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  • 文章类型: Journal Article
    在这项工作中,我们提出了一种从工业聚合物生产模型微塑料的新协议,并将其与传统方法进行比较,冷冻研磨。选择聚丙烯工业颗粒是由于其广泛的生产和频繁存在于环境中,使它们成为微塑料的重要来源。两种方案都从颗粒在紫外光下的老化开始,但在随后施加的机械应力方面有所不同-强与软-将光降解颗粒分解成微塑料。所有产生的颗粒都在尺寸方面得到了充分的表征,形状,氧化速率,在水介质中的稳定性。通过低温研磨生产的微塑料表现出明显的尺寸和氧化异质性,并倾向于在水中聚集。尽管涉及软机械应力的新方案需要更长的准备时间,它更准确地模拟了原塑料的环境降解。该方法成功地生产了具有受控尺寸分布的氧化微塑料,该尺寸分布在50μm左右,在没有稳定剂的情况下在水中保持稳定。
    In this work, we propose a new protocol for producing model microplastics from an industrial polymer and compare it to a conventional method, cryomilling. Polypropylene industrial pellets were chosen due to their widespread production and frequent presence in the environment, making them a notable source of microplastics. Both protocols start with aging under Ultra-Violet light of the pellets but differ in the subsequent mechanical stress applied-strong vs. soft-to break down the photodegraded pellets into microplastics. All generated particles were fully characterized in terms of size, shape, oxidation rate, and stability in aqueous media. Microplastics produced via cryomilling exhibited significant size and oxidation heterogeneity and tended to aggregate in water. Although the new protocol involving soft mechanical stress required a longer preparation time, it simulated more accurately the environmental degradation of raw plastic. This method successfully produced oxidized microplastics with a controlled size distribution centered around 50 µm which remained stable in water without stabilizers.
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  • 文章类型: Journal Article
    由于覆盖间隔是广泛使用的测量不确定度的表达式,本贡献回顾了《测量不确定度表达指南》(GUM)中定义的覆盖间隔,并将它们与应用统计学和测量科学中常用的概率区间的主要类型进行比较。虽然形式上与传统的均值置信区间相同,GUM将覆盖间隔更多地解释为贝叶斯可信间隔,或公差间隔。我们专注,特别是,关于从GUM补充1(GUM-S1)的蒙特卡洛方法的结果得出的间隔的常见误解,并为这些间隔提供新颖的解释,我们相信这将培养人们对它们能提供什么的现实期望,以及它们如何以及何时在实践中有用。
    Since coverage intervals are widely used expressions of measurement uncertainty, this contribution reviews coverage intervals as defined in the Guide to the Expression of Uncertainty in Measurement (GUM), and compares them against the principal types of probabilistic intervals that are commonly used in applied statistics and in measurement science. Although formally identical to conventional confidence intervals for means, the GUM interprets coverage intervals more as if they were Bayesian credible intervals, or tolerance intervals. We focus, in particular, on a common misunderstanding about the intervals derived from the results of the Monte Carlo method of the GUM Supplement 1 (GUM-S1), and offer a novel interpretation for these intervals that we believe will foster realistic expectations about what they can deliver, and how and when they can be useful in practice.
