Development of a Double Vacuum Furnace Tube and Its Application in Gas Composition Determination during Rock Heating Degassing
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摘要: 分析岩石矿物中的气体化学组成，可为岩石圈地幔的不同地球化学过程、地球内部氧化还原环境以及水在深部地球中的循环等研究提供重要的信息与约束条件。对岩矿样品加热使气体脱出是一种常用的实验手段，使用单石英玻璃管作为样品管，石英玻璃结构中不规则的空隙使得气体在高温下易发生扩散与渗透；由钼、钽坩埚组成的双真空炉管一般用于稀有气体同位素组成分析，较少用于气体化学组成分析，且该装置结构复杂，不易组装拆解，也易被损坏。针对以上问题，本文研制了石英玻璃与金属零件组成的双真空盛样炉管，该炉管具有体积小、易于组装、拆解和移动等特点。在相同的实验条件下与单石英玻璃管进行对照实验。根据实验结果，尤其是H2浓度的测量结果表明：不论哪种类型的样品在500℃和950℃加热脱气时，应用本文研制的双真空盛样炉管，测量的H2浓度均高于同等实验条件下应用单石英玻璃管测量的H2浓度，该双真空炉管的气密性优于单石英玻璃管，有利于获得样品中更加真实的气体化学组成。Abstract:
BACKGROUNDThe analysis of gas chemical composition in rock and mineral can provide important information and constraints for the study of different geochemical processes of lithospheric mantle, redox environment in the earth, and water circulation in the deep earth. Heating rock and ore samples to remove gas is a common experimental method. A single quartz glass tube is used as the sample tube. Irregular voids in quartz glass structure make gas easy to diffuse and permeate at high temperature. The double vacuum furnace tubes consisting of molybdenum and tantalum crucibles are generally used for the analysis of rare gas isotope composition, but seldom used for the analysis of gas chemical composition. The device has a complex structure, is not easy to assemble and disassemble, and is easily damaged. OBJECTIVESTo solve the problems contained in the sample-filling tube proposed in the background research. METHODSA double vacuum sampling furnace tube composed of quartz glass and metal parts had been developed. The furnace tube had the characteristics of small size, easy assembly, disassembly and movement. Under the same experimental conditions, the result was compared with that of a single quartz glass tube. RESULTSH2 concentration measured by the double vacuum sampling tube was higher than that measured by the single quartz glass tube under the same experimental conditions, no matter which type of sample was heated to degas at 500℃ or 950℃. CONCLUSIONSThe closure of the double vacuum furnace tube is better than that of the single quartz glass tube, which is conducive to obtain more real gas chemical composition in the sample. -
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表 1 各样品脱出气体的组分含量百分比
Table 1. Percentage of component content for gases released from each sample
样品编号 加热温度(石英管类型) 样品质量
(g)气体含量百分比(%) H2 O2+Ar N2 CH4 CO CO2 MAS-KC-2 500℃(单石英管) 0.3817 2.944 0.233 0.336 0.692 6.211 88.657 950℃(单石英管) 0.3817 0.044 0.295 2.748 0.054 0.382 94.875 500℃(双真空炉管) 0.3813 4.487 0.086 0.214 5.439 5.210 82.006 950℃(双真空炉管) 0.3813 0.982 0.142 1.619 0.837 2.240 93.891 HXZ-2 500℃(单石英管) 0.6384 2.035 0.448 1.040 21.009 5.016 68.313 950℃(单石英管) 0.6384 0.034 0.004 0.274 0.049 0.389 99.121 500℃(双真空炉管) 0.6369 7.351 0.186 0.420 10.186 1.873 75.907 950℃(双真空炉管) 0.6369 0.403 0.029 0.367 0.196 1.244 97.641 FDX-NT-1 500℃(单石英管) 0.5313 7.813 0.425 1.588 5.860 4.184 72.103 950℃(单石英管) 0.5313 0.860 0.004 0.044 0.078 14.796 84.096 500℃(双真空炉管) 0.5300 20.33 0.479 1.119 19.962 4.363 48.435 950℃(双真空炉管) 0.5300 1.465 0.014 0.034 0.623 14.542 83.126 MAS-ZC-1 500℃(单石英管) 0.2402 1.770 0.008 0.022 3.126 15.028 76.591 950℃(单石英管) 0.2402 0.754 0.116 0.452 0.200 0.982 96.897 500℃(双真空炉管) 0.2391 2.428 0.026 0.057 4.316 10.795 82.027 950℃(双真空炉管) 0.2391 1.292 0.148 0.637 0.587 1.219 94.911 黑钨矿 500℃(单石英管) 0.9403 5.016 0.032 0.265 0.785 9.341 84.328 950℃(单石英管) 0.9403 0.991 0.282 2.587 0.077 4.747 89.863 500℃(双真空炉管) 0.9398 6.391 0.070 0.439 3.242 1.454 74.501 950℃(双真空炉管) 0.9398 3.203 0.126 1.426 5.545 22.298 65.621 
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表 2 各样品在不同温度点释出的气体量
Table 2. Amount of gas released from each sample at different temperature
加热脱气炉管及温度 气体量(μL) MAS-KC-2 HXZ-2 FDX-NT-1 MAS-ZC-1 黑钨矿 500℃(单石英管) 330.34 34.14 16.03 532.76 260.34 950℃(单石英管) 29.31 541.38 582.76 86.21 34.48 500℃(双真空炉管) 268.97 208.97 66.20 379.31 270.67 950℃(双真空炉管) 127.59 406.90 637.93 60.69 98.97
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表 3 重复性测试以及钼管试验结果
Table 3. Repeatability test and Mo-tube test results
样品 加热温度
(℃)样品质量
(g)气体含量百分比(%) H2 O2 +Ar N2 CH4 CO CO2 FRS
(11月21日)500 0.3352 25.252 0.346 2.351 24.638 9.076 36.767 950 0.3352 25.830 0.143 2.931 9.049 46.980 14.790 FRS重复
(11月25日)500 0.3357 27.832 0.333 2.433 22.901 7.848 33.761 950 0.3357 25.503 0.142 2.966 12.586 41.506 16.573 FRS钼管
(不开V1)500 0.3277 4.603 0.236 1.120 12.881 21.280 57.422 950 0.3277 14.077 0.361 2.467 10.026 22.534 43.388 FRS钼管
(开V1，关V4)500 0.3374 7.098 0.229 1.515 15.918 15.943 53.892 950 0.3374 10.939 0.264 7.122 9.996 41.897 23.739
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