Applications with a brighter X-ray source and new detectors from Agilent

Agilent Technologies develop and supply X-ray systems for single-crystal diffraction research, including the SuperNova; a compact, highly reliable and very low maintenance instrument providing X-ray data of the highest quality; and the PX Scanner for testing and characterization of protein crystals in their original crystallization drops (in-situ). The SuperNova and PX Scanner are constantly improving, with recent enhancements including a new range of detectors using an Intelligent Measurement System. The Eos S2, Atlas S2 and Titan S2 detector range employs a smart sensitivity control of the electronic gain and is capable of instantaneously switching its binning modes thus providing unprecedented flexibility in tuning every exposure to provide the highest data quality for a wide range of experiments. We have also developed a completely new micro-focus X-ray source based on Gradient Vacuum technology, with novel filament and target designs. This novel source is an integral part of the new Agilent GV1000 X-ray diffractometer, which has been designed for applications that require even higher brightness of the X-ray beam.

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X-Ray Fluorescence Analysis of a Gold Ibex and other Artifacts from Akrotiri

HNPS Proceedings ◽

10.12681/hnps.2224 ◽

2019 ◽

Vol 11 ◽

Author(s):

A. G. Karydas ◽

T. Pantazis ◽

C. Doumas ◽

A. Vlachopoulos ◽

P. Nomikos ◽

...

Keyword(s):

Bulk Composition ◽

Fluorescence Analysis ◽

Wall Painting ◽

Inorganic Elements ◽

X Ray ◽

Wide Range ◽

Soldering Technology ◽

Excavation Area

In-situ X-ray fluorescence analysis (XRF) of ancient artifacts from the excavation area was performed using a novel X-ray instrumentation, composed of a portable silicon PIN thermoelectrically cooled X-ray detector, a miniature X-ray source, and portable data acquisition devices. The main objective of the analyses in Akrotiri was to explore the potential of the technique to provide answers to a wide range of archaeometric questions regarding the bulk composition of metal alloys, especially of gold, the characterization of corrosion products in bronze artifacts, identification of inorganic elements which are fingerprints of the minerals used in wall-painting pigments, and of the painting materials and techniques used for the decoration of clay vase surfaces. Among the analysed artifacts are a unique gold ibex, a bronze dagger and blade, various pigments from the wall paintings of room 3 in Xeste 3, decoration pigments from rosettes of faience, a bichrome jug, and other clay vases. The results of the in-situ XRF survey, primarily those of the bulk composition and soldering technology of the gold ibex, are discussed and compared with literature.

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Synthesis and Characterization of Tetraphenylphosphonium Tetraazidoborate

Zeitschrift für Naturforschung B ◽

10.1515/znb-2002-0605 ◽

2002 ◽

Vol 57 (6) ◽

pp. 621-624 ◽

Cited By ~ 12

Author(s):

Wolfgang Fraenk ◽

Heinrich Nöth ◽

Thomas M. Klapötke ◽

Max Suter

Keyword(s):

Single Crystal ◽

Synthesis And Characterization ◽

X Ray Diffraction ◽

X Ray

AbstractTetraphenylphosphonium tetraazidoborate, [P(C6H5)4][B(N3)4], was obtained from B(N3)3 - in situ prepared from BH3 · O(C2H5)2 and HN3 - and [P(C6H5)4][N3]. Recrystallization from an acetonitrile / hexane mixture yielded colorless crystals in 60% yield. The molecular structurewas determined by single crystal X-ray diffraction and the [B(N3)4]- anionwas shown to possess S4 symmetry.

