I searched for "mass spectrometry" on the user powered news site, digg.com, and got no results. First, I checked under the science topic. Oh, wait there are some stories that come up when the whole site is searched.
Fairly interesting stuff, not newsworthy according to the digg community, but I don't think there are many scientist on there.
At Georgia Tech, this is what they call a nanoscale probe, or the Scanning Mass Spectrometry probe (SMS). It seems like what they are trying to do is take some mass spectrums of protiens, metabolites, and peptides without separating them from the cell/tissue. The associate professor responsible for doing this work is Andrei G. Fedorov. His research is pretty hardcore, talking about crazy ideas for ion sources, see project 7.
I think the way it works is the substrate gets a positive charge, the scanning tip has a negative charge. The scanning tip pulls molecules by charge, but also uses something called Taylor electrohydrodynamic focusing of jets to produce charged ions.
Sunday, November 26, 2006
Wednesday, October 18, 2006
Why can't power plug configurations be universal?
We have all this excess noise in the lab, mostly from instrumentation, not from chatty n00bie employees. The lab I work in has two icp optical emission spectrometers and one icp mass spectrometer. Each instrument has a chiller and the mass spec also has a big ole vacuum pump. So, to prevent us from having to yell "WHAT" across the lab to one another, the boss had the idea to put the two chillers and the vacuum pump in another little room right next to the lab. That conversation was two months ago.
All we had to do was put some holes in the wall and get some longer power cords for everything. Sounds easy, but of course, it wasn't. The easy thing to do would be to plug the stuff in in the little room. But it all has to be on UPS and the only UPS outlets are in the lab. One chiller has a 110V power cord, not a problem at all, that is the normal plug in your house. The mass spec chiller has a 220V plug and it's from Europe. I never knew there were so many different power cord configurations. The power cord from the vacuum pump is also 220V, European, and different than the chiller cord from Europe.
There's a bunch of phone calls made, some red tape in the way, so we decide to move the mass spec right in front of the hole we made in the wall, so we don't need longer power cords. Genius.
Have a Guinness!
All we had to do was put some holes in the wall and get some longer power cords for everything. Sounds easy, but of course, it wasn't. The easy thing to do would be to plug the stuff in in the little room. But it all has to be on UPS and the only UPS outlets are in the lab. One chiller has a 110V power cord, not a problem at all, that is the normal plug in your house. The mass spec chiller has a 220V plug and it's from Europe. I never knew there were so many different power cord configurations. The power cord from the vacuum pump is also 220V, European, and different than the chiller cord from Europe.
There's a bunch of phone calls made, some red tape in the way, so we decide to move the mass spec right in front of the hole we made in the wall, so we don't need longer power cords. Genius.
Have a Guinness!
Saturday, September 16, 2006
Plumbing better than Mario and Luigi
Instead of dealing with large green pipes you have to jump into,
I have to deal with peristaltic pump tubing.
These little tubes are used to carry liquids into the mass spec. Other people use them too, such as chemists who use HPLC, IC, and SFA.
About twice a month, I have to run an analysis called FIAS or TTRA. Too make a long expanation short, the samples are mixed with buffer (pH 5.5) and internal standard (Y, In, Tb) all "online", then pushed through a column with an affinity resin that grabs the transition metals and lets the group I metals pass through. Then, the column is washed with acid, which rinses the transition metals into the mass spec which sorts them and counts them.
The way the literature describes to do this was unecessarily complicated. It explained using a sample loop and employing a water line to wash the column. It involved two valves, two pumps, four peristaltic pump lines, a double six-way valve, and finally the column.That's the way I did it and it worked for a while, but eventually it stopped working properly and I couldn't fix it. So instead of spending multiple days troubleshooting, I decided to just completely start over and re-think the whole thing.
I re-plumbed it much more simple and straight forward. Both valves, half of the double six-way valve, and the water line ended up being unnecessary. Now, loads of para-film were no longer needed to prevent leaks in the peristaltic pump tube connections. Also, less sample is used.
I have to deal with peristaltic pump tubing.
These little tubes are used to carry liquids into the mass spec. Other people use them too, such as chemists who use HPLC, IC, and SFA.
About twice a month, I have to run an analysis called FIAS or TTRA. Too make a long expanation short, the samples are mixed with buffer (pH 5.5) and internal standard (Y, In, Tb) all "online", then pushed through a column with an affinity resin that grabs the transition metals and lets the group I metals pass through. Then, the column is washed with acid, which rinses the transition metals into the mass spec which sorts them and counts them.
The way the literature describes to do this was unecessarily complicated. It explained using a sample loop and employing a water line to wash the column. It involved two valves, two pumps, four peristaltic pump lines, a double six-way valve, and finally the column.That's the way I did it and it worked for a while, but eventually it stopped working properly and I couldn't fix it. So instead of spending multiple days troubleshooting, I decided to just completely start over and re-think the whole thing.
I re-plumbed it much more simple and straight forward. Both valves, half of the double six-way valve, and the water line ended up being unnecessary. Now, loads of para-film were no longer needed to prevent leaks in the peristaltic pump tube connections. Also, less sample is used.
Wednesday, September 13, 2006
How to make a 1000 fold dilution
Making dilutions is an everyday thing when analyzing environmental samples. It's either diluting salt water samples by 10 because they have such a high ion content they suppress the plasma and cause internal standards to drop too low or diluting sediment samples because it takes more acid to digest them than is in the calibration standards.
