scholarly journals Validation of XRD phase quantification using semi-synthetic data

2020 ◽  
Vol 35 (4) ◽  
pp. 262-275
Author(s):  
Nicola Döbelin
Keyword(s):  
Reference Materials ◽  
Certified Reference Materials ◽  
Synthetic Data ◽  
Statistical Validation ◽  
Validation Parameters ◽  
Phase Quantification ◽  
Characteristic Features ◽  
Diffraction Patterns ◽  
Synthetic Datasets ◽  
Multi Phase

Validating phase quantification procedures of powder X-ray diffraction (XRD) data for an implementation in an ISO/IEC 17025 accredited environment has been challenging due to a general lack of suitable certified reference materials. The preparation of highly pure and crystalline reference materials and mixtures thereof may exceed the costs for a profitable and justifiable implementation. This study presents a method for the validation of XRD phase quantifications based on semi-synthetic datasets that reduces the effort for a full method validation drastically. Datasets of nearly pure reference substances are stripped of impurity signals and rescaled to 100% crystallinity, thus eliminating the need for the preparation of ultra-pure and -crystalline materials. The processed datasets are then combined numerically while preserving all sample- and instrument-characteristic features of the peak profile, thereby creating multi-phase diffraction patterns of precisely known composition. The number of compositions and repetitions is only limited by computational power and storage capacity. These datasets can be used as input files for the phase quantification procedure, in which statistical validation parameters such as precision, accuracy, linearity, and limits of detection and quantification can be determined from a statistically sound number of datasets and compositions.

Development of reference materials with the composition of propyl and isopropyl alcohol solutions

2020 ◽  
pp. 66-72
Author(s):  
Irina A. Piterskikh ◽  
Svetlana V. Vikhrova ◽  
Nina G. Kovaleva ◽  
Tatyana O. Barynskaya
Keyword(s):  
Reference Materials ◽  
Measurement Errors ◽  
Isopropyl Alcohol ◽  
Certified Reference Materials ◽  
Toxic Substances ◽  
Biological Objects ◽  
Margin Of Error ◽  
Measurement Results ◽  
And Control ◽  
Characteristic Mass

Certified reference materials (CRM) composed of propyl (11383-2019) and isopropyl (11384-2019) alcohols solutions were created for validation of measurement procedures and control of measurement errors of measurement results of mass concentrations of toxic substances (alcohol) in biological objects (urine, blood) and water. Two ways of establishing the value of the certified characteristic – mass consentration of propanol-1 or propanol-2 have been studied. The results obtained by the preparation procedure and comparison with the standard are the same within the margin of error.

scholarly journals G-Tric: generating three-way synthetic datasets with triclustering solutions

2021 ◽  
Vol 22 (1) ◽  
Author(s):  
João Lobo ◽  
Rui Henriques ◽  
Sara C. Madeira
Keyword(s):  
State Of The Art ◽  
Synthetic Data ◽  
Ground Truth ◽  
Real Data ◽  
Three Dimensions ◽  
Additional Advantage ◽  
Urban Dynamics ◽  
Data Generator ◽  
Real World Datasets ◽  
Synthetic Datasets

Abstract Background Three-way data started to gain popularity due to their increasing capacity to describe inherently multivariate and temporal events, such as biological responses, social interactions along time, urban dynamics, or complex geophysical phenomena. Triclustering, subspace clustering of three-way data, enables the discovery of patterns corresponding to data subspaces (triclusters) with values correlated across the three dimensions (observations $$\times$$ × features $$\times$$ × contexts). With increasing number of algorithms being proposed, effectively comparing them with state-of-the-art algorithms is paramount. These comparisons are usually performed using real data, without a known ground-truth, thus limiting the assessments. In this context, we propose a synthetic data generator, G-Tric, allowing the creation of synthetic datasets with configurable properties and the possibility to plant triclusters. The generator is prepared to create datasets resembling real 3-way data from biomedical and social data domains, with the additional advantage of further providing the ground truth (triclustering solution) as output. Results G-Tric can replicate real-world datasets and create new ones that match researchers needs across several properties, including data type (numeric or symbolic), dimensions, and background distribution. Users can tune the patterns and structure that characterize the planted triclusters (subspaces) and how they interact (overlapping). Data quality can also be controlled, by defining the amount of missing, noise or errors. Furthermore, a benchmark of datasets resembling real data is made available, together with the corresponding triclustering solutions (planted triclusters) and generating parameters. Conclusions Triclustering evaluation using G-Tric provides the possibility to combine both intrinsic and extrinsic metrics to compare solutions that produce more reliable analyses. A set of predefined datasets, mimicking widely used three-way data and exploring crucial properties was generated and made available, highlighting G-Tric’s potential to advance triclustering state-of-the-art by easing the process of evaluating the quality of new triclustering approaches.

