TY - JOUR A1 - Ramirez Caro, Alejandra A1 - Pauli, Jutta A1 - Mota, Berta A1 - Simon, Sebastian A1 - Schmidt, Wolfram A1 - Resch-Genger, Ute T1 - C⁠3A passivation with gypsum and hemihydrate monitored by optical spectroscopy N2 - Tricalcium aluminate (C⁠3A) is found with less than 10% wt. of the total composition; however, during hydration, C⁠3A plays an important role in the early hydration of cement in the presence of gypsum as a set retarder. The aim of this investigation is to assess the suitability of optical spectroscopy and a dye-based optical probe to monitor early hydration of C⁠3A in the presence of gypsum and hemihydrate. Optical evaluation was performed using steady-state fluorescence and diffuses reflectance spectroscopy (UV-VisDR). Phase characterization during hydration was done with in-situ X-ray diffraction. UV-VisDR with a cyanine dye probe was used to monitor the formation of metastable phases and was employed together with fluorescence spectroscopy, to follow the Aggregation and disaggregation of the dye during hydration. In conclusion, for the first time, a cyanine dye was identified as a feasible and stable probe to monitor C⁠3A hydration changes in the presence of calcium sulfate. KW - Dye KW - Photoluminescence KW - Fluorescence KW - Reflection spectroscopy KW - Cement KW - Hydration KW - Method development PY - 2020 DO - https://doi.org/10.1016/j.cemconres.2020.106082 VL - 133 SP - 106082 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-50952 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Adorjan, I. A1 - Rosenau, Th. A1 - Potthast, A. A1 - Kosma, P. A1 - Mereiter, K. A1 - Pauli, Jutta A1 - Jäger, Christian T1 - Crystal and molecular structure of methyl 4-O-methyl-beta-D-ribo-hex-3-ulopyranoside N2 - Methyl 4-O-methyl-?-Image-ribo-hex-3-ulopyranoside (2), a model compound for partially oxidized anhydroglucose units in cellulose, was crystallized from CHCl3/n-hexane by vapor diffusion to give colorless plates. Crystal structure determination revealed the monoclinic space group P21 with Z=2C8H14O6 and unit cell parameters of a=8.404(2), b=4.5716(10), c=13.916(3) Å, and ?=107.467(4)°. The structure was solved by direct methods and refined to R=0.0476 for 1655 reflections and 135 parameters. The hexulopyranoside occurs in a distorted chair conformation. Both hydroxyls are involved in hydrogen bonding and form zigzag bond chains along the b-axis. One of the two hydrogen bonds is bifurcated. The solid-state 13C NMR spectrum of 2 exhibits eight carbon resonances, with well-separated signals for the two methoxyls (1-OMe: 55.72 ppm, 4-OMe: 61.25 ppm) and a keto resonance with relatively large downfield shift (206.90 ppm). Differences in the C-4 and the methoxyls’ chemical shifts in the solid and liquid states were found KW - Crystal structure KW - Solid-state NMR KW - Cellulose KW - Carbonyl groups PY - 2004 DO - https://doi.org/10.1016/j.carres.2004.01.006 SN - 0008-6215 SN - 1873-426X VL - 339 IS - 4 SP - 795 EP - 799 PB - Elsevier CY - Amsterdam AN - OPUS4-5341 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mackie, I.D. A1 - Röhrling, J. A1 - Gould, R.O. A1 - Pauli, Jutta A1 - Jäger, Christian A1 - Walkinshaw, M. A1 - Potthast, A. A1 - Rosenau, Th. A1 - Kosma, P. T1 - Crystal and molecular structure of methyl 4-O-methyl-beta-D-glucopyranosyl-(1->4)-beta-D-glucopyranoside N2 - The cellulose model compound methyl 4-O-methyl-?-Image-glucopyranosyl-(1?4)-?-Image-glucopyranoside (6) was synthesised in high overall yield from methyl ?-Image-cellobioside. The compound was crystallised from methanol to give colourless prisms, and the crystal structure was determined. The monoclinic space group is P21 with Z=2 and unit cell parameters a=6.6060 (13), b=14.074 (3), c=9.3180 (19) Å, ?=108.95(3)°. The structure was solved by direct methods and refined to R=0.0286 for 2528 reflections. Both glucopyranoses occur in the 4C1 chair conformation with endocyclic bond angles in the range of standard values. The relative orientation of both units described by the interglycosidic torsional angles [? (O-5?---C-1?