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  • 文章类型: Journal Article
    全球的土壤环境,特别是在农业环境中,现在已经被证明被微塑料污染了。农业塑料-例如地膜-用于与土壤紧密或直接接触,越来越多的证据表明它们是微塑料的潜在来源。需要进行命运和影响研究,以了解这种污染的行为和潜在的长期生态风险。然而,缺乏可用于此目的的测试材料。这项研究描述了五批大型(1-40kg)来自农业地膜的微塑料测试材料的制造和表征。批次由基于聚乙烯的常规覆盖膜或淀粉-聚丁二烯己二酸酯对苯二甲酸酯共混物覆盖膜生产,这些覆盖膜在土壤中被证明是可生物降解的。在微粉化过程中遇到和克服的挑战为从这些材料类型生成微塑料测试材料的未来提供了有价值的见解。这包括将原始聚乙烯薄膜材料微粉化的困难。所有五个批次都进行了彻底的物理和化学表征-原始原膜和随后产生的微塑料颗粒-包括筛选化学添加剂的存在。这是提供必要信息以解释科学测试中的粒子命运或影响的关键步骤。阐明了获得首选粒子类型与时间和成本限制之间的权衡。从这项研究中获得的经验中提出了一些建议,以推动研究领域朝着与环境相关的测试材料的更大协调和利用方向发展。
    Soil environments across the globe, particularly in agricultural settings, have now been shown to be contaminated with microplastics. Agricultural plastics - such as mulching films - are used in close or direct contact with soils and there is growing evidence demonstrating that they represent a potential source of microplastics. There is a demand to undertake fate and effects studies to understand the behaviour and potential long-term ecological risks of this contamination. Yet, there is a lack of test materials available for this purpose. This study describes the manufacture and characterisation of five large (1-40 kg) batches of microplastic test materials derived from agricultural mulching films. Batches were produced from either polyethylene-based conventional mulching films or starch-polybutadiene adipate terephthalate blend mulching films that are certified biodegradable in soil. Challenges encountered and overcome during the micronisation process provide valuable insights into the future of microplastic test material generation from these material types. This includes difficulties in micronising virgin polyethylene film materials. All five batches were subjected to a thorough physical and chemical characterisation - both of the original virgin films and the subsequent microplastic particles generated - including a screening for the presence of chemical additives. This is a critical step to provide essential information for interpreting particle fate or effects in scientific testing. Trade-offs between obtaining preferred particle typologies and time and cost constraints are elucidated. Several recommendations emerging from the experiences gained in this study are put forward to advance the research field towards greater harmonisation and utilisation of environmentally relevant test materials.
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  • 文章类型: English Abstract
    OBJECTIVE: To assess the adequacy of linear function of calibration according to GOST R ISO 11095-2007 for ethanol mass concentration measurement using internal reference materials (RMs).
    METHODS: An experiment on calibration in accordance with the GOST R ISO 11095-2007 National standard of the RF was carried out using internal RMs, namely aqueous solutions of ethanol at different concentrations. Measurements were performed for two subbands of ethanol concentrations at RMs: 0.15-1.05 and 1.0-7.0 mg/ml - according to the certified methodology.
    RESULTS: The graphs of the calibration\'s functions based on experimental data are consistent with the assumption of the calibration function\'s linearity, as well as the assumption of the standard deviation\'s constance of residues is equitable for two subbands of RMs.
    CONCLUSIONS: Proven linear models in the calibration experiment may be recommended for use in the ethanol mass concentration measurement.
    UNASSIGNED: Оценка адекватности линейной функции калибровки по ГОСТ Р ИСО 11095-2007 для измерения массовой концентрации этанола с применением внутренних образцов сравнения (Reference Material, RM).
    UNASSIGNED: Проведен эксперимент по калибровке в соответствии с Национальным стандартом РФ ГОСТ Р ИСО 11095-2007 с применением внутренних RM — водных растворов этанола в разных концентрациях. Измерения выполняли для двух поддиапазонов концентраций этанола на RM: 0,15—1,05 и 1,0—7,0 мг/мл — в соответствии с аттестованной методикой.
    UNASSIGNED: Графики функций калибровки, построенные по экспериментальным данным, согласуются с предположением о линейности функции калибровки, а также предположение о постоянстве стандартного отклонения остатков является справедливым для двух поддиапазонов RM.
    UNASSIGNED: Подтвержденные линейные модели в ходе эксперимента по калибровке могут быть рекомендованы к применению на практике для измерения массовой концентрации этанола.