Before entering into environmental analytical chemistry I would say to make a 1000 fold dilution, add 1000mL to 1 mL of what you're trying to dilute. But that's wrong, you add 999mL to 1mL of what you're trying to dilute. Reason is, it's already diluted once. If you start with pure copper for example, and stuck it in a beaker, then you would have to add 1000mL to dilute it 1000 fold. But if the copper is already dissolved in 1mL, then you would have to add 999mL to dilute to 1000 fold. I'm pretty sure you typically don't see pure metals, sitting around an environmental chemistry laboratory waiting to be dissolved into standards. It's much easier and cost effective to buy the metals already dissolved in water in nice, guaranteed concentrations, like 10,000ppm.
I can grow orchids --->
Before entering into environmental analytical chemistry I would say to make a 1000 fold dilution, add 1000mL to 1 mL of what you're trying to dilute. But that's wrong, you add 999mL to 1mL of what you're trying to dilute. Reason is, it's already diluted once. If you start with pure copper for example, and stuck it in a beaker, then you would have to add 1000mL to dilute it 1000 fold. But if the copper is already dissolved in 1mL, then you would have to add 999mL to dilute to 1000 fold. I'm pretty sure you typically don't see pure metals, sitting around an environmental chemistry laboratory waiting to be dissolved into standards. It's much easier and cost effective to buy the metals already dissolved in water in nice, guaranteed concentrations, like 10,000ppm.
I can grow orchids --->
Wednesday, August 30, 2006
How to get motivated for work
Someone asked me the other day how I got motivated for work. It didn't come out of the blue, we've been having some serious mass spec problems we just can't figure out. Turns out now, the technician can't really figure it out either. I replied I have to get paid, just kind of as a joke. I didn't really have time to think about it.
Maybe it's actually competition. Not just from people around me in the present, but people in the past. Stories of old chemists discovering things, having moments of clearity, and thinking "eureka!" actually motivates me. Maybe if I don't give in to working and feeling like a slave I'll get better at what I'm doing. The only way to solve a problem is to see the answer. It's hard to keep an open vision and look at things in a new way when you give into the stress of work problems.
So, to get motivated for work, seek inspiration from the past.
Maybe it's actually competition. Not just from people around me in the present, but people in the past. Stories of old chemists discovering things, having moments of clearity, and thinking "eureka!" actually motivates me. Maybe if I don't give in to working and feeling like a slave I'll get better at what I'm doing. The only way to solve a problem is to see the answer. It's hard to keep an open vision and look at things in a new way when you give into the stress of work problems.
So, to get motivated for work, seek inspiration from the past.
Tuesday, August 15, 2006
Unheard of ICPMS drift: Rabbit Pump Drift
Fellow mass spectrometerists, check this out. I'm running some calibration standards and all the sudden, from the 100ppb to the 200ppb, internal standard recovery changes from 100% to 80%. Naturally thought it was sample introduction; checked for clogs, changed cones, changed to new nebuliser, still same drift, sometimes after 5 cups. Then it eventually, 5 cups or so, it kind of creeps back up around 100%.
Today, I was looking at the real time display, in deep thought while I watched the 115In and 209Bi signal intertwine bouncing across the 20 in. flat screen when I figured it out. I accessed the accessory window and switched the peristaltic pump into rabbit mode[1]. Sure enough, the signal drops, probably around 80%, but just going off counts per second at the time. Let it equilibrate and switch it back to regular pump speed, 24%. Oh, man, took like 3 or 4 minutes for the counts to get back up to where they were before rabbit pump.
Edited ACL script, no rabbit pump, calibrated fine, loaded samples, got to name a new type of drift: Rabbit Pump Drift.
I also named Seesaw Drift, this is when the low mass internal standards drift up while the high mass internal standards drift down, or the other way around.
[1] This is what the software that runs the ICPMS calls max speed pumping. Good for washing the probe during rinse.
Today, I was looking at the real time display, in deep thought while I watched the 115In and 209Bi signal intertwine bouncing across the 20 in. flat screen when I figured it out. I accessed the accessory window and switched the peristaltic pump into rabbit mode[1]. Sure enough, the signal drops, probably around 80%, but just going off counts per second at the time. Let it equilibrate and switch it back to regular pump speed, 24%. Oh, man, took like 3 or 4 minutes for the counts to get back up to where they were before rabbit pump.
Edited ACL script, no rabbit pump, calibrated fine, loaded samples, got to name a new type of drift: Rabbit Pump Drift.
I also named Seesaw Drift, this is when the low mass internal standards drift up while the high mass internal standards drift down, or the other way around.
[1] This is what the software that runs the ICPMS calls max speed pumping. Good for washing the probe during rinse.
Monday, August 14, 2006
Typical drift problems
Links to help solve drift problems: link 1 , Perkin Elmer, Spectroscopy magazine, PlasmaChem.
It's not the sample introduction, it can't be.
If you don't want to turn your head, translation for above, Wanted: Experienced Dog Catcher/Trapper to catch "one" small, smart, sneaky dog. Please call .... How great is that? Anybody up to it?
Random shot from the lab, do you think the guys who made this piece of equipment had a little laugh?
It's not the sample introduction, it can't be.
If you don't want to turn your head, translation for above, Wanted: Experienced Dog Catcher/Trapper to catch "one" small, smart, sneaky dog. Please call .... How great is that? Anybody up to it?
Random shot from the lab, do you think the guys who made this piece of equipment had a little laugh?
Sunday, August 06, 2006
Cones before and after
A sample cone looks like this after you clean it:
And a skimmer cone looks like this after some samples:
I think that is permanganate built up on there. Anybody else have an idea?
And a skimmer cone looks like this after some samples:
I think that is permanganate built up on there. Anybody else have an idea?
Friday, July 21, 2006
Slow down
It's hard to keep up in the blog world when your trying to move. I mean moving to a different residence. You always forget how much of a pain it is. I've got everything packed up in I-CHEM boxes swiped from work. Well they're not really swiped, they were getting thrown away.
