There are open databases of organic spectral data online now. I found even CD-3 and CD-4. You can also now do this with your android phone with an attachment to the camera iirc.
Glycin Synthesis/Production
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There are open databases of organic spectral data online now. I found even CD-3 and CD-4. You can also now do this with your android phone with an attachment to the camera iirc.
OP
OP
Catechol goes at $5/100g, so that is no issue. NIR spectroscopy cannot be carried out in a way as simple as using one's phone (there are apps vor visible light spectroscopy, but it's mainly qualitative. I'll contact some friends and see if I can't get is tested in a mass spectrometer.
OP
OP
Well, I'd rather leave the spectro work to the professionals, given that I only have cursory knowledge of analysis, doing anything on my own will be little more than a waste of time.
Another remark not directly related to glycin synthesis, but generally useful(I think) : It may be possible to regenerate old brown glycin if you dissolve it in an alkaline solution and add ascorbic acid at 1/10 of the weight of the glycin. Boil until solution clears up and its color lightens. Note that this works for me, but your results may vary, so try it on a small (1/8g) amount and see if it works before going for a large batch.
Another remark not directly related to glycin synthesis, but generally useful(I think) : It may be possible to regenerate old brown glycin if you dissolve it in an alkaline solution and add ascorbic acid at 1/10 of the weight of the glycin. Boil until solution clears up and its color lightens. Note that this works for me, but your results may vary, so try it on a small (1/8g) amount and see if it works before going for a large batch.
Spectral analysis might be easier than you think.
Run the spectrum you wish, then look up glycin in a table of spectra. Compare them. If they match, you are ok. If they are similar, it is probably impure glycin, and if they are totally different, you will know you don't have glycin.
The ascorbic acid method looks interesting to me.
PE
Run the spectrum you wish, then look up glycin in a table of spectra. Compare them. If they match, you are ok. If they are similar, it is probably impure glycin, and if they are totally different, you will know you don't have glycin.
The ascorbic acid method looks interesting to me.
PE
OP
OP
Well, in that case I might be doing it with the school's spectrophotometer, it's a standard unit I've seen in most manuals, so I believe I'd be able to test the glycin.
Ascorbic acid seems to be a very useful reducing agent, in the color chem. section I posted my tests of making a color developer with CD1( I know, I know, but it's the only thing I've got, and time, I have some time on my hands
), and I've substituted hydroxylamine, which I am reluctant to purchase in the kg range, as it is offered here, with 500mg/l ascorbic acid, which seems to retard oxidation enough to make a reasonably stable developer. Anyhow, I digress 
Ascorbic acid seems to be a very useful reducing agent, in the color chem. section I posted my tests of making a color developer with CD1( I know, I know, but it's the only thing I've got, and time, I have some time on my hands
), and I've substituted hydroxylamine, which I am reluctant to purchase in the kg range, as it is offered here, with 500mg/l ascorbic acid, which seems to retard oxidation enough to make a reasonably stable developer. Anyhow, I digress
Make sure the spectrophotometer is an IR unit and do NOT dissolve the sample in water. None of the items in the beam are made of glass, but rather are made of huge, specially grown and polished NaBr or NaCl crystals. They are phenomenally expensive. Of course there are special cuvettes that are transparent to IR as well.
There are some new words for you!
PE
There are some new words for you!
PE
OP
OP
I do have some quartz cuvettes I used in my dye laser project, I think their transmission values should reach IR. I have seen people growing NaBr crystals for CO2 lasers, and worrying about water leaks from the cooling jackets. Anyhow, I'll check up the unit soon...
If you have any interpretatoin problems, I have one spectrum textbook here, but it is not very inclusive. However, I might be able to recall enough of my course in interpretation to help you out. (no promises-I'm very rusty at this)
PE
PE
> in the range or $10-15 to the gram
You can get photographyc glycin by a much lower price
http://www.bhphotovideo.com/c/produ...0_0610_10G_Glycin_N_Parahydroxyphenyl_10.html
You can get photographyc glycin by a much lower price
http://www.bhphotovideo.com/c/produ...0_0610_10G_Glycin_N_Parahydroxyphenyl_10.html
OP
OP
Purity Test/Risk and safety assessment
OK, so today I got some preliminary results from testing, carried out by a third party; The (anhydrous) sample I sent seems to be 96.5-97% glycin, with the balance sodium chloride (from the neutralized MCA), and sodium acetate (pH balancing agent used during synthesis). There are trace amounts of p-aminophenol (<0.1%), suggesting a proper ratio and full conversion. I'm satisfied...
