The difficulties encountered in quantitative analysis by gas chromatography are discussed, with particular reference to detection systems. The properties of an ideal detector for quantitative analysis are listed. A description is given of the mode of operation of detectors for gas chromatography, and the extent to which they are suitable for quantitative work is assessed. It was concluded that no one detector possessed all the properties required or an ideal detector. In particular a qualitative knowledge of the sample for analysis was required by all detectors; and calibration was required by the majority of detectors. The extent to which the Brunel mass detector overcomes these limitations was assessed. It is shown that the response of the mass detector depends solely on weight changes caused by adsorption of materials eluted from the chromatographic column thus completely eliminating the need for calibration and qualitative information. The response of the detector is integral, so that the problems associated with peak area measurement do not arise. The sensitivity of the detector is of a similar order to conventional hot wire detectors. The detector gave a quantitative response to all materials analysed, covering a wide boiling range: the upper limit was determined by the maximum column operating temperature, and the lower limit by the extent to which the detector was cooled. The detector responded quantitatively to water. At room temperature the detector responded on a qualitative basis to organic and inorganic gases. The detector was used for the calibration of other detector, and was operated in conjunction with the Martin gas density balance to determine the molecular weights of eluted materials.

The neutron-neutron (n-n) scattering length is a fundamental parameter in nuclear physics; however, measurements are plagued with large uncertainties caused by neutron detector cross talk. Many experimentalists also rely upon computer code to calibrate their neutron detectors. Experiments give one of two different numbers but there is still no adequate explanation for this discrepancy. We have developed a new neutron detector expressly for the purpose of improving the n-n scattering length measurement. It offers two important advantages: 1) minimal cross talk and 2) high counting efficiency. We calibrated the detector from 1 MeV to 6 MeV at 1 MeV increments. We have shown that the computer code, MCNP, does not always give the correct detector efficiency, and that reliance upon this code for calibration could be a large factor for error in previous experiments. Preliminary tests show no cross talk between two like detectors and suggest that these detectors in a n-n scattering length measurement.

Simulations have demonstrated that high-energy neutrinos (E > 1017 eV) are detected cost-efficiently via the Askaryan effect in ice, where a particle cascade induced by the neutrino interaction produces coherent radio emission that can be picked up by antennas installed below the surface. A good knowledge of the near surface ice (aka firn) properties is required to reconstruct the neutrino properties. In particular, a continuous monitoring of the snow accumulation (which changes the depth of the antennas) and the index-of-refraction profile are crucial for an accurate determination of the neutrino's direction and energy. 14 months of data of the ARIANNA detector on the Ross Ice Shelf, Antarctica, are presented where a prototype calibration system was successfully used to monitor the snow accumulation with unprecedented precision of 1 mm. Several algorithms to extract the time differences of direct and reflected (off the surface) signals (D'n'R time difference) from noisy data (including deep learning) are explored. This constitutes an in-situ test of the neutrino vertex distance reconstruction using the D'n'R technique which is needed to determine the neutrino energy. Additionally, an in-situ calibration system is proposed that extends the radio detector station with a radio emitter to continuously monitor the firn properties by measuring D'n'R time difference. In a simulation study the station layout is optimized and the achievable precision is quantified.

High-energy neutrino physics offers a unique way to investigate the most violent phenomena in our universe. The detection of energies above E > 1017 eV is most efficient using the Askaryan effect, where a neutrino-induced particle shower produces coherent radio emission that is detectable with radio antennas. By using radio techniques large volumes can be covered with few stations at moderate cost exploiting the large attenuation length of radio in cold ice. Key to the reconstruction of the neutrino properties visa precise and continuous monitoring of the firn properties. In particular the snow accumulation (changing the absolute depth of the antennas thus the propagation path of the signal) and the index-of-refraction profile are crucial for the neutrino energy and direction reconstruction. This work presents an in-situ calibration design that acts as an detector extension by adding additional emitter antennas to the station design to continuously monitor the firn properties by measuring the direct and reflected signals (D’n’R). In a simulation study the optimal station layout is determined and the achievable precision is quantified. Furthermore 14 months of data from an ARIANNA station at the Ross Ice Shelf, Antarctica, are presented where a prototype of this calibration system has been successfully installed to monitor the snow accumulation with unprecedented precision of 1 mm. Several algorithms, including deep learning algorithms, to compute the D’n’R time difference from radio traces are considered.

No description available.

Tato práce se zabývá možnostmi kvantitativního zobrazování ve skenovacím (transmisním) elektronovém mikroskopu (S|T|EM) společně s jejich korelativní aplikací. Práce začíná popisem metody kvantitativního STEM (qSTEM), kde lze stanovenou lokální tloušťku vzorku dát do spojitosti s ozářenou dávkou, a vytvořit tak studii úbytku hmoty. Tato metoda byla použita při studiu ultratenkých řezů zalévací epoxidové pryskyřice za různých podmínek (stáří, teplota, kontrastování, čištění pomocí plazmy, pokrytí uhlíkem, proud ve svazku). V rámci této části jsou diskutovány a demonstrovány možnosti kalibračního procesu detektoru, nezbytné pozadí Monte Carlo simulací elektronového rozptylu a dosažitelná přesnost metody. Metoda je pak rozšířena pro použití detektoru zpětně odražených elektronů (BSE), kde byla postulována, vyvinuta a testována nová kalibrační technika založená na odrazu primárního svazku na elektronovém zrcadle. Testovací vzorky byly různě tenké vrstvy v tloušťkách mezi 1 až 25 nm. Použití detektoru BSE přináší možnost měřit tloušťku nejen elektronově průhledných vzorků jako v případě qSTEM, ale také tenkých vrstev na substrátech - qBSE. Obě výše uvedené metody (qSTEM a qBSE) jsou založeny na intenzitě zaznamenaného obrazu, a to přináší komplikaci, protože vyžadují správnou kalibraci detektoru, kde jen malý posun úrovně základního signálu způsobí významnou změnu výsledků. Tato nedostatečnost byla překonána v případě qSTEM použitím nejpravděpodobnějšího úhlu rozptylu (zachyceného pixelovaným STEM detektorem), namísto integrální intenzity obrazu zachycené prstencovým segmentem detektoru STEM. Výhodou této metody je její použitelnost i na data, která nebyla předem zamýšlena pro využití qSTEM, protože pro aplikaci metody nejsou potřeba žádné zvláštní předchozí kroky. Nevýhodou je omezený rozsah detekovatelných tlouštěk vzorku způsobený absencí píku v závislosti signálu na úhlu rozptylu. Obecně platí, že oblast s malou tloušťkou je neměřitelná stejně tak jako tloušťka příliš silná (použitelný rozsah je pro latex 185 - 1 000 nm; rozsah je daný geometrií detekce a velikostí pixelů). Navíc jsou v práci prezentovány korelativní aplikace konvenčních a komerčně dostupných kvantitativních technik katodoluminiscence (CL) a rentgenové energiově disperzní spektroskopie (EDX) spolu s vysokorozlišovacími obrazy vytvořenými pomocí sekundárních a prošlých elektronů.