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Isotopic ratio mass spectrometer, sulfur isotope testing method and milk powder tracing method

A technology of isotope ratio and mass spectrometer, which is applied in the field of milk powder traceability and isotope ratio mass spectrometer, can solve the problems of poor accuracy and precision, oxygen isotope interference, etc., and achieve the effect of quality inspection, stable analysis and simple test method

Pending Publication Date: 2019-04-05
FOOD INSPECTION CENT OF CIQ SHENZHEN +1
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  • Application Information

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Problems solved by technology

[0004] The isotope ratio mass spectrometry is to prepare sulfur dioxide gas from the sulfur element in the sample. Compared with the sulfur hexafluoride method, the sulfur dioxide method has the advantages of simple operation and high safety. However, due to the viscosity of sulfur dioxide samples and defects such as oxygen isotope interference, its Less accurate and precise

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  • Isotopic ratio mass spectrometer, sulfur isotope testing method and milk powder tracing method
  • Isotopic ratio mass spectrometer, sulfur isotope testing method and milk powder tracing method
  • Isotopic ratio mass spectrometer, sulfur isotope testing method and milk powder tracing method

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Embodiment 1

[0041] An isotope ratio mass spectrometer such as figure 1 As shown, it includes a sample inlet 1, an oxidation tube 2 communicated with the sample inlet 1, a reduction tube 3 communicated with the oxidation tube 2, the top of the reduction tube 3 is connected with a drying tube 4, and the drying tube 4 is completely filled with desiccant ( not shown in the figure). Drying pipe 4 comprises the horizontal drying pipe 41 that is connected with reducing pipe 3 tops, and horizontal drying pipe 41 is communicated with longitudinal drying pipe 42. In other embodiments, the horizontal drying pipe 41 and the vertical drying pipe 42 may also be serpentine or spherical. This makes the sample gas dry immediately after coming out of the high-temperature reducing tube 3, avoiding the interference of water, and obtaining a stable sulfur isotope ratio. Generally, the stability of S determination is required to be better than 0.5 per thousand, and the stability can reach 0.3 per thousand af...

Embodiment 2

[0044]A method for testing sulfur isotopes, the steps are: take an appropriate amount of sample and wrap it in a tin cup and then enter the isotope ratio mass spectrometer in Example 1. The sample is first carried by helium into the oxidation tube 2 for oxidation reaction, and then through the reduction tube 3 to generate In the reduction reaction, the generated sulfur dioxide gas directly reaches the drying tube 4 for drying, and then is further purified by the adsorption column 5 and then enters the stable isotope mass spectrometer 6 for detection. The present invention has analyzed 10 international standard items USGS43, and the standard deviation (SD) reaches 0.25‰. At the same time, the same milk powder sample is taken for 10 parallel measurements, and its SD reaches 0.22‰ (see the following table 1 for specific data). Generally speaking, the stability requirement of S stable isotope ratio analysis process is better than 0.5‰, and the stability after improvement is better ...

Embodiment 3

[0051] The method for milk powder traceability includes the following steps:

[0052] S1 Obtain samples of milk powder imported from multiple countries;

[0053] S2 uses the isotope ratio mass spectrometer in embodiment 1 to carry out the detection of stable sulfur isotopes respectively with a plurality of samples;

[0054] S3 analyzed the characteristics of the above-mentioned sulfur isotope ratios to obtain the characteristic elements of different countries;

[0055] S4 tests the stable sulfur isotope of the unknown sample, and judges the origin attribute of the unknown sample based on the analysis data of S3.

[0056] In the preferred S2, the sample is also detected and analyzed for stable carbon and nitrogen isotopes; in the preferred S2, the sample is also detected and analyzed for stable hydrogen and oxygen isotopes. Samples were also analyzed for trace elements in S2. Trace elements include Mn, Ni, Cu, Rb, Sr, Ba, As, Li, V, Co, Y, Cs, La, Ce, Nd.

[0057] 1 Materia...

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Abstract

The invention relates to the field of isotope detection, in particular to an isotopic ratio mass spectrometer, a sulfur isotope testing method and a milk powder tracing method. According to the technical key points, the isotopic ratio mass spectrometer comprises a sample inlet, an oxidation tube, and a reduction tube, wherein the oxidation tube communicates with the sample-injecting port, the reduction tube communicates with the oxidation tube, a drying tube communicates with the top end of the reduction tube, and the drying tube is completely filled with a desiccant. According to the isotopicratio mass spectrometer, the sulfur isotope testing method and the milk powder tracing method, a traditional straight-type drying tube is replaced, thus sample gas is dried immediately after being discharged from the high-temperature reduction tube, the influence of vapor condensation at the junction of the reduction tube and the traditional straight-type drying tube on SO2 in the sample gas is lowered, and analysis is more stable. The measurement stability of S is generally required to be better than 0.05% while the stability after adopting the methods can reach 0.03%.

Description

technical field [0001] The invention relates to the field of isotope detection, more specifically, it relates to an isotope ratio mass spectrometer, a method for testing sulfur isotopes, and a method for traceability of milk powder. Background technique [0002] Sulfur is widely distributed in nature, commonly exists in air, water, rock, soil and other media, and exists in the form of sulfide, sulfate, etc.; sulfur has 25 isotopes, four of which are stable: 32 S (95.02%), 33 S(0.75%), 34 S (4.21%) and 36 S (0.02%), the different contents of sulfur isotopes can be used to determine the origin of minerals in forest ecosystems, which has good research significance. [0003] Isotope ratio mass spectrometers are good at isotope analysis, can analyze various forms of samples, detect multiple components simultaneously or sequentially, provide rich structural information, can quickly analyze and monitor in real time, and use less samples and have high sensitivity. [0004] The i...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/72G01N30/54G01N27/62G01N1/44
CPCG01N1/44G01N27/62G01N30/02G01N30/54G01N30/72G01N2030/025
Inventor 吴浩田玲易冰清李月梅罗洁郭秀秀曹刚红葛丽雅谢丽琪
Owner FOOD INSPECTION CENT OF CIQ SHENZHEN
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