Also, in respect to the safety of the production, I sat down and assessed the safety factors in a system I use for any lab work. It's a 10-grade relative system, 0 being no immediate danger, 10 being work with chemicals like methylmercury, dioxin, extreme flammables and caustics, very high temperatures, etc. The grades are founded on standard lab protocol, i.e. no food, drinks, smoking, common sense . Following are the salient points:
Fire Hazard: 2 - use of solvents for testing and cleanup, solid chemicals and their solutions are unflammable
Vapor Toxicity: 1 - MCA and acetic acid emit light vapors, but work under a fume hood, or in a properly ventilated room keeps concentrations well bellow minimum thresholds
Contact toxiciy: 5 - prolonged skin contact with mild alkalis and p-aminophenol can result in a persisting dermatitis, possibly promoting an allergy. Glacial acetic acid can cause chemical burns. Monochloroacetic acid is highly toxic and resorbed through the skin quickly. Nitrile gloves are a minimum requirement, along with a rubber apron over the lab coar, eye protection for splashes. Most chemicals are crystalline and handling them gives little rise to dust in the air, though a simple filter mask is appropriate.
Reaction Procedure: 2 - no immediate hazard of runaway reaction, improper mixing can cause gas evolution and fizzing that releases a mist, improper heating of reactant mixture can cause bumping(superheating of liquid and spontaneous evaporation, resulting in liquid losses).
Glassware Procedure and handling: 2, hot glass looks the same as cold glass, temperatures of up to 130C are required, thermal burns can result from carelessness, broken glassware can be vary sharp (and painful to say goodbye to );
Well, if general lab rules are observed, there is no particular danger to the synthesis. The most hazardous chemical is MCA, but adhering to MSDS recommendations and common sense are sufficient to prevent exposure and harm. Disposal of the liquid waste,provided that synthesis is carried out to completion, should present no problems, as all the MCA is converted, and in solutio remain NaCl and CH3COONa.
If general lab procedures are followed, there is
OK, so today I got some preliminary results from testing, carried out by a third party; The (anhydrous) sample I sent seems to be 96.5-97% glycin, with the balance sodium chloride (from the neutralized MCA), and sodium acetate (pH balancing agent used during synthesis). There are trace amounts of p-aminophenol (<0.1%), suggesting a proper ratio and full conversion. I'm satisfied...
Also, in respect to the safety of the production, I sat down and assessed the safety factors in a system I use for any lab work. It's a 10-grade relative system, 0 being no immediate danger, 10 being work with chemicals like methylmercury, dioxin, extreme flammables and caustics, very high temperatures, etc. The grades are founded on standard lab protocol, i.e. no food, drinks, smoking, common sense
. Following are the salient points:Fire Hazard: 2 - use of solvents for testing and cleanup, solid chemicals and their solutions are unflammable
Vapor Toxicity: 1 - MCA and acetic acid emit light vapors, but work under a fume hood, or in a properly ventilated room keeps concentrations well bellow minimum thresholds
Contact toxiciy: 5 - prolonged skin contact with mild alkalis and p-aminophenol can result in a persisting dermatitis, possibly promoting an allergy. Glacial acetic acid can cause chemical burns. Monochloroacetic acid is highly toxic and resorbed through the skin quickly. Nitrile gloves are a minimum requirement, along with a rubber apron over the lab coar, eye protection for splashes. Most chemicals are crystalline and handling them gives little rise to dust in the air, though a simple filter mask is appropriate.
Reaction Procedure: 2 - no immediate hazard of runaway reaction, improper mixing can cause gas evolution and fizzing that releases a mist, improper heating of reactant mixture can cause bumping(superheating of liquid and spontaneous evaporation, resulting in liquid losses).
Glassware Procedure and handling: 2, hot glass looks the same as cold glass, temperatures of up to 130C are required, thermal burns can result from carelessness, broken glassware can be vary sharp (and painful to say goodbye to
); Well, if general lab rules are observed, there is no particular danger to the synthesis. The most hazardous chemical is MCA, but adhering to MSDS recommendations and common sense are sufficient to prevent exposure and harm. Disposal of the liquid waste,provided that synthesis is carried out to completion, should present no problems, as all the MCA is converted, and in solutio remain NaCl and CH3COONa.
If general lab procedures are followed, there is
Good job so far.
PE
PE
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