Today not much work was done in the laboratory. The GC run of the retrieval 2 samples at first glance showed the same type of contamination as retrieval 1. This is only a provisional statement until I can look at the chromatograms more in depth. It looks as if the reagent blank is fairly clean though. This leads me to believe that the contamination either was introduce during the storage of the LFT prior to use or during construction. I think we can come to a better conclusion when the data is actually worked up and the blank LFT from the lab is analyzed. I feel that determining where this contamination came from is an absolute must before any other LFT can be made, deployed, or processed.
I performed a thorough review of the bench sheets created during this project and found that more attention to detail is needed when filling these out. I had Anna, Marie, and Adama go over the bench sheets to verify that they were filled out correctly and fix errors that had occurred. It is obvious that some sort of error correction code system or protocol needs to be implemented such as OSU's SOP1200.
A party was thrown in my honor to thank me for my time and effort. It was very much appreciated.
Friday, March 13, 2009
Week 6 - Thursday
Today I had a meeting with Hama, Makhfousse, Baba, Amadou, and Papa Sam Gueye. During this meeting I discussed in length my summary of the training; what had been accomplished, challenges, some suggestions I had for the laboratory. This meeting lasted much of the afternoon.
In the morning we prepared the samples from retrieval 2 and started a run on the GC that will not be over until the morning on Friday. The computer froze after a few injections so we had to start the run over in the afternoon unfortunately. We are still seeing degradation of some analytes in the inlet, but chose to run the samples anyway to better facilitate training. The samples can always be run again at a later date when the inlet problems are resolved. The problem in the inlet seems most likely to be the glass wool. If I had more time I would have removed the glass wool from the liners and evaluated the degradation and compare the two set-ups. Unfortunately during the preparation of the samples which included bringing the final volume up to 2 ml, drawing off 1 mL, and inserting an internal standard spike Adama noticed that the milliliter marks on the centrifuge tubes were not accurately done. I suspect that this was caused by someones incorrect or sloppy pipeting technique. To ensure it was done correctly and to retrain the staff I marked new centrifuge tubes and we quantitatively transferred all the samples to these new tubes before proceeding. This added about two hours to the whole process unfortunately.
Anna was busy most of the day re-updating the calibration table with the new standards that were run last night. We saved this new calibration table under a new processing method name specific to retrieval two. I was with Anna helping her off and on during the day. Adama prepared the samples and seems to be more and more comfortable in the lab.
Much of the staff's time today was shared between working on this project and another project that had come in a few days earlier looking at pesticides in what I believe was peanut oil.
In the morning we prepared the samples from retrieval 2 and started a run on the GC that will not be over until the morning on Friday. The computer froze after a few injections so we had to start the run over in the afternoon unfortunately. We are still seeing degradation of some analytes in the inlet, but chose to run the samples anyway to better facilitate training. The samples can always be run again at a later date when the inlet problems are resolved. The problem in the inlet seems most likely to be the glass wool. If I had more time I would have removed the glass wool from the liners and evaluated the degradation and compare the two set-ups. Unfortunately during the preparation of the samples which included bringing the final volume up to 2 ml, drawing off 1 mL, and inserting an internal standard spike Adama noticed that the milliliter marks on the centrifuge tubes were not accurately done. I suspect that this was caused by someones incorrect or sloppy pipeting technique. To ensure it was done correctly and to retrain the staff I marked new centrifuge tubes and we quantitatively transferred all the samples to these new tubes before proceeding. This added about two hours to the whole process unfortunately.
Anna was busy most of the day re-updating the calibration table with the new standards that were run last night. We saved this new calibration table under a new processing method name specific to retrieval two. I was with Anna helping her off and on during the day. Adama prepared the samples and seems to be more and more comfortable in the lab.
Much of the staff's time today was shared between working on this project and another project that had come in a few days earlier looking at pesticides in what I believe was peanut oil.
Week 6 - Wednesday
We ran into problems with the GC today. It looks as if some of our analytes are being degraded in the inlet more and more each injection. From the Friday of week 5 to today I can see a definite progression of either lost or smeared peaks for several analytes. It is most noticeable for propanil, fipronil, dimethoate, and DDT.
Most of my time was spent working with Anna on interpreting chromatograms, manual integrations, compiling data into a raw data master spreadsheet for data work-up, and general troubleshooting of the inlet problems. The other staff, especially Adama were observing the training as well.
Adama and I vialed up new standards specifically for the retrieval 2 samples and set up a run on the GC over night. Anna should be working on reviewing the run tomorrow and updating the calibration table.
Most of my time was spent working with Anna on interpreting chromatograms, manual integrations, compiling data into a raw data master spreadsheet for data work-up, and general troubleshooting of the inlet problems. The other staff, especially Adama were observing the training as well.
Adama and I vialed up new standards specifically for the retrieval 2 samples and set up a run on the GC over night. Anna should be working on reviewing the run tomorrow and updating the calibration table.
