic, but it´s pretty hard to find, and when you do, it´s super expencive.
I found some 99,85%. Can It be used too?
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[*] posted on 28-5-2014 at 10:36


I made some copper chloride the other day, it's pretty fun, great colors.

Quote:

I found some 99,85%. Can It be used too?
Yes, go for it. Here is some for a good price.


Quote:

[...] then weigh how much salt is left over, and whether the distillate is salty.

It won't be obviously, no need to even check:cool:.




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[*] posted on 30-5-2014 at 07:25




Quote:

[...] then weigh how much salt is left over, and whether the distillate is salty.

It won't be obviously, no need to even check:cool:. [/rquote]

You'd be surprised what dissolved solids can be carried over during a distillation. NaCl? Perhaps not so easily but since nannah is only starting to learn lab technique, perhaps he/she would best serve his/her own interest by going through the steps, even if we see it as unnecessary.
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[*] posted on 30-5-2014 at 09:14


Quote: Originally posted by Rogeryermaw  

You'd be surprised what dissolved solids can be carried over during a distillation.


Please try to post useful suggestions for a noob.

Either me or nannah - take your pick, we're both noobs.

Your comment contains nothing do-able.

Please give suggestions of What to do, seeing as you are obviously So knowledgeable, and try to make it fit what skills/reagents/aparatus a noob may have.

Personally i do not care at all if ou are the best chemist in history.
So far all you have displayed is aloof arrogance, and have imparted 0 in terms of knowledge.

I doubt You were born all-knowing, and would know Less now if your teachers had taken the same attitude.

[Edited on 30-5-2014 by aga]




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[*] posted on 30-5-2014 at 10:34


I'm with Arkoma too. Building your own equipment is super rewarding, fun, and generally cheaper then buying them.

Making an electrolysis power-supply from a computer supply was a really fun project and helped me to understand some things in chemistry I wouldn't have other-wise. Electrons are also cheap reagents, and lots of little effects can be observed! Be careful with computer power supplies of course. They pack a pretty high current, so you know, implement safety features and research before experimenting.

Extractions are also fun entry level experiments(caffeine from coffee/tea, etc). TLC is great too and teaches some of the basics of separation science. Could start with grass/chlorophyll and then if you make good TLC plates(or buy them) then you could even analyze your caffeine extract :).

My advice for starting chemistry is maybe not have a specific field to investigate in the beggining. Start with some basic fun observable things. By observable I mean color changes, crystal shapes, scent changes(aroma chemistry is so often over-looked). See what you think is interesting. Expand from there as you develop your interests/skills.




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[*] posted on 30-5-2014 at 11:10


Quote: Originally posted by Zyklonb  
I made some copper chloride the other day, it's pretty fun, great colors.

Quote:

I found some 99,85%. Can It be used too?
Yes, go for it. Here is some for a good price.


Quote:

[...] then weigh how much salt is left over, and whether the distillate is salty.

It won't be obviously, no need to even check:cool:.


Thanks, i will check out the link. :) Great price, but i have to see what the shipping charges will be.
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[*] posted on 30-5-2014 at 11:43


I also made myself a HUGE (4.5 x 2 foot) Periodic Table on the backside of a piece of wallpaper. It's hanging proudly in the living room. As I get element samples I tape/glue them in their boxes. My friends 7 year old daughter helps with this*. I also have made "flash cards" of various anions and cations with their charges and M(olecular)W(eights) wrote on them.

Having a balance is VERY important; I made my own with wood scraps and razor blades. Sensitive to one drop of water.

Same so with a notebook-you can't repeat anything unless you write down everything you do, even if it doesn't seem important at the time. Plus, I suffer bad from "CRS" (can't remember shit)



*she's buying my plane ticket to Stockholm when she wins the Nobel!

(edit)Also for pH indicators, grab ya some flowers, hot water extract them, and soak coffee filters and dry. Also red cabbage. believe it or not roses and petunias work well :D

[Edited on 5-30-2014 by arkoma]
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[*] posted on 30-5-2014 at 11:47


Quote: Originally posted by aga  
Quote: Originally posted by Rogeryermaw  

You'd be surprised what dissolved solids can be carried over during a distillation.


Please try to post useful suggestions for a noob.

Either me or nannah - take your pick, we're both noobs.

Your comment contains nothing do-able.

Please give suggestions of What to do, seeing as you are obviously So knowledgeable, and try to make it fit what skills/reagents/aparatus a noob may have.

Personally i do not care at all if ou are the best chemist in history.
So far all you have displayed is aloof arrogance, and have imparted 0 in terms of knowledge.

I doubt You were born all-knowing, and would know Less now if your teachers had taken the same attitude.

[Edited on 30-5-2014 by aga]


First, I was speaking to zykon and only pointing out that when one is so new to lab techniques, that they should not skip steps some may see as superfluous if for no other reason than to embed proper technique to combat complacency.

Second, I'm not arrogant to any one. I try to help people who ask. I observe several others argue and call names. You seem to fit right in with those folks.

Third, I have made contributions around this board a good bit. Apparently you haven't read the P4 thread. Or thread about amines in organic. There have been others. Pick your battles and try to get over yourself.

