Friday
Still no oven. GC care package did not arrive at CERES.
Adama made the PRC standard today, but Anna, Marie, and Vieux were present. We were experiencing power outages all day long, but mostly for only a minute or two at a time. We were going to check the standard on the GC to verify it, but during the run the power went out for good. Needless to say the battery back-up and it's capacitors only held up for about 35 minutes. I would add that the capacity of the back-up was probably compromised due to the frequent losses of power earlier in the day. This failure of the back-up occurred around 1:45 PM during the middle of a GC run. The CERES staff and I had already agreed to come in on Saturday to make LFT, but since we could not confirm the PRC standard we'll see what tomorrow holds. We still have part of the day on Tuesday to finish LFT if need be.
Saturday
We made open-ended LFT today for the upcoming deployment. This means we essentially made the LFT with one looped end and with one open end so that it can be easily fortified with the PRC solution at a later date.
Since we had to wait on the GC before we could proceed, we spent the rest of our afternoon cleaning the cages with Alconox and water and gathering materials need for the deployment next week.
I spent much of the morning bringing the GC back online after the power failure on Friday. It had lost power just after an injection so it took a while for the compounds to come off the column and by the time we left for the day the baseline was still not that low. I will wait to see what the PRC solution looks like on the GC on Monday.
Friday, February 6, 2009
Thursday, February 5, 2009
Week 2 - Thursday
Still no oven. I was told by Baba that the manufacturer had forgot to send it over here. It very much sounds like we are being given the "run around" by this company or an intermediary.
Baba and I paid a visit to Air Liquid our helium supplier to confirm the purity of the helium sent to us. After a very lengthy discussing I found that it is currently grade 4.5 or 99.995%.
We wanted to make the Performance Reference Compound spike today but it did not happen. There were many factors delaying this. The main problem was the purity of hexanes we were going to use was in question. After doing an air injection on the gc which turned out clean shown below in first picture. I suspect the contamination from yesterday came from the hexanes (VWR brand new bottle) not the GC itself. This was confirmed by injection a different brand of hexanes (Panreac) shown below in second picture. It shows much smaller peaks (same scale on left) if you compare it the chromatogram from the previous day. We also injected another new bottle of hexanes (VWR) of the same lot and got similar results as yesterdays runs. Anna and I worked on most of this together.
There was not enough time in the day to make the standard and we will proceed tomorrow and if it checks out on the GC we will begin making LFT. If need be the CERES staff will be happy to work on Saturday to ensure the success of this project.
Good news, we found a 10-100 ul pipet. This should aid us in making standards very much and these pipets seems to be of decent quality...brand name Hightech lab series LM.
We will try to pick up the "GC-care" package that glenn sent to CERES on friday morning.
Baba and I paid a visit to Air Liquid our helium supplier to confirm the purity of the helium sent to us. After a very lengthy discussing I found that it is currently grade 4.5 or 99.995%.
We wanted to make the Performance Reference Compound spike today but it did not happen. There were many factors delaying this. The main problem was the purity of hexanes we were going to use was in question. After doing an air injection on the gc which turned out clean shown below in first picture. I suspect the contamination from yesterday came from the hexanes (VWR brand new bottle) not the GC itself. This was confirmed by injection a different brand of hexanes (Panreac) shown below in second picture. It shows much smaller peaks (same scale on left) if you compare it the chromatogram from the previous day. We also injected another new bottle of hexanes (VWR) of the same lot and got similar results as yesterdays runs. Anna and I worked on most of this together.
There was not enough time in the day to make the standard and we will proceed tomorrow and if it checks out on the GC we will begin making LFT. If need be the CERES staff will be happy to work on Saturday to ensure the success of this project.Good news, we found a 10-100 ul pipet. This should aid us in making standards very much and these pipets seems to be of decent quality...brand name Hightech lab series LM.
We will try to pick up the "GC-care" package that glenn sent to CERES on friday morning.
Week 2 - Wednesday
Still no oven, manufacturer could not be reached
Baba, Marie, and I visited blacksmith. He's working on the spiders and was drilling holes for water flow through top and bottom of cage. Told him to refocus efforts on the spiders as those are most crucial to the project not the holes. Told him Monday afternoon was the very very latest to get them done.
After the shut down yesterday it took a long time today to bring the GC back online and have a low baseline. After the baseline leveled out we ran some hexane reagent blanks. The chromatograms is shown below. As you can see this is not ideal for a reagent blank. The large peak is usually around 2,000 Hz
For standards we really need a 100 ul pipet, but have not found one that works well.
Baba, Marie, and I visited blacksmith. He's working on the spiders and was drilling holes for water flow through top and bottom of cage. Told him to refocus efforts on the spiders as those are most crucial to the project not the holes. Told him Monday afternoon was the very very latest to get them done.
After the shut down yesterday it took a long time today to bring the GC back online and have a low baseline. After the baseline leveled out we ran some hexane reagent blanks. The chromatograms is shown below. As you can see this is not ideal for a reagent blank. The large peak is usually around 2,000 Hz
For standards we really need a 100 ul pipet, but have not found one that works well.
Tuesday, February 3, 2009
Week 2 - Tuesday
Still no oven. I haven't heard back from Makhfousse on the status yet.
The GC ran at over night and the baseline this morning was steady at 500 Hz for the front detector and 750 for the back detector at 300 C. At 110 C the baseline was around 250 Hz for each, which is much better than before. We replaced the injector needles and rinsed the auto sampler rinse vials and added new solvent. We ran several injections of hexanes (all solvents were newly opened bottles). There are 2 or 3 stubborn peaks that show up in both front and back chromatograms starting at 24 minutes and some high grassy baseline towards the end of the run. Each successive injection showed the peaks at the same height. Most of this work was down by me, Anna also was there to observe and learn. Much of today the CERES staff was working on bring up a Varian GC for some pesticide verification work they had to do. Baba helped them with all of this.