---O-4---C-4) -89.1°, phi (C-1?---O-4---C-4---C-5) -152.0°] is responsible for the very flat shape of the molecule and is similar to those found in other cellodextrins. Different rotamers at the exocyclic hydroxymethyl group for both units are present. The hydroxymethyl group of the terminal glucose moiety displays a gauche–trans orientation, whereas the side chain of the reducing unit occurs in a gauche–gauche conformation. The solid state 13C NMR spectrum of compound 6 exhibits all 14 carbon resonances. By using different cross polarisation times, the resonances of the two methyl groups and C-6 carbons can easily be distinguished. Distinct differences of the C-1 and C-4 chemical shifts in the solid and liquid states are found. KW - Crystal structure KW - Cellulose KW - Methyl cellobioside KW - Solid state NMR PY - 2002 DO - https://doi.org/10.1016/S0008-6215(01)00299-3 SN - 0008-6215 SN - 1873-426X VL - 337 IS - 2 SP - 161 EP - 166 PB - Elsevier CY - Amsterdam AN - OPUS4-11023 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hamann, F. A1 - Brehm, Robert A1 - Pauli, Jutta A1 - Grabolle, Markus A1 - Frank, W. A1 - Kaiser, W.A. A1 - Fischer, D. A1 - Resch-Genger, Ute A1 - Hilger, I. T1 - Controlled modulation of serum protein binding and biodistribution of asymmetric cyanine dyes by variation of the number of sulfonate groups N2 - To assess the suitability of asymmetric cyanine dyes for in vivo fluoro-optical molecular imaging, a comprehensive study on the influence of the number of negatively charged sulfonate groups governing the hydrophilicity of the DY-67x family of asymmetric cyanines was performed. Special attention was devoted to the plasma protein binding capacity and related pharmacokinetic properties. Four members of the DY-67x cyanine family composed of the same main chromophore, but substituted with a sequentially increasing number of sulfonate groups (n = 1−4; DY-675, DY-676, DY-677, DY-678, respectively), were incubated with plasma proteins dissolved in phosphate-buffered saline. Protein binding was assessed by absorption spectroscopy, gel electrophoresis, ultrafiltration, and dialysis. Distribution of dye in organs was studied by intraveneous injection of 62 nmol dye/kg body weight into mice (n = 12; up to 180 minutes postinjection) using whole-body near-infrared fluorescence imaging. Spectroscopic studies, gel electrophoresis, and dialysis demonstrated reduced protein binding with increasing number of sulfonate groups. The bovine serum albumin binding constant of the most hydrophobic dye, DY-675, is 18 times higher than that of the most hydrophilic fluorophore, DY-678. In vivo biodistribution analysis underlined a considerable influence of dye hydrophilicity on biodistribution and excretion pathways, with the more hydrophobic dyes, DY-675 and DY-676, accumulating in the liver, followed by strong fluorescence signals in bile and gut owing to accumulation in feces and comparatively hydrophilic DY-678-COOH accumulating in the bladder. Our results demonstrate the possibility of selectively controlling dye-protein interactions and, thus, biodistribution and excretion pathways via proper choice of the fluorophore's substitution pattern. This underlines the importance of structure-property relationships for fluorescent labels. Moreover, our data could provide the basis for the rationalization of future contrast agent developments. PY - 2011 DO - https://doi.org/10.2310/7290.2011.00005 SN - 1535-3508 SN - 1536-0121 VL - 10 IS - 4 SP - 258 EP - 269 PB - Decker CY - Hamilton, Ont. AN - OPUS4-24311 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Würth, Christian A1 - Grabolle, Markus A1 - Pauli, Jutta A1 - Spieles, Monika A1 - Resch-Genger, Ute T1 - Comparison of methods and achievable uncertainties for the relative and absolute measurement of photoluminescence quantum yields N2 - The photoluminescence quantum yield (Φf) that presents a direct measure for the efficiency of the conversion of absorbed photons into emitted photons is one of the spectroscopic key parameters of functional fluorophores. It determines the suitability