Today was the last day at the lab. I spent the morning updated the LIMS spreadsheet with the new callibration table and fixing a few misdirected links.
The spreadsheet is now back up to 100% and Anna went through several samples entering data and saving the sheets for subsequent upload to the VM machine.
I went through the other materials (computer files) I brought for the lab to use showing her what some of the folders contained. The rest of the time was spent working briefly with the Agilent 5973 helping Anna set up a simple method for a couple of pyrethroids.
Since tomorrow (Wednesday 31Aug11) is a holiday here there is no option for any additional work. All details of the data processing and machine QC have been covered and all is progressing well. By early next week all the samples should be run and then it will just be a matter of data processing.
Tuesday, August 30, 2011
Monday, August 29, 2011
Running Again - 29Aug11
All back in operation today. The CCV passed and blanks were blank. ALL of the samples were diluted by a factor of 10 today and the appropriate amount of Internal Standard added.
The first batch of the diluted samples are running now, and we'll look at data tomorrow.
The LIMS testing went poorly. The connection was so slow that LIMS quit responding and finally the connection was lost. We were unable to reconnect so we are going to try again tomorrow. So I switched to the data processing spreadsheet and went over how it is used to feed information into LIMS. Tmorrow I will have Anna process some data and send it to the VM via the drop box app.
TAH
The first batch of the diluted samples are running now, and we'll look at data tomorrow.
The LIMS testing went poorly. The connection was so slow that LIMS quit responding and finally the connection was lost. We were unable to reconnect so we are going to try again tomorrow. So I switched to the data processing spreadsheet and went over how it is used to feed information into LIMS. Tmorrow I will have Anna process some data and send it to the VM via the drop box app.
TAH
Sunday, August 28, 2011
All Samples ready for GC Analysis - 28Aug11
Today was spent briefly in the lab preparing the last group of samples for GC analysis. All from this current batch have now been extracted and prepared for GC analysis.
The first group has been run and the samples that require dilution have been identified. The GC was dirty after this first group and the injector liners and septa were changed today. The GC was left injecting several runs of hexane to clean out any residual contamination. The GC detectors and liners were left set above the normal run method limits to bake off anything else that was missed. A CCV will be run in the morning.
Monday's plans are to work on LIMS and address any questions about data processing. This is also pretty much the agenda for the rest of the week as well as help with any sample processing.
Today was an interesting day at the lab. One of the staff brought a Chameleon to the lab, and he had caught it somewhere in the back forty of the lab site (see Picture du jour).
Picture du Jour:
Friday, August 26, 2011
Sampling the samples - 26Aug2011
Today was spent running samples. So far all is going well. Several of the final samples will need to be diluted and re-run, but all of the machine QC, blanks and CCV (Continuing Calibration Verification), passed with no problems.
The GC did have a faux pas today. The front injector needle took a turn for the worse and decided to commit ritual suicide. It just curled itself up into a nice ball and of course all requisite GC errors ensued. Thank goodness a couple of extra syringes were sent with the standards, so after a few moments of silence to honor the fallen syringe, it was replaced and the system back up and running.
This afternoon was spent getting the "dropbox" software installed on Anna's computer and on the Ceres VM login. This was done and all is working tres magnifique.
All is on schedule and progressing well.
Au revoir et bonsoir.
TAH
The GC did have a faux pas today. The front injector needle took a turn for the worse and decided to commit ritual suicide. It just curled itself up into a nice ball and of course all requisite GC errors ensued. Thank goodness a couple of extra syringes were sent with the standards, so after a few moments of silence to honor the fallen syringe, it was replaced and the system back up and running.
This afternoon was spent getting the "dropbox" software installed on Anna's computer and on the Ceres VM login. This was done and all is working tres magnifique.
All is on schedule and progressing well.
Au revoir et bonsoir.
TAH
Thursday, August 25, 2011
25Aug2011
All is progressing well with the GC-ECD method. The method is adding a calibration for PCB-180 and samples are being checked for contamination from the roto-vap systems.
The roto-vaps have been cleaned and are now being used to reduce samples in preparation for GC-ECD analysis.
I have updated the spreadsheet with the local calibration settings, e.g. updated retention times, cal table, etc.
I am installing the software to allow computers to cache documents and syncronize files as there is a latency problem ttrying to send files to the virtual machine. This will minimize some of the LIMS training, but plans are to cover input of samples, and batch preparation, so when files are synchronized they can just be linked to the appropriate batch.
There has been some minor consternation over my leaving on September 1st but I'm not too sure what an additional day or two would accomplish. I have tried to put to rest any concerns but showing them all is going well so far. I think from talking with several folks here that training is the biggest issue, and the lab personnel just need to have someone come over solely to train. Training in the use of the all the features in chemstation, using Excel to analyze data, LIMS, and all other associated computer related items, e.g. data management, archiving, etc. is warranted. The lab personnel have a good basic skill set but some of the items outlined above seem to cause them a bit of concern.