Anyways, anyone know how to clean an extraction lens or re-install instrument controlling software without getting a headache?
Anyways, anyone know how to clean an extraction lens or re-install instrument controlling software without getting a headache?
Wednesday, July 05, 2006
Silver crashes
The other day I took on the rather long task of making a multi-element solution. A multi-element solution is exactly what it sounds like, a solution (a mixture of dissolved stuff), the dissolved stuff being many different elements. This particular solution was to be composed of 27 different metal elements such as chromium, arsenic, and manganese. One way to start making this solution is to dissolve different metallic salts, like As2O3, into a diluted acid (HNO3 or nitric acid) solution. But, I don't have to do that, we buy the metals already dissolved in acidic solutions.
So all I have to do is successfully pipette certain amounts like 10mL, 1mL, or 0.1mL. Then dilute the solution to 1 or 2L in a class A volumetric flask. It's not that hard if you got good lab technique, but you do have 27 chances to accidently add the wrong amount. Anyways, silver is always a little tricky to get into a solution. It always wants to precipitate out. I think it forms AgCl. The Cl anions come from the HCl I add to the solution along with the HNO3 to stabilize the metals. One way to prevent precipitation is to add the HCl last after the silver has already been added and is diluted throughout everything else. But in general, silver can't be put in a multi-element solution above 500ppb. Well for some reason I forgot everything I knew for 30 seconds and messed up the entire solution on the 27th metal, silver. As soon as I pipetted 0.5mL of a 1000ppm silver solution into about 1L of other dissolved metals + acid + water it crashed out into a white haze in the flask and eventually combined into what looks like normal table salt at the bottom of the volumetric flask, but I wouldn't put that salt on my fries.
So all I have to do is successfully pipette certain amounts like 10mL, 1mL, or 0.1mL. Then dilute the solution to 1 or 2L in a class A volumetric flask. It's not that hard if you got good lab technique, but you do have 27 chances to accidently add the wrong amount. Anyways, silver is always a little tricky to get into a solution. It always wants to precipitate out. I think it forms AgCl. The Cl anions come from the HCl I add to the solution along with the HNO3 to stabilize the metals. One way to prevent precipitation is to add the HCl last after the silver has already been added and is diluted throughout everything else. But in general, silver can't be put in a multi-element solution above 500ppb. Well for some reason I forgot everything I knew for 30 seconds and messed up the entire solution on the 27th metal, silver. As soon as I pipetted 0.5mL of a 1000ppm silver solution into about 1L of other dissolved metals + acid + water it crashed out into a white haze in the flask and eventually combined into what looks like normal table salt at the bottom of the volumetric flask, but I wouldn't put that salt on my fries.
Sunday, June 25, 2006
Plasma in the window
You know a lot of people play Sudoku and work crossword puzzles to exercise their mind. Any chemists out there ever try to draw out syntheses for natural products or any other molecules to gain extra brain power? Here's a shot of the plasma from the lab.
The color of the plamsa is actually white, but the window is tinted green with something that prevents the UV light from harming our eyes. The ultraviolet light is emitted from the metals in the water samples after they gain energy from the plasma. There is actually no reason for the window at all, it just looks cool.
The color of the plamsa is actually white, but the window is tinted green with something that prevents the UV light from harming our eyes. The ultraviolet light is emitted from the metals in the water samples after they gain energy from the plasma. There is actually no reason for the window at all, it just looks cool.
Monday, June 19, 2006
Quality Control Explained
Quality control in ensuring your product, or scientific result falls in between a set of guidelines determined by the necessary amount of accuracy and precision required. It allows a customer to know how reliable a scientific result is.
For instance, say you want to analyze some water samples from off the coast of Louisiana to check if there is any lead contamination because the battery factory was flooded and damaged from a hurricane. To start with, you might want to take samples in various locations and record some type of data like distance from shore and maybe depth of sample taken along with the pH of the water. To tell that the guy or girl sampling the water hasn't contaminated it themselves, they'll need to take some DI water up with their water sampling equipment and bottle that up to go with all the sea water samples.
Then, it'll get back to the lab and it will have to be prepared to be analyzed, the preparer will include another blank with the batch of sea water samples to ensure that he or his lab did not contaminate the samples. These blank samples are representative of the whole batch of samples, if they have any lead in them, then all the other sea water samples would be expected to have the same amount. That's why you gotta keep it all clean, with a mass spec you're usually looking for pretty low amounts.
To be continued... as a series or possibly just a trilogy.
For instance, say you want to analyze some water samples from off the coast of Louisiana to check if there is any lead contamination because the battery factory was flooded and damaged from a hurricane. To start with, you might want to take samples in various locations and record some type of data like distance from shore and maybe depth of sample taken along with the pH of the water. To tell that the guy or girl sampling the water hasn't contaminated it themselves, they'll need to take some DI water up with their water sampling equipment and bottle that up to go with all the sea water samples.
Then, it'll get back to the lab and it will have to be prepared to be analyzed, the preparer will include another blank with the batch of sea water samples to ensure that he or his lab did not contaminate the samples. These blank samples are representative of the whole batch of samples, if they have any lead in them, then all the other sea water samples would be expected to have the same amount. That's why you gotta keep it all clean, with a mass spec you're usually looking for pretty low amounts.
To be continued... as a series or possibly just a trilogy.