We searched for the 1,000-10,000 ul pipet that was in the lab the previous week and it could not be located. It would be nice to have had it along with pipet tips that fit that autopipet, but this was overlooked until after the shipment from OSU. The other item that would be nice to have would be GC vial inserts to limit wasting standards, but we can make do if we have to.
We washed some ground glass stoppers so we could start making standards tomorrow. We are using an oven that is in the biology lab here that can heat up and past the 400 C mark needed. They are in the oven and will remain there until the morning. Marie, Adama, Vieux, and I participated in that.
My GC work was cut short ~3:00 pm as the electricians had to shut down the power to replace a part in the power house.
The GC ran at over night and the baseline this morning was steady at 500 Hz for the front detector and 750 for the back detector at 300 C. At 110 C the baseline was around 250 Hz for each, which is much better than before. We replaced the injector needles and rinsed the auto sampler rinse vials and added new solvent. We ran several injections of hexanes (all solvents were newly opened bottles). There are 2 or 3 stubborn peaks that show up in both front and back chromatograms starting at 24 minutes and some high grassy baseline towards the end of the run. Each successive injection showed the peaks at the same height. Most of this work was down by me, Anna also was there to observe and learn. Much of today the CERES staff was working on bring up a Varian GC for some pesticide verification work they had to do. Baba helped them with all of this.
We searched for the 1,000-10,000 ul pipet that was in the lab the previous week and it could not be located. It would be nice to have had it along with pipet tips that fit that autopipet, but this was overlooked until after the shipment from OSU. The other item that would be nice to have would be GC vial inserts to limit wasting standards, but we can make do if we have to.
We washed some ground glass stoppers so we could start making standards tomorrow. We are using an oven that is in the biology lab here that can heat up and past the 400 C mark needed. They are in the oven and will remain there until the morning. Marie, Adama, Vieux, and I participated in that.
My GC work was cut short ~3:00 pm as the electricians had to shut down the power to replace a part in the power house.
Monday, February 2, 2009
Week 2 - Monday
Today I was hoping to bring the GC online as well as load the new method for the current list of analytes. It did ultimately happen but not without faults. The nitrogen generator we were going to use would not hold pressure so after further investigation we noticed the other generator that had many many hours counted hours even when not running. We are attempting to used this nitrogen generator now. We brought up to temperature of the inlet oven and detectors and they will continue to be held at typical operating temperature overnight. I will assess the baseline then. When I left for the day the detector were reading ~2,000 to 1,500 and dropping somewhat slowly. Adama, Anna, Marie, and Vieux (Trainee) and I were present for the first bit, but once I ramped up the temperatures I mostly was alone, but was showing Anna, Marie, and Adama what I was doing and explained why.
Once again we experienced prolems with the He pressure regulator but I think we have "hopefully" fixed it. Adama, Anna, Marie, Vieux, Baba, Makhfousse, and I were present.
Baba, Adama, and I paid a visit to the fellow making the cages. I guess there was some mis-communication somewhere because there was only 1 spider per cage made, not the 2 like I was expecting. It does not look like we will be going out to the field for a deployment until Tuesday and Wednesday of week 3. The cages and spiders that were produced however were of nice quality. There was a problem however that I alluded to last week. The cages and spiders are a bit small. The cage dimensions are as follows; diameter = 15.5 cm, height = 15 cm. Spider dimensions; diameter = 15 cm, height = 4 to 3.5 cm. We were able to take two cages and 4 spiders back with us to the lab to see if a regular length (1 m) LFT would fit. We found that if a spring were to be used the length of each LFT would need to be anwhere from 93-95 cm long. But as can be seen in the picture below we found a way of winding it around the center pin to make a 1-m LFT work (shown in the bottom picture). It does seem quite secure, so I think we can make it work
As is evident by the pictures above we practice making LFT today. Adama, Marie, Anna, Vieux, and I were present. All seem to be proficient after some practice. Now we need to work on efficiency.
Tomorrow I will further evaluate the GC and we may begin standards paperwork and gather of supplies for the upcoming field deployment if we have time.
Once again we experienced prolems with the He pressure regulator but I think we have "hopefully" fixed it. Adama, Anna, Marie, Vieux, Baba, Makhfousse, and I were present.
Baba, Adama, and I paid a visit to the fellow making the cages. I guess there was some mis-communication somewhere because there was only 1 spider per cage made, not the 2 like I was expecting. It does not look like we will be going out to the field for a deployment until Tuesday and Wednesday of week 3. The cages and spiders that were produced however were of nice quality. There was a problem however that I alluded to last week. The cages and spiders are a bit small. The cage dimensions are as follows; diameter = 15.5 cm, height = 15 cm. Spider dimensions; diameter = 15 cm, height = 4 to 3.5 cm. We were able to take two cages and 4 spiders back with us to the lab to see if a regular length (1 m) LFT would fit. We found that if a spring were to be used the length of each LFT would need to be anwhere from 93-95 cm long. But as can be seen in the picture below we found a way of winding it around the center pin to make a 1-m LFT work (shown in the bottom picture). It does seem quite secure, so I think we can make it work
As is evident by the pictures above we practice making LFT today. Adama, Marie, Anna, Vieux, and I were present. All seem to be proficient after some practice. Now we need to work on efficiency.Tomorrow I will further evaluate the GC and we may begin standards paperwork and gather of supplies for the upcoming field deployment if we have time.