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In Situ Observation of the Oxygen Nucleation in Silicon with X-Ray Single Crystal Diffraction

Solid State Phenomena ◽

10.4028/www.scientific.net/ssp.178-179.353 ◽

2011 ◽

Vol 178-179 ◽

pp. 353-359 ◽

Cited By ~ 2

Author(s):

Johannes Will ◽

Alexander Gröschel ◽

Christoph Bergmann ◽

Andreas Magerl

Keyword(s):

Single Crystal ◽

Waller Factor ◽

Dynamical Theory ◽

Mean Value ◽

Single Crystal Diffraction ◽

X Ray ◽

Float Zone ◽

Debye Waller Factor ◽

The Mean

The measurement of Pendellösungs oscillations was used to observe the time dependent nucleation of oxygen in a Czochralski grown single crystal at 750°C. It is shown, that the theoretical approach of the statistical dynamical theory describes the data well. Within the framework of this theory it is possible to determine the static Debye-Waller-factor as a function of the annealing time by evaluating the mean value of the Bragg intensity and the period length. The temperature influence on the Pendellösungs distance was corrected for by measurement of a Float-zone sample at the same temperature.

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Synthesis and Characterization of Binuclear Ruthenium Vinyl Complexes with Dithienylethene Unit

Advanced Materials Research ◽

10.4028/www.scientific.net/amr.834-836.259 ◽

2013 ◽

Vol 834-836 ◽

pp. 259-262

Author(s):

Yan Lin ◽

Han Feng Cui ◽

Hao Fan

Keyword(s):

Single Crystal ◽

Elemental Analysis ◽

Nmr Spectra ◽

Synthesis And Characterization ◽

Single Crystal Diffraction ◽

X Ray

A novel binuclear ruthenium vinyl complexes with dithienylethene unit II [RuCl (CO)(PMe3)3]2(μ-CH=CH-DTE-CH=CH) has been synthesized and characterized by elemental analysis and NMR spectra. Meanwhile, the crystal of II was obtained and determined by X-ray single-crystal diffraction.

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Lactide polymerization with iron alkoxide complexes

Canadian Journal of Chemistry ◽

10.1139/cjc-2014-0561 ◽

2015 ◽

Vol 93 (6) ◽

pp. 594-601 ◽

Cited By ~ 7

Author(s):

Arek Keuchguerian ◽

Berline Mougang-Soume ◽

Frank Schaper ◽

Davit Zargarian

Keyword(s):

Single Crystal ◽

Room Temperature ◽

Side Reactions ◽

X Ray Diffraction ◽

Iron Cluster ◽

X Ray ◽

H Nmr ◽

Exchange Product

This report presents the results of a study on the preparation of iron alkoxide complexes chelated by diiminopyridine ligands and their role in the room temperature polymerization of rac-lactide. Reaction of N,N′-(p-R-C6H4CH2)2-diiminopyridines (R = H (1), F (2)) with FeX2 (X = Cl, Br) yielded the homoleptic complexes [(1)2Fe][FeX4] or [(2)2Fe][FeX4], respectively. Treating the latter with Na[BPh4] afforded the anion exchange product [(2)2Fe][BPh4]2, which was characterized by 1H NMR and absorption spectroscopy, combustion analysis, and single crystal X-ray diffraction. Various attempts to grow crystals of [(1)2Fe][FeX4] and [(2)2Fe][FeX4] culminated in the isolation of single crystals of [(2)2Fe][Cl6Fe2O] that was characterized by X-ray diffraction. Attempted synthesis of well-defined, mononuclear alkoxide derivatives from [(1)2Fe]2+ or [(2)2Fe]2+ gave mostly intractable products, but in one case we obtained the crystallographically characterized sodium iron cluster Na4Fe2(OC6H4F)8(THF)2. An aryloxide derivative proved accessible by reaction of NaOC6H4F with the mono-ligand precursor LFeCl2 (L = N,N′-dimesityl-diiminopyridine), but characterization of LFe(OC6H4F)2 was limited to a single crystal X-ray diffraction analysis, owing to unsuccessful attempts at isolating pure samples. The difficulties encountered in the isolation of pure alkoxide derivatives prompted us to use in-situ generated LFe(OEt)2 for studying the polymerization of rac-lactide. This system was found to be moderately active at room temperature and with a slight preference for the formation of a heterotactic polymer (Pr = 0.54–0.65). Large polydispersities of 1.5–2.0 indicated the presence of transesterification side-reactions, which were confirmed by the presence of peaks with m/z = n 144 + M(EtOH) + M(Na+) and m/z = (n + 0.5) 144 + M(EtOH) + M(Na+) in MALDI-MS.