PROGRESS ON THE DEVELOPMENT OF CERTIFIED REFERENCE MATERIALS FOR Aβ1-42

2017 ◽  
Vol 13 (7) ◽  
pp. P1512
Author(s):  
Sébastien Boulo ◽  
Julia Kuhlmann ◽  
Andreas Leinenbach ◽  
Tobias Bittner ◽  
Leentje Demeyer ◽  
...  
Keyword(s):  
Reference Materials ◽  
Certified Reference Materials

scholarly journals Development and certification of a reference material for zearalenone in maize germ oil

2021 ◽  
Author(s):  
Juliane Riedel ◽  
Sebastian Recknagel ◽  
Diana Sassenroth ◽  
Tatjana Mauch ◽  
Sabine Buttler ◽  
...  
Keyword(s):  
Reference Material ◽  
Reference Materials ◽  
Mass Fraction ◽  
High Performance ◽  
Certified Reference Materials ◽  
Maximum Level ◽  
Whole Process ◽  
Commission Regulation ◽  
Maize Oil ◽  
Maize Germ

AbstractZearalenone (ZEN), an estrogenic mycotoxin produced by several species of Fusarium fungi, is a common contaminant of cereal-based food worldwide. Due to frequent occurrences associated with high levels of ZEN, maize oil is a particular source of exposure. Although a European maximum level for ZEN in maize oil exists according to Commission Regulation (EC) No. 1126/2007 along with a newly developed international standard method for analysis, certified reference materials (CRM) are still not available. To overcome this lack, the first CRM for the determination of ZEN in contaminated maize germ oil (ERM®-BC715) was developed in the frame of a European Reference Materials (ERM®) project according to the requirements of ISO Guide 35. The whole process of CRM development including preparation, homogeneity and stability studies, and value assignment is presented. The assignment of the certified mass fraction was based upon an in-house study using high-performance liquid chromatography isotope dilution tandem mass spectrometry. Simultaneously, to support the in-house certification study, an interlaboratory comparison study was conducted with 13 expert laboratories using different analytical methods. The certified mass fraction and expanded uncertainty (k = 2) of ERM®-BC715 (362 ± 22) μg kg−1 ZEN are traceable to the SI. This reference material is intended for analytical quality control and contributes to the improvement of consumer protection and food safety. Graphical abstract

Development of Certified Reference Materials for Diarrhetic Shellfish Poisoning Toxins, Part 2: Shellfish Matrix Materials

2016 ◽  
Vol 99 (5) ◽  
pp. 1163-1172 ◽  
Author(s):  
Pearse McCarron ◽  
Kelley L Reeves ◽  
Sabrina D Giddings ◽  
Daniel G Beach ◽  
Michael A Quilliam
Keyword(s):  
Reference Materials ◽  
Matrix Effects ◽  
Certified Reference Materials ◽  
Standard Addition ◽  
Tissue Homogenate ◽  
Shellfish Poisoning ◽  
Diarrhetic Shellfish Poisoning ◽  
Preliminary Work ◽  
Seafood Industry ◽  
Human Illness

Abstract Okadaic acid (OA) and its analogs, dinophysistoxins-1 (DTX1) and -2 (DTX2) are lipophilic biotoxins produced by marine algae that can accumulate in shellfish and cause the human illness known as diarrhetic shellfish poisoning (DSP). Regulatory testing of shellfish is required to protect consumers and the seafood industry. Certified reference materials (CRMs) are essential for the development, validation, and quality control of analytical methods, and thus play an important role in toxin monitoring. This paper summarizes work on research and development of shellfish tissue reference materials for OA and DTXs. Preliminary work established the appropriate conditions for production of shellfish tissue CRMs for OA and DTXs. Source materials, including naturally incurred shellfish tissue and cultured algae, were screened for their DSP toxins. This preliminary work informed planning and production of a wet mussel (Mytilus edulis) tissue homogenate matrix CRM. The homogeneity and stability of the CRM were evaluated and found to be fit-for-purpose. Extraction and LC-tandem MS methods were developed to accurately certify the concentrations of OA, DTX1, and DTX2 using a combination of standard addition and matrix-matched calibration to compensate for matrix effects in electrospray ionization. The concentration of domoic acid was also certified. Uncertainties were assigned following standards and guidelines from the International Organization for Standardization. The presence of other toxins in the CRM was also assessed and information values are reported for OA and DTX acyl esters.

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