This study assessed the potential of five fluorochromes in marking shells of the abalone Haliotis rubra, using an immersion technique. Such marks are required to 'time stamp' the shells and thus determine whether shell layers are deposited regularly enough to be used to age abalone. The stains used were: oxytetracycline and tetracycline at 300-1000 mg L-1; calcein at 10-120 mg L-1; alizarin red S at 10-60 mg L-1; and xylenol orange at 20-100 mg L-1. Immersion times were 12, 24 and 48 h. Mortality rates were low in all treatments, and clearly discernible marks were produced when abalone were immersed for 24 and 48 h at high concentrations in all the stains. Three problems were encountered when tetracyclines were employed: (i) the solutions were acidic, so the pH had to be adjusted with NaOH to prevent mortality; (ii) there was excessive foaming of the solutions; and (iii) a natural fluorescence in the shells closely resembled that of the tetracyclines. Problems also arose in assessing alizarin red and xylenol orange because they have long emission wavelengths, so that simultaneously viewing natural layers on the sections is difficult. Calcein, although expensive, was the most effective, as at high concentrations it consistently produced bright, extensive marks. The success of marking appeared to depend on the growth rate of the abalone, as feeding before staining increased the intensity of marks, and marking varied between batches of abalone collected at different times.
Two-week-old straight-run white broiler chicks and 2-week-old straight-run white turkey poults were fed seed or whole plants Cymopterus watsonii or seed of Cymopterus longipes at 0.4, 0.8, and 1.6% of body weight, and then placed in sunlight for 5 hours each day for 7 days. All plant material produced moderate to severe photosensitivity in chicks. Toxic signs included photophobia; red discoloration of beak, comb, and feet; loss of feathers in the periorbital area; dried serous fluid on comb and edge of beak; keratoconjunctivitis; and multiple lesions on feet and legs. Turkey poults showed a syndrome similar to that of chicks. Mortality was particularly high in turkeys fed C. longipes seed. Toxic signs in turkeys 6 weeks after treatment included tremors in the legs; upturning and shortening of the upper beak; and shortening disfigurement, and gangrene of the toes. Two phototoxic furocoumarins, oxypeucedanin and isoimperitorin, were isolated from C. longipes seed. Either compound, administered orally, produced photosensitivity in 2-week-old chicks.
At Texaco's Research Center, X-ray Fluorescence (XRF) is our workhorse method for the determination of additive elements in lubricating materials. Other analysis techniques are used to assist in method development by confirming compositions of standards and quality control samples, or by verifying analysis results from newly developed XRF methods. Often it is impractical to make a determination of all analytes in a sample by XRF due to inherent limitations of X-ray fluorescence measurements and the complexity of calibrating for many analytes in a single method. Analyses of high volumes of samples can be made more efficient by omitting difficult or infrequently encountered elements. When a unique sample comes along, alternative analytical techniques are used to determine elements for which the X-ray spectrometer is not sensitive or not calibrated. These concentrations can be combined with theoretical influence coefficients to correct existing XRF calibrations for the effects of unanalyzed elements. A working example, sodium in research samples, is given. Another example, barium in oils, shows the serious shortcomings of this approach. Alternative techniques such as inductively coupled plasma atomic emission spectroscopy, atomic absorption spectrometry, sulfur determination by high temperature combustion with infrared detection, and wet chemical methods can be used to complete an analysis or to confirm the accuracy of XRF methods for determinations of additive elements in lubricants. Examples of our elemental analysis methods, how they relate to ASTM procedures, and how we use our techniques are described.
Environmental regulations specify the analysis of recycled oil for arsenic, cadmium, chromium, lead, and total halogens. Waste oils for disposal must be analyzed for arsenic, barium, cadmium, chromium, lead, mercury, selenium, and silver. Inductively coupled plasma mass spectrometry (ICP-MS) is a multielement technique with sufficient sensitivity to determine most metals and some nonmetals at the parts-per-billion level. Direct aspiration of the sample after dilution in a suitable solvent eliminates the tedious and potentially dangerous acid digestion process and the loss of volatile elements. The heat generated in the plasma and the addition of oxygen in the gas streams aid the breakdown of complexes of metals and the destruction of the organic matrix. The detection limits in a multielement analytical batch for elements of high mass [>80 atomic mass units (amu)] approach 5 to 50 μg/m3 for undiluted samples. Elements of lower mass suffer from isobaric or polyatomic interferences, which degrade detection limits.
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