Monday, March 9, 2009
Tuesday, March 3, 2009
Week 6 - Tuesday
Good and bad news...today we re-looked at the chromatograms and realized there was a switch that must have happened between the reagent blank and a real sample during a transfer step during processing. This was confirmed through our duplicate analysis. The reagent blank looks exactly like the sample "field site #3 duplicate". We can never know for sure but the chromatograms are fairly undeniable. We still don't know where the other contamination came from in the other QC samples (which is the bad news). Tomorrow when we run our 2nd retrieval samples we will have a better idea. If I don't find out what caused it by the time I leave the staff here are very motivated in finding where it came from....they want to succeed. Anna has picked up fairly fast on the GC training I'm happy to say. I will post if and when we find out what might have happened...or any other interesting revelations.
Here are the internal dimensions of the oven shown as actual(usable): DxWxH 55cm(53), 33cm(29, shelf braces), 31cm(31). We can fit a maximum of 7 cages inside (more practically 6). I do not think it is possible to put an exhaust fan or a port on it, it is the wrong type of oven for that. If there are any more questions about the oven feel free to ask.
Today we re-updated the calibration table for the front and back detector (Anna and I, Marie, Adama, and Vieux were present too). We keep running into problems with some compounds continually shifting retention times (propanil, dimethoate, fipronil). We ran in to some other problems with the back column. I think we may need to invest in some backup and/or new columns. I don't think the back column is in all that good of shape as near as I can tell. We vialed up some new standards and are running those tonight.
Tomorrow we will run the 2nd retrieval samples on the GC and start working on the calculation spreadsheet.
We did a dialysis on the blank LFT we put out into the lab. I'm not sure if we can run these on the GC before I leave though. If I don't I am confident the staff can.
Here are the internal dimensions of the oven shown as actual(usable): DxWxH 55cm(53), 33cm(29, shelf braces), 31cm(31). We can fit a maximum of 7 cages inside (more practically 6). I do not think it is possible to put an exhaust fan or a port on it, it is the wrong type of oven for that. If there are any more questions about the oven feel free to ask.
Today we re-updated the calibration table for the front and back detector (Anna and I, Marie, Adama, and Vieux were present too). We keep running into problems with some compounds continually shifting retention times (propanil, dimethoate, fipronil). We ran in to some other problems with the back column. I think we may need to invest in some backup and/or new columns. I don't think the back column is in all that good of shape as near as I can tell. We vialed up some new standards and are running those tonight.
Tomorrow we will run the 2nd retrieval samples on the GC and start working on the calculation spreadsheet.
We did a dialysis on the blank LFT we put out into the lab. I'm not sure if we can run these on the GC before I leave though. If I don't I am confident the staff can.
Week 6 - Monday
The 1st retrieval samples ran over the weekend on the GC.
GC training was done with Anna mostly (Adama, Marie, and Vieux were watching, but were also in and out). We processed the front column chromatograms and looked at the standards we ran with the samples. While viewing and processing the QC samples it was obvious that there was a cross contamination (of most of the analytes in our method) issue happening, which is unfortunate. The worst sample was probably the reagent blank, which during the dialysis was the last sample to be transferred and processed to see if we had cross contamination.
Part of the day was spent trying to track down where this contamination occurred. There was a centrifuge tube that had hexanes in it that was in the blow down module that had been exposed to the air in the lab for ~1 week and we ran that and found no peaks that were identifiable, so the contamination is probably not coming from the ambient air. I had previously not seen any contamination with solvent blown down on the rotovap, so that is likely not the source.
We made 4 blank LFT and set them up in the hood, bench top, freezer, and LFT construction rig to see a worse case scenario. If we see nothing in these samples then I don't really know where the contamination came from. If you have any ideas please post them as a comment to this post.
Tuesday I hope to prepare and run samples from the 2nd retrieval. We will also finish updating the the calibration curve for the back column and hopefully finish analyzing chromatograms so we can start looking at the calculation spreadsheet.
GC training was done with Anna mostly (Adama, Marie, and Vieux were watching, but were also in and out). We processed the front column chromatograms and looked at the standards we ran with the samples. While viewing and processing the QC samples it was obvious that there was a cross contamination (of most of the analytes in our method) issue happening, which is unfortunate. The worst sample was probably the reagent blank, which during the dialysis was the last sample to be transferred and processed to see if we had cross contamination.
Part of the day was spent trying to track down where this contamination occurred. There was a centrifuge tube that had hexanes in it that was in the blow down module that had been exposed to the air in the lab for ~1 week and we ran that and found no peaks that were identifiable, so the contamination is probably not coming from the ambient air. I had previously not seen any contamination with solvent blown down on the rotovap, so that is likely not the source.
We made 4 blank LFT and set them up in the hood, bench top, freezer, and LFT construction rig to see a worse case scenario. If we see nothing in these samples then I don't really know where the contamination came from. If you have any ideas please post them as a comment to this post.
Tuesday I hope to prepare and run samples from the 2nd retrieval. We will also finish updating the the calibration curve for the back column and hopefully finish analyzing chromatograms so we can start looking at the calculation spreadsheet.
Week 5 - Saturday
We have a lot of work to do still, especially on the GC and thus we Anna, Adama, and I came in to work from 9 to 3:30.
