Last post

This blog is no longer active. It will remain up until the training report (of which the blog is a draft) is completed. This is estimated to be Friday, November 2, 2007

Please send comments or suggestions to Greg Sower at sowerg@onid.orst.edu.

Thanks to everyone who participated for their help on this project.

Last day

The GC autosampler misaligned a wash vial and destroyed the syringe on the front injector. The reagent blank, lab spike, trip and field blanks completed, but no samples were injected.

Take a slow . . . deep . . . breath.

The power failed early last night and the GC crashed before finishing the standards, let alone the samples. We will get the GC up and load the generator with fuel to run the GC overnight.

In an effort to provide the staff with a cursory exposure to PSD data analysis, I presented the spreadsheets used for calculating water concentration. The basic spreadsheet is derived from reference material given to CERES during their 2006 training. We discussed the how previous research by others had established the equations, how the variables affected the results and how the GC data is incorporated into a much larger spreadsheet to calculate for multiple analytes at multiple sites and exposures durations.

Additionally, I demonstrated the proper technique for preparing raw LFT for PSD construction. This small detail is critical to proper PSD development and can significantly affect the GC results.

Cheikh, Makhfousse, and I met with Baba and discussed point by point the Issues and Recommendations section of this report.

Pending electrical repairs

An electrician evaluated the power issue and surmised that there are two big problems: The batteries in the UPS are dead (probably because the incoming power signal is insufficient to charge them) and the incoming service cables are inadequate and should be replaced. A permanent solution and invoice are pending.

Retrieval 3 samples are in vials and running on the GC overnight. There is not enough fuel for the generator to run all night (which is what we did previously to guarantee operation) so hopefully the incoming power is sufficient.

More progress

Adama and Marie built a new set of standards because the results from the first set were unsatisfactory. Anna and Sokhna trained Emmanuel on PSD cleaning using the samples from field retrieval 3 and also finished cleaning the glassware. The PSD extraction was completed and substantial improvements were made in bench organization, cleanup and bench sheet use. Cheikh restructured the bench sheets to reflect the SAM modifications and as a result are much more organized.

Wednesday the 24^th is blowdown, vial up, and GC prep.

Home stretch

We started the week by sequestering all the CERES/OSU samples from retrieval 2 and prepping for extraction of retrieval 3 PSDs. RBFs were collected and cleaned with boiling hexanes in a Soxhlet setup (80% RBF volume of hexanes boiled for 30 minutes, two times). We cleared the work area of all material and wiped the countertop with acetone. The inlets on the GC were changed. The back inlet had extensive septum material on it. The injector tower on the back inlet was borrowed from the lab’s GC-MS unit. The syringe may not be in good shape compared to that of the new tower on the front.

Cheikh also worked on building the calibration curve for the GC based on the standards that had been run Oct 4^th.

Week in Review 5

We started the week with a setback due to contamination. While the cause was determined to be inadequately cleaned laboratory glassware, the incident revealed issues that need to be addressed. CERES will need to upgrade or obtain certain equipment (e.g. countertops, an oven, and perhaps a lab water purification system) as well as develop staff lab skills for the increased analytical requirements of the project. However, temporary fixes will likely allow for continued training on the retrieved PSDs in week 6. An extraction will be attempted on the third set of PSDs and the OSU/CERES split samples will be stored until demonstration of successful extraction and analysis can be completed.

FAO accompanied the CERES team on the final field retrieval at Pont Gendarme. Sokhna, Marie, and Anna trained Emmanuel in proper PSD retrieval which demonstrates their competence and comfort in the procedure. All equipment was retrieved from the Pont Gendarme sites.

We were delayed getting back to the Dakar lab, but expect to begin the PSD extraction on Monday the 22^nd by carefully preparing glassware and paperwork and cleaning the PSD.

I provided Cheikh with the Training Evaluations and Informed Consent forms that OSU developed for collecting the CERES staff’s perceptions of this training so he could translate them into French. He will retain them until OSU IRB clearance has been obtained.

