55327
2022
eng
1
9
9
33
article
IOP Publishing
Bristol, UK
1
--
--
--
Validation of a fast and traceable radiographic scale calibration of dimensional computed tomography
A fast and highly precise method of determining the geometrical scale factor of computed tomography (CT) measurements has been validated successfully by Bundesanstalt für Materialforschung und -prüfung (BAM), the Federal Institute of Metrology (METAS) and Physikalisch-Technische Bundesanstalt (PTB) within the scope of AdvanCT (Advanced Computed Tomography for dimensional and surface measurements in industry), a project funded in the European Metrology Programme for Innovation and Research (EMPIR). The method has been developed by PTB and requires only two radiographic images of a calibrated thin 2D standard (hole grid standard) from two opposite directions. The mean grid distance is determined from both radiographs. From this and with the help of the calibration result, the radiographic scale and therefore the voxel size is determined. The procedure takes only a few minutes and avoids a time-consuming CT scan. To validate the method, the voxel sizes determined via this method were compared with voxel sizes determined from CT scans of calibrated objects. Relative deviations between the voxel sizes in the range of 10−5 were
achieved with minimal effort using cone-beam CT systems at moderate magnifications.
Measurement Science and Technology
10.1088/1361-6501/ac74a3
0957-0233
urn:nbn:de:kobv:b43-553271
publish
21.07.2022
false
true
Creative Commons - CC BY - Namensnennung 4.0 International
U. Neuschaefer-Rube
J. Illemann
M. Sturm
B. Bircher
F. Meli
Carsten Bellon
Sergei Evsevleev
eng
uncontrolled
Dimensional metrology
eng
uncontrolled
Voxel size
eng
uncontrolled
Industrial CT
eng
uncontrolled
Geometrical magnification
Analytische Chemie
8 Zerstörungsfreie Prüfung
8.5 Röntgenbildgebung
Chemie und Prozesstechnik
Verlagsliteratur
Datei für die Öffentlichkeit verfügbar ("Open Access")
Wissenschaftliche Artikel der BAM
Bundesanstalt für Materialforschung und -prüfung (BAM)
https://opus4.kobv.de/opus4-bam/files/55327/Neuschaefer-Rube_2022_Meas._Sci._Technol._33_094007.pdf
55316
2022
eng
106502
195
article
Elsevier B.V.
1
--
--
--
Features of hydrogen reduction of SiF4 in ICP plasma
Probe diagnostics is used to determine the electron temperature and electron number density in a low pressure inductively coupled plasma (ICP) ignited in the mixture of SiF4, Ar and H2. Emission spectra of mixtures with different stoichiometry of components are investigated and the electron density distribution function (EDDF) is estimated. The optimal conditions for high conversion of SiF4 into Si are found by studying the dependence of the yield of silicon upon the ratio of reagents. The maximum achieved yield of silicon is 85% under the optimal conditions. Based on the analysis of IR and MS spectra of exhaust gases, 5% of initial SiF4 converts into volatile fluorosilanes. A rate of production of Si is 0.9 g/h at the energy consumption 0.56 kWh /g.