Lastly, not that you are the one to dictate who should post what where, a simple process nannah might like to try at home would be procure a bottle of household ammonia, a liter bottle and some distilled water. Two flasks, stoppers and some hose. Use gentle heat to drive NH3 from the dilute solution, through hose, into the distilled water to obtain concentrated ammonia of good purity.
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[*] posted on 30-5-2014 at 12:47


Quote: Originally posted by smaerd  
I'm with Arkoma too. Building your own equipment is super rewarding, fun, and generally cheaper then buying them.

Making an electrolysis power-supply from a computer supply was a really fun project and helped me to understand some things in chemistry I wouldn't have other-wise. Electrons are also cheap reagents, and lots of little effects can be observed! Be careful with computer power supplies of course. They pack a pretty high current, so you know, implement safety features and research before experimenting.

Extractions are also fun entry level experiments(caffeine from coffee/tea, etc). TLC is great too and teaches some of the basics of separation science. Could start with grass/chlorophyll and then if you make good TLC plates(or buy them) then you could even analyze your caffeine extract :).

My advice for starting chemistry is maybe not have a specific field to investigate in the beggining. Start with some basic fun observable things. By observable I mean color changes, crystal shapes, scent changes(aroma chemistry is so often over-looked). See what you think is interesting. Expand from there as you develop your interests/skills.

I've made a very useful magnetic stirrer from some household stuff, saves a good $50 for having to buy one.




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[*] posted on 30-5-2014 at 14:21


Quote: Originally posted by Rogeryermaw  

First, I was speaking to zykon and only pointing out that when one is so new to lab techniques, that they should not skip steps some may see as superfluous if for no other reason than to embed proper technique to combat complacency.


The direction of your comment was not obvious, and i clearly made the wrong assumption.
I assumed that you were replying to my post, as you quoted it.
Skipping Experience is definitely dangerous.
Appologies if my mistaken assumption caused annoyance.

Quote: Originally posted by Rogeryermaw  

Second, I'm not arrogant to any one. I try to help people who ask. I observe several others argue and call names. You seem to fit right in with those folks.


In the limited Context, your post appeared arrogant, in that this thread is from a noob, requesting Information about What to do, rather than What is Not Worth Bothering with.

I assume you are a very experienced Chemist, and where people like me are starting is so far Behind you, the things we Need to learn seem irrelevant and obvious to you, as it is already second nature.

To people like us, it is not, and is more than likely worth learning.

Quote: Originally posted by Rogeryermaw  
Third, I have made contributions around this board a good bit. Apparently you haven't read the P4 thread. Or thread about amines in organic. There have been others. Pick your battles and try to get over yourself.


The P4 thread is so far advanced from where i am at in the learning process that i fail to understand the words, never mind the chemistry.

Quote: Originally posted by Rogeryermaw  
Lastly, not that you are the one to dictate who should post what where, a simple process nannah might like to try at home would be procure a bottle of household ammonia, a liter bottle and some distilled water. Two flasks, stoppers and some hose. Use gentle heat to drive NH3 from the dilute solution, through hose, into the distilled water to obtain concentrated ammonia of good purity.


A Chemist speaks !

Thank you for suggesting that process.
I will certainly give it a go.

Appologies again for any offence caused.

[Edited on 30-5-2014 by aga]




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[*] posted on 30-5-2014 at 20:01


we're all here to learn together. i'm not that experienced in lab processes as my accident making PCl3 showed...i read quite a bit more than i experiment as it is so expensive.

here are a couple that are fun and easy. sorry if they have been mentioned already. i noticed someone mention copper sulfate. easy to get as root killer at any hardware store. also fun to make electrolytically with H2SO4 and copper metal. recrystallize your copper sulfate and make a saturated solution in water. add some of that ammonia you concentrated to get the amino complex. then you can evaporate that and the crystals are quite pretty.

another fun and quite useful thing to do is go around hardware stores and small, non-chain type pharmacies and see what chemicals you can find. some of them have saltpeter and cold packs with ammonium nitrate. those are fun and easy to practice re-crystallization with. and if you can find ammonium nitrate, add strong base in a stoppered flask with a hose lead into water as another way to make concentrated ammonia solution.

you can get impure manganese dioxide from lantern batteries and add 3% hydrogen peroxide to make O2 gas. concentrate the H2O2 by fractional crystallization (fancy for partially freezing the peroxide). the peroxide freezes at a slightly lower temp than water so if you filter out the slush, the liquid will be more concentrated and react more vigorously with the MnO2.

also useful from the batteries are the carbon rods which can be used in electrolysis projects.

[Edited on 31-5-2014 by Rogeryermaw]
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[*] posted on 1-6-2014 at 11:11


Nice Ideas Rogeryermaw! All simple, well explained (Especially Fractional Dist.!). This is what we need here, not argument.

Convert some of your metal salts to their carbonates (w/ Baking soda, I'm sure you know) so you can get corresponding salts from the acids you have. Do some practice with double displacement, try Epsom salt (MgSO4) for starters.




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