IP Library › Granted Patent US 11,075,066
Granted Patent B2
US 11,075,066 · App. 16/591,442 · Granted Jul 27, 2021

Automated detection of nanoparticles using single-particle inductively coupled plasma mass spectrometry (SP-ICP-MS)

Inventors: Takayuki Itagaki (Hachioji, JP); Steven Wilbur (Lopez Island, WA); Michiko Yamanaka (Kodaira, JP)
Assignee: Agilent Technologies, Inc.
H01J49/105H01J49/0036H01J49/24H01J49/4225
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Quick Facts
Patent No.
US 11,075,066
App. No.
16/591,442
Granted
Jul 27, 2021
Kind
B2
Abstract

Particles such as nanoparticles in a sample are analyzed by single-particle inductively coupled plasma-mass spectrometry (spICP-MS). The sample is processed in an ICP-MS system to acquire time scan data corresponding to ion signal intensity versus time. A signal distribution, corresponding to ion signal intensity and the frequency at which the ion signal intensity was measured, is determined from the time scan data. A particle detection threshold is determined as an intersection point of an ionic signal portion and a particle signal portion of the signal distribution. The particle signal portion corresponds to measurements of particles in the sample, and the ionic signal portion corresponds to measurements of components in the sample other than particles. The particle detection threshold separates the particle signal portion from the ionic signal portion, and may be utilized to determine data regarding the particles.

Claims (25)

1. A method for analyzing nanoparticles in a sample by single-particle inductively coupled plasma-mass spectrometry (spICP-MS), the method comprising:

processing the sample in an ICP-MS system to acquire raw sample data corresponding to ion signal intensity as a function of time measured by an ion detector of the ICP-MS system;

determining a signal distribution of the raw sample data corresponding to a plurality of data points, each data point corresponding to ion signal intensity and the frequency at which the ion detector measured the ion signal intensity; and

determining a particle detection threshold as an intersection point of an ionic signal portion of the signal distribution and a particle signal portion of the signal distribution,

wherein the particle signal portion corresponds to measurements of nanoparticles in the sample, the ionic signal portion corresponds to measurements of components in the sample other than nanoparticles, and the particle detection threshold separates the particle signal portion from the ionic signal portion.

2. The method of claim 1 , wherein determining the particle detection threshold comprises evaluating a characteristic of the ionic signal portion.

3. The method of claim 2 , wherein evaluating a characteristic of the ionic signal portion comprises approximating the ionic signal portion as an exponential function.

4. The method of claim 1 , wherein determining the particle detection threshold comprises:

calculating a plurality of approximate curves approximating the ionic signal portion, based on an exponential function in which data points of the signal distribution are inputs;

calculating coefficients of determination of the data points within the approximate curves;

determining which of the coefficients of determination is a maximum correlation; and

determining the data point corresponding to the maximum correlation to be the particle detection threshold.

5. The method of claim 1 , comprising, after determining the particle detection threshold, determining nanoparticle data based on the particle signal portion.

6. The method of claim 5 , wherein determining nanoparticle data is selected from the group consisting of: determining a mass spectrum; determining particle number concentration; determining elemental composition; determining particle size; determining particle size distribution; and a combination of two or more of the foregoing.

7. The method of claim 1 , wherein processing the sample comprises producing ions by exposing the sample to an inductively coupled plasma, and transmitting at least some of the ions into a mass analyzer, and transmitting at least some of the ions from the mass analyzer to the ion detector.

8. The method of claim 7 , wherein processing the sample comprises generating the inductively coupled plasma in a torch box, transmitting the ions from the torch box into a collision/reaction cell to suppress interferences, and transmitting at least some of the ions from the collision/reaction cell into the mass analyzer.

9. The method of claim 1 , wherein processing the sample comprises flowing the sample into an ion source from a nebulizer or a spray chamber.

10. An inductively coupled plasma-mass spectrometry (ICP-MS) system for analyzing nanoparticles in a sample by single-particle inductively coupled plasma-mass spectrometry (spICP-MS), the ICP-MS system comprising:

a torch box configured to generate plasma and produce ions from the sample in the plasma;

a mass analyzer configured to separate the ions according to mass-to-charge ratio;

an ion detector configured to count ions received from the mass analyzer; and

a controller comprising an electronic processor and a memory, and configured to control the steps of the method of claim 1 .

11. The ICP-MS system of claim 10 , comprising a collision/reaction cell positioned between the ion source and the mass analyzer and configured to suppress interferences.

12. A non-transitory computer-readable medium, comprising instructions stored thereon, that when executed on a processor, control or perform the steps of the method of claim 1 .

13. A system comprising the computer-readable storage medium of claim 12 .

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 2, 2019
From: ITAGAKI, TAKAYUKI; WILBUR, STEVEN; YAMANAKA, MICHIKO
To: AGILENT TECHNOLOGIES, INC.
Reel/Frame 050608/0577 →
Continuity (2)
Provisional Application 62751259 · Oct 26, 2018
Related Publication 20200135443A1 · Apr 30, 2020
Cited By (1)
US 12,482,642