Spectrochimica Acta Part B
10.1016/j.sab.2022.106502
0584-8547
publish
08.09.2022
R. Kornev
Igor B. Gornushkin
V. Nazarov
V. Shkrunin
A. Ermakov
eng
uncontrolled
Plasma enhanced chemical vapor deposition
eng
uncontrolled
PECVD
eng
uncontrolled
Silicon tetrafluoride
eng
uncontrolled
Emission spectroscopy
eng
uncontrolled
Probe diagnostics
Analytische Chemie
1 Analytische Chemie; Referenzmaterialien
1.3 Instrumentelle Analytik
Chemie und Prozesstechnik
Verlagsliteratur
Datei im Netzwerk der BAM verfügbar ("Closed Access")
54993
2022
eng
1
7
article
Royal Society of Chemistry
1
--
--
--
Quantitative reversible one pot interconversion of three crystalline polymorphs by ball mill grinding
We demonstrate here using a disulfide system the first example of reversible, selective, and quantitative transformation between three crystalline polymorphs by ball mill grinding. This includes the discovery of a previously unknown polymorph. Each polymorph is reproducibly obtained under well-defined neat or liquid-assisted grinding conditions, revealing subtle control over the apparent thermodynamic stability. We discovered that the presence of a contaminant as low as 1.5% mol mol−1 acting as a template is required to enable all these three polymorph transformations. The relative stabilities of the polymorphs are determined by the sizes of the nanocrystals produced under different conditions and by surface interactions with small amounts of added solvent. For the first time, we show evidence that each of the three polymorphs is obtained with a unique and reproducible crystalline size. This mechanochemical approach gives access to bulk quantities of metastable polymorphs that are inaccessible through recrystallisation.
Crystengcomm
10.1039/D2CE00393G
urn:nbn:de:kobv:b43-549934
publish
13.06.2022
false
true
Creative Commons - CC BY - Namensnennung 4.0 International
A. Belenguer
G. Lampronti
Adam Michalchuk
Franziska Emmerling
J. Sanders
eng
uncontrolled
Mechanochemistry
eng
uncontrolled
Polymorph
eng
uncontrolled
XRD
Analytische Chemie
Ingenieurwissenschaften und zugeordnete Tätigkeiten
6 Materialchemie
6.3 Strukturanalytik
Material
Chemie und Prozesstechnik
Verlagsliteratur
Datei für die Öffentlichkeit verfügbar ("Open Access")
Wissenschaftliche Artikel der BAM
6.0 Abteilungsleitung und andere
Materialdesign
Bundesanstalt für Materialforschung und -prüfung (BAM)
https://opus4.kobv.de/opus4-bam/files/54993/quantitative.pdf
55287
2022
eng
1
6
211
article
Elsevier Ltd.
1
--
--
--
Experimental investigation of the local environment and lattice distortion in refractory medium entropy alloys
EXAFS analysis of pure elements, binary and ternary equiatomic refractory alloys within the Nb-Zr-Ti-Hf- Ta system is performed at the Nb and Zr K-edges to analyze the evolution of the chemical local environ- ment and the lattice distortion. A good mixing of the elements is found at the atomic scale. For some compounds, a distribution of distances between the central atom and its neighbors suggests a distortion of the structure. Finally, analysis of the Debye-Waller parameters shows some correlation with the lat- tice distortion parameter δ², and allows to quantify experimentally the static disorder in medium entropy alloys.
Scripta Materialia
10.1016/j.scriptamat.2022.114532
1359-6462
publish
18.07.2022
false
true
L. Lilensten
K. Provost
L. Perrière
E. Fonda
J. Couzinié
F. Amman
Martin Radtke
G. Dirras
I. Guillot
eng
uncontrolled
BAMline
eng
uncontrolled
Refractory alloys
eng
uncontrolled
EXAFS
eng
uncontrolled
Debye-Waller parameter
Analytische Chemie
6 Materialchemie
6.3 Strukturanalytik
Chemie und Prozesstechnik
Chemische Charakterisierung und Spurenanalytik
Verlagsliteratur
Datei im Netzwerk der BAM verfügbar ("Closed Access")
55288
2022
eng
1
14
article
Wiley online library
1
--
--
--
Investigations on fire-gilding
Fire-gilding is a historic technique for the application of golden layers on a number of different base materials utilizing a gold amalgam. This technique leaves a significant amount of Hg in the golden layer, giving archeometrists a reliable indicator to identify firegildings.