Wednesday, June 14, 2006
Alpha hydroxy garbage
This is kinda funny. After studying organic chemistry, whenever those commercials came on TV about "alpha hydroxys" in skin creams and stuff I would laugh and say that doesn't mean anything. I tried to explain to my girlfriend that the term alpha hydroxy just describes a location on a molecule, like the next carbon over from something has an alcohol bonded to it. In other words, the alcohol (hydroxy) is alpha (next to) something, but you can't really tell what that something is when you say alpha hydroxy.
Glycolic acid
Some of the commercials say "alpha hydroxy acids". This makes much more sense, turnes out, there is a group of molecules called alpha hydroxy acids. And they do have an effect on skin.
Another thing that tickles my fancy is seeing all those little multi-colored beads mixed in and suspended in the face wash or shampoo. That is actually some hot research because just the way it looks sitting on the grocery store shelf makes people buy it. So there were actually scientist out there trying to find out how to suspend little colored balls in a hair gel, making and spending loads of money. It's just the way it goes. Kinda seems like a waste of scientific talent to me, maybe the project only took a couple years.
Next up, beta hydroxy acids.
Glycolic acid
Some of the commercials say "alpha hydroxy acids". This makes much more sense, turnes out, there is a group of molecules called alpha hydroxy acids. And they do have an effect on skin.
Another thing that tickles my fancy is seeing all those little multi-colored beads mixed in and suspended in the face wash or shampoo. That is actually some hot research because just the way it looks sitting on the grocery store shelf makes people buy it. So there were actually scientist out there trying to find out how to suspend little colored balls in a hair gel, making and spending loads of money. It's just the way it goes. Kinda seems like a waste of scientific talent to me, maybe the project only took a couple years.
Next up, beta hydroxy acids.
Friday, June 09, 2006
New calibration standards
Calibration standards have to be made in order for the mass spec to correlate the intensity of the ion signal to concentration. You can't just turn it on and stick a sample in and get a result of 50ppb Cd like on CSI. (A mass spec finds atoms of interest in big piles of random atoms). What would happen if you did that is you would get some random result such as 564,000 CPS (counts per second). When I "calibrate" the instrument by analyzing a 25ppb (10,000CPS), 50ppb (20,000CPS), and 100ppb (40,000CPS) at the beggining of the run, then the instrument knows what 564,000 CPS is. Yes, if you graphed intensity (CPS) vs. concentration (ppb), it would be linear, that's how it works. Technically, 564,000 CPS is obviously overcal in this example and would have to be rerun diluted.
Back to the calibration standards, or multi-element solutions, these are a pain to make. You take bottles off the shelf such as 10,000ppm Sb, it's dissolved in acidified D.I. water from some kind of compound like Sb2O3. You take about 20 to 30 of these bottles off the shelf including things like Tl, Pb, Mn, and Ag. The tricky part is dispensing a very small and precise amount of each element into a 250 or 500mL volumetric flask to arrive at a solution where each element is exactly 50ppb. There is a quite simple calculation to find out how much 10,000ppm Sb to add to a 500mL flask to get 50 ppb. M1*V1 = M2*V2
(10,000ppm Sb)*(x mL) = (0.050ppm)*(500mL)
x = 0.0025mL or 2.5uL
In this case I would have to make an intermediate of say 10ppm and then dilute that down to 50ppb because our pipettes don't go down to 2.5uL.
Then I have your basic quality control guidelines and if the solution I made doesn't "pass", it has to be remade. One can see where it can become frustrating. And besides just calibration standards, I need to make a second source calibration check, an interference check solution, as well as all the spiking solutions used in the lab.
Thursday, June 08, 2006
On global warming from a sceptical chemist
I got into a very interesting and controversial conversation while on a trip to Chicago with a jaunt to Green Bay last week.
The topic of global warming came up from someone who believes it is happening and that something must be done about it. I made a little remark about how I was still somewhat sceptical of the whole global warming argument. And the reaction was surprisal, especially me being a scientist and everything. They went on to talk about how scientist views are being put down or hushed by Washington government. That in itself is very alarming and really requires its own post.
It gets real messy when politics get mixed in with science. You really don't know whose views are swayed by whatever. Really, what I think the problem is, I can't find information on the subject that I don't feel has been politically influenced. What I have read is mostly from science articles on the web that are conflicting. That is how it appears to me, is that scientist actually don't agree on global warming.
Instead of commenting about how I know nothing about global warming (I admit, I'm not an expert), please give me a link to some scientific literature about global warming that you believe to be the truth. I mean the facts, some evidence, you know, experimentation. I'll take a sceptical look at computer models.
By the way, I noticed I made an appearance on the Mass Spectrometry Blog.
An interesting blog by a fellow mass spectrometerist.
Cutting edge literature_, Chemistry facts_, Rants and raves_,
The topic of global warming came up from someone who believes it is happening and that something must be done about it. I made a little remark about how I was still somewhat sceptical of the whole global warming argument. And the reaction was surprisal, especially me being a scientist and everything. They went on to talk about how scientist views are being put down or hushed by Washington government. That in itself is very alarming and really requires its own post.
It gets real messy when politics get mixed in with science. You really don't know whose views are swayed by whatever. Really, what I think the problem is, I can't find information on the subject that I don't feel has been politically influenced. What I have read is mostly from science articles on the web that are conflicting. That is how it appears to me, is that scientist actually don't agree on global warming.
Instead of commenting about how I know nothing about global warming (I admit, I'm not an expert), please give me a link to some scientific literature about global warming that you believe to be the truth. I mean the facts, some evidence, you know, experimentation. I'll take a sceptical look at computer models.
By the way, I noticed I made an appearance on the Mass Spectrometry Blog.
An interesting blog by a fellow mass spectrometerist.