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  • 文章类型: Journal Article
    定期监测诺如病毒在环境和食物样本中的存在至关重要,因为它的高传播率和爆发潜力。为了检测诺如病毒GI,逆转录qPCR方法是常用的,但其灵敏度会受到检测性能的影响。这项研究显示,当使用针对诺如病毒GI基因组5291-5319(NC_001959)的引物时,数字PCR或qPCR的检测性能显着降低,位于预测的RNA结构的发夹上。强烈建议在商业试剂盒开发或诊断中避免该区域,以最大程度地减少假阴性的潜在风险。
    Regular monitoring of Norovirus presence in environmental and food samples is crucial due to its high transmission rates and outbreak potential. For detecting Norovirus GI, reverse transcription qPCR method is commonly used, but its sensitivity can be affected by assay performance. This study shows significantly reduced assay performance in digital PCR or qPCR when using primers targeting Norovirus GI genome 5291-5319 (NC_001959), located on the hairpin of the predicted RNA structure. It is highly recommended to avoid this region in commercial kit development or diagnosis to minimizing potential risk of false negatives.
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  • 文章类型: Journal Article
    tri的复杂行为和环境中释放的tri浓度增加的可能性是实验室方法研究和开发的促进剂,该方法能够准确确定各种形式的tri,包括有机结合的tri(OBT),以用于公共和监管保证。tri的测量是剂量和风险评估的关键步骤。罗马尼亚的Cernavoda核电站(NPP)改进了制备方法,并通过相互比较练习测试了用于OBT分析的环境矩阵。本文介绍了国际有机结合氚(OBT)比对练习,由Cernavoda核电站(NPP)于2019-2020年组织,使用来自Cernavoda镇的水果样品(quince)。使用ISO13528:2015标准中描述的稳健分析(算法A)方法和ANOVA方法进行来自参与实验室的结果的评估。获得的结果令人鼓舞,因为参与实验室数量的增加并未改变在50Bq/L燃烧水的活性浓度水平下观察到的结果分散性。将及时检查剩余样品的稳定性,以研究其在环境水平上用作OBT分析的参考材料。
    The complex behavior of tritium and the probability of increasing tritium concentrations released in the environment were the promotors for the research and development of laboratory methods that enable to accurately determine the various forms of tritium including organically-bound tritium (OBT) for public and regulatory assurance. The measurement of tritium is a key step for dose and risk assessment. The Cernavoda Nuclear Power Plant (NPP) in Romania improved preparation methods and tested environmental matrices for OBT analysis through intercomparison exercises. This paper describes the international Organically-Bound Tritium (OBT) intercomparison exercise, organized by the Cernavoda Nuclear Power Plant (NPP) in 2019-2020, using fruit sample (quince) from Cernavoda town. Evaluation of the results from the participating laboratories was performed using both robust analysis (Algorithm A) method described in the ISO 13528:2015 standard and ANOVA method. The results obtained are encouraging as an increased number of participating laboratories did not change the observed dispersion of the results for activity concentration level around 50 Bq/L of combustion water. The stability of the remaining sample will be checked in time to investigate its use as a reference material for OBT analysis at the environmental levels.
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  • 文章类型: Journal Article
    血糖仪为循证诊断提供快速的血糖状态,监测,和糖尿病的治疗。我们旨在评估经处理的血液材料(PBM)的可交换性及其在血糖仪性能评估中的用途。分析了通过固定细胞方法获得的两个PBM的同质性,稳定性,和可交换性。质谱和每个血糖仪之间的十对相容性被分类为相容(平均配对差异≤5%)和不相容(平均配对差异>5%)。评估葡萄糖计1(n=767)和葡萄糖计2(n=266)的性能。PBM中的葡萄糖保持均质化和稳定至少180天。十分之六具有可交换的PBM。在良好相容和不相容的葡萄糖结果中观察到PBM的可交换性。来自质谱的目标葡萄糖值与一组葡萄糖计的一致值显着不同(p≤0.05)。当使用可交换的PBM时,血糖仪1表现出比血糖仪2更好的性能,并且当使用来自质谱和共识值的葡萄糖目标值时,满意度百分比是相关的,但与血糖仪2的性能无关。来自固定电池方法的PBM可以以可接受的均匀性和稳定性大量生产。在血糖仪的性能评估中使用之前,需要对PBMs进行可交换性测试。因为通过固定细胞方法获得的PBMs中葡萄糖的可交换性是可变的,并且取决于单个血糖仪。
    Glucose meters provide a rapid blood glucose status for evidence-based diagnosis, monitoring, and treatment of diabetes mellitus. We aimed to evaluate the commutability of processed blood materials (PBMs) and their use in the performance evaluation of glucose meters. Two PBMs obtained by the fixed-cell method were analyzed for homogeneity, stability, and commutability. The compatibility of ten pairs between mass spectrometry and each glucose meter was categorized as compatible (mean paired difference ≤ 5%) and incompatible (mean paired difference > 5%). The performance of glucose meter 1 (n = 767) and glucose meter 2 (n = 266) was assessed. The glucose in the PBMs remained homogenized and stable for at least 180 days. Six out of ten pairs had commutable PBMs. Commutability of PBMs was observed in both well-compatible and incompatible glucose results. Target glucose values from mass spectrometry were significantly different (p ≤ 0.05) from consensus values in one group of glucose meters. When commutable PBMs were used, glucose meter 1 showed better performance than glucose meter 2, and the percentage of satisfaction was associated when using target values for glucose from mass spectrometry and consensus values, but the performance of glucose meter 2 was not associated. PBM from a fixed-cell method could be mass produced with acceptable homogeneity and stability. Commutability testing of PBMs is required prior to use in the performance evaluation of glucose meters, as the commutability of glucose in the PBMs obtained by a fixed-cell method was variable and depended on the individual glucose meter.
