High-reliability zircon separation for hunting the oldest material on Earth： An automatic zircon separator with image-processing/microtweezers-manipulating system and double-step dating

Despite the recent development in radiometric dating of numerous zircons by LA-ICPMS, mineral separation still remains a major obstacle, particularly in the search for the oldest material on Earth. To improve the efficiency in zircon separation by an order of magnitude, we have designed/developed a new machine-an automatic zircon separator（AZS）. This is designed particularly for automatic pick-up of100 μm-sized zircon grains out of a heavy mineral fraction after conventional separation procedures. The AZS operates in three modes：（1） image processing to choose targeted individual zircon grains out of all heavy minerals spread on a tray,（2） automatic capturing of the individual zircon grains with microtweezers, and（3） placing them one-by-one in a coordinated alignment on a receiving tray. The automatic capturing was designed/created for continuous mineral selecting without human presence for many hours. This software also enables the registration of each separated zircon grain for dating, by recording digital photo-image, optical（color） indices, and coordinates on a receiving tray. We developed two new approaches for the dating; i.e.（1） direct dating of zircons selected by LA-ICPMS without conventional resin-mounting/polishing,（2） high speed U-Pb dating, combined with conventional sample preparation procedures using the new equipment with multiple-ion counting detectors（LA-MIC-ICPMS）.With the first approach, Pb-Pb ages obtained from the surface of a mineral were crosschecked with the interior of the same grain after resin-mounting/polishing. With the second approach, the amount of time required for dating one zircon grain is ca. 20 s, and a sample throughput of 〉150 grains per hour can be achieved with sufficient precision（ca. 0.5%）.We tested the practical efficiency of the AZS, by analyzing an Archean Jack Hills conglomerate in Western Australia with the known oldest（〉4.3 Ga） zircon on Earth. Preliminary results are positive; we were able to obtain more than 194 zircons that are over 4.0 Ga out of ca. 3800 checked grains, and 9 grains were over 4300 Ma with the oldest at 4371 ± 7 Ma. This separation system by AZS, combined with the new approaches, guarantees much higher yield in the hunt for old zircons.

Stability of selenium and its speciation analysis in water using automatic system separation and HR-ICP-MS measurement

A simple and convenient method has been developed for the pre-concentration and separation of inorganic selenium species from environmental water samples using anion exchange chromatographic column combined with high resolution inductively coupled plasma mass spectrometry(HR-ICP-MS)measurement.^(75)Se(Ⅳ) and ^(75)Se(Ⅵ)were prepared and used as tracers during the experiments.The volatility of selenium during solution evaporation was investigated to establish a reliable water samples pretreatment procedure.The parameters which affect the uptake of Se(Ⅳ)and Se(Ⅵ)on Dowex1×8 resin was optimized and the procedure for Se(Ⅳ)and Se(Ⅵ)separation was proposed.Both Se(Ⅳ)and Se(Ⅵ)are retained on the column in natural or alkaline solution with high distribution coefficient.The successive gradient elution of pre-concentrated species of selenium with HNO_(3)solution allows to differentiate between them.Se(Ⅳ)and Se(Ⅵ)finally were eluted with 0.05 mol/L HNO_(3) and 5.0 mol/L HNO_(3),respectively.The proposed method has been successfully verified using the certified reference materials(CRMs)of real water samples,and spiked recoveries for real samples were 98%-104%with 5%relative standard deviations(RSDs).The developed procedure is proved to be reliable and can be used for the rapid determination of selenium species in environmental water samples.