Field Retrieval 3

CERES completed Field Retrieval 3 without a problem. CERES staff in attendance included Adama, Marie, Anna, Sokhna, Makhfousse, Cheikh, and Emmanuel. Emmanuel had been occupied with another project so hadn’t been able to join us previously; but now every CERES lab member has experienced field training with PSDs.

CERES staff appear very comfortable and capable working with the PSD in the field. Their retrievals are coordinated, cooperative and efficient. This was the strongest aspect by far of the training.

We observed the same fouling pattern as before: Site 1 the worst, and Site 3 the best with 4 and 2 very similar. This gives no indication of contaminant load, but may be useful in the context of additional information such as pH, total dissolved or solids or salinity. It does demonstrate, however, that performance/permeability reference compounds (PRCs) will be important for maintaining accurate and comparable data.

We also observed the same activities as before: washing clothes and dishes, bathing, fishing, household water collection and watering livestock.

We leave for Dakar Friday morning and will head directly to the lab to clean the PSD and clean glassware (likely with hot solvent) to begin the dialysis on Monday. We hope to have retrieval 3 data by the end of the training on October 26^th.

The Source of the Contamination

We have been analyzing various samples to determine the source of the contamination. It appears that the source is indeed dirty glassware. The round bottom flasks used in the dialysis appear to be the most significant contributor to the contamination.

The glassware sample is blue, while the blank is red.
The peaks on the glassware sample represent compounds
not removed during the cleaning procedure.
Other issues are present and noted.

After stepping through SOP 2110.03 entitled Laboratory Glassware Cleaning, some issues with CERES equipment became clear. The SOP requires baking the glassware at 400 °C, however, the CERES oven can only achieve 100 °C. Also, where rinses with 18 Mohm·cm water are required, CERES only has access to basic distilled water. The flasks are more difficult to clean than other glassware due to the narrow mouth and high relative volume, making these cleaning steps all the more important. However, all lab glassware is now suspect.

The GC-ECD combined with helium as a carrier gas provides levels of detection approximately two orders of magnitude greater than CERES could previously obtain. The levels of contamination were such that they would likely have been hidden in the higher former baseline. CERES’s increased analytical capabilities have exposed new issues, but the steps necessary to fix the situation should not be difficult. An oven capable of 400 °C will need to be obtained. This should not be prohibitively expensive and CERES has the counter space next to the other ovens. This oven should not be used for any purpose other than cleaning lab equipment.

As a result of this incident, the CERES/OSU split will not be immediately processed. An attempt will be made to clean glassware by different, solvent intensive, method and the PSD from Retrieval 3 will be extracted and analyzed.

To put this incident in perspective, brief commentary is necessary. CERES has quality equipment and staff, and the potential to deliver the required results. The increased analytical requirements of this project (and, inevitably, most if not all future work for pesticide analysis not related to this project) have pushed the limits of other points in the chain of analysis. Parts per million levels (CERES previous capabilities) will not suffice and the move to parts per billion capabilities exposed the weak spots that should be addressed.

Minor pieces of equipment are needed to increase performance. A hotter oven will help significantly, but one of the laboratory hoods should have the countertop covered in either high-grade (e.g. 316) stainless steel or replaceable Teflon paper with adhesive backing. The grout on the existing tile countertops is a high risk for harboring contamination. Additionally, high purity water (HPLC grade) would also help.

On another note, Bill and Hama will be joining us on the 3rd and final retrieval at Pont Gendarme today through Friday.

Contaminated Extracts

We viewed the chromatograms before performing the PSD cleaning and found severe contamination in the last extraction. The hexane blank that had been removed from the reagent bottle and placed on the GC was clean. However, the reagent blank that had been through the PSD method (dialysis, blow down, transfers, etc.) was very contaminated. A chromatographic comparison between the reagent blank and the lab spike (which also went through the method) is shown below (lab spike consists of 200 uL of a 1ppm dilution of Chemservice organochlorine pesticides mixture #1 – 508 in MTBE, cat # OCP508-1JM spiked into 100 mL hexanes, then extracted by the PSD method). Note that retention times, compound labels, and baselines have been removed for clarity.