Anna, Adama, and I spent most of the day updating the calibration table and doing training on the GC. We also now have all compound retention times in the calibration table correctly. While updating, it was clear that a few compounds don't show up on the GC here as well as they do at OSU, especially fipronil, dimethoate, and propanil. These compounds may need to be dropped from the method. A lot of time was lost today because of a software glitch with Chemstation. The calibration table would not communicate correctly with it's own software and had to be rebuilt a few times. It was good practice for the staff, but a set back nonetheless.
We prepared the 1st retrieval samples to be run on the GC over Saturday night and Sunday. Adama brought the samples up to volume, I transferred them to the GC vials at 1 mL, and Anna administered the I.S. spike. One sample was compromised as a result of a bad spike, but the samples were analyzed in duplicate.
Anna, Adama, and I spent most of the day updating the calibration table and doing training on the GC. We also now have all compound retention times in the calibration table correctly. While updating, it was clear that a few compounds don't show up on the GC here as well as they do at OSU, especially fipronil, dimethoate, and propanil. These compounds may need to be dropped from the method. A lot of time was lost today because of a software glitch with Chemstation. The calibration table would not communicate correctly with it's own software and had to be rebuilt a few times. It was good practice for the staff, but a set back nonetheless.
We prepared the 1st retrieval samples to be run on the GC over Saturday night and Sunday. Adama brought the samples up to volume, I transferred them to the GC vials at 1 mL, and Anna administered the I.S. spike. One sample was compromised as a result of a bad spike, but the samples were analyzed in duplicate.
Week 5 - Friday
The results from the GC run overnight shows that there is little difference between using centrifuge tubes marked at 1 and 2 ml and using an automated pipet for 1 mL. The key is being accurate with the marks on the centrifuge tubes. Given this information we prepared standards for the calibration table with internal standards (Adama pipeting each composite standard dilution and me introducing the internal standard). These ran over night.
We also performed a dialysis of the 2nd retrieval samples and some of the QC. I will be taking some QC samples (1 trip blank, 1 field exposure blank, 1 lab cleaning blank) back with me to OSU. I observed the dialysis and corrected technique where needed but for the most part did not physically help. The staff's technique had improved since the 1st retrieval's samples were processed. (Adama, Anna, Vieux, and Marie were present)
We also performed a dialysis of the 2nd retrieval samples and some of the QC. I will be taking some QC samples (1 trip blank, 1 field exposure blank, 1 lab cleaning blank) back with me to OSU. I observed the dialysis and corrected technique where needed but for the most part did not physically help. The staff's technique had improved since the 1st retrieval's samples were processed. (Adama, Anna, Vieux, and Marie were present)
Friday, February 27, 2009
Week 5 - Thursday
Last night Anna and I ran the I.S. and mix of PRC and 14 analytes so that we could update the calibration table retention times in Chemstation. At first glance the chromatograms looked great, but we are starting to lose a little resolution between some compounds...yet gaining some with others. The elution order and peak identification were hard to place a finger on with a few compounds near the middle of the run (Chlorpyrifos, Fipronil, PCB 100, Fenitrothion). The peak height ratios didn't really help much either. We found some standards in the freezer that had been previously used for other projects and did some dilutions and ran them for retention time. We are still sorting out two compounds. The back column was straight forward from the beginning. Also I am not seeing the breakdown in the inlet of compounds like I was before.
At the end of the day we realized that we were going to have a problem with pipeting 1 ml into or out of GC auto-sampler vials due to the pipet tip being too wide. After several email exchanges with Glenn and a Skype conversation with Paul we decided that we could just use the 1 and 2 ml graduations on the centrifuge tubes as volumes. This would simplify everything.
Overnight Anna and I ran on the GC 2 samples each of 1 mL of hexanes transferred using a 1 mL automated pipet and 1 mL hexanes transferred using graduations on a centrifuge tube and spiked all samples with the internal standard at 100 PPB. I wanted to know how accurate the centrifuge tube method was compared to the automated pipet method.
Adama, Marie, and Vieux arrived from St. Louis and performed the solvent cleaning of the 2nd retrieval samples. We will do the dialysis of these samples tomorrow. We will run the calibration standards on the GC tomorrow as well.
At the end of the day we realized that we were going to have a problem with pipeting 1 ml into or out of GC auto-sampler vials due to the pipet tip being too wide. After several email exchanges with Glenn and a Skype conversation with Paul we decided that we could just use the 1 and 2 ml graduations on the centrifuge tubes as volumes. This would simplify everything.
Overnight Anna and I ran on the GC 2 samples each of 1 mL of hexanes transferred using a 1 mL automated pipet and 1 mL hexanes transferred using graduations on a centrifuge tube and spiked all samples with the internal standard at 100 PPB. I wanted to know how accurate the centrifuge tube method was compared to the automated pipet method.
Adama, Marie, and Vieux arrived from St. Louis and performed the solvent cleaning of the 2nd retrieval samples. We will do the dialysis of these samples tomorrow. We will run the calibration standards on the GC tomorrow as well.
Week 5 - Wednesday
Sorry for the delay in posts, we've been working late and the internet at Hacienda had been down.
In the morning the staff (Adama, Anna, Marie, Vieux, and I) performed the sample blow down. That is, we used the Rotovaps and performed the nitrogen final blow down. The blow down took a very long time as only one rotovap can be used at a time due to the glassware compatibility problem I posted about before.