Cutting edge literature_, Chemistry facts_, Rants and raves_,
Tuesday, May 30, 2006
Everybody should read this
I read a story on Wired news about garage chemistry. I wish they still sold chemistry sets that I thought would be fun to use. Like all the chemicals and equipment necessary to isolate and characterize natural products. I think I would specialize in marine natural products, they don't seem to be a passing fad.
Organic chemistry_, Cutting edge literature_
Thursday, May 25, 2006
The Golden Run
Last night's run was what we analytical chemists call a golden run. This means that all the analytes that I needed to analyze for, for each sample, had the yellow highlighter run over them on the cover page of the lab report. The yellow highlighter means that the result is good to go and I don't need to reanalyze. This has only happened one other time in the year I have been running the mass spec.
Talk about staying steady, the mass spec was on point for at least 12 to 14 hours. Now, sales people for mass specs say their instruments can stay "in cal." for like 2 or 3 days. What they don't tell is they are analyzing nice clean pretty sample in D.I. water. Get some real samples in there with loads of salt or suspended solids and your instrument might not make it past the first sample like that.
In the lab_,
Talk about staying steady, the mass spec was on point for at least 12 to 14 hours. Now, sales people for mass specs say their instruments can stay "in cal." for like 2 or 3 days. What they don't tell is they are analyzing nice clean pretty sample in D.I. water. Get some real samples in there with loads of salt or suspended solids and your instrument might not make it past the first sample like that.
In the lab_,
Tuesday, May 23, 2006
Backwards chromatography with Mass Spec
I've been trying to run the FIAS analysis for three days now, the column just doesn't seem to be doing its job. I think the problem might be that I have it backwards. I believe the way the flow should be is into the large end and out the small end. This way, the front of the column will bind the most metals, then, when the flow reverses to rinse the metals off the column with dilute acid, the metals will be at the end of the column, so they come off together.
Sunday, May 21, 2006
More from the blogosphere
I've been reading a few other chemistry blogs around the web.
The Sceptical Chymist
This blog is from the editors of Nature. They have several different authors and many chemstry topics. Somehow they know about In the pipeline and Tenderblog. Powered by Moveable Type.
TotallySynthetic.com
This blog must be from some grad student trying to keep up on "the literature." I do enjoy the review natural product molecules in current literature I can't read about due to enormous subscription fees.
The Endless Frontier
Ph.D student at Harvard.
Interfacial Science
California post-doc.
post doc ergo propter doc
Canadian post-doc.
Check them out and enjoy.
In the blogosphere_
The Sceptical Chymist
This blog is from the editors of Nature. They have several different authors and many chemstry topics. Somehow they know about In the pipeline and Tenderblog. Powered by Moveable Type.
TotallySynthetic.com
This blog must be from some grad student trying to keep up on "the literature." I do enjoy the review natural product molecules in current literature I can't read about due to enormous subscription fees.
The Endless Frontier
Ph.D student at Harvard.
Interfacial Science
California post-doc.
post doc ergo propter doc
Canadian post-doc.
Check them out and enjoy.
In the blogosphere_
Tuesday, May 16, 2006
Busy as Hell
Sometimes you're waiting around for the chemistry to happen, but I haven't been. It goes like this, I run the mass spec everyday which includes first, turning it on. Sometimes the plasma flickers, arcs, and starts melting the torch. This pisses me off, and it pisses my boss off because they are over $300 bucks. I still use them if they didn't melt all the way through.
Then, I move on to "optimizing" the "signal." This consists of aspirating a "tuning" solution and looking at a real time graph of "intensity" vs. time. And basically, you just move some voltages around to create high intensity of what you want, while creating low intensity for things you don't want.
Getting mid-way throught the morning now, I need to find some time to review the run from last night and prepare all the data in a type of lab report. The best time to start this is right after I start the calibration. I usually see some drift during the first calibration, so I restart it right about lunch time, so the lab keeps working while I'm off the clock.
Getting back from lunch, I have to quickly check the calibration and find some samples to run because there is no point in even thinking of running any samples until I know the instrument is going to work right. So I type in a sample sequence, make sure the QC is kosher, and then start making dilutions for pretty much everything but freshwater samples.
Now it's about 4pm and I have to finish reviewing yesterdays data, make any solutions that need to be made, and deal with email. Then I just schedule the MS to shutdown when it's done, which is usually between midnight and 3 in the morning.
Then, I move on to "optimizing" the "signal." This consists of aspirating a "tuning" solution and looking at a real time graph of "intensity" vs. time. And basically, you just move some voltages around to create high intensity of what you want, while creating low intensity for things you don't want.
Getting mid-way throught the morning now, I need to find some time to review the run from last night and prepare all the data in a type of lab report. The best time to start this is right after I start the calibration. I usually see some drift during the first calibration, so I restart it right about lunch time, so the lab keeps working while I'm off the clock.
Getting back from lunch, I have to quickly check the calibration and find some samples to run because there is no point in even thinking of running any samples until I know the instrument is going to work right. So I type in a sample sequence, make sure the QC is kosher, and then start making dilutions for pretty much everything but freshwater samples.
Now it's about 4pm and I have to finish reviewing yesterdays data, make any solutions that need to be made, and deal with email. Then I just schedule the MS to shutdown when it's done, which is usually between midnight and 3 in the morning.
Sunday, May 14, 2006
In my backyard
Thursday, May 11, 2006
Copper in seawater
This is the worst analysis ever, it's called Time Transient Resolved Analysis (TTRA) or Flow Injection Analysis of Seawater (FIAS). The methods are the same, they remove the salt from the seawater so I can measure the concentration of copper. The problem is the flow, there are two pumps, two valves, four lines, a 5mL loop, column, and six way valve, and the flow has got to be steady. A simple calculation reveals 7 to the 10th ways for it to screw up.