A discussion with the CERES staff resulted in a careful evaluation of the entire extraction process. As this contamination occurred in the reagent blank, it could not be from the field extraction and therefore must have occurred during the dialysis, blow down, or transfer.

Today we are extracting a new reagent blank, a blank LFT, and the acetone from the wash bottle (used to clean the Rotavap-RBF joint between samples). Dirty glassware is suspected, however, several measures are being taken to rectify the situation. All glassware for the CERES/OSU split extraction is being cleaned again. The split extraction will not proceed until the situation is satisfactorily remedied.

In contrast, the standards appear much better. Below is an example.

Retrieval 2

Oct 8th

The electricity failed soon after the GC run was initiated (and we had left) on Friday afternoon. As described to me by Cheikh, the incoming grid electricity is of poor condition and the UPS uses battery power to compensate thus draining the UPS batteries. When the batteries are drained the grid power is insufficient to maintain the equipment and the UPS shuts down. The backup generator does not turn on because it still recognizes the grid power input regardless of quality.

Therefore, we have no data from last week’s extraction.

We are attempting to run the GC entirely off the backup generator while we are in Saint Louis in hopes that the clean signal from the generator will allow the GC to complete its run.

I am of the opinion that CERES needs a power conditioning unit to prevent abuse of the UPS and maintain instrument operation. Or a replacement UPS that is capable of better power conditioning.

Seraphim Dorego joined us to perform GIS work at the site then we left for St. Louis about 2:30 pm.

Oct 9^th

We arrived at Site 1 at about 8:15 and proceeded to retrieve two sets of PSDs, one set for CERES extraction and analysis and one set for OSU extraction and analysis. CERES staff in attendance were: Cheikh, Makhfousse, Anna, Marie, Adama, Sokhna, Madame Ndaiye. Abdoulaye Djiop again assisted with retrieval. CERES staff performed all work with minimal oversight and field bench sheets were competed in detail.

When we approached Site 1 we found the cages were lying horizontally on the bottom of the concrete canal. The PSD had significant fouling, but some may be rust from the non-stainless steel portions of the cages.

An interesting observation of the PSD is the increasing amount of fouling with increasing distance from the river. Site 3 cages are positioned in the Goron-Lamspar tributary and are very clean after two weeks, Site 2 in the main irrigation canal shows some fouling, while Site 1 at the drainage pump station shows the most severe fouling. It is not clear, however, if the fouling is rust, sediment, or biological.

From left to right: Site 3 in the river, Site 2 in the irrigation canal,

and Site 1 at the drainage pumping station.

In addition to the four PSD sites, we visited the drainage area south of the pumping station to allow Seraphim to collect GIS data. We observed livestock drinking at this site.

We observed bathing, washing of utensils and household water collection, as well as fishing at Site 1, and household water collection at Sites 2 and 3.

October 10^th

We left St. Louis too late to get back to Dakar early enough to perform the PSD cleaning, but we received word that the GC had successfully run all the loaded samples.

Week in Review 3

The third week is the halfway point for the PSD training. The first field retrieval went well, though there were issues with cage positioning and air exposure. Modifications were made and the remaining cages successfully redeployed.

We recognized that the bench sheets should be in French as well as English, not necessarily one or the other, but bilingual would be best. Locustox staff are working on this. Also, we are working on collecting more information in the bench sheets.

After retrieval Locustox extracted the PSD and prepared the field and quality control samples for GC analysis (9 samples total). The lab equipment was well suited to the procedure, though a TurboVap LV is preferable for high sample throughput (greater than 10 - 15 samples at a time).

The GC successfully ran the OC pesticide standards (using OSU's OCPQUANT.M method), though neither a calibration curve nor data analysis was completed. The GC was loaded with the extracts to run over the weekend. We attempted to perform the analysis in a manner consistent with OSU's approach to facilitate future data comparisons.

Next week we will again travel to Saint Louis for the second of three retrievals. This next retrieval is particularly important as two sets of PSDs will be collected with one going back to OSU for analysis and comparison with Locustox's analysis.

We are a couple days behind on lab work, but as this is the first such training attempt we will use it to frame future training schedules.