Some calibration standards and the internal standards were checked on the GC today.
We washed dishes today in preparation of the field samples from retrieval 2.
In the morning the staff (Adama, Anna, Marie, Vieux, and I) performed the sample blow down. That is, we used the Rotovaps and performed the nitrogen final blow down. The blow down took a very long time as only one rotovap can be used at a time due to the glassware compatibility problem I posted about before.
Some calibration standards and the internal standards were checked on the GC today.
We washed dishes today in preparation of the field samples from retrieval 2.
Wednesday, February 25, 2009
Week 5 - Tuesday
Update
Make serial dilutions of PRC and mix of analytes for calibration curve DONE
Make internal standard composite DONE
Solvent cleaning of field samples from the first retrieval DONE
Dialysis of first retrieval samples and QC DONE
Run practice samples on GC NO
Check some calibration standards on GC NO
Tuesday was a long day. The staff arrived at 8:00 am and we left at 7:00 pm. The decision was made to have Anna and I not go out to the field on Wednesday. We felt that we could use that time to train Vieux in the field and Anna and I could spend some much needed time on the GC. We got a lot done, but still have a lot of work ahead of us.
Make serial dilutions of PRC and mix of analytes for calibration curve DONE
Make internal standard composite DONE
Solvent cleaning of field samples from the first retrieval DONE
Dialysis of first retrieval samples and QC DONE
Run practice samples on GC NO
Check some calibration standards on GC NO
Tuesday was a long day. The staff arrived at 8:00 am and we left at 7:00 pm. The decision was made to have Anna and I not go out to the field on Wednesday. We felt that we could use that time to train Vieux in the field and Anna and I could spend some much needed time on the GC. We got a lot done, but still have a lot of work ahead of us.
Monday, February 23, 2009
Week 5 - Monday
This weeks outline
Monday - Create a blow-down module, do final blow down of practice samples, bake out glassware
Tuesday - Make serial dilutions of PRC and mix of analytes for calibration curve, make internal standard composite, log in samples, do solvent cleaning of field samples from the first retrieval, do dialysis of field samples and QC, run practice samples on GC, check some calibration standards on GC
Wednesday - Blow down samples, run calibration standards on GC, travel to St. Louis
Thursday - 2nd and final retrieval, travel back to Dakar
Friday - Log in samples, solvent cleaning of 2nd retrieval samples, run 1st retrieval samples on GC, clean glassware
Today Adama and I were able to create a blow down system (seen in picture below) that should work until a suitable replacement can be purchased (like a turbo-vap). We thoroughly cleaned all the parts of the new blow-down system we could. We tested the oven today and we found that the oven takes a long time to cool down. There is no exhaust fan, it is all internal. This will increase the time that the glassware will be unavailable to us as it is cooling. We can crack the door and get a decent rate of cool down, but when the oven shuts the heating coils off in the middle of the night it does not cool much before we arrive in the morning unfortunately. We started working on the paperwork for the standards to make tomorrow go faster.
On Friday I talked to Baba about getting the hood motors fixed since only one worked and it was underpowered. A technician came by today to check it out and told Baba, he would need to upgrade all the motors and replace them for the hoods to work effectively...I would agree. Also we had a guy come about the stainless steel counter-top and hood. He made measurements and can probably start this week. I think Baba said it would take about 2 to 3 days to complete when he starts. I believe it will be made with nice 1.5 mm stainless.
Monday - Create a blow-down module, do final blow down of practice samples, bake out glassware
Tuesday - Make serial dilutions of PRC and mix of analytes for calibration curve, make internal standard composite, log in samples, do solvent cleaning of field samples from the first retrieval, do dialysis of field samples and QC, run practice samples on GC, check some calibration standards on GC
Wednesday - Blow down samples, run calibration standards on GC, travel to St. Louis
Thursday - 2nd and final retrieval, travel back to Dakar
Friday - Log in samples, solvent cleaning of 2nd retrieval samples, run 1st retrieval samples on GC, clean glassware
Today Adama and I were able to create a blow down system (seen in picture below) that should work until a suitable replacement can be purchased (like a turbo-vap). We thoroughly cleaned all the parts of the new blow-down system we could. We tested the oven today and we found that the oven takes a long time to cool down. There is no exhaust fan, it is all internal. This will increase the time that the glassware will be unavailable to us as it is cooling. We can crack the door and get a decent rate of cool down, but when the oven shuts the heating coils off in the middle of the night it does not cool much before we arrive in the morning unfortunately. We started working on the paperwork for the standards to make tomorrow go faster.
On Friday I talked to Baba about getting the hood motors fixed since only one worked and it was underpowered. A technician came by today to check it out and told Baba, he would need to upgrade all the motors and replace them for the hoods to work effectively...I would agree. Also we had a guy come about the stainless steel counter-top and hood. He made measurements and can probably start this week. I think Baba said it would take about 2 to 3 days to complete when he starts. I believe it will be made with nice 1.5 mm stainless.
Week 4 - Friday
Today was a short day, I left at 2:00-ish, so did the rest of the staff.