I have to use a bunch of para-film to keep the tube joints together because the pump builds up so much pressure in the peri pump tube to push everything throught the column.
The sample flows through a tube, mixes with a buffer (the whole shabang is pH sensitive), and flows onto the column. The metals, including copper and sodium, stick to the resin in the column. The column is rinsed with water, supposedly, the sodium washes off. Then the column is rinsed with diluted nitric acid and the copper comes off and goes into the spectrometer. The metals binding strength to the iminodiacetate resin in the column depends on pH.
Wednesday, May 03, 2006
Mass Spec at home?
There is a reason why you can't have a mass spec at your house. It's not because it's so big, it's because they cost so much to fix. I had a service technician come out the other day and his visit to fix one part for one day was a cool $25,000. Ya, thats just to fix it. You could buy a pretty nice house for what they can cost new.
Parts break all the time, and you can't just keep running it like a car, a mass spec has to be fully optimized at all times to work properly. The technology is always pushed to the furthest point. If old designers of mass specs stuck with the original design and just improved on it, like a clothes washer, maybe they could last 30 years. But, then it would have run off of DOS.
The picture is not me or the mass spec I run, that thing is huge. And whats with all the multi-colored lights.
Monday, May 01, 2006
Ophiobolin C
I worked on the synthesis of this molecule while in school at FSU as an undergraduate. It was one of my better academic experiences in Tallahassee. I had my own lab bench, my own glassware, and my own chemicals. I guess it was a taste of graduate school without the 80 hours a week. I met a lot of great people in there; post docs and graduate students who have all dispersed across the world from England to China. When I retire, I'm going to build a
laboratory and make natural products.
Wednesday, April 26, 2006
Plasma goes out
So I'm just calibrating the mass spec after getting it nicely optimized and out of nowhere, the plasma goes out. That basically means I have to start all over again. I could not find a reason for it to go out. The software that runs the instrument just gave this generic error that it displays anytime anything goes wrong. The software has more bugs than Windows 98.
It's not just pushing buttons all day folks, these things happen all the time. At least half my job is troubleshooting. Finding out why the mass spec is doing what it is doing. So, like a computer, I turned it off and then back on, and everything was fine.
It's not just pushing buttons all day folks, these things happen all the time. At least half my job is troubleshooting. Finding out why the mass spec is doing what it is doing. So, like a computer, I turned it off and then back on, and everything was fine.
Monday, April 24, 2006
DARTs and MS
I'm sure all the mass spec people have heard about this before because it is so cool and also one year old news. It's a new ionization method called DART (direct analysis in real time) invented by Robert B. Cody of JEOL USA and James A. Laramee of EAI Corp. It is a sample introduction system that can be coupled to a mass spectrometer, currently only coupled to a MS by JEOL.
The major difference here, compared to other mass specs, is the sample inlet is at atmospheric pressure. You can hold an object, such as an orange, up in front of the sample cone and get a reading of masses detected and find fungicides.
This technique works by applying an electrical potential to a gas (N2 or H2) to form a plasma that interacts with the sample and the atmosphere.
It took me a minute to picture the instrument layout in my head, I couldn't, so I went to the website. The path of the ion: First, gas is fed in, a plasma is formed, then the instrument opens up to the atmosphere. So, the open region is between the plasma torch and the sample cone. Then, the rest of the mass spec, the one they use happens to be a time-of-flight.
The major difference here, compared to other mass specs, is the sample inlet is at atmospheric pressure. You can hold an object, such as an orange, up in front of the sample cone and get a reading of masses detected and find fungicides.
This technique works by applying an electrical potential to a gas (N2 or H2) to form a plasma that interacts with the sample and the atmosphere.
It took me a minute to picture the instrument layout in my head, I couldn't, so I went to the website. The path of the ion: First, gas is fed in, a plasma is formed, then the instrument opens up to the atmosphere. So, the open region is between the plasma torch and the sample cone. Then, the rest of the mass spec, the one they use happens to be a time-of-flight.
Friday, April 21, 2006
MS at PittCon
Well, I didn't get to go to PittCon, even though it was only a 4 or 5 hour drive from here. And it looks like I missed out on a lot of cool analytical instrumentation as well as possible job leads.
My favorite company Thermo (read with sarcastic tone) introduced a new type of mass spec. In fact, they claim it is "the first totally new mass analyzer to be introduced to the market in more than 20 years." It is called the LTQ Orbitrap mass spectrometer. To read about its initial research, Anal. Chem. 2000, 72, 1156.
Apparently, the orbitrap takes the place of the quadrupole to separate the ions based on m/z. The orbitrap "has ions spinning around a carefully shaped central electrode while shuttling back and forth over its long axis in harmonic motion at frequencies dependent only on their mass-to-charge ratios," says R. Graham Cooks of Purdue University.
More interesting news from PittCon to come.
My favorite company Thermo (read with sarcastic tone) introduced a new type of mass spec. In fact, they claim it is "the first totally new mass analyzer to be introduced to the market in more than 20 years." It is called the LTQ Orbitrap mass spectrometer. To read about its initial research, Anal. Chem. 2000, 72, 1156.
Apparently, the orbitrap takes the place of the quadrupole to separate the ions based on m/z. The orbitrap "has ions spinning around a carefully shaped central electrode while shuttling back and forth over its long axis in harmonic motion at frequencies dependent only on their mass-to-charge ratios," says R. Graham Cooks of Purdue University.
More interesting news from PittCon to come.
Labels:
analytical chemistry,
cutting edge literature,
ICPMS,
research
Sunday, April 16, 2006
Bismuth
Interesting facts about Bi, mass 209 (the only stable isotope), atomic number 83.
