Solid reference substance for laser ablation inductively coupled plasma mass spectrometry and quantitative analysis method

A reference material, inductive coupling technology, applied in the field of analytical chemistry, can solve the problem of lack of reference material, and achieve the effect of short time consumption, simple operation and high data accuracy

Active Publication Date: 2020-09-08
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to overcome the problem of lack of solid standard reference substances for LA-ICP-MS analysis, the p...

Method used

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  • Solid reference substance for laser ablation inductively coupled plasma mass spectrometry and quantitative analysis method
  • Solid reference substance for laser ablation inductively coupled plasma mass spectrometry and quantitative analysis method
  • Solid reference substance for laser ablation inductively coupled plasma mass spectrometry and quantitative analysis method

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Experimental program
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Effect test

Embodiment 1

[0058] The preparation of embodiment 1 solid reference substance

[0059] The present invention uses an aluminum alloy plate with a thickness of 0.12 cm that does not contain nickel, and uniformly cuts the aluminum alloy plate into six base material samples with a size specification of 2.5 cm×2.5 cm. Substrate samples were ultrasonically cleaned for 4 minutes and then dried. A Ni element target with a purity of 99.99% is selected. Put the dried substrate into a vacuum ion coating instrument, set the coating speed to 48nm / min, and control the time to 0min, 1min, 2min, 5min, 10min and 20min respectively, to obtain aluminum-based solid reference materials containing different concentration gradients of Ni. substances such as figure 1 shown.

Embodiment 2

[0060] Embodiment 2 performance investigation

[0061] Select any piece of solid reference material obtained in Example 1, adopt the method of surface scanning (multi-line composition surface), denudate the random area on the surface of the reference material, and collect data to obtain the element distribution map of Ni element on the surface of Al base ( like figure 2 Shown), and calculate the mass spectrum response signal RSD of Ni element with time. Experiments show that the Ni element distribution on the surface of the sample using vacuum ion plating is very uniform, and under continuous laser ablation, a stable signal can be generated, with RSD<10%.

[0062] The samples with different concentration gradients were denuded by line scanning and the mass spectrum response signals were collected. The concentration of the Ni element in the denuded area was selected as the abscissa and the mass spectrum response signal as the ordinate, and a linear regression diagram was draw...

Embodiment 3

[0063] Embodiment 3 actual sample analysis and result verification

[0064] Select an aluminum alloy sample containing Ni element, use the same laser ablation parameters to analyze the unknown sample, and combine the above standard curve equation to obtain the content of Ni element in the sample.

[0065] In addition, grind the sample into powder, weigh 0.1g and place it in a polytetrafluoroethylene container, add 3mL HNO 3 and 9mL HCl, heated at 100°C for 2h until the sample was completely digested, and the volume was set to 100mL, and measured by inductively coupled plasma spectroscopy. The obtained results were compared with those obtained by laser ablation-inductively coupled plasma mass spectrometry, and the results are shown in Table 1.

[0066] Table 1 Laser ablation inductively coupled plasma mass spectrometry analysis and inductively coupled plasma spectroscopy measurement results table

[0067]

[0068] The results showed that the element contents obtained by LA...

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Abstract

The invention discloses a solid reference substance for laser ablation inductively coupled plasma mass spectrometry and a quantitative analysis method. A to-be-detected metal element is adopted as a target material, and the surface of a flat and smooth solid base material is coated with a film through a vacuum ion coating method to form a solid reference substance coating film with the to-be-detected element uniformly distributed. Compared with an existing solid reference substance for laser denudation inductively coupled plasma mass spectrometry and a quantitative analysis method, the disclosed method is suitable for detection of any metal element in any matrix sample; the operation is easy, consumed time is short, finally, a precise calculation method is adopted for valuing, and data accuracy is higher.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, in particular to a solid reference substance for laser ablation inductively coupled plasma mass spectrometry analysis and a quantitative analysis method using the reference substance. Background technique [0002] Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is a method for direct sampling and microanalysis of solids. The method has the advantages of good spatial resolution, high sensitivity, wide dynamic linear range, and simultaneous determination of multiple elements. Due to the direct injection of solids, it can effectively avoid the problems of complex sample pretreatment and contamination of the elements to be measured during wet analysis, and greatly reduce the interference of mass spectrometry. Therefore, it is widely used in the fields of geology, metals, biology, etc. analyze. However, quantitative analysis has always been one of the biggest challenges fa...

Claims

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Application Information

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IPC IPC(8): G01N27/62G01N27/626
CPCG01N27/62
Inventor 张国霞汪正李青陈奕睿郭琳倩
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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