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4th Mission Report _KE3_Jan –Feb 2013i) To accommodate this erroneous recommendation of installing a UPS, an inadequate 13 amp householdplug was used for the high power electrical supply. Furthermore other inadequate connections usingsimple wire connections with insulating tape had been used rather than the proper connectors.This electrical system was considered dangerous by the KE3 and he recommended that a professionalelectrician reconfigure the connections , who was immediately engaged to undertake this. He installed, asa temporary measure, a heavy duty 2 pole switch, with the third earth wire directly connected. Also thedangerous connection was replaced with a direct heavy duty connector. This was satisfactory as atemporary basis but it was recommended that the 2 pole switch should be replaced with a 3 pole switchand a heavy duty plug and socket should be installed.ii) Following the rectification of the electrical supply, the operation of the AAS 600 was investigated. Therewere three hollow cathode lamps (HCL) installed for Zn, Cu, Fe Ni and Pb analysis and also an EDL lamp forCadmium. The AAS was computer controlled using Perkin Elmer Windows software. According to thecomputer display, the AAS appeared to initialise correctly for the Spectrophotometer, Furnace andAutosampler. However the highest output energies from the lamps was only about 30% which seemedtoo low and the EDL lamp produced no energy at all. When the analysis was carried out even for the topstandards of copper of 5µl of 50µg/l, no atomic absorption was noted with or without backgroundcorrection.iii) The carbon furnace tube was removed and the energy was checked again and no difference wasnoted, indicating that the alignment was satisfactory.iv) The autosampler appeared to function correctly and to verify that this was not causing the problemthe highest copper standard (50µg/l) was manually injected and again no atomic absorption was noted.v) The above checks indicated that this problem could originate from a faulty detector as it seemedunlikely that all the lamps were faulty. It was recommended that the above information is passed on tothe Perkin Elmer Engineer, to assist the diagnosis and resolution of the problem.2) Fluorescence SpectrophotometerThe Perkin Fluorescence Spectrophotometer (FS 45) had been delivered about 5 years ago but had neverreally been used. It can be used for the analysis of any compound that fluoresce or luminesce such as:petroleum hydrocarbon products, and polyaromatic hydrocarbons. This technique is useful, as theindividual methods are usually very specific and avoid interferences by other compounds. Furthermore itis also sensitive, achieving low limits of detection, especially if the excitation and emission wavelengthsare specified within the method. The FS 45 had limited facilities compared to other models, so that the slitwidths were fixed at 10 nm and could not be changed, and there were no other accessories such as anautosampler and flow cells. It had just one cell holder and two 1 cm silica cells were supplied. Thissimplified the operation and settings for the instrument.The following issues were addressed:i) The FS45 was computer controlled but the CD drive was faulty, and was replaced and the WinFlowsoftware was reinstalled.ii) There were a number of methods already installed in the software, which were all tested by KE3 butthe one that was easily applicable was the “Time Drive” method. With this method one could specify theemission and excitation wavelengths and then scan the fluorescence over a period of time, which couldbe specified by the operator.Page 14 of 36
4th Mission Report _KE3_Jan –Feb 2013When the Time Drive method is set up, one can preset the emission, and excitation wavelengths togetherwith the duration of each integration period (set at 5 seconds). The duration of the scan could also be sete.g. 100 seconds. One could also set up the file name (td file) so that the graphical results could be saved.The instrument uses a simple traffic light icon to be clicked to start the analysis, which then initiated the100 second scan showing the fluorescence emission value graphically.iii) Using the above technique, this method was tested by using a range of crude oil standardsconcentrations from 0.5 to 10µg/l in hexane, which produced emissions from 200 to about 996, with ablank of about 27. This indicated that the LOD for this method could, in theory, reach at least 0.05µg/l,though would depend on the liquid/liquid extraction, and concentration efficiencies.iv) The KE3 recommended that this method should be developed for specific hydro carbons such as crudeoil, diesel oils & total petroleum products where standard methods are available by:a. Initially making up at least 6 concentration standards in the extraction solvent (hexane) to producea calibration graph to determine the linearity range.b. Following this, carry out the ISO extraction procedure on a similar series of standards made up indistilled water in order to determine the ideal recoveries.c. Repeat (b) using standards in the Pilot River water of the Chorokhi – Adjaristkali taken from a goodreference site (site with no anthropogenic activity so that the water should be pure as possible) toestablish the extraction efficiencies from the river water.d. It was also recommended to repeat this process from similar pure water from the Black Sea, whichwould be important for the department in analyzing the sea and also for the imminent new EUsister project investigating the coastal regions.If the Department does not have the available time to undertake this method development, it could be anideal project for a research M.Sc. postgraduate study, which would also minimise costs.v) The FS 45 does have other useful facilities, such as scanning fluorescence at differing wavelengths,which could be useful for determining new methods for compounds where there are no ISO methodsavailable. When this is required, the KE3 expert could investigate this new operational procedure duringfuture missions to further develop the application of this equipment.3) Other Equipment ProblemsThe KE3 also checked the inoperative microwave digester, unfortunately there was insufficient time tofully investigate this problem and it was recommended that this is progressed in the next appropriatemission as this apparatus is not as vital as the others.The Laboratory also had a Scalar Continuous Bubble Flow Analyser dedicated for measuring nitrates,phosphates and ammonia. This had recently broken down and appeared to have a power problem andwas due to be fixed soon.The Chemical Laboratory had so many problems with their expensive sensitive equipment, could becaused by poor electrical supplies. It was recommended that, where possible, to using anti surge electricalsockets, and power regulators to avoid electrical spikes, and safeguard the equipment, though this mightnot be possible for the AAS.4) Analytical Quality ControlPage 15 of 36
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