Field retrieval 1 extractions

Oct. 4^th 2007

The sample extractions were started first thing in the morning (~8:00 am). Adama and Anna added 100 mL of hexanes to the samples and prepared a reagent blank and lab OC pesticide spike. The OCP spike consisted of 200uL of a 1,000 ppb concentration standard prepared from the Chemservice OC pesticide standard OSU provided. Adama, Marie, Anna, and Sokhna worked on the second dialysis.

Dialysis of retrieved PSDs.

Cheikh ran the standards on the GC using the OSU methods. Results should be available Friday.

A review of the field bench sheets revealed substantial deviations, mostly in the form of unrecorded data. I discussed this with Cheikh and we will work with the staff on the next retrieval to increase completion.

Oct. 5^th 2007

The standards finished without incident on the GC but there was not time for anything but a cursory review of the runs. Background was low, many of the 5 ppb peaks were identified, but specifics will not be available until Monday at the earliest, possibly Wednesday due to the field work at Saint Louis.

Today Locustox performed the sample blow down on Rotavaps and the Techne Dri-block. In attendance: Adama, Marie, Sokhna and Cheikh.

Adama performing the the initial sample blow down with a Rotavap.

Transfer from round bottom flask to smaller tube.

One sample, the trip blank, became contaminated with water on the Rotavap blow down. We used it as an example on how to remove water from a sample and where to keep accurate notes on the bench sheet.

After the extraction the samples were loaded onto the GC with the standards for analysis over the weekend.

Pont Gendarme field sites map

This is a modification to an existing slide. The field sampling sites are represented by the white circles with red outline. We have had poor luck with our GPS receiver, so coordinates are pending.

PSD cleanup

We performed the field cleanup steps for the samples collected yesterday. For the UN-GEF project, this cleanup is performed in the lab, not in the field. The following Locustox staff were in attendance: Cheikh, Adama, Anna, and Marie.

I demonstrated the proper PSD cleanup procedure using the field and trip blanks from yesterday’s retrieval. Note that these blanks do not normally get this cleanup, but this was for demonstration purposes. The staff then completed the remaining sample cleanup including an extraction blank. These samples will be extracted tomorrow.

The OSU field benchsheets have a location to record the manufacturer and lot numbers of the cleanup reagents. I neglected to move this information from the field to the extraction benchsheet and as a result it was not recorded. I will rectify the problem when Cheikh and I review the benchsheets.

The PSD dialysis portion of the extraction needs to be completed in a single day; therefore, the extraction will not begin until Thursday morning. The entire extraction should be complete by Friday afternoon.

The prep blank, lab spike, and field and trip blanks from the deployment will not be extracted this round. This first extraction will familiarize the staff with the procedures. As the mentioned samples are valuable and irreplaceable quality control, they will be part of the second extraction to take place after retrieval of the Locustox/OSU duplicates next week.

One thing has become clear: It would be preferable to have the SOPs and SAMs translated into French. This is something that is important not just to Locustox, but to future partner labs.

Also, a number of the details are lab specific, which is to be expected for a SOP, but they need to be modified for Locustox and the UN-GEF project in general (such as the cleanup reagents info). I can help consult on the specifics and Cheikh could translate but we are limited on time; therefore, we are assigning the staff the documents to translate. This should help familiarize them with the procedures and benchsheets.

After the translation we will review the documents and make necessary changes. All the translated documents will be emailed to OSU for further review and backup.

Field retrieval 1

The first retrieval at Pont Gendarme went well, though there were some unexpected issues with the cage positioning. In attendance for the retrieval training were Adama, Marie, Anna, Sokhna, Cheikh and Makhfousse. Abdoulaye Djiop again joined us and helped significantly during retrieval.

We left for Saint Louis Monday, the 1^st in the afternoon and arrived that evening. We left the hotel at about 7 am (first light) and headed to the field site.

At the first site, the main drainage pumping station, we found the cages exposed to air (about 15 cm above the water line). The water level had been lowered to facilitate fishing, which was ongoing when we arrived (the fishermen declined to allow photos). Exposure to air prevents water sampling and, in fact, allows for air sampling; neither condition is suitable for this project.

