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Device and method for preparing graphite by Zn/Fe flame sealed-tube method

A tube sealing method, graphite technology, applied in chemical instruments and methods, inorganic chemistry, non-metallic elements, etc., can solve problems such as affecting the efficiency of graphite preparation, time-consuming, etc., to improve practical performance, avoid atmospheric leakage, and improve safety. Effect

Pending Publication Date: 2019-08-20
INST OF HYDROGEOLOGY & ENVIRONMENTAL GEOLOGY CHINESE ACAD OF GEOLOGICAL SCI
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Problems solved by technology

[0008] The above methods have their own advantages and disadvantages, but the device structure used in the implementation of each method is basically the same, which is divided into two parts: the vacuum maintenance system and the graphite preparation system. preparation efficiency

Method used

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  • Device and method for preparing graphite by Zn/Fe flame sealed-tube method
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  • Device and method for preparing graphite by Zn/Fe flame sealed-tube method

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preparation example Construction

[0099] Filled with CO 2 Before the preparation of raw materials, the present invention preferably CO 2 The oxidizing agent in the preparation raw material is subjected to decarbonization treatment, and the decarbonization treatment is preferably kept at 800-950°C, more preferably at 850-930°C, and more preferably at 900°C; the holding time is preferably 1.5-2.5h, more preferably 1.7-2.2h, more preferably 2h.

[0100] The CO of the present invention 2 The methods of filling, vacuuming and flame sealing of the prepared raw materials are described in Example 1.

[0101] In the present invention, for CO 2When the preparation raw materials are heated, the heating temperature is preferably 840-860°C, more preferably 845-855°C, and more preferably 850°C, and the heating time (ie reaction time) is preferably ≥12h, more preferably 12-850°C. 15h, more preferably 13-14h. The heating in the present invention is preferably carried out in a muffle furnace.

[0102] When producing CO ...

Embodiment 1

[0114] according to Figure 1~2 The structural construction device shown: the main pipeline Z-1 is composed of a glass-welded high-vacuum glass valve (Kimble, USA) with an outer diameter of 9.5mm, and the detachable parts are connected by Ultra-Torr stainless steel joints (Swagelok, USA);

[0115] Vacuum system 1 is supported by a Hicube 80 vacuum pump unit and a composite vacuum gauge PKR 251 (Pfeiffer Vacuum, Germany); the backing pump of the turbomolecular pump is an oil-free diaphragm pump;

[0116] First CO 2 Preparation unit 2, the second CO 2 Preparation unit 6, the first CO 2 Purification unit 3, the second CO 2 Purification unit 5, CO 2 The sampling unit consists of 4, where CO 2 Sampling unit 4 consists of sequentially arranged CO 2 Constant volume tube 4-1, double-layer casing reactor 4-2, 13 The C sampling tube 4-3 and the backup sample sampling tube 4-4 are composed, and the setting method is fixed at the connecting nozzle of the connecting pipe H-2 through...

Embodiment 2

[0138] Same as Example 1, the difference is that the inorganic carbon sample is used in a Y-type acid hydrolysis tube to carry out acid hydrolysis reaction with 6mL phosphoric acid (85% V / V, Tianjin Kermel Chemical Reagent) to generate CO 2 . The inorganic carbon sample used in this example is calcite (IHEG Cal, inorganic carbon). Calcite crystals were collected from the Yangliugang Formation (Middle Cambrian ~ 520 Ma), with high crystallinity, pure white and no impurities. The crystals were crushed in an agate mortar and then soaked in 1% (V / V) hydrochloric acid for 4 hours to remove the influence of surface inorganic carbon. After washing and drying with deionized water, they were used for the preparation of graphite and the purification and collection of carbon dioxide.

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Abstract

The invention belongs to the technical field of graphite preparation, and specifically relates to a device and method for preparing graphite by a Zn / Fe flame sealed-tube method. The provided device can shorten the vacuumizing period and improve the CO2 sample collection efficiency. According to the Zn / Fe flame sealed-tube method, Zn powder is taken as a reducing agent, the shortage that when H2 orTiH2 is taken as a reducing agent, methane is generated in the system is overcome; moreover, the flame sealed-tube method can solve the problem that due to long time of an online reducing method, leakage of a vacuum system happens, the background values of the test result are reduced, and the sampling efficiency is improved.

Description

technical field [0001] The invention belongs to the technical field of graphite preparation, and in particular relates to a device and a method for preparing graphite by a Zn / Fe flame sealing method. Background technique [0002] With the development and application of accelerator mass spectrometer (AMS), 14 C (half-life 5730ya) isotope dating and tracing technology has provided important technical support for innovative research in many disciplines such as geology, oceanography, environmental science, groundwater science, archaeology and biomedicine, and these applications are all important Established 14 Based on high-precision analysis of C isotopes. [0003] Traditional beta decay counting method measurement 14 At C, it is necessary to convert the sample into benzene for decay counting. This method has the disadvantages of long sample preparation period, large sample volume (>1g carbon), long measurement time, and low test accuracy, which seriously restricts 14 Th...

Claims

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Application Information

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IPC IPC(8): C01B32/205
CPCC01B32/205
Inventor 刘圣华杨庆华史慧霞
Owner INST OF HYDROGEOLOGY & ENVIRONMENTAL GEOLOGY CHINESE ACAD OF GEOLOGICAL SCI
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