NanoSIMS measurements of sub‐micrometer particles using the local thresholding technique

Hao, Jialong; Yang, Wei; Huang, Wenjuan; Xu, Yuchen; Lin, Yangting; Changela, Hitesh

doi:10.1002/sia.6711

Cited by 7 publications

(4 citation statements)

References 16 publications

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“…The acquired ion images were processed and analyzed using ImageJ with the Open MIMS plugin. The 30 frames of ion images of each isotope were automatically aligned and added using the TurboReg ImageJ plugin ( Hao et al, 2020 ). Then the Region of Interesting (ROI)s were selected depended the Experimental requirements.…”

Section: Methodsmentioning

confidence: 99%

NanoSIMS sulfur isotopic analysis at 100 nm scale by imaging technique

et al. 2023

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NanoSIMS has been widely used for in-situ sulfur isotopic analysis (32S and 34S) of micron-sized grains or complex zoning in sulfide in terrestrial and extraterrestrial samples. However, the conventional spot mode analysis is restricted by depth effects at the spatial resolution < 0.5–1 μm. Thus sufficient signal amount cannot be achieved due to limited analytical depths, resulting in low analytical precision (1.5‰). Here we report a new method that simultaneously improves spatial resolution and precision of sulfur isotopic analysis based on the NanoSIMS imaging mode. This method uses a long acquisition time (e.g., 3 h) for each analytical area to obtain sufficient signal amount, rastered with the Cs+ primary beam of ∼100 nm in diameter. Due to the high acquisition time, primary ion beam (FCP) intensity drifting and quasi-simultaneous arrival (QSA) significantly affects the sulfur isotopic measurement of secondary ion images. Therefore, the interpolation correction was used to eliminate the effect of FCP intensity variation, and the coefficients for the QSA correction were determined with sulfide isotopic standards. Then, the sulfur isotopic composition was acquired by the segmentation and calculation of the calibrated isotopic images. The optimal spatial resolution of ∼ 100 nm (Sampling volume of 5 nm × 1.5 μm2) for sulfur isotopic analysis can be implemented with an analytical precision of ∼1‰ (1SD). Our study demonstrates that imaging analysis is superior to spot-mode analysis in irregular analytical areas where relatively high spatial resolution and precision are required and may be widely applied to other isotopic analyses.

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Section: Methodsmentioning

confidence: 99%

NanoSIMS sulfur isotopic analysis at 100 nm scale by imaging technique

et al. 2023

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“…A NanoSIMS was used due to its high spatial resolution and multi-collection mode to measure Li isotopes with other elements. 32,35,36,40,41,43,[47][48][49][50][51][52][53][54][55][56][57][58] 2. Samples and analytical procedures…”

Section: Introductionmentioning

confidence: 99%

“…A NanoSIMS was used due to its high spatial resolution and multi-collection mode to measure Li isotopes with other elements. 32,35,36,40,41,43,47–58…”

Section: Introductionmentioning

confidence: 99%

A silica-related matrix effect on NanoSIMS Li isotopic analysis of glasses and its online calibration

Li,

Hao,

Yang

et al. 2023

J. Anal. At. Spectrom.

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“…On the one hand, the unique co-axial design of NanoSIMS reduces the spot size, which permits the analysis of much smaller minerals and mapping of the elemental distribution in crystal micro-structures. 9,27,28,31,[38][39][40][41][42][43][44][45][46] On the other hand, NanoSIMS has a smaller analysis chamber which is helpful in decreasing the chamber vacuum and thus, the hydrogen background. Although previous studies have reduced the background for water analysis to < 10 ppm by using NaonSIMS, the spatial resolution was restricted to > 10 μm.…”

Section: Introductionmentioning

confidence: 99%

High-Spatial-Resolution Measurement Of Water Content In Olivine Using NanoSIMS 50L

Hao¹,

Yang²

2022

At.Spectrosc.

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Olivine is the most abundant mineral in the planetary mantle. Its water content provides critical constraints on the processes and dynamics of the planetary interior. Olivine usually develops zonings with typical widths of 5-20 μm, which requires high spatial resolution. For secondary ion mass spectrometry (SIMS) measurements, primary beams with low currents were utilized to achieve high spatial resolution. However, this strategy also resulted in high background, which cannot be applied to nominally anhydrous minerals, e.g., olivine. Therefore, achieving high spatial resolution with low background is essential but challenging. For example, even though the NanoSIMS is designed for high-spatial-resolution measurements, the spatial resolution remained at > 10 μm for water content analysis in order to maintain a low water background of < 10 ppm. In this study, we optimized the primary beam settings and raster size for water content analysis of olivine using a CAMECA NanoSIMS 50L to improve the spatial resolution and the background simultaneously. Olivine standard samples (KLB-1, ICH-30, Mongok) with a water content ranging from 11.2 ppm to 70.6 ppm were measured for water content calibration with 1 H -/ 16 Oratio. San Carlos olivine with a water content of 1.42 ppm was used for background monitoring. The results showed that a spatial resolution of ~6 μm (primary beam size + raster size) with a background of 6 ± 2 ppm could be achieved by applying a Cs + beam current of 2 nA with a diameter of ~2 μm, rastering an area of 4 × 4 μm 2 . The analytical reproducibility of this method is better than 13% for standard samples with a water content of > 10 ppm. Overall, this method improved the spatial resolution for measuring water content by a factor of ~2 (in comparison to previous studies) and could be applied to olivine grains with complex zoning.

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NanoSIMS measurements of sub‐micrometer particles using the local thresholding technique

Cited by 7 publications

References 16 publications

NanoSIMS sulfur isotopic analysis at 100 nm scale by imaging technique

NanoSIMS sulfur isotopic analysis at 100 nm scale by imaging technique

A silica-related matrix effect on NanoSIMS Li isotopic analysis of glasses and its online calibration

High-Spatial-Resolution Measurement Of Water Content In Olivine Using NanoSIMS 50L

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