High-sensitivity emitter and method for thermal ionization mass spectrometer for ultra-micro sample strontium isotope test

An ultra-trace sample, off-mass spectrometer technology, which is applied in the field of strontium isotope analysis of ultra-trace samples, can solve the problems of difficulty in producing satisfactory data, poor test accuracy, and no strontium isotope propellant has been developed, and achieves easy preparation and purification. , the effect of improving analytical sensitivity and strong application prospects

Inactive Publication Date: 2019-04-30
INST OF GEOLOGY & GEOPHYSICS CHINESE ACAD OF SCI
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  • Abstract
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  • Application Information

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Problems solved by technology

However, for sample amounts of 200pg or less, due to TaF 5 The emitter cannot further improve the ionization efficiency of Sr, and the sensitivity cannot meet the test requirements, so it is difficult to produce satisfactory data
The lack of Sr isotope testing technology for ultra-trace samples has greatly restricted the development of earth science and environmental science, especially for some precious samples (extraterrestrial materials, mantle xenoliths, biological shell microfossils) or samples with low strontium concentrations ( Water samples, animal and plant samples), due to the inability to provide sufficient samples, the test accuracy is poor and cannot meet the needs of scientific research
[0006] In summary, so far, no emitter suitable for strontium isotopes in ultra-trace (30pg-200pg) samples has been developed.

Method used

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  • High-sensitivity emitter and method for thermal ionization mass spectrometer for ultra-micro sample strontium isotope test
  • High-sensitivity emitter and method for thermal ionization mass spectrometer for ultra-micro sample strontium isotope test
  • High-sensitivity emitter and method for thermal ionization mass spectrometer for ultra-micro sample strontium isotope test

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Experimental program
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Effect test

Embodiment 1

[0037] 1. Preparation of propellants

[0038] 1) Weigh the sample size of silicotungstic acid powder to be 110±1mg, and the volume of deionized water added is 5mL;

[0039] 2) After the silicotungstic acid is dissolved, the silicotungstic acid solution is purified through an AG50 cation exchange column filled with 1.5mL resin to reduce the sample bottom.

[0040] 3) preparing phosphoric acid with a concentration of 0.8M;

[0041] 2. Sample loading detection

[0042] 1) Take 1 μL of 0.8M phosphoric acid emitter and apply it on the surface of the high-purity Re filament. After the phosphoric acid is evaporated to dryness, apply 1 μL of silicotungstic acid emitter. Spot the NIST 987 sample on the surface of the filament, evaporate the sample to dryness at low temperature, increase the filament current until the filament turns dark red and keep for 3-5 seconds, then return the current to zero.

[0043] 2) The sample is loaded into the Triton Plus thermal ionization mass spectrome...

Embodiment 2

[0047] Embodiment 2 is roughly the same as Embodiment 1, except that this implementation selects 100 pg of NIST 987 to test the sensitivity and test accuracy of the emitter. 87 Sr / 86 Sr detection results are shown in Table 2:

[0048] Table 2. Analysis results of 100pg international standard sample NIST 987

[0049]

Embodiment 3

[0051] Embodiment 3 is roughly the same as Embodiment 1, except that this implementation selects 50 pg of NIST 987 sample amount to test the sensitivity and test accuracy of the emitter. 87 Sr / 86 Sr detection results are shown in Table 3:

[0052] Table 3. Analysis results of 50pg international standard sample NIST 987

[0053]

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Abstract

The invention discloses a high-sensitivity emitter and method for a thermal ionization mass spectrometer for the ultra-micro sample strontium isotope test and employs silicotungstic acid and phosphoric acid as high-sensitivity cast charges for the thermal ionization mass spectrometer. The method is advantaged in that properties of high sensitivity, low cost and simple operation are realized, the method is an important innovation of ultra-micro sample strontium isotope analysis, compared with a traditional analysis method, a sample consumption ratio is 1-50ng, the method only needs 30-200pg toobtain satisfactory test accuracy, test sensitivity is greatly improved, and the method has wide application prospects.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, and in particular relates to a method for analyzing strontium isotopes of ultra-trace samples using silicotungstic acid as a propellant. Background technique [0002] Strontium has four natural isotopes 88 Sr, 87 Sr, 86 Sr and 84 Sr, the isotopic abundances are 82.58%, 7.00%, 9.86% and 0.56%, respectively. Sr is widely distributed in various rocks, minerals, soils, water bodies and organisms in nature. The strontium isotope ratio varies greatly in different reservoirs in nature, which can be used not only for Rb-Sr isotopic dating of common minerals in geological bodies (mica, feldspar, metal sulfides), but also for a wider range of research objects (extraterrestrial matter , rock minerals, dust, water, food, animals and plants, archaeological samples, etc.) Sr isotope tracer. Currently, 87 Sr / 86 As an isotope tracer, the Sr ratio has been widely used in environmental scienc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/64
CPCG01N27/64B01D15/362H01J49/16H01J49/049H01J49/0031
Inventor 李潮峰
Owner INST OF GEOLOGY & GEOPHYSICS CHINESE ACAD OF SCI
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