A french language version of LIMS is highly recommended for the CERES lab on the VM. Most here can speak a bit of english, but for routine use french is the preferred language. This issue has been voiced several times and should be one of the first issues addressed. LIMS being in english is a big concern for several of the lab staff and I see LIMS tasks being pushed off to the best english reader/speaker.
TAH
The roto-vaps have been cleaned and are now being used to reduce samples in preparation for GC-ECD analysis.
I have updated the spreadsheet with the local calibration settings, e.g. updated retention times, cal table, etc.
I am installing the software to allow computers to cache documents and syncronize files as there is a latency problem ttrying to send files to the virtual machine. This will minimize some of the LIMS training, but plans are to cover input of samples, and batch preparation, so when files are synchronized they can just be linked to the appropriate batch.
There has been some minor consternation over my leaving on September 1st but I'm not too sure what an additional day or two would accomplish. I have tried to put to rest any concerns but showing them all is going well so far. I think from talking with several folks here that training is the biggest issue, and the lab personnel just need to have someone come over solely to train. Training in the use of the all the features in chemstation, using Excel to analyze data, LIMS, and all other associated computer related items, e.g. data management, archiving, etc. is warranted. The lab personnel have a good basic skill set but some of the items outlined above seem to cause them a bit of concern.
A french language version of LIMS is highly recommended for the CERES lab on the VM. Most here can speak a bit of english, but for routine use french is the preferred language. This issue has been voiced several times and should be one of the first issues addressed. LIMS being in english is a big concern for several of the lab staff and I see LIMS tasks being pushed off to the best english reader/speaker.
TAH
Wednesday, August 24, 2011
Calibration Success - 24August2011
The calibration of the GC-ECD went well. All the target compounds worked and only a few individual targets were needed to be run to verify peaks. The method is up and running and calibrated ready for samples.
I put together a quick start guide on how to access the VM, settings that need to be addressed in the remote desktop manager, what items to open to get to various programs, and all with a few associated screen shots. I will give this to the CERES folks as there was quite a bit of anxiety over using LIMS.
A test of the VM was attempted by myself and my computer to determine what kind of data transfer rate was going to be possible. The VM access went without problem, but as soon as it was put to the test of copying data from Senegal to OSU it suffered greatly but kept trying even though the connection was dropped several times. The computers kept reconnecting and files crept toward OSU ever so slowly. It took well over an hour to copy a couple of data files that in a local copy from a USB stick to my computer took seconds. The CERES lab has wireless connectivity, but a bandwidth test to any internet sites was very slow. A drop box solution has been proposed, files are placed in local folder and syncronized as time permits. This will be tested to see if it is a viable option. Further testing of the VM with LIMS will proceed to see what kind of results that produces.
Photo du jour - arbre de pamplemousse <--See I'm learning some French!
Tuesday, August 23, 2011
Testing testing testing.... 23Aug2011
Today the calibration set is running. The rotovap systems are now clean. I showed the others how to clean the system and now they are consistently getting much cleaner aliquots from the rotovap systems. It appears that the rotovaps are used for a lot of work and need a sodium hydroxide cleaning to remove most of the residue built up from all the other testing. After finding a bottle of NaOH pellets I went through safe handling and cleaning using a 1M solution. This removed the ever present background in the samples. The procedure I outlined for them was to use about 100mL of 1M NaOH in the flask, swirl it about every 10-15 minutes, and let it sit for about 1 hour. Then rinse the flask at least 3 times with DI water testing for neutral pH at the end, then rinse with solvent.
The access to LIMS was established today, but by the time I got the cal series running and the test samples run (checking the rotovaps, see above) we were out of time to do any work with the connection. It does appear that there is adequate speed to be able to perform analysis on the CERES-ANALYST system. I will see how long it takes to send a few files that direction tomorrow.
Here is the picture du jour:
The access to LIMS was established today, but by the time I got the cal series running and the test samples run (checking the rotovaps, see above) we were out of time to do any work with the connection. It does appear that there is adequate speed to be able to perform analysis on the CERES-ANALYST system. I will see how long it takes to send a few files that direction tomorrow.
Here is the picture du jour:
Banana plant growing behind the lab
Monday, August 22, 2011
Pictures above are a few shots of the labs and front gate.
The box of standards arrived today and there was no physical damage to any of the contents. The samples were warm as the freezer pack had thawed. All of the samples were placed in the freezer for analysis to begin tomorrow.
Today was spent seeing if the background noise on the ECD detectors could be lowered. I tried raising the temperature to 350 degrees centigrade but no luck. The detectors seem to be running right on the upper limit of being useful and no additional baking seems to make any difference. The ECD cells are probably getting toward the end of their lifespan in this environment. I would expect that they will perform adequately for at least another year or two before needing to be replaced. The power system here has many brown-outs during the day and I would guess that these power dips and spikes have hastened the demise of these detectors.