It melts at 520 F, maybe possible in the oven.
It boils at 1833 K (2840 F). The ICP plasma I use is 8,000 - 10,000 K.
Not quite as toxic as other elements in the same group, arsenic and antimony. Bismuth is used in cosmetics. And it's in Pepto-Bismol
The most diamagnetic metal, a weak type of magnatism compared to ferro- or paramagnatism. It wouldn't stick to your fridge.
It is used as an internal standard, it is run through the mass spec with every sample at the same concentration, and I make sure the instrument gives the same result. One way to tell if the instrument drifts.
Around $8 / kg.
It melts at 520 F, maybe possible in the oven.
It boils at 1833 K (2840 F). The ICP plasma I use is 8,000 - 10,000 K.
Not quite as toxic as other elements in the same group, arsenic and antimony. Bismuth is used in cosmetics. And it's in Pepto-Bismol
The most diamagnetic metal, a weak type of magnatism compared to ferro- or paramagnatism. It wouldn't stick to your fridge.
It is used as an internal standard, it is run through the mass spec with every sample at the same concentration, and I make sure the instrument gives the same result. One way to tell if the instrument drifts.
Around $8 / kg.
Tuesday, April 11, 2006
Water droplet
I may have found the answer to my question of why that one drop of liquid always jumps up at me (see previous post), at physicsweb.org/articles/news/10/4/4/1
If I knew how to put the link in, I would.
If I knew how to put the link in, I would.
Blogroll
I finally found out how to write some code and put some more crap on the sidebar over there. It is now cool to put pictures on your blog, relevent to what you're talking about. And if you want to be really cool, you can put clever little captions on the picture for some comic relief.
But seriously, Dylan's blog about synthetic organic grad school life is great. I can now live my dream vicariously through his daily posts. I've been reading In the pipeline written by Derek Lowe for a while now, it's about life as a wonder drug maker in the pharmaceutical industry.
I also found out how to make your blog come into the top ten on Google. Actually, I read about it on some other dude's blog and I forgot his name. I've noticed people are as serious about getting referenced on the internet as in chemistry journals. To get your blog to the top ten, write about something specific, then email all the top read bloggers in that subject and kindly ask them to link your blog. Once you get enough links and enough people coming by, you are one of the first links for that specific subject on a google search. Or maybe that was the way to get more visitors to your blog?
Anyways, pictures are coming, and if I'm in a good mood, clever captions.
But seriously, Dylan's blog about synthetic organic grad school life is great. I can now live my dream vicariously through his daily posts. I've been reading In the pipeline written by Derek Lowe for a while now, it's about life as a wonder drug maker in the pharmaceutical industry.
I also found out how to make your blog come into the top ten on Google. Actually, I read about it on some other dude's blog and I forgot his name. I've noticed people are as serious about getting referenced on the internet as in chemistry journals. To get your blog to the top ten, write about something specific, then email all the top read bloggers in that subject and kindly ask them to link your blog. Once you get enough links and enough people coming by, you are one of the first links for that specific subject on a google search. Or maybe that was the way to get more visitors to your blog?
Anyways, pictures are coming, and if I'm in a good mood, clever captions.
Tuesday, April 04, 2006
Outsourcing
It is here. We are losing oppurtunities everyday. I'll make a future prediction: India and China will produce most of the new drugs simply because they have a lot more people actually doing research. They have four times as many people as we do, producing more scientist and engineers than we do. That's if their governments don't tear the country down.
It's fairly obvious to me why Americans don't want to go into science. It does not pay well. I read somewhere, adjusted for IQ, scientists are the lowest paid workers in the country. Especially for PhD's, they go to school for 4 to 6 years, then struggle to get a job. Even better of a question, why are we telling American college students to go into science when there are no jobs to get when you get out? Getting an academic research professor job for a chemist is like getting to the Major League in baseball. Only the elite can make it, it takes natural talent. So please, current professors out there, tell your students the truth: If they don't have a 4.0 and work for a "famous" scientist, they won't get their dream job doing whatever research interests them. If you're smart and you have the ability to go past a bachelors degree, the law or medical degree will earn you money after you have no problem finding a job. I wonder what the unemployment rate would look like between chemistry PhD's, lawyers, and doctors. I guess it would look better if you only looked at people working in the field of their degree.
By the way, I'm a happy scientist.
It's fairly obvious to me why Americans don't want to go into science. It does not pay well. I read somewhere, adjusted for IQ, scientists are the lowest paid workers in the country. Especially for PhD's, they go to school for 4 to 6 years, then struggle to get a job. Even better of a question, why are we telling American college students to go into science when there are no jobs to get when you get out? Getting an academic research professor job for a chemist is like getting to the Major League in baseball. Only the elite can make it, it takes natural talent. So please, current professors out there, tell your students the truth: If they don't have a 4.0 and work for a "famous" scientist, they won't get their dream job doing whatever research interests them. If you're smart and you have the ability to go past a bachelors degree, the law or medical degree will earn you money after you have no problem finding a job. I wonder what the unemployment rate would look like between chemistry PhD's, lawyers, and doctors. I guess it would look better if you only looked at people working in the field of their degree.
By the way, I'm a happy scientist.
Tuesday, March 21, 2006
March Update
Hopefully I'll be able to blog more than once a month. I started out thinking I could post everyday, like there would be plenty to talk about. Well, there is plenty going on, it's just a matter of remembering events and getting to a computer and thinking of a clever way to present things.
Anyways, the arsenic situation: Dumb mistake. It's too embarrasing to tell here where the false positives were coming from. Email me if you fall into a similar situation.