Recent findings on presumably fire-gilded objects have shown in several cases significantly lower Hg content than previously studied objects. This prompted a synchrotron-based X-ray fluorescence investigation into the Hg distribution along the material–gilding interface, as well as a series of measurements regarding the Hg content development in fire-gilded samples during artificial aging. This work presents findings on laboratory-prepared fire-gildings, indicating an Hg enrichment at the interface of firegilded silver samples. Notably, such an enrichment is missing in fire-gilded copper samples. Further, it is confirmed that fire-gilded layers typically do not undercut an Hg bulk content of 5%. In this light, it seems improbable that ancient samples that contain <5% Hg are fire-gilded. The results presented in this study might lead to a non-destructive method to identify the Hg enrichment at the interface. This might be obtained by a combination of different non-destructive measurements and might also work unambiguously in samples in which the gold top layer is altered.
Archaeometry
10.1111/arcm.12797
0003-813X
urn:nbn:de:kobv:b43-552885
publish
18.07.2022
false
true
Creative Commons - CC BY-NC-ND - Namensnennung - Nicht kommerziell - Keine Bearbeitungen 4.0 International
R. Margreiter
J. Baumann
I. Mantouvalou
Martin Radtke
Uwe Reinholz
E. Strub
eng
uncontrolled
BAMline
eng
uncontrolled
X-Ray Fluorescence
eng
uncontrolled
Gilding
eng
uncontrolled
Depth profile
eng
uncontrolled
Archaeometry
Analytische Chemie
6 Materialchemie
6.3 Strukturanalytik
Chemie und Prozesstechnik
Chemische Charakterisierung und Spurenanalytik
Verlagsliteratur
Datei für die Öffentlichkeit verfügbar ("Open Access")
Wissenschaftliche Artikel der BAM
Bundesanstalt für Materialforschung und -prüfung (BAM)
https://opus4.kobv.de/opus4-bam/files/55288/Archaeometry-2022-Margreiter-InvestigationsonFireGilding.pdf
55207
2022
eng
1
13
article
Wiley-VCH-Verlag
Weinheim, Germany
1
--
--
--
Quantification of the Activator and Sensitizer Ion Distributions in NaYF4:Yb3+, Er3+ Upconverting Nanoparticles Via Depth-Profiling with Tender X-Ray Photoemission
The spatial distribution and concentration of lanthanide activator and sensitizer dopant ions are of key importance for the luminescence color and efficiency of upconverting nanoparticles (UCNPs). Quantifying dopant ion distributions and intermixing, and correlating them with synthesis methods require suitable analytical techniques. Here, X-ray photoelectron spectroscopy depth-profiling with tender X-rays (2000–6000 eV), providing probe depths ideally matched to UCNP sizes, is used to measure the depth-dependent concentration ratios of Er3+ to Yb3+, [Er3+]/[Yb3+], in three types of UCNPs prepared using different reagents and synthesis methods. This is combined with data simulations and inductively coupled plasma-optical emission spectroscopy (ICP-OES) measurements of the lanthanide ion concentrations to construct models of the UCNPs’ dopant ion distributions. The UCNP sizes and architectures are chosen to demonstrate the potential of this approach. Core-only UCNPs synthesized with XCl3·6H2O precursors (β-phase) exhibit a homogeneous distribution of lanthanide ions, but a slightly surface-enhanced [Er3+]/[Yb3+] is observed for UCNPs prepared with trifluroacetate precursors (α-phase). Examination of Yb-core@Er-shell UCNPs reveals a co-doped, intermixed region between the single-doped core and shell. The impact of these different dopant ion distributions on the UCNP's optical properties is discussed to highlight their importance for UCNP functionality and the design of efficient UCNPs.