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Raman Spectroscopy and Single-Crystal High-Temperature Investigations of Bentorite, Ca6Cr2(SO4)3(OH)12·26H2O

Minerals ◽

10.3390/min10010038 ◽

2019 ◽

Vol 10 (1) ◽

pp. 38

Author(s):

Rafał Juroszek ◽

Biljana Krüger ◽

Irina Galuskina ◽

Hannes Krüger ◽

Martina Tribus ◽

...

Keyword(s):

Crystal Structure ◽

High Temperature ◽

Single Crystal ◽

Chemical Formula ◽

Crystal Chemical Formula ◽

Single Crystal Diffraction ◽

Bending Vibrations ◽

X Ray ◽

First Time

The crystal structure of bentorite, ideally Ca6Cr2(SO4)3(OH)12·26H2O, a Cr3+ analogue of ettringite, is for the first time investigated using X-ray single crystal diffraction. Bentorite crystals of suitable quality were found in the Arad Stone Quarry within the pyrometamorphic rock of the Hatrurim Complex (Mottled Zone). The preliminary semi-quantitative data on the bentorite composition obtained by SEM-EDS show that the average Cr/(Cr + Al) ratio of this sample is >0.8. Bentorite crystallizes in space group P31c, with a = b = 11.1927(5) Å, c =21.7121(10) Å, V = 2355.60(18) Å3, and Z = 2. The crystal structure is refined, including the hydrogen atom positions, to an agreement index R1 = 3.88%. The bentorite crystal chemical formula is Ca6(Cr1.613Al0.387)Σ2[(SO4)2.750(CO3)0.499]Σ3.249(OH)11.502·~25.75H2O. The Raman spectra of bentorite from two different localities exhibit the presence of the main stretching and bending vibrations related to the sulfate group at 983 cm−1 (ν1), 1109 cm−1 (ν3), 442 cm−1 (ν2), and 601 cm−1 (ν4). Moreover, the presence of bands assigned to the symmetric Cr(OH)63− stretching mode and hydroxyl deformation vibrations of Cr–OH units at ~540 cm−1 and ~757 cm−1, respectively, may be used to distinguish between ettringite and bentorite. In situ high temperature single crystal XRD experiments show that the decomposition of bentorite starts at ca. 45 °C and that a dehydroxylation product similar to metaettringite is formed.

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Hydrothermal Synthesis and Luminescent Characterization of Zn (II) Complex with 1,4-Bis(2’-formylphenyl)-1,4-dioxabutane Isonicotinoylhydrazone

Advanced Materials Research ◽

10.4028/www.scientific.net/amr.424-425.23 ◽

2012 ◽

Vol 424-425 ◽

pp. 23-26

Author(s):

Li Hua Wang

Keyword(s):

Schiff Base ◽

Hydrothermal Synthesis ◽

Single Crystal ◽

Diffraction Analysis ◽

Schiff Base Ligand ◽

Ir Spectrum ◽

Luminescent Properties ◽

Single Crystal Diffraction ◽

X Ray

A aroylhydrazone Schiff-base ligand (1, 4-Bis(2’-formylphenyl)-1,4-dioxabutane isonicotinoylhydrazone) and its Zn (II) complex were synthesized by hydrothermal method. The ligand was characterized by IR spectrum, MS spectrum and X-ray single crystal diffraction analysis. The luminescent properties of the ligand and Zn (II) complex material have been investigated in solid and in organic solvents. The results show that the ligand has strong luminescent emission at ca. 454 nm and the fluorescence of Zn (II) complex is very weak.

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