The PSD cages as we found them at the first site.

Also, a cage had clearly been tampered with, the shell removed and the retention nuts missing. The shell had been dented, but the PSDs were still intact. We collected this cage for analysis.

The cage that had been tampered with lost it's shell on retrieval.


A rusted spring and accompanying discoloration on the PSD.


The dented shell.

The cages were repositioned lower in the water column.

The retention springs on the cages are not stainless steel and had rusted. These should be replaced with stainless springs.

Staff washed the two PSD in local water and packaged them in a clip-sealed Teflon bag according to the SOP. (Note: this project necessitates a deviation from the OSU SOP. The OSU SOP requires the local water rinse, then subsequent rinses in HCL, 18 Mohm/cm water, acetone, and finally isopropanol. For the UN-GEF project, the PSDs are washed in local water and then sealed in a Teflon bag. The rinses are performed at the laboratory. This modification is a logistical requirement and has been vetted by OSU/ Locustox work from the summer of 2006.) A trip blank accompanied our retrieval and a field blank remained exposed for the entire operation at this site.

At the second site, the main irrigation canal, the cages were again exposed, this time about 20cm above the water line. Staff retrieved, cleaned and stored the PSD without incident and according to the SOP. After retrieval, the cages were repositioned so they rested horizontally in the water column.

The cages as we found them at the second site.

Removing the PSDs for the local water wash (L to R: Anna, Marie, Sokhna).

Cheikh and Mr. Djiop helping to reposition the cages horizontally in the water column.

We discussed the possibility of manufacturing new shell retention nuts with an eye hook on them. This would allow easy horizontal deployment, prevent the nut from inadvertently unscrewing, and may help prevent tampering.

The PSDs at this site had about the same amount of fouling as those at the first site.

The third site is the main irrigation pumping station with the cages deployed in the Goron-Lampsor tributary. The cage and PSDs here were extremely clean; no signs of rusting or fouling. Additionally, the cages remained completely submerged. Staff retrieved, cleaned and stored the PSDs without incident in accordance with the SOP.

We again witnessed local household water collection and fishing in the area.

Retrieval of the cages and water quality data collection at site 3

(L to R: Anna, Adama, Mr. Djiop).

At the fourth site, the main drainage canal, the cages remained well positioned. Again, staff retrieved, cleaned and stored the PSDs without incident in accordance with the SOP.

Cage retrieval at site 4 (L to R: Marie, Sokhna, Mr. Djiop, Anna, Makhfousse).

After the final collection we returned to Dakar and deposited the samples at the laboratory that afternoon.

The staff have become comfortable with handling the PSDs and benchsheets. While I was initially disappointed that the first two sites’ cages were partially exposed, Makhfousse pointed out that the incident helps training. It also underscores the fact that these data should be limited to training purposes only.

The PSD extraction, GC analysis and data evaluation steps remain and we will accomplish as much as we can in the remainder of the week.

Week in Review 2

This week started with a great deal of progress, but several issues arose that slowed things down by the end.

The field deployment of the PSDs went very well. Most of the Locustox staff were able to participate, the weather was good, and the sites well suited to the training (see previous posts for details).

Numerous other engagements limited PSD work on Wednesday and Thursday. I fell ill on Thursday and was unable to work at the lab. The standards that were ordered for us by Amanda on September 18th finally arrived today (Friday) after some miscommunication with FEDEX. This more than anything limited the work we could perform as our next step is to run the standards on the GC with the modified method and helium.

We are prepared, however, for the first field retrieval this coming week.

Congratulations everyone

Thank you Greg, for this latest posting. A great help to able to see the locations and hear about deployment. The GPS data will be useful. I was pleased to hear that the pumps coped with the excessive rainfall.

We have started discussions about development of a project database that would provide a permanent archive that connects protocols and procedures with the data that are collected, locations sampled, photographs, GPS coordinates etc. Michael is going to help us with this, and we are going to send the blog address to him also.