Small
10.1002/smll.202107976
1613-6813
urn:nbn:de:kobv:b43-552075
publish
07.07.2022
false
true
Creative Commons - CC BY - Namensnennung 4.0 International
P.C.J Clark
Elina Andresen
M. J. Sear
M. Favaro
L. Girardi
R. van de Krol
Ute Resch-Genger
D.E. Starr
eng
uncontrolled
Shell
eng
uncontrolled
Nanomaterial
eng
uncontrolled
Nano
eng
uncontrolled
Upconversion nanoparticle
eng
uncontrolled
Lanthanide
eng
uncontrolled
Photoluminescence
eng
uncontrolled
Quantum yield
eng
uncontrolled
Photophysics
eng
uncontrolled
Excitation power density
eng
uncontrolled
Surface
eng
uncontrolled
Coating
eng
uncontrolled
Core-shell
eng
uncontrolled
XPS
eng
uncontrolled
Intermixing
eng
uncontrolled
HAXPES
eng
uncontrolled
Method
Analytische Chemie
1 Analytische Chemie; Referenzmaterialien
1.2 Biophotonik
Material
Chemie und Prozesstechnik
Verlagsliteratur
Datei für die Öffentlichkeit verfügbar ("Open Access")
Wissenschaftliche Artikel der BAM
Nano
Bundesanstalt für Materialforschung und -prüfung (BAM)
https://opus4.kobv.de/opus4-bam/files/55207/Clark_EA_Small 2022_Quantification of the Activator and Sensitizer Ion Distributions.pdf
55272
2022
eng
1203
1207
6
37
article
Royal Society of Chemistry
1
--
--
--
Size determination of nanoparticles by ICP-ToF-MS using isotope dilution in microdroplets
Within this work, the combination of a microdroplet generator and an ICP-ToF-MS for nanoparticle analysis is presented. For the size determination of platinum nanoparticles an on-line isotope dilution analysis approach was developed. The 194Pt/195Pt isotopic ratio was used for the characterization of the particles, while the 182W/183W isotopic ratio was monitored simultaneously for mass bias correction. The on-line ID-MDG-sp-ICP-ToF-MS approach was deployed for the size determination of three platinum nanoparticle samples (50 nm, 63 nm, 70 nm); for validation, complementary size characterization techniques (sp-ICP-ToF-MS and TEM) were used. The robustness of this technique was evidenced, by using sodium chloride concentrations up to 100 mg L−1 as a matrix component. Our new on-line ID MDG-sp-ICP-ToF-MS approach is a promising tool for the fast and reliable determination of nanoparticles' size in severe matrix concentrations, e.g., environmental samples.
Journal of Analytical Atomic Spectrometry
10.1039/D2JA00072E
0267-9477
urn:nbn:de:kobv:b43-552727
publish
13.07.2022
false
true
Creative Commons - CC BY - Namensnennung 4.0 International
Marcus von der Au
Sebastian Faßbender
Michail Chronakis
Jochen Vogl
Björn Meermann
eng
uncontrolled
ICP-ToF-MS
eng
uncontrolled
Nanoparticles
eng
uncontrolled
Isotope Dilution
Analytische Chemie
1 Analytische Chemie; Referenzmaterialien
1.1 Anorganische Spurenanalytik
Chemie und Prozesstechnik
Chemische Charakterisierung und Spurenanalytik
Verlagsliteratur
Datei für die Öffentlichkeit verfügbar ("Open Access")
Wissenschaftliche Artikel der BAM
Bundesanstalt für Materialforschung und -prüfung (BAM)
https://opus4.kobv.de/opus4-bam/files/55272/JAAS2022.pdf
54972
2021
eng
08001
1A
59
article
0
--
--
--
PAWG Pilot Study on Quantification of SARS-CoV-2 Monoclonal Antibody - Part 1