The plan for today was to blow down our practice samples in preparation to run them on the GC. It became apparent that only certain parts of the N2 blow-down module (similar in function to the Anderson Lab's turbo-vap) worked properly. I was able to confirm with the staff that it had only kind of work as of late. Even with the functioning parts i don't think the flow through the 1/8 copper supply tubing would be sufficient for several simultaneous samples. I took apart the blow-down module to inspect it and can understand why it doesn't work very well. There is a design flaw and is needs new parts from the manufacturer to work correctly. We set in motion an idea to construct our own blow-down apparatus and will finish setting it up and testing it on Monday.
The blow-down via the roto-vap and transfer of samples was performed by me first followed by Adama, Marie, and Viex. Anna was present, but did not do/practice the transfer.
The plan for today was to blow down our practice samples in preparation to run them on the GC. It became apparent that only certain parts of the N2 blow-down module (similar in function to the Anderson Lab's turbo-vap) worked properly. I was able to confirm with the staff that it had only kind of work as of late. Even with the functioning parts i don't think the flow through the 1/8 copper supply tubing would be sufficient for several simultaneous samples. I took apart the blow-down module to inspect it and can understand why it doesn't work very well. There is a design flaw and is needs new parts from the manufacturer to work correctly. We set in motion an idea to construct our own blow-down apparatus and will finish setting it up and testing it on Monday.
The blow-down via the roto-vap and transfer of samples was performed by me first followed by Adama, Marie, and Viex. Anna was present, but did not do/practice the transfer.
Friday, February 20, 2009
Week 4 - Wednesday and Thursday
Wednesday in the lab:
We started the dialysis of our practice samples today at 9:00 am. Anna, Marie, Adama, Vieux, and I were present. As it takes at least 4 hours to travel to St. Louis, we left Vieux to finish the 2nd half of the dialysis. Anna, Marie, Adama, and I left for St. Louis Wednesday around 3:00 pm.
Thursday - The retrieval
As we were heading to the first site the pick-up decided to leak all of the water and coolant out of a fitting on the water pump about 10 miles from the site. We had to hitch a ride with what I believe was one of the driver's friends. For the rest of the retrieval we used a horse cart to travel from site to site. The retrieval was successful and all cages were still present and accounted for. Something did happen to the cages though...something i feared after taking a look at the old style cages. They had rusted. Some more than others. It seems as though the stainless used was either a bad batch or low grade. Most of the rust occurred along the welds. I will take some pictures on Monday and post them. I added one picture that kind of shows the rust.
The pickup was towed back to St. Louis and fixed relatively fast though we did have to wait several hours after the retrieval and our horse drawn carriage ride was over.
Sorry I did not post earlier, but I didn't get back to the hotel until about 9 pm.
We started the dialysis of our practice samples today at 9:00 am. Anna, Marie, Adama, Vieux, and I were present. As it takes at least 4 hours to travel to St. Louis, we left Vieux to finish the 2nd half of the dialysis. Anna, Marie, Adama, and I left for St. Louis Wednesday around 3:00 pm.
Thursday - The retrieval
As we were heading to the first site the pick-up decided to leak all of the water and coolant out of a fitting on the water pump about 10 miles from the site. We had to hitch a ride with what I believe was one of the driver's friends. For the rest of the retrieval we used a horse cart to travel from site to site. The retrieval was successful and all cages were still present and accounted for. Something did happen to the cages though...something i feared after taking a look at the old style cages. They had rusted. Some more than others. It seems as though the stainless used was either a bad batch or low grade. Most of the rust occurred along the welds. I will take some pictures on Monday and post them. I added one picture that kind of shows the rust.
The pickup was towed back to St. Louis and fixed relatively fast though we did have to wait several hours after the retrieval and our horse drawn carriage ride was over.
Sorry I did not post earlier, but I didn't get back to the hotel until about 9 pm.
Tuesday, February 17, 2009
Week 4 - Tuesday
Great news...at about 5:15 pm the oven arrived. If we ever need to bake anything out at 3000 C we are set. See picture below. I was told they will install it on Wednesday. The size is a little deceptive, it has a lot of insulation.
We are still trying to get a hold of a pesticide grade hexanes distributor. I'm not sure we can get high quality hexanes before my time is up here.
We made the stock solution for the 14 analytes with the ethyl acetate we found yesterday. I ran several injections of the ethyl acetate on the GC to make sure it was clean....it was. We decided to make some practice samples. We will use the reagent grade hexanes and see what happens. The samples are LFT that were spiked with both our PRC mix and our mix of 14 analytes. While running the ethyl acetate I noticed one peak that shows up in both detectors very consistently. It is definitely higher in the first run of the day if the GC remains idle overnight.
Wednesday we will do a dialysis of the practice samples then leave for St. Louis. We will retrieve on Thursday then head back to Dakar in the afternoon.
We are still trying to get a hold of a pesticide grade hexanes distributor. I'm not sure we can get high quality hexanes before my time is up here.
