Institute of Analytical and Bioanalytical Chemistry, Ulm University, Albert-Einstein-Allee 11, 89081, Ulm, Germany.
Anal Bioanal Chem. 2019 Jul;411(19):4551-4558. doi: 10.1007/s00216-019-01606-7. Epub 2019 Feb 27.
Recently, graphite furnace atomic absorption spectrometry (GFAAS) has been suggested as a tool for detection and sizing of metal nanoparticles (NPs) providing several advantages, such as direct analysis of solid samples, high sample throughput, and robust and cost-efficient instrumentation. For this purpose, evaluation of newly introduced criteria of the absorbance signal, namely, atomization delay (t) and atomization rate (k), is performed. However, in real samples, NPs are typically stabilized by either engineered coating reagents or natural materials and occur in unknown concentration. Hence, systematic investigation of possible influences of nine different coating reagents and of Ag concentration on the atomization behavior of silver nanoparticles (AgNPs) was studied. Evaluation of absorption signal characteristics revealed no influence of the coating or Ag concentration on the observed parameters. Furthermore, size-dependent measurements gave reproducible size correlation independent from the coating. Validity of sizing AgNPs with the proposed approach was successfully proven by investigation of two reference materials. The found size of 74.3 ± 5.9 nm in RM 8017 (NIST) agrees very well with the certified size of 74.6 ± 3.8 nm. Moreover, AgNP size of 25.1 ± 2.5 nm found by direct slurry sampling GFAAS in matrix reference material "NanoLyse13"-chicken meat homogenate spiked with PVP-AgNPs-was in very good agreement with the reference value of 27.3 ± 5.3 nm as determined by TEM.
最近,石墨炉原子吸收光谱法(GFAAS)被认为是一种用于检测和测定金属纳米粒子(NPs)大小的工具,具有直接分析固体样品、高样品通量、坚固且经济高效的仪器等优点。为此,对新引入的吸光度信号标准,即原子化延迟(t)和原子化速率(k)进行了评估。然而,在实际样品中,NPs 通常通过工程涂层试剂或天然材料稳定存在,且浓度未知。因此,系统研究了九种不同涂层试剂和 Ag 浓度对银纳米粒子(AgNPs)原子化行为的可能影响。吸收信号特征的评估表明,涂层或 Ag 浓度对观察到的参数没有影响。此外,尺寸依赖性测量给出了与涂层无关的可重复的尺寸相关性。通过对两种参考材料的研究,成功证明了用所提出的方法对 AgNPs 进行尺寸测定的有效性。在 NIST 的 RM 8017 中发现的 74.3±5.9nm 的尺寸与认证的 74.6±3.8nm 的尺寸非常吻合。此外,通过直接在基质参考材料“NanoLyse13”-鸡肌肉匀浆中进行悬浮液采样 GFAAS 发现的 PVP-AgNPs 掺杂的“NanoLyse13”-鸡肌肉匀浆中的 AgNP 尺寸为 25.1±2.5nm,与 TEM 测定的 27.3±5.3nm 的参考值非常吻合。