Os element secondary oxidative distillation separation device and separation method and application thereof

A technology of secondary oxidation and distillation separation, which is applied to measurement devices, analytical materials, preparation of samples for testing, etc., can solve the problems of poor signal intensity of Os element measurement, low enrichment of Os element, and high acidity of absorption liquid, etc. Achieve the effect of improving the measurement signal strength and measurement accuracy, reducing the risk of explosion, and high content

Active Publication Date: 2020-11-24
INST OF GEOLOGY & GEOPHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In view of the insufficient oxidation degree of the Os element existing in the prior art, the enrichment of the Os element is small, and the OsO 4 The acidity of the absorption liquid is high, and the signal intensity of Os element measurement is poor. The present invention provides a secondary oxidation distillation separation device and separation method for Os element

Method used

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  • Os element secondary oxidative distillation separation device and separation method and application thereof
  • Os element secondary oxidative distillation separation device and separation method and application thereof
  • Os element secondary oxidative distillation separation device and separation method and application thereof

Examples

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Effect test

Embodiment 1

[0109] Accurately weigh 0.8g pyrite sample, 0.1g molybdenite standard substance JDC, 185 Re- 190 The Os mixed diluent was put into the Carius tube, and then the Carius tube containing the mineral sample was placed in the ethanol-liquid nitrogen mixed freezing solution at -80°C to -50°C, and then 9 mL of reverse aqua regia was added to the Carius tube. After the material in the Carius tube is completely frozen, use an oxygen-gas torch to heat the Carius tube to melt and seal it. The sealed Carius tube was then heated in an oven at 220 °C for 48 h.

[0110] After heating, take out the Carius tube and cool it down to room temperature, then put it into the ethanol-liquid nitrogen mixed freezing solution at -80°C to -50°C to open the tube, and add 9 mL of high-purity water to dilute after opening the tube. Then install the Carius tube in the electric heating steam bath, pass in ozone, and after verifying the air tightness, adjust the gas flow to 40-50mL / min, start the electric he...

Embodiment 2

[0116] The operation is the same as that of Re-Os isotope dating test example 1, except that 0.01 g of molybdenite standard substance HLP (GBW04435) is used instead of 0.1 g of molybdenite standard substance JDC (GBW04436).

[0117] Embodiment 2 repeats three times, and the results are as shown in table 2:

[0118] Table 2

[0119]

[0120] Among them, the first 2S in Table 2 is taken as an example, which indicates the standard deviation of twice the Re content. As can be seen from Table 2, the ages in the molybdenite standard substance HLP (GBW04435) and JDC (GBW04436) measured in the present invention are respectively 219.8 ± 1.1Ma and 139.6 ± 0.9Ma, while the molybdenite standard substance HLP (GBW04435) and The content of JDC (GBW04436) is 221.4±5.6Ma and 139.6±3.8Ma, which shows that the determination method in the present invention has high precision.

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Abstract

The invention relates to an Os element secondary oxidative distillation separation device comprising a gas source device, a gas washing device, a sample dissolving device, a heating device and an OsO4collecting device, wherein the gas source device is an ozone generator, and a washing liquid in the gas washing device is ethanol. Ozone with strong oxidizing property is used for carrying out secondary oxidation on the Os element in a decomposition liquid, and effective separation of the Re element and the Os element is realized under an ozone carrier band. Comparing with an air carrier band, under the same condition, the ozone carrier band has the advantages that the collection time can be shortened, the acidity of an OsO4 absorption liquid is reduced, the measurement signal of the Os element is improved by 1.2-10 times, the accuracy of dating analysis of the Re-Os isotope system is improved favorably, and the device is particularly suitable for treating sulfide mineral samples with theOs element content of 100 ppt or below.

Description

technical field [0001] The invention relates to the field of Re-Os isotope dating, in particular to an Os element secondary oxidation distillation separation device, separation method and application thereof, and an Os element content determination method. Background technique [0002] Re-Os isotopic dating is the most direct and effective dating method for metal deposits, and has developed into one of the most important dating techniques in ore depositology. Distillation is the main Os element separation method in the Re-Os isotope dating process. This method mainly uses an oxidant to oxidize Os in the sample into volatile OsO 4 , so as to separate and enrich Re and Os elements. [0003] Since the distillation method needs to occupy a large space, the cleaning workload is large, and a large amount of acid and alkali waste liquid will be discharged at the same time, therefore, the predecessors improved on the basis of the distillation method and established the in-situ dist...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/62G01N1/40G01N1/44
CPCG01N27/626G01N1/4055G01N1/44
Inventor 李文君高炳宇张连昌
Owner INST OF GEOLOGY & GEOPHYSICS CHINESE ACAD OF SCI
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