We made the stock solution for the 14 analytes with the ethyl acetate we found yesterday. I ran several injections of the ethyl acetate on the GC to make sure it was clean....it was. We decided to make some practice samples. We will use the reagent grade hexanes and see what happens. The samples are LFT that were spiked with both our PRC mix and our mix of 14 analytes. While running the ethyl acetate I noticed one peak that shows up in both detectors very consistently. It is definitely higher in the first run of the day if the GC remains idle overnight.
Wednesday we will do a dialysis of the practice samples then leave for St. Louis. We will retrieve on Thursday then head back to Dakar in the afternoon.
Week 4 - Monday
The project of the day was to track down pesticide grade hexanes in Senegal since the only grade in the lab is standard reagent grade. It looks as if there is none in Senegal. It would take at least 2 weeks to ship it, probably more since most of the companies we have contacted, including Fisher seem to take their sweet time answering inquiries. Also, the french websites are not as nicely laid out as the American ones and they are not the same product numbers, so it took a very long time to do to say the least. We did happen upon some pesticide grade ethyl acetate which will work great for standards in the mean time. Baba, Anna, and I spent a lot of time working this out so far.
We ran into a problem with the rotovaps and our glassware but found a solution. The rotovaps have a larger fitting than the round bottom flasks we shipped over previously. Adama found an adapter in a storage room and it works. The problem is that we only have one....so only one operational rotovap. This will increase blow down time unfortunately. We will search harder for another fitting. We have been steadily baking what glassware we can until the new oven arrives.
I'm still running into degradation in the inlet of our third PRC dibutylchlorendate. I re-did the liner for the front inlet, but kept the back the same to compare. It does look much better than before but the dibutylchlorendate is still a problem. Maybe we should not use it. I will be able to better evaluate the situation once we make a standard of the analytes (14 components).
We ran into a problem with the rotovaps and our glassware but found a solution. The rotovaps have a larger fitting than the round bottom flasks we shipped over previously. Adama found an adapter in a storage room and it works. The problem is that we only have one....so only one operational rotovap. This will increase blow down time unfortunately. We will search harder for another fitting. We have been steadily baking what glassware we can until the new oven arrives.
I'm still running into degradation in the inlet of our third PRC dibutylchlorendate. I re-did the liner for the front inlet, but kept the back the same to compare. It does look much better than before but the dibutylchlorendate is still a problem. Maybe we should not use it. I will be able to better evaluate the situation once we make a standard of the analytes (14 components).
Saturday, February 14, 2009
Week 3 - Friday
Today was a short day. It took the morning to bring the GC back online. Adama, Anna, and I were the only ones that came in today. We checked the rotovaps to make sure they were in working condition. They worked just fine, but some replacement parts will probably be needed soon. We also tested the N2 blow-down module. This took a long time to do that since we had to find another gas regulator that worked. So far we have not located any GC-grade hexanes in Senegal yet. They are expecting some soon at one location but it seems as if they really don't know any details beyond that. I ran out of time today and will pursue this more in depth on Monday. Baba knows of our need for high purity hexanes and it being essential for the success of this project.
Week 3 - Wednesday and Thursday (deployment)
Before we left, Adama and I went over the deployment benchsheets. Anna, Adama, the driver and I left mid-day and picked up Marie along the way. We did not have enough time on Wednesday to visit the sampling sites so we did everything on Thursday.
We were only able to find 3 sites to deploy at. Two sites were the same as when Greg was here (the inlet and outlet). The two sites in the irrigation canal that Greg sampled in were dry due to one of the pumps being broken. The third site we sampled was at some other canal that had water in it. It was very stagnant water though. Pictures of the three sites are listed below. I also included a picture of the dry land around the old dried up
sites.
Photo 1: Us at the first sampling site (drainage pump station). From left to right; Me (Lucas), Adama, Marie, Anna.
Photo 2, Site 1: The pump station. Evidence of fishing practices were obvious. There were also plenty of fish present. People were seen near by fetching water.
Photo 3, Site 2: In the adjacent river near the other pump station. 1.5 to 2 m deep. People and livestock were observed either drinking, fetching water, or washing their clothes.
Photo 4, Site 3: A stagnant canal, one of the few other places with any water. It was about 1 m deep. This area seemed to be a well travel route so we hid the rope lines near the bridge/culvert that the picture was taken from.
Photo 5: This is adjacent to the old middle sites that Greg sampled. As you can tell it is very dry.
We were only able to find 3 sites to deploy at. Two sites were the same as when Greg was here (the inlet and outlet). The two sites in the irrigation canal that Greg sampled in were dry due to one of the pumps being broken. The third site we sampled was at some other canal that had water in it. It was very stagnant water though. Pictures of the three sites are listed below. I also included a picture of the dry land around the old dried up
sites.Photo 1: Us at the first sampling site (drainage pump station). From left to right; Me (Lucas), Adama, Marie, Anna.
Photo 2, Site 1: The pump station. Evidence of fishing practices were obvious. There were also plenty of fish present. People were seen near by fetching water.
Photo 3, Site 2: In the adjacent river near the other pump station. 1.5 to 2 m deep. People and livestock were observed either drinking, fetching water, or washing their clothes.Photo 4, Site 3: A stagnant canal, one of the few other places with any water. It was about 1 m deep. This area seemed to be a well travel route so we hid the rope lines near the bridge/culvert that the picture was taken from.