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  • 文章类型: Journal Article
    N末端B型利钠肽原(NT-proBNP)是心力衰竭(HF)诊断和预后的重要生物标志物。然而,没有SI可追溯的认证参考材料(CRM)或参考测量程序(RMP)可用于此生物标志物,因此,在不同实验室获得的临床试验结果不能追溯到更高的标准,导致无与伦比的测量。蛋白质水解和蛋白质裂解同位素稀释质谱(AAA-IDMS和PepA-IDMS)用于开发CRM。通过高分辨率质谱鉴定结构相关的杂质。根据杂质的氨基酸组成校正定量AAA-IDMS结果。使用PepA-IDMS,来自蛋白水解产物的两种肽被证实为特征肽。为了获得可追溯和准确的结果,使用杂质校正的AAA-IDMS对特征肽进行定量.将候选NT-proBNP溶液变性并使用Glu-C内切蛋白酶酶消化。使用同位素稀释方法测量释放的特征肽。对候选CRM的均匀性和稳定性进行了表征,并将其不确定性与价值分配过程相结合。开发的CRM可以被认为是独特的SI可追溯的NT-proBNP参考材料,并有望用作矩阵NT-proBNPCRM开发的主要校准物。
    N-Terminal pro-B-type natriuretic peptide (NT-proBNP) is a pivotal biomarker for the diagnosis and prognosis of heart failure (HF). However, no SI-traceable certified reference material (CRM) or reference measurement procedure (RMP) is available for this biomarker, and so clinical testing results obtained in different laboratories cannot be traced to a higher-order standard, leading to incomparable measurements. Protein hydrolysis and protein cleavage isotope dilution mass spectrometry (AAA-IDMS and PepA-IDMS) were used to develop a CRM. Structurally related impurities were identified by high-resolution mass spectrometry. The quantitative AAA-IDMS results were corrected according to the amino acid compositions of the impurities. Using PepA-IDMS, two peptides from the proteolyzed product were confirmed as signature peptides. To obtain traceable and accurate results, the signature peptides were quantified using impurity-corrected AAA-IDMS. The candidate NT-proBNP solution was denatured and enzymatically digested using the Glu-C endoproteinase. The released signature peptides were measured using an isotopic dilution approach. The homogeneity and stability of the candidate CRM were characterized, and their uncertainties were combined with the value assignment process. The developed CRM can be considered a unique SI-traceable NT-proBNP reference material and is expected to be used as a primary calibrator for matrix NT-proBNP CRM development.