The rest of the day was spent assisting Anna and her group getting another rotovap operational. The effluent from this rotovap and the others in the lab were being tested for contamination via the GC-ECD. So this and running the samples occupied a good portion of the day.
The newest version of the LIMS spreadsheet was provided to the lab and this along with calibrating the method will begin tomorrow.
A note on the internet service here; The service is very slow and prone to frequent loss of service. There appears to be wireless service almost every where I turn on my computer. Expect fairly basic service and slow access to anything out of the immediate area.
Today was spent seeing if the background noise on the ECD detectors could be lowered. I tried raising the temperature to 350 degrees centigrade but no luck. The detectors seem to be running right on the upper limit of being useful and no additional baking seems to make any difference. The ECD cells are probably getting toward the end of their lifespan in this environment. I would expect that they will perform adequately for at least another year or two before needing to be replaced. The power system here has many brown-outs during the day and I would guess that these power dips and spikes have hastened the demise of these detectors.
The rest of the day was spent assisting Anna and her group getting another rotovap operational. The effluent from this rotovap and the others in the lab were being tested for contamination via the GC-ECD. So this and running the samples occupied a good portion of the day.
The newest version of the LIMS spreadsheet was provided to the lab and this along with calibrating the method will begin tomorrow.
A note on the internet service here; The service is very slow and prone to frequent loss of service. There appears to be wireless service almost every where I turn on my computer. Expect fairly basic service and slow access to anything out of the immediate area.
Monday August 22, 2011
The box of standards arrived today and all looked to be in good shape physically. The ice pack had thawed and the samples were warm. All were put in the freezer for storage, and we will begin analysis tomorrow.
Today was spent checking the ECD signals in the morning, and working with Anna and her group to get an additional rotovap up and running. The ECD signals were still running a bit high but in the range where they should perform with no problem. I tried raising the temperature on both detectors to 350
Today was spent checking the ECD signals in the morning, and working with Anna and her group to get an additional rotovap up and running. The ECD signals were still running a bit high but in the range where they should perform with no problem. I tried raising the temperature on both detectors to 350
Friday, August 19, 2011
19August2011 - In the Lab
Today the GC-ECD was tested and appears to be working well. The detectors are running a bit high so a bake out is in progress for the weekend. The bake-out will degrade and volatilize any residual coatings on/in the detector thus lowering the background signal. The detectors were baked briefly yesterday and the background signal did significantly come down. The current background for both ECD detectors is currently around 750, optimally a value below 500 is desired, so I'll see what a longer bake out does. The original background before any work began had the front at about 2500 and the rear about 1200, so both were dirty.
The GC-ECD was tested with hexane samples today and it does not appear that there is any residual contamination. Samples taken from the roto-vaps to check for contamination did confirm that these were initially contaminated. A subsequent washing of the systems removed the contamination, and all was happy again in the lab.
Anna and her crew worked on finishing the LFT extractions. These extractions are progressing well and all are doing a good job following procedures. I have not seen any problems to note so far with the extractions.
Once the box of supplies from OSU shows we can begin final preparation of the samples and the method calibration.
So far all is progressing as expected.
Reporting from Senegal, Good night and Good Luck. TAH
The GC-ECD was tested with hexane samples today and it does not appear that there is any residual contamination. Samples taken from the roto-vaps to check for contamination did confirm that these were initially contaminated. A subsequent washing of the systems removed the contamination, and all was happy again in the lab.
Anna and her crew worked on finishing the LFT extractions. These extractions are progressing well and all are doing a good job following procedures. I have not seen any problems to note so far with the extractions.
Once the box of supplies from OSU shows we can begin final preparation of the samples and the method calibration.
So far all is progressing as expected.
Reporting from Senegal, Good night and Good Luck. TAH
Thursday, August 18, 2011
Week 1 Day 1 - The Beginning
Today was the first day at the CERES lab.
Items accomplished and discussed.
1. New columns installed on the GC-ECD system, and the new method put on the system.
2. New injector liners installed (and septa also)
3. Detectors reading very high so a bake out was warranted, system is currently baking the detectors. The detectors responses were still coming down, so it was decided to let them bake overnight.
4. MS-Office was installed on the GC-ECD so the spreadsheets and Word documents could be opened and manipulated.
5. The new bench sheets are being used, as Anna and company began LFT extractions (see pics plus several general lab shots included for free).
6. Anna and I discussed the other files and documents and we will cover the new SOP and calculations in more detail in the coming days.
7. An exploration of the internet connection finds it to be present but very slow. A test of the connection to the OSU server will be attempted in the next working day or two to see if the CERES lab can get into LIMS.