Photo 5: This is adjacent to the old middle sites that Greg sampled. As you can tell it is very dry.
Week 3 - Tuesday
Today we (Adama, Marie, Anna, Vieux, and I) spiked LFT and finished their construction for the upcoming field deployment on Thursday.
We (same people) had to do some sanding of the spiders. Some of the edges were sharp and could easily cut through LFT and skin. After this we cleaned the spiders with detergent; soaking and scrubbing them, then thoroughly rinsing them with tap water. We further cleaned the spiders by submersion and agitation in acetone then hexanes and were left to dry. Once dry the spiders were packaged in clean plastic bags.
I installed new liners for the GC inlet, removing some of the glass wool prior to installation. I also changed out the gold seals and snugged up all the column connections. The new liners seem only to make the multiple peak problem worse, especially for the front detector. At the end of the day I cooled and shut down the GC. The recent power failures led to this decision. I did not want the GC turning off hot while we were in the field. (Anna and Adama were present for most of the GC troubleshooting)
We also gathered more materials for the trip to the field.
We (same people) had to do some sanding of the spiders. Some of the edges were sharp and could easily cut through LFT and skin. After this we cleaned the spiders with detergent; soaking and scrubbing them, then thoroughly rinsing them with tap water. We further cleaned the spiders by submersion and agitation in acetone then hexanes and were left to dry. Once dry the spiders were packaged in clean plastic bags.
I installed new liners for the GC inlet, removing some of the glass wool prior to installation. I also changed out the gold seals and snugged up all the column connections. The new liners seem only to make the multiple peak problem worse, especially for the front detector. At the end of the day I cooled and shut down the GC. The recent power failures led to this decision. I did not want the GC turning off hot while we were in the field. (Anna and Adama were present for most of the GC troubleshooting)
We also gathered more materials for the trip to the field.
Monday, February 9, 2009
Week 3 - Monday
I was paid a visit today by a couple of gentleman by the names of Jeff, Paul, Bill, Hama, and Makhfousse. I accompanied them during their visit until about 1:oo or so when they left.
The retrieval has to be pushed back to Wednesday/Thursday. 32 complete cages have arrived and are in need of cleaning due to all the oil more than likely used in their manufacture. 3 spiders however were made way too small and had to be retrofitted....which the blacksmith did today and we received them shortly before the end of the day. Today we cleaned/scrubbed the cages with Alconox and tap water. Tomorrow we will do the same for the spiders but also we'll do a quick solvent rinse of them since we have no oven.
We had a problem with PRC mix on the GC, mainly with dibutylchlorendate. After some discussion with Jeff Jenkins we think it may be degrading in the inlet. We are seeing consistently two peaks even when we shoot dibutylchlorendate singly. This second peak does not show up in any of our solvent or air injections. I have a few things to try tomorrow to get to heart of this problem.
The retrieval has to be pushed back to Wednesday/Thursday. 32 complete cages have arrived and are in need of cleaning due to all the oil more than likely used in their manufacture. 3 spiders however were made way too small and had to be retrofitted....which the blacksmith did today and we received them shortly before the end of the day. Today we cleaned/scrubbed the cages with Alconox and tap water. Tomorrow we will do the same for the spiders but also we'll do a quick solvent rinse of them since we have no oven.
We had a problem with PRC mix on the GC, mainly with dibutylchlorendate. After some discussion with Jeff Jenkins we think it may be degrading in the inlet. We are seeing consistently two peaks even when we shoot dibutylchlorendate singly. This second peak does not show up in any of our solvent or air injections. I have a few things to try tomorrow to get to heart of this problem.
Friday, February 6, 2009
Week 2 - Friday and Saturday
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.
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.
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.
Friday, January 30, 2009
TGIF
Today we were met with many new challenges. The goal was to re-plumb the GC helium and nitrogen gas lines and insert working traps. Before this could happen we notice the pressure regulator on the helium was not functioning correctly and leaked. I removed it and took it apart. The regulator was very corroded (rusted shut) on the inside. I pieced together and cleaned another regulator from old ones and it seems to be working properly and hold pressure well. We relocated the helium tank, which was previously kept outside, into the lab. I am positive this is why the regulator was functioning so poorly (sea air). We were successful in re-plumbing both gas systems and the nitrogen generator seems to being working well at the moment. I hope that next Monday i can bring the GC online and start trouble shooting potential contamination issues.
1/29/2009
Today was another day of GC maintenance. We put the inlets back together, trimmed and re-installed the columns. Also we got the balance in working order and verified a few pipets. The pipets we found a few days earlier are in great condition (never been used) and seem to be very accurate. I saw the stock room today with Adama's help and we found several more pipets. The volumes for each pipet are 2-20ul, 100-1000ul, and 1000-5000ul. We only have tips for the 2-20 and 100-1000 and the tips do fit just fine. Below you will see picture of the previously posted cages that should be done on monday. As you can see they are a bit smaller than the standard cages from EST. 1/30/09 we should be re-blumbing the gas lines and practice making some LFT
Wednesday, January 28, 2009
1/28/09
I was able to view the cages and the building operation. There are 32 caged being built. They do appear to be smaller in diameter (maybe 7-8 inches vs the EST cages ? inches). They all need more finishing and welding. The spiders were being made while we were there. The spiders also seems a bit small. I will post pictures later.
