摘要
随着加速器质谱(AMS)^(14)C测年需求的增长,高效、低本底的石墨化制样装置成为年代学实验室核心设备。传统手动制样因流程存在效率低、现代碳污染严重、难以在短期找到或培养经验丰富的人员等问题的限制,使得多种商业自动石墨化装置得到快速发展。目前国内已大量使用CEGS、AGE3、μGRAPHILINE等石墨化制样装置,满足日常样品制备工作,其工作原理、系统性能与适用范围尚缺乏系统对比。文章从仪器设计(结构及性能、自动化控制、功能拓展)、石墨化流程(样品氧化方式、CO_(2)纯化技术、催化还原方法)等多方面进行了详细介绍;并基于本底样品(邻苯二甲酸酐、天然石墨)及国际标准物质(OXⅡ、IAEA-C系列)的石墨化数据为依据,对3种自动石墨化装置的系统性能(石墨转化率、本底水平、运行效率)进行了对比。研究得出的结论,旨在为相关研究人员未来认识与选购此类设备提供参考依据。以下为本文结论:CEGS具备在线/离线氧化与酸解功能,液氮冷阱纯化使本底达>50000 a B.P.,石墨转化率>91%,最高可达99.8%,但顺序处理模式限制了运行效率,适合高本底需求样品或复杂样品的前处理研究;AGE3通过元素分析仪和沸石分子筛吸附实现了高效运行,本底可稳定在45000~50000 a B.P.,常规样品的石墨转化率可维持在90%以上,但对微量样品(初始碳量<200μg)的石墨转化率较低,适合均质样品的批量处理;μGRAPHILINE采用无液氮无气体的石墨化方法及特殊的CO_(2)转移技术与模块化设计,据官方资料其本底可维持在45000 a B.P.,石墨转化率>95%,单日样品通量可达24个,运维成本低,具备故障隔离能力,适合大样品量的处理。
With the growing demand for accelerator mass spectrometry(AMS) ^(14)C dating,high-efficiency,low-background graphitization systems have become core equipment in modern laboratories.Traditional manual sample preparation processes suffer from limitations such as low efficiency and poor reproducibility.While several commercial automated graphitization systems(CEGS,AGE3,μGRAPHILINE)have been developed,a systematic comparison of their technical characteristics and applicable scenarios remains lacking.This study provides a detailed introduction from many aspects such as instrument design(structural performance,automated control,functional expansion),graphitization process(sample oxidation method,CO_(2) purification techniques,catalytic reduction method).And based on the CEGS graphitization data of background samples(phthalic anhydride,natural graphite)and international reference materials(OXⅡ,IAEA-C series),the system performance(graphite conversion rate,background level,operational efficiency)of the three automatic graphitization systems was compared.The conclusions drawn from the study aim to provide a reference for relevant researchers to understand and purchase such equipment in the future.The following conclusions can be drawn:(1)CEGS has online/offline oxidation and acid hydrolysis functions.Its liquid nitrogen cold trap purification achieves a background level of>50000 a B.P.and a graphite conversion rate of>91%,up to 99.8%.However,its sequential processing mode limits operational efficiency.It is suitable processing samples with high background requirements and complex samples.(2)AGE3 achieves efficient operation through an elemental analyzer and zeolite molecular sieve adsorption,maintaining a stable background level between 45000~50000 a B.P.The graphite conversion rate of conventional samples can be maintained above 90%.However,it exhibits a lower graphite conversion rate for trace samples(initial carbon content<200μg),making it suitable for batch processing of homogenized samples.(3)μGRAPHILINE adopts no liquid nitrogen,no gas,special CO_(2) transfer technology and modular design.The background can be maintained at 45000 a B.P.,the graphite conversion rate is>95%,and the sample throughput of a single day can reach 24 samples in the standard modular configuration.It has fault isolation capabilities,low operation and maintenance costs,and is suitable for processing large sample volumes.
作者
徐子琪
许冰
陈实
赵亚茹
张俊杰
XU Ziqi;XU Bing;CHEN Shi;ZHAO Yaru;ZHANG Junjie(State Key Laboratory of Lithospheric Evolution and Environmental Coevolution,Institute of Geology and Geophysics,Chinese Academy of Sciences,Beijing 100029,China;College of Earth and Planetary Sciences,University of Chinese Academy of Sciences,Beijing 100049,China;Institute of Vertebrate Paleontology and Paleoanthropology,Chinese Academy of Sciences,Beijing 100044,China)
出处
《第四纪研究》
北大核心
2025年第6期1394-1404,共11页
Quaternary Sciences
基金
中国科学院(B类)战略性先导科技专项项目(批准号:XDB0710000)
中国科学院青年创新促进会项目(批准号:2021060)共同资助。