of such materials for applications in, for example, (bio)analysis, biosensing, and fluorescence imaging as well as as active components in optical devices. The reborn interest in accurate Φf measurements in conjunction with the controversial reliability of reported Φf values of many common organic dyes encouraged us to compare two relative and one absolute fluorometric method for the determination of the fluorescence quantum yields of quinine sulfate dihydrate, coumarin 153, fluorescein, rhodamine 6G, and rhodamine 101. The relative methods include the use of a chain of Φf transfer standards consisting of several 'standard dye' versus 'reference dye' pairs linked to a golden Φf standard that covers the ultraviolet and visible spectral region, and the use of different excitation wavelengths for standard and sample, respectively. Based upon these measurements and the calibration of the instruments employed, complete uncertainty budgets for the resulting Φf values are derived for each method, thereby providing evaluated standard operation procedures for Φf measurements and, simultaneously, a set of assessed Φf standards. KW - Fluorescence KW - Photoluminescence KW - Quantum yield KW - Dye KW - Uncertainty KW - Absolute quantum yield KW - Method comparison KW - Integrating sphere PY - 2011 DO - https://doi.org/10.1021/ac2000303 SN - 0003-2700 SN - 1520-6882 VL - 83 IS - 9 SP - 3431 EP - 3439 PB - American Chemical Society CY - Washington, DC AN - OPUS4-23632 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauli, Jutta T1 - Characterization of a new near infrared dyes for molecular imaging T2 - Method and Application of Fluerescence (MAF10) CY - Salzburg, Austria DA - 2007-09-09 PY - 2007 AN - OPUS4-16407 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauli, Jutta T1 - Certified Fluorescence Quantum Yield Standards as New Optical Reference Materials N2 - Luminescence techniques are amongst the most commonly used analytical methods in life and material sciences due to their sensitivity and their nondestructive and multiparametric character. Photoluminescence signals are, however, affected by wavelength, polarization and time dependent instrument specific effects, and provide only relative intensities. This hampers the comparability of fluorescence measure-ments and calls for simple tools for instrument characterization and the quantification of measured fluorescence intensities. Well characterized fluorescence standards for instrument calibration and performance validation (IPV) can be used as references for fluorescence signals. Of special importance is the correct determination of photoluminescence quantum yields (QF) (number of emitted per absorbed photons) that provides a direct comparison of the fluorescence efficiency of emitters. Such well characterized standards have been successfully developed by BAM for the relative determination of f values of transparent solutions of molecular and nanoscale emitters in the wavelength range from 350 and 1100 nm and will be soon certified. These standards can also be used to evaluate integrating sphere setups, which are increasingly being used for absolute measurements of QF values. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2091 KW - Fluoreszenz KW - Referenzmaterial PY - 2019 AN - OPUS4-47795 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauli, Jutta T1 - Brilliant and Functional Herceptin Conjugates with a Remarkably High Number of Bound Fluorophores T2 - MOBI 2013 CY - Heidelberg, Germany DA - 2013-10-28 PY - 2013 AN - OPUS4-29576 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauli, Jutta T1 - Bright Functional Herceptin Conjugates with a Remarkably High Number of Fluorophores for Optical Imaging T2 - 5th EuCheMS CY - Istanbul, Turkey DA - 2014-08-31 PY - 2014 AN - OPUS4-31849 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauli, Jutta T1 - Analytical and Spctroscopic tools for the Design of Highly Flourescent Conjugates T2 - ANAKON 2013 CY - Essen, Germany DA - 2013-03-04 PY - 2013 AN - OPUS4-28471 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -