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Organisationseinheit der BAM
Mechanochemical synthesis of [Zn3(C2O4)3(4,4'-bipy)4] and its reorganization at high temperatures
(2014)
The metal organic layered structure catena-(bis(µ2-4,4'-bipyridine)-tris(µ2-oxalato)-bis(4,4'-bipyridine)-tri-zinc(ii)) ([Zn3(C2O4)3(4,4'-bipy)4]) was synthesized mechanochemically applying three different routes. The synthesis succeeded by i) simultaneously neat grinding the three starting materials zinc acetate dihydrate, oxalic acid dihydrate and 4,4'bipyridine, ii) grinding two compounds and adding the third afterwards, independent of the sequence. The products were characterized using powder X-ray diffraction, Raman spectroscopy, gas adsorption measurements, and scanning electron microscopy. Temperature-dependent synchrotron XRD measurements revealed that the monoclinic structure of [Zn3(C2O4)3(4,4'-bipy)4] rearranges reversibly to a higher ordered orthorhombic structure [Zn(C2O4)(4,4'-bipy)] at high temperatures.
The VSSA approach has the important advantage over classifying, imaging and counting techniques that it does not involve dispersion protocols. Further, the BET technique as the basis for VSSA determination it is in widespread use, generates low costs and is specified for many commercial materials. Finally, the same equipment allows for a deeper analysis by full isotherm evaluation.
The present deliverable assesses all NanoDefine powders, supplemented by further real-world materials (in total 26 powders), and quantitatively compares the relationship between the median size (by Electron Microscopy – considered as benchmark for the EC nanomaterial definition) vs. the size derived from VSSA. The VSSA method mitigates the challenges of EM to assess the thickness of platelets, but worked as well on fibbers and particles of irregular shapes. A screening strategy is proposed. If applied to the further data from real-world materials as validation set, this screening does achieve a correct classification, leaving only borderline materials for tier 2 assessment.
Zeolite synthesis was studied using two silica rich filtration residues (FR 1 and FR 2) as Si-source
and sodium aluminate in a direct synthesis at 60°C at strong alkaline conditions (8 M - 16 M NaOH).
In addition to these one-pot syntheses, a two-step process was investigated. Here, an alkaline digestion
of FR at 60°C was followed by gel precipitation with sodium aluminate and gel crystallization
under usual conditions of 80°C - 90°C. The results show that the substitution of chemical
reagent sodium silicate by a waste material like FR as Si-source is possible but requires fine tuning
of the reaction conditions as zeolite crystallization is a process under kinetic control. The
solubility behaviour and impurities of the inserted filtration residues strongly influenced the
course of reaction. Thus zeolites like hydrosodalite or intermediate zeolite between cancrinite
and sodalite, or zeolite NaA or Z-21 in cocrystallization with hydrosodalite could be observed in
the one pot syntheses already in a short time interval between 1 - 4 h depending on the alkalinity.
The two step process yield to zeolites NaA and NaX in very good quality. The reaction process of FR
in both reaction methods was characterized by chemical analyses, X-ray powder diffraction,
Fourier transform infrared spectroscopy as well as scanning electron microscopy. Surface area
and water content of selected products were further characterized by the BET-method and by
thermogravimetry. Summing up the results, we can show that zeolite formation from filtration residues
is possible by several reaction procedures as model cases for a re-use of industrial waste
materials. Beside the importance for environmental protection, the reactions are of interest for
zeolite chemistry as the re-use of FR is possible under economically conditions of low energy consumption
at 60°C and short reaction periods.
