Evaluation of Carboxen carbon molecular sieves for trapping replacement chlorofluorocarbons

A method has been developed for trapping and preconcentrating the very volatile replacement chlorofluorocarbons (hydrofluorocarbons and hydrochlorofluorocarbons) using microtraps filled with Carboxen, a carbon molecular sieve type material, without the need for extensive cryotrapping using liquid nitrogen. We present here the adsorption characteristics of four Carboxen materials, Carboxen 569, 1000, 1001, and 1002, used to trap a range of replacement chlorofluorocarbons varying in boiling point from −48.4 to −9.8°C. The application of these traps for the automated analysis of trace gases in atmospheric and environmental chemistry could prove extremely useful.     

Über Perrhenate. 1. Zur Kenntnis von LiReO4

About Perrhenates. 1. On LiReO₄ For the very first time anhydrous LiReO₄ was prepared in transparent, colourless single crystals from Li₂O₂ and Re₂O₇ (closed Au-pipe; 350°C; 14 d). The crystal structure, P1 , with a = 9.652(1), b = 8.455(1), c = 6.928(1) Å, α = 101,53° (1), β = 106.55° (1), γ = 97.22° (1), Z = 6, d_x = 4.92 g/cm³, d_pyk = 4,81 g/cm³ was solved (four-circle-diffractometer data PW 1100, 2151 I₀ (hkl), AgKα; R = 0.073, R_w = 0.076). There are three kinds of functionally different Li⁺. The Madelung Part of the Lattice Energy, MAPLE, was calculated.     

High-resolution/higher-order derivative spectrophotometry in microanalytical chemistry

Summary Examples are given of the application of higher-order derivative spectrophotometry to microanalytical problems, including the increase in sensitivity for estimation of Zn and Cd dithizonates and the quantitative detection of arenes, aniline and phenols. We also describe the estimation of saccharin in soft drinks, and the characterization and estimation of dyes in solution and after absorption on a thin layer of alumina. Only ng-g amounts of substance are needed.

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Hochauflösende UV/VIS-Derivativspektrophotometrie höherer Ordnung in der Mikroanalytik

Zusammenfassung Einige Beispiele für die Anwendung der Derivativspektrophotometrie höherer Ordnung in der Mikroanalyse wurden angegeben. Im besonderen wurden die Erhöhung der Empfindlichkeit der Zn- und Cd-Dithizonat-Bestimmung, die quantitative Bestimmung von Arenen, Anilin, Phenol, die Erfassung von Saccharin in Limonaden und sowohl die Charakterisierung als auch die quantitative Bestimmung von Farbstoffen in Lösung oder adsorbiert an einer dünnen Schicht Aluminiumoxid beschrieben. Es werden nur einige Mikrogramm bis Nanogramm Substanz für die Untersuchungen benötigt.

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Presented at the 8th International Microchemical Symposium, Graz, August 25–30, 1980.     

Locked by Design: A Conformationally Constrained Transglutaminase Tag Enables Efficient Site‐Specific Conjugation

Based on the crystal structure of a natural protein substrate for microbial transglutaminase, an enzyme that catalyzes protein crosslinking, a recognition motif for site‐specific conjugation was rationally designed. Conformationally locked by an intramolecular disulfide bond, this structural mimic of a native conjugation site ensured efficient conjugation of a reporter cargo to the therapeutic monoclonal antibody cetuximab without erosion of its binding properties.     

The caffeine contents of dietary supplements commonly purchased in the US: analysis of 53 products with caffeine-containing ingredients

As part of a study initiating the development of an analytically validated Dietary Supplement Ingredient Database (DSID) in the United States (US), a selection of dietary supplement products were analyzed for their caffeine content. Products sold as tablets, caplets, or capsules and listing at least one caffeine-containing ingredient (including botanicals such as guarana, yerba mate, kola nut, and green tea extract) on the label were selected for analysis based on market share information. Two or three lots of each product were purchased and analyzed using high-pressure liquid chromatography (HPLC). Each analytical run included one or two National Institute of Standards and Technology (NIST) Standard Reference Materials (SRMs) and two products in duplicate. Caffeine intake per serving and per day was calculated using the maximum recommendations on each product label. Laboratory analysis for 53 products showed product means ranging from 1 to 829 mg caffeine/day. For products with a label amount for comparison (n = 28), 89% (n = 25) of the products had analytically based caffeine levels/day of between −16% and +16% of the claimed levels. Lot-to-lot variability (n = 2 or 3) for caffeine in most products (72%) was less than 10%.     

Spectroscopy of highly excited states in29Si

Particleγ-ray coincidences have been measured in the²⁸Si (d,pγ) reaction at 6.5 and 7 MeV bombarding energy, in the²⁶Mg (α,nγ) reaction at 12, 14 and 15 MeV, and in the²⁷A1 (τ,pγ) reaction at 9 MeV. Theγ-decay has been observed for all bound states of²⁹Si and for 56 unbound states up to 12,960 KeV excitation energy. Particleγ-ray angular correlations were measured in the²⁸Si (d,pγ) reaction at 6.5 MeV and in the²⁶Mg (α,nγ) reaction at 12 MeV. Spin (-parity) assignments or restrictions were obtained for nearly all bound states and some high-spin states above the binding energy. The assignment of mirror levels in²⁹Si and²⁹P has been extended to 8.2 MeV excitation energy. The excitation energies of 41 positive-parity states are reproduced by shell model calculations. The possible existence of aK ^π=5/2⁺ band with prolate deformation is discussed.