Best wihes to everyone there,

Paul

Update check in

The field sites look great. It was nice to see that you all were able to get such nice individual locations. The cages also look wonderful, we should have them make us some....
Good to hear that He, hexanes, etc are arriving. However, has the standard arrived yet?
I am also impressed that someone successful made you (Greg) pose for a picture. On the pictures is it possible to let us know who is who? I am trying to match names to faces.
Excellent work all !

Kim Anderson

Field deployment

On Monday the 24^th we departed Dakar and traveled to the Pont Gendarme field site for PSD deployment. In attendance: Makhfousse Sarr, Cheikh Toure, Madame Ndaiye, Adama, Anna, Marie, Madame Ndao. When we arrived in the afternoon we inspected the field sites with Abdoulaye Djiop to ensure access and inform him of our research and intent.

After scouting the sites we returned to Saint Louis for the evening. In the morning we left at dawn and traveled to the field site which is currently under rice cultivation. We met Abdoulaye Djiop and proceeded to deploy the PSDs at each sampling site. Each site received 4 cages with 2 PSD in each cage. A trip blank was kept in the glove compartment of one of the trucks in a sealed (clipped) Teflon bag. Staff collected water depth and cage depth (taken at the middle of the cages) measurements at each site. Mr. Djiop assisted greatly in the deployment at all sites. He ventured into the water, positioned the cages and took the depth measurements. I took photos with a digital camera, but the GPS unit’s batteries were dead so no coordinates were taken. We will try again on the first retrieval.

The first site sampled was the main drainage pumping station south of the fields. A field blank remained exposed for the duration of the deployment at this site. I presented a brief demonstration of proper handling and mounting of the PSD and then the staff continued on their own for the remaining cages. The PSDs were deployed after the pumping station for several reasons. In front of the station there was considerable activity the evening before by local residents playing in and collecting the water. Behind the station the area was secured by a locked gate providing security from tampering. Even though the pumps churn the water considerably when they are on, there was not any sediment due to the basin’s concrete lining.

Click on photos for larger image.

Positioning cages behind the main drainage pumping station.
Adama (left) and Mr. Djiop (right)

I had received reports of flooding in the area. Mr.Djiop informed us that the drainage pumping station removed the excess water from the canals. I observed cattle grazing to the west of the station.

I believe this location might be a good site for a meteorological station as it can be secured behind the locked gate and positioned well off the ground. Cons included the location near the pump building and proximity to a moderately traveled road.

The second site deployed was the primary irrigation canal located between the irrigation pumping station and the drainage pumping station. We took care to discretely position the cages and anchors to minimize their exposure. We observed local residents collecting household water from the canal. The water at this location was much more turbid than at the drainage pump station.

Loading PSD into cages
Left to right: Adama, Mdm. Ndao


Positioning cages in main irrigation canal.
Front to back: Mr. Djiop, Adama

The third site deployed was the primary irrigation pumping station (north). A local resident was seen fishing in the area. Water clarity was better than at the previous location, but this area is not lined with concrete. We attempted to minimize sediment disruption during deployment.

Greg Sower

Local fisherman at the main irrigation pumping station.
Cheikh (fore), Makhfousse

Loading PSD into cages.
Mdm. Ndao (front), Marie (L), and Anna

The PSDs were located ~3-4 m northwest of the canal and near the shore of the tributary. This was done to prevent interference with the boats and fisherman that use the canal mouth. The area was difficult to properly position the cages due to the extensive sediment and shallow approach.

Preparing to deploy cages at the irrigation pumping station.
Adama and Mr. Djiop

The final sampling site was the main drainage canal to the west. As in all previous locations the PSD cages were suspended from a rope spanning the canal. The staff positioned the anchors just above the water line and covered them with debris.

Positioning cages at the main drainage canal.

A water pumping station was located near this site and I was informed that it provided water to the tower located in a nearby village.

The complete deployment took approximately 1.5 hours and afterwards the remaining equipment was secured and we traveled back to Dakar.

While in Saint Louis I made phone contact with Tim Krupnik and we agreed to try to meet on Monday, October 1^st during our field retrieval.