Mikrostrukturelle und mineralogische Eigenschaften leichter Gesteinskörnungen aus Mauerwerkbruch
(2015)
Poröse RC-Leichtgranulate mit Rohdichten zwischen 600 kg/m³ und 1400 kg/m³ können nach einem mehrstufigen mechanischen Prozess durch thermische Erhärtung bei 1180 °C aus ziegelhaitigern Mauerwerkbruch hergestellt werden. Diese Granulate erfüllen die Anforderungen an leichte Gesteinskörnungen nach DIN EN 13055 und es lassen sich damit Leichtbetone nach DIN EN 206-1/DIN 1045-2 herstellen. Ihre Festigkeits- und Dauerhaftigkeitseigenschatten sind mit denen herkömmlicher Leichtbetone mit Blähtonkörnungen sehr gut vergleichbar. Das ist das Fazit aus dem in den letzten Jahren durchgeführten Verbundforschungsvorhaben "Aufbaukörnungen". Um jedoch die Granulatentstehung bzw. den Vorgang der Porosierung besser verstehen, den Herstellungsprozess optimieren und die Eigenschaften der Granulate maßschneidern zu können, wurden zusätzlich zu den makroskopischen Charakteristika, wie beispielsweise Porosität und Wasseraufnahme, die chemisch-mineralogischen und mikrostrukturellen Eigenschaften der Leichtgranulate untersucht. Dazu dienten Analysen mittels ICP-Emissionsspektrometrie, Röntgenpulverdiffraktometrie, Quecksilberporosimetrie und mikroskopischen Verfahren. Im Beitrag wird über die Ergebnisse der Gefüge- und Porenstrukturuntersuchungen an Leichtgranulaten im Vergleich zu herkömmlichem Blähton berichtet.
Nonporous corundum powder, known as an abrasive material in the industry, was functionalized covalently with protein binders to isolate and enrich specific proteins from complex matrices. The materials based on corundum were characterized by TEM, ESEM, BET, DLS, and zeta potential measurements. The strong Al-O-P bonds between the corundum surface and amino phosphonic acids are used to introduce functional groups for further conjugations. The common cross-linker glutaraldehyde was compared with a hyperbranched polyglycerol (PG) of around 10 kDa. The latter is oxidized with periodate to generate aldehyde groups that can covalently react with the amines of the surface and the amino groups from the protein via a reductive amination process. The amount of bound protein was quantified via aromatic amino acid analysis (AAAA). This work shows that oxidized polyglycerol can be used as an alternative to glutaraldehyde. With polyglycerol, more of the model protein bovine serum albumin (BSA) could be attached to the surface under the same conditions, and lower nonspecific binding (NSB) was observed. As a proof of concept, IgG was extracted with protein A from crude human plasma. The purity of the product was examined by SDS-PAGE. A binding capacity of 1.8 mg IgG per g of corundum powder was achieved. The advantages of corundum are the very low price, extremely high physical and chemical stability, pressure resistance, favorable binding kinetics, and flexible application.
These data sets serve as models for calculating the specific surface area (BET method) using gas sorption in accordance with ISO 9277.
The present measurements were carried out with nitrogen at 77 Kelvin and argon at 87 Kelvin.
It is recommended to use the following requirements for the molecular cross-sectional area:
Nitrogen: 0.1620 nm²
Argon: 0.1420 nm²
Expected specific surface area for nitrogen (BET): 24 to 25 m²/g
Expected specific surface area for argon (BET): 20 m²/g
Titanium dioxides certified with nitrogen sorption and additionally measured with argon for research purposes were used as sample material.
The resulting data sets are intended to serve as comparative data for own measurements and show the differences in sorption behaviour and evaluations between nitrogen and argon.
These data are stored in the universal AIF format (adsorption information format), which allows flexible use of the data.
These data sets serve as models for calculating the specific surface area (BET method) using gas sorption in accordance with ISO 9277.
The present measurements were carried out with nitrogen at 77 Kelvin and argon at 87 Kelvin.
It is recommended to use the following requirements for the molecular cross-sectional area:
Nitrogen: 0.1620 nm²
Argon: 0.1420 nm²
Expected specific surface area for nitrogen (BET): 140 to 154 m²/g
Expected specific surface area for argon (BET): 129 to 135 m²/g
Titanium dioxides certified with nitrogen sorption and additionally measured with argon for research purposes were used as sample material.
The resulting data sets are intended to serve as comparative data for own measurements and show the differences in sorption behaviour and evaluations between nitrogen and argon.
These data are stored in the universal AIF format (adsorption information format), which allows flexible use of the data.
These data sets serve as models for calculating the specific surface area (BET method) using gas sorption in accordance with ISO 9277.
The present measurements were carried out with nitrogen at 77 Kelvin and argon at 87 Kelvin.
It is recommended to use the following requirements for the molecular cross-sectional area:
Nitrogen: 0.1620 nm²
Argon: 0.1420 nm²
Titanium dioxides certified with nitrogen sorption and additionally measured with argon for research purposes were used as sample material.
The resulting data sets are intended to serve as comparative data for own measurements and show the differences in sorption behaviour and evaluations between nitrogen and argon.
These data are stored in the universal AIF format (adsorption information file), which allows flexible use of the data.