Under the auspices of the Protein Analysis Working Group (PAWG) of the Comité Consultatif pour la Quantité de Matière (CCQM) a pilot study, CCQM-P216, was coordinated by the Chinese National Institute of Metrology (NIM), National Research Council of Canada (NRC) and the Bureau International des Poids et Mesures (BIPM). Eleven Metrology Institutes or Designated Institutes and the BIPM participated in the first phase of the pilot study (Part 1). The purpose of this pilot study was to develop measurement capabilities for larger proteins using a recombinant humanized IgG monoclonal antibody against Spike glycoprotein of SARS-CoV-2 (Anti-S IgG mAb) in solution. The first phase of the study was designed to employ established methods that had been previously studies by the CCQM Protein Analysis Working Group, involving the digestion of protein down to the peptide or amino acid level. The global coronavirus pandemic has also led to increased focus on antibody quantitation methods. IgG are among the immunoglobulins produced by the immune system to provide protection against SARS-CoV-2. Anti-SARS-CoV-2 IgG can therefore be detected in samples from affected patients. Antibody tests can show whether a person has been exposed to the SARS-CoV-2, and whether or not they potentially show lasting immunity to the disease. With the constant spread of the virus and the high pressure of re-opening economies, antibody testing plays a critical role in the fight against COVID-19 by helping healthcare professionals to identify individuals who have developed an immune response, either via vaccination or exposure to the virus. Many countries have launched large-scale antibody testing for COVID-19. The development of measurement standards for the antibody detection of SARS-CoV-2 is critically important to deal with the challenges of the COVID-19 pandemic. In this study, the SARS-CoV-2 monoclonal antibody is being used as a model system to build capacity in methods that can be used in antibody quantification. Amino acid reference values with corresponding expanded uncertainty of 36.10 ± 1.55 mg/kg, 38.75 ± 1.45 mg/kg, 18.46 ± 0.78 mg/kg, 16.20 ± 0.67 mg/kg and 30.61 ± 1.30 mg/kg have been established for leucine, valine, phenylalanine, isoleucine and proline, respectively. Agreement between nearly all laboratories was achieved for the amino acid analysis within 2 to 2.5 %, with one participant achieving markedly higher results due to a technical issue found in their procedure; this result was thus excluded from the reference value calculations. The relatively good agreement within a laboratory between different amino acids was not dissimilar to previous results for peptides or small proteins, indicating that factors such as hydrolysis conditions and calibration procedures could be the largest sources of variability. Peptide reference values with corresponding expanded uncertainty of 4.99 ± 0.28 mg/kg and 6.83 ± 0.65 mg/kg have been established for ALPAPIEK and GPSVFPLAPSSK, respectively. Not surprisingly due to prior knowledge from previous studies on peptide quantitation, agreement between laboratories for the peptide-based analysis was slightly poorer at 3 to 5 %, with one laboratory's result excluded for the peptide GPSVFPLAPSSK. Again, this level of agreement was not significantly poorer than that achieved in previous studies with smaller or less complex proteins. To reach the main text of this paper, click on Final Report.
Metrologia
10.1088/0026-1394/59/1a/08001
publish
false
true
W. Mi
R. D. Josephs
J. E. Melanson
X. Dai
Y. Wang
R. Zhai
Z. Chu
X. Fang
M.-P. Thibeault
B. B. Stocks
J. Meija
M. Bedu
G. Martos
S. Westwood
R. I. Wielgosz
Q. Liu
T. L. Teo
H. Liu
Y. J. Tan
M. Öztuğ
E. Saban
T. Kinumi
K. Saikusa
Rudolf Schneider
Michael G. Weller
Zoltán Konthur
Carsten Jaeger
M. Quaglia
C. Mussell
G. Drinkwater
C. Giangrande
H. Vaneeckhoutte
A. Boeuf
V. Delatour
J. E. Lee
G. O'Connor
R. Ohlendorf
A. Henrion
P. J. Beltrão
S. M. Naressi Scapin
Y. B. Sade
deu
uncontrolled
Antibody quantification
deu
uncontrolled
Amino acid analysis
deu
uncontrolled
Peptide analysis
deu
uncontrolled
Round robin test
Analytische Chemie