Anybody else hate when you pour a liquid out of a container into another container containing liquid with a wide mouth, like a bucket and the first drop hits and there's always that one drop that jumps out. Whats the deal with that? Is it the liquid that was being poured in or is it the liquid that is already sitting in the container that you poured into? Confusing? Yes.
Also, I'm going to create a blogroll on the sidebar over there to list cool scientific blogs like Derek Lowe's on Corante and Dylan something's that talks about synthetic organic grad school.
Anyways, the arsenic situation: Dumb mistake. It's too embarrasing to tell here where the false positives were coming from. Email me if you fall into a similar situation.
Anybody else hate when you pour a liquid out of a container into another container containing liquid with a wide mouth, like a bucket and the first drop hits and there's always that one drop that jumps out. Whats the deal with that? Is it the liquid that was being poured in or is it the liquid that is already sitting in the container that you poured into? Confusing? Yes.
Also, I'm going to create a blogroll on the sidebar over there to list cool scientific blogs like Derek Lowe's on Corante and Dylan something's that talks about synthetic organic grad school.
Tuesday, February 28, 2006
Phosphorus and methamphetamine
A great idea, all this time, and no comments. Well, fellow mass spectrometrists of the world, I've got some new things to talk (write, type, blog) about.
Short side note, anyone ever hear a hissing noise comming from the torch box. It's not an electrical arc or I just can't see one. I have produced an electrical arc on the torch itself before and gave it a nice melted dimple. This noise seems to be something else, almost sounds like gas or water blowing out a small hose, but I think if that was the case, things wouldn't be working as well as they have been. No visible damage or drift caused by noise.
Next up, I just got word that I will be analyzing some samples from a meth lab bust. I'll be looking for phosphorus. I imagine I'll find some since the samples are taken from powder made by grinding up match heads. So, I don't think I'll have any actual meth in the lab, sorry. I know detection limits are crappy, like 1ppm, anyone know about any interferences or any other problems analyzing phosphorus.
Methamphetamine has quite a history. It's a farely new drug, first synthesized in 1919 in Japan. It was distributed during WWII to Nazi soldiers as a stimulant. In the 50's it saw such uses as a cure for narcolepsy, post-encephalitic parkinsonism, alcoholism, depression, and obesity. What a wonder drug back then. Made illegal sometime in the 80's when its recreational use started up.
Easily made by even non-chemists from pseudoephedrine hydrochloride, various different procedures found in chemistry journals or sketchy websites. There is a wealth of information found on Wikipedia (who checks the facts on this website?)
Short side note, anyone ever hear a hissing noise comming from the torch box. It's not an electrical arc or I just can't see one. I have produced an electrical arc on the torch itself before and gave it a nice melted dimple. This noise seems to be something else, almost sounds like gas or water blowing out a small hose, but I think if that was the case, things wouldn't be working as well as they have been. No visible damage or drift caused by noise.
Next up, I just got word that I will be analyzing some samples from a meth lab bust. I'll be looking for phosphorus. I imagine I'll find some since the samples are taken from powder made by grinding up match heads. So, I don't think I'll have any actual meth in the lab, sorry. I know detection limits are crappy, like 1ppm, anyone know about any interferences or any other problems analyzing phosphorus.
Methamphetamine has quite a history. It's a farely new drug, first synthesized in 1919 in Japan. It was distributed during WWII to Nazi soldiers as a stimulant. In the 50's it saw such uses as a cure for narcolepsy, post-encephalitic parkinsonism, alcoholism, depression, and obesity. What a wonder drug back then. Made illegal sometime in the 80's when its recreational use started up.
Easily made by even non-chemists from pseudoephedrine hydrochloride, various different procedures found in chemistry journals or sketchy websites. There is a wealth of information found on Wikipedia (who checks the facts on this website?)
Saturday, February 18, 2006
Message board
My original idea was to create a message board where mass spec researchers and analysts could discuss trouble shooting. I suggested it to the company which makes the mass spec I work with, but I havn't recieved any reply and didn't really expect it.
So, I'm taking it upon myself. I am currently an environmental chemist using mass spectrometry to analyze water and sediment samples for metals. The mass spec I use uses a quadrupole to filter the ions and it also has a type of collision cell that all the companies are putting out now. The collision cell is supposed to reduce interferents by colliding the interferents with other gas molecules supplied into the collision cell. It also has kinetic energy discrimination which uses some various lens voltages within the collision cell to limit the range of kinetic energies in the ion beam coming out of the collision cell.
I've got everything working pretty well after battling for 6 to 8 months. But I still have some elusive problems which is why I'm creating this blog, or message board.
Anybody analyze Arsenic in salt water with a collision cell? I can't get rid of some interferent at mass 75 which gives me a constant result of 6 - 10ppb in salt water samples that are confirmed having less arsenic by a optical method (ICP emission.) I can discuss a lot more if anybody else knows anything about this.
So, I'm taking it upon myself. I am currently an environmental chemist using mass spectrometry to analyze water and sediment samples for metals. The mass spec I use uses a quadrupole to filter the ions and it also has a type of collision cell that all the companies are putting out now. The collision cell is supposed to reduce interferents by colliding the interferents with other gas molecules supplied into the collision cell. It also has kinetic energy discrimination which uses some various lens voltages within the collision cell to limit the range of kinetic energies in the ion beam coming out of the collision cell.
I've got everything working pretty well after battling for 6 to 8 months. But I still have some elusive problems which is why I'm creating this blog, or message board.
Anybody analyze Arsenic in salt water with a collision cell? I can't get rid of some interferent at mass 75 which gives me a constant result of 6 - 10ppb in salt water samples that are confirmed having less arsenic by a optical method (ICP emission.) I can discuss a lot more if anybody else knows anything about this.
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