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  • 文章类型: Journal Article
    对饮用水和环境样品中微塑料颗粒的尺寸分辨识别和定量的需求不断增加,需要对可用于此目的的方法和技术进行充分验证。反过来,这种验证的可行性取决于是否存在合适的认证参考材料(CRM)。新的候选参考材料(RM),由聚对苯二甲酸乙二醇酯(PET)颗粒和水基质组成,已经开发了。这里,我们检查了其在各个单位中均匀和稳定的微塑料颗粒数浓度方面的适用性。采用定制软件进行颗粒自动计数和分析的测量系列(TUM-ParticleTyper2)与拉曼显微光谱法相结合,显示了候选RM均一性的证据,其中PET颗粒计数的相对标准偏差为12%,涉及粒径>30μm。在所有选择的候选RM单位中,不同尺寸类别内的总颗粒计数和各自的总和都是可比的。我们证明了生产相对于颗粒数浓度足够均匀且稳定的参考材料的可行性。
    Increasing demand for size-resolved identification and quantification of microplastic particles in drinking water and environmental samples requires the adequate validation of methods and techniques that can be used for this purpose. In turn, the feasibility of such validation depends on the existence of suitable certified reference materials (CRM). A new candidate reference material (RM), consisting of polyethylene terephthalate (PET) particles and a water matrix, has been developed. Here, we examine its suitability with respect to a homogeneous and stable microplastic particle number concentration across its individual units. A measurement series employing tailor-made software for automated counting and analysis of particles (TUM-ParticleTyper 2) coupled with Raman microspectroscopy showed evidence of the candidate RM homogeneity with a relative standard deviation of 12% of PET particle counts involving particle sizes >30 µm. Both the total particle count and the respective sums within distinct size classes were comparable in all selected candidate RM units. We demonstrate the feasibility of production of a reference material that is sufficiently homogeneous and stable with respect to the particle number concentration.
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  • 文章类型: Journal Article
    D-二聚体是凝血和纤溶活性的敏感指标,作为血管内血栓形成的生物标志物尤其有价值。血浆D-二聚体水平的测定在深静脉血栓形成等疾病的诊断和监测中起着至关重要的作用。肺栓塞,和弥散性血管内凝血。各种免疫测定,包括酶联免疫吸附测定,乳胶增强免疫比浊法,全血聚集分析,和免疫层析分析,在临床中广泛用于确定D-二聚体水平。然而,从不同的D-二聚体测定获得的结果差异显著.这些检测方法内的变异系数在6.4%到17.7%之间,不同测定之间的测量差异可高达20倍。由于缺乏国际认可的参考测量系统(包括参考材料和参考测量程序),无法保证D-二聚体测试的准确性和可靠性,这可能会导致误诊和诊断不足,限制了其完整的临床应用。在这次审查中,我们对临床D-二聚体检测进行了深入分析,总结现有的挑战,计量学的当前状态,以及在协调方面的进展。我们还回顾了D-二聚体检测技术的最新进展,其中包括质谱和电化学和光学免疫测定。通过比较基本原理,被测量的定义,以及这些方法的分析性能,我们对D-二聚体临床试验的潜在改善进行了展望.
    The D-dimer is a sensitive indicator of coagulation and fibrinolysis activation, especially valuable as a biomarker of intravascular thrombosis. Measurement of plasma D-dimer levels plays a crucial role in the diagnosis and monitoring of conditions such as deep vein thrombosis, pulmonary embolism, and disseminated intravascular coagulation. A variety of immunoassays, including enzyme-linked immunosorbent assays, latex-enhanced immunoturbidimetric assays, whole-blood aggregation analysis, and immunochromatography assays, are widely used in clinical settings to determine D-dimer levels. However, the results obtained from different D-dimer assays vary significantly. These assays exhibit intra-method coefficients of variation ranging from 6.4% to 17.7%, and the measurement discrepancies among different assays can be as high as 20-fold. The accuracy and reliability of D-dimer testing cannot be guaranteed due to the lack of an internationally endorsed reference measurement system (including reference materials and reference measurement procedures), which may lead to misdiagnosis and underdiagnosis, limiting its full clinical application. In this review, we present an in-depth analysis of clinical D-dimer testing, summarizing the existing challenges, the current state of metrology, and progress towards harmonization. We also review the latest advancements in D-dimer detection techniques, which include mass spectrometry and electrochemical and optical immunoassays. By comparing the basic principles, the definition of the measurand, and analytical performance of these methods, we provide an outlook on the potential improvements in D-dimer clinical testing.
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