We did inlet maintenance on the GC today. The gold seals were both fairly dirty and the inserts were very dirty. We attempted to clean the gold seals them with some success, but we won't really know until we reconnect the columns and put the inlets back together. It would be best to order two new gold seals I believe.
There is another nitrogen generator that we will use that has much less time on the filter and had an electrician connect it to the power conditioner to keep it running when power is poor.
I met with Hama and Baba today to discuss the project and the discrepancies with the inventory survey I did yesterday.
Tomorrow, I hope to put the inlets back together on the GC and re-install the columns. Also we should be re-plumb some of the gas tubing and insert traps for the N2 and He gases. After that we should have a better idea of contamination on the GC and the condition of the columns and/or detectors.
We did inlet maintenance on the GC today. The gold seals were both fairly dirty and the inserts were very dirty. We attempted to clean the gold seals them with some success, but we won't really know until we reconnect the columns and put the inlets back together. It would be best to order two new gold seals I believe.
There is another nitrogen generator that we will use that has much less time on the filter and had an electrician connect it to the power conditioner to keep it running when power is poor.
I met with Hama and Baba today to discuss the project and the discrepancies with the inventory survey I did yesterday.
Tomorrow, I hope to put the inlets back together on the GC and re-install the columns. Also we should be re-plumb some of the gas tubing and insert traps for the N2 and He gases. After that we should have a better idea of contamination on the GC and the condition of the columns and/or detectors.
Tuesday, January 27, 2009
1st day 1/27/09 overview
The focus for the day was to start GC troubleshooting and maintenance and to do an inventory of supplies that had been previously shipped to the lab in the summer of 2008. It was brought to my attention that the front column or DB-17ms was broken. at first glance it appeared to be broken in half, but I later found that only a 1-m section from the end was broken...so that is great news. We quickly took apart the GC inlet and it was found to be fairly dirty, especially the gold seals. The GC should have high purity helium for the inlet and nitrogen for the make-up gas, but both were plumbed with the He line. We fixed this problem but will not install new gas traps until we are ready to make GC runs. The outlet for the gases was venting into the lab onto the lab bench. It was discussed how to fix this and run tubing to the outside for contaminantion and health reasons.
The nitrogen generator used for nitrogen in the lab is showing a red light indicating nearest as I can tell (no manual) that the filter is bad. The members indicated that it has never been changed. I recommend we make changing the filter a priority. Without it we can't do reliable chromatography.
There is one full tank of class 2 helium.
During inventory the 2 Rainin pipets that were shipped over in the summer of 2008 were missing, but we did find 3 pipets that may work just as well. We will test them on tomorrow. Most of the glassware was present, but some beakers and flasks were missing. It became apperant that the if volumetric flasks are to be used to make standards then ground glass stoppers are needed as they very few.
I indicated to Adama that I need to see the deployment cages for the LFT asap since they are not in the lab yet....to be finished by saturday was what I was told. I hope to view them tomorrow.
Tomorrow we will be doing mostly GC maintenance and pipet verification. I will try to post tomorrow if I have internet.
The nitrogen generator used for nitrogen in the lab is showing a red light indicating nearest as I can tell (no manual) that the filter is bad. The members indicated that it has never been changed. I recommend we make changing the filter a priority. Without it we can't do reliable chromatography.
There is one full tank of class 2 helium.
During inventory the 2 Rainin pipets that were shipped over in the summer of 2008 were missing, but we did find 3 pipets that may work just as well. We will test them on tomorrow. Most of the glassware was present, but some beakers and flasks were missing. It became apperant that the if volumetric flasks are to be used to make standards then ground glass stoppers are needed as they very few.
I indicated to Adama that I need to see the deployment cages for the LFT asap since they are not in the lab yet....to be finished by saturday was what I was told. I hope to view them tomorrow.
Tomorrow we will be doing mostly GC maintenance and pipet verification. I will try to post tomorrow if I have internet.
Saturday, January 24, 2009
General timeline of 2009 training
Week 1
Orientation, introductions, performance evaluations, GC training and trouble shooting
Week 2
Standards, Passive sampling device (PSD) construction, field deployment
Week 3
PSD processing and training, GC training, review and data analysis of practice PSD samples, calculation spreadsheet
Week 4
1st field retrieval and processing of samples, GC run of 1st retrieval
Week 5
2nd field retrieval and processing of samples, GC run of 2nd retrieval
Week 6
GC training, performance evaluations, discuss method validation packet, follow up on inadequate training indicated by performance evaluations
Orientation, introductions, performance evaluations, GC training and trouble shooting
Week 2
Standards, Passive sampling device (PSD) construction, field deployment
Week 3
PSD processing and training, GC training, review and data analysis of practice PSD samples, calculation spreadsheet
Week 4
1st field retrieval and processing of samples, GC run of 1st retrieval
Week 5
2nd field retrieval and processing of samples, GC run of 2nd retrieval
Week 6
GC training, performance evaluations, discuss method validation packet, follow up on inadequate training indicated by performance evaluations