Week in Review

The accomplishments this week have been significant. The staff have substantially increased their LFT construction skills and are much improved over the initial attempts. Fortunately, they came into this with some familiarity and practice and good attention to detail. Staff constructed all the LFT required for the deployment and we are using aldrin as the PRC. Both Cheikh and Makhfousse agreed that aldrin should not be present at Pont Gendarme. The locally built cages should work perfectly.

Hama paid a visit and was updated on the project's progress. The necessary supplies, notably helium, but also hexanes, nitrogen and glassware, are on site. The staff were easy to work with despite my inability to grasp French, and appear enthusiastic about the project. They put in considerable time (and patience) this week and this is not the only project they are working on. Their efforts are appreciated.

In summary: The lab is prepared and we are well positioned to complete the remaining work as scheduled.

Continued field preparations

I know you are waiting for this: The helium arrived today. We will start Wednesday the 26th with lab PSD extractions and GC analysis thereof.

Field preparations continue, this time with paperwork and equipment. The benchsheets are modeled off OSU's with project specific modifications. Cheikh is preparing the necessary personnel paperwork and organizing the equipment (rope, cages, etc.). I recommended building an equipment checklist for future trips, but we will determine what exactly might be needed outside the usual after this one.

Pont Gendarme, the field site, is ~200 km away and will take 4 - 5 hours to get there. Once we arrive on Monday we will choose the specific sites, then head to Saint Louis for the night. In the morning, we will deploy the PSDs and head back to Locustox. Since each site will get four cages, everyone should have ample opportunity to load and deploy PSDs.

Field preparations

Still no helium.

An email to the heat sealer company asking about repair or local service resulted in a referral to a southern California distributor.

Met Hama Garba today and we discussed the training progress.

Preparation for the field deployment continues with construction of the field LFTs. The lab staff are increasing the quality and consistency of the PSDs as well as the pace of production. They currently make 20 spiked PSDs per hour; the deployment requires 45. The spiking solution is 100uL of 1 ppm aldrin in ethyl acetate. This concentration should be easily detected even with significant loss in the field or poor extractions, high background, etc. All the PSD are completed for the deployment, we only need a few more cages.

Some good fortune: A chemical distributor cold called today and Cheikh tells me they have plenty of hexanes. Initially, there was some question as to whether hexanes would be readily available so this helps.

I've included a couple of photos of the LFT construction for the field. Note the location of the preparation blank on the frame. This serves two purposes: it keeps the blank near the production location but out of the way, and ensures that all the LFT are the same length.

Preparing PSD for field deployment.
Front to back: Emmanuel, Adama, Cheikh

Spiking the PSD with a PRC.
Marie

LFT progress and PRC selection

Adama, Emmanuel, Marie and Anna continue to practice LFT construction now focusing on proper spiking technique and removal of air prior to the final heat seal. It is clear that they have practiced previously as they are using techniques that were shown to Cheikh and Makhfousse during their visit. They all seem very comfortable with the process and are working to increase their pace. I noted some small details to look for to ensure high quality construction.

Cheikh and I were discussing the performance reference compound to be used in the Pont Gendarme deployment. We are leaning toward Aldrin as it is unlikely to be found in the area (or already degraded/metabolized to dieldrin) and has a similar Kow to the other OCs (5.1 - 7.4). Also, it is easily identifiable on the OSU method.

Concerning the blog, as suggested by Paul, I've added a way to easily track training progress. The sidebar indicates desired tasks to be completed. I will make a note as we accomplish them.

Locustox LFT frame

Test communication from OSU

Thank you Greg. The summary of activities and details of plans that you provide are extremely helpful. This is a test message to confirm that I will be able to respond to technical questions as required. I will also try to add comments to test the system. Best wishes to you and everyone at LOCUSTOX. Paul

LFT construction practice and cages

Makhfousse, Cheikh and I reviewed the blog and how it is intended to serve the training.

Cheikh attached a nitrogen generator to the Techne Dri-block DB-3 sample concentrator. The unit is operational and will be used as an acceptable equivalent to the TurboVap LV in SOP 406.00.

The staff (Adama, Emmanuel, Marie, and Anna) began practice on building LFT with special attention to the heat seals. They practiced for several hours on old LFT. On Wednesday they will practice proper spiking technique.