1 Analytische Chemie; Referenzmaterialien
1.5 Proteinanalytik
1.8 Umweltanalytik
Chemie und Prozesstechnik
Chemische Charakterisierung und Spurenanalytik
Verlagsliteratur
Datei im Netzwerk der BAM verfügbar ("Closed Access")
54973
2022
eng
1
8
3
17
article
AVS
1
--
--
--
In-depth analysis of iodine in artificial biofilm model layers by variable excitation energy XPS and argon gas cluster ion sputtering XPS
Here, we present a study on agarose thin-film samples that represent a model system for the exopolysaccharide matrix of biofilms. Povidone-iodide (PVP-I) was selected as an antibacterial agent to evaluate our x-ray photoelectron spectroscopy (XPS)-based methodology to trace specific marker elements, here iodine, commonly found in organic matrices of antibiotics. The in-depth distribution of iodine was determined by XPS analyses with variable excitation energies and in combination with argon gas cluster ion beam sputter cycles. On mixed agarose/PVP-I nanometer-thin films, both methods were found to solve the analytical task and deliver independently comparable results. In the mixed agarose/PVP-I thin film, we found the outermost surface layer depleted in iodine, whereas the iodine is homogeneously distributed in the depth region between this outermost surface layer and the interface between the thin film and the substrate. Depletion of iodine from the uppermost surface in the thin-film samples is assumed to be caused by ultrahigh vacuum exposure resulting in a loss of molecular iodine (I2) as reported earlier for other iodine-doped polymers.
Biointerphases
10.1116/6.0001812
1934-8630
publish
09.06.2022
false
true
P. M. Dietrich
Marit Kjærvik
E. A. Willneff
Wolfgang Unger
eng
uncontrolled
Biofilm
eng
uncontrolled
XPS
eng
uncontrolled
Argon gas cluster ion sputtering
eng
uncontrolled
Variable excitation
eng
uncontrolled
Iodine
Analytische Chemie
Ingenieurwissenschaften und zugeordnete Tätigkeiten
6 Materialchemie
6.1 Oberflächen- und Dünnschichtanalyse
Material
Chemie und Prozesstechnik
Verlagsliteratur
Datei im Netzwerk der BAM verfügbar ("Closed Access")
Nano
54983
2022
eng
14461
14477
9
30
article
Optica
Washington, DC
1
--
--
--
Compact and versatile neutron imaging detector with sub-4μm spatial resolution based on a single-crystal thin-film scintillator
A large and increasing number of scientific domains pushes for high neutron imaging resolution achieved in reasonable times. Here we present the principle, design and performance of a detector based on infinity corrected optics combined with a crystalline Gd3Ga5O12 : Eu scintillator, which provides an isotropic sub-4 μm true resolution. The exposure times are only of a few minutes per image. This is made possible also by the uniquely intense cold neutron flux available at the imaging beamline NeXT-Grenoble. These comparatively rapid acquisitions are compatible with multiple high quality tomographic acquisitions, opening new venues for in-operando testing, as briefly exemplified here.
Optics Express
10.1364/oe.448932
urn:nbn:de:kobv:b43-549836
publish
09.06.2022
Creative Commons - CC BY - Namensnennung 4.0 International
A Tengattini
N Kardjilov
L Helfen
P A Douissard
N Lenoir
Henning Markötter
A Hilger
T Arlt
M Paulisch
T Turek
Ingo Manke
eng
uncontrolled
Neutron imaging
eng
uncontrolled
Scintillator
eng
uncontrolled
Resolution
Analytische Chemie
8 Zerstörungsfreie Prüfung
8.5 Röntgenbildgebung
Chemie und Prozesstechnik
Verlagsliteratur
Datei für die Öffentlichkeit verfügbar ("Open Access")
Wissenschaftliche Artikel der BAM
Bundesanstalt für Materialforschung und -prüfung (BAM)
https://opus4.kobv.de/opus4-bam/files/54983/final_high-res_n-detector.pdf