I inspected several cages that were built for the field deployment. I was told that 7 were at Locustox and the others being constructed at the contracted shop. They are excellent duplications and should work well for deployment. Photos below. The third one down from the top is the OSU purchased cage.

The cages were locally built for 15,000 Fcfa or 30 USD per cage.

The TEW impulse heat sealer is not working properly. The timer is broke and the operator has to practice and be careful to create a good seal. Fortunately the staff have each practiced enough to make it work. The heat sealer that OSU shipped is 110V not 220V. Locustox is using a locally purchased step-down transformer to make it work. I am not sure if this affected the timer.

Helium should be delivered on Wednesday the 19th.

Cheikh and I are choosing a PRC for the spiking solution for Pont Gendarme deployments next week.

Senegalese cages compared to U.S. cage. The U.S. cage is the third from the top.

LFT construction practice.

Front to back: Marie, Adama, Anna

Introductions and equipment review

Introductions to the all CERES/Locustox personnel. Afterwards, an in-depth meeting with the relevant Locustox lab staff (those participating directly in the PSD work) took place and covered Locustox and OSU expectations and detailed objectives for the training. In attendance: Cheikh Toure, Makhfousse Sarr, Auditrice Ndaiye, Adama Ndaiye, Marie Ndao, Ndeye Sokhna Fall Ndao, Anna Ndiaye, and Emmanuel Senghor. We discussed training evaluations of both myself and the Locustox staff as well as the training schedule. The lab staff will continue to work on other projects through PSD training; however, all staff will be attending field sampling.

Some concern was expressed about the method requiring significant blow down and handling of resulting quantities (<1 mL). There is interest in obtaining a TurboVap LV. As is, the blowdown will be attempted with a nitrogen/syringe setup. I believe the TurboVap would be a great advantage, but the method is possible with the existing equipment considering the training requires so few samples. If high throughput is expected for future work a TurboVap LV would be required.

There was a problem with the lab A/C unit and refrigerant leaked. The odor prevented the lab from being occupied for several hours.

The training schedule was adapted to account for arrival on Thursday the 20th of a Chemservice OC pesticide sample and helium for the GC-ECD. In the meantime, extra LFT will be sacrificed to develop PSD production skills.

Meeting with Locustox

I met with Cheikh Toure and Makhfousse Sarr at about 3:30 pm. We discussed expectations briefly, # of personnel on the field trips, some GC issues, and miscellaneous details concerning my housing, office space, etc. Point by point:

1. As planned, Monday the 17th will be a day of meeting staff, going over the lab and required equipment and settling in.

2. Cheikh asked if Chemstation files could be viewed on the OSU computers. I mentioned concern’s that the GC computer’s Chemstation is old, but my laptop Chemstation might work. If it does, we might be able to install the latest Chemstation we have on a computer in the lab that’s not hooked up to an instrument. As needed.

3. Makhfousse told me all the lab staff (whose CVs we received) will be participating in the field trips. This is good news: The more people that do it, and the more often, the better.

4. Miscellaneous details were discussed concerning my cell phone access, housing, lab space and after hours access.

The current hotel accommodations are fine, but I’ll be picked up by a driver at 8 am to head to Locustox and then continue my stay in a private apartment closer to the lab.

Travel

Sept 15
Depart PDX, 7:18 am
Arrive at Hotel Hacienda in Dakar @ 5:50 am Sept 16.

Purpose of Visit

While other goals may be attempted, the main purpose of this visit is to complete Specific Goal 3:

Analysis of PSD in field conditions. Deployment will be done at Pont Gendarme, one of the villages of the GEF project PDF-B. In this location two cages will be deployed at each of the sampling places: the main irrigated canal (at the pumping station), the main drainage canal (at the draining station) and at the wetland where waste water is drained. The deployment of PSD which is a part of the training will be done with CERES/Locustox staff. One set will be analyzed at CERES/Locustox and the other will be sent to OSU. All the necessary consumable and material will purchased by FAO to avoid any delay on delivery time which could affect the analytical process.