<sup>14</sup>C Sample Preparation Vacuum Line and Graphite Preparation Method for <sup>14</sup>C-AMS Measurement

Sheng-hua LIU; Yu-zhen YANG; Sheng XU; Hui ZHANG; Ya-xin JIANG; Hui-xia SHI

doi:10.15898/j.cnki.11-2131/td.201807120084

Rock and Mineral Analysis > 2019 > 38(3): 270-279. > DOI: 10.15898/j.cnki.11-2131/td.201807120084

Sheng-hua LIU, Yu-zhen YANG, Sheng XU, Hui ZHANG, Ya-xin JIANG, Hui-xia SHI. ¹⁴C Sample Preparation Vacuum Line and Graphite Preparation Method for ¹⁴C-AMS Measurement[J]. Rock and Mineral Analysis, 2019, 38(3): 270-279. DOI: 10.15898/j.cnki.11-2131/td.201807120084

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¹⁴C Sample Preparation Vacuum Line and Graphite Preparation Method for ¹⁴C-AMS Measurement

1.
Institute of Hydrogeology and Environmental Geology, Chinese Academy of Geological Sciences, Shijiazhuang 050061, China
2.
Central South Geo-Exploration Institute, China Metallurgical Geology Bureau, Wuhan 430081, China
3.
Scottish Universities Environmental Research Centre, Scottish Enterprise Technology Park, East Kilbride G75 0QF, UK

More Information

Received Date: July 11, 2018
Revised Date: March 08, 2019
Accepted Date: April 08, 2019
Published Date: April 30, 2019

Abstract

HIGHLIGHTS
(1) Compared with Zn/Fe online method, Zn/Fe sealed tube method was more suitable in overcoming air leakage and low background.

(2) A novel sample preparation vacuum system and graphitization method based on Zn/Fe flame sealed tube method were developed in this study.

(3) Higher ultimate radiocarbon age (47000-48000ya) and good precision (RSD=0.35%) have been achieved by Zn/Fe flame sealed tube method.

ABSTRACT

BACKGROUNDThe technical keys of high-quality ¹⁴C-Accelerator Mass Spectrometry (AMS) analysis with low-background is the sample preparation method and the vacuum line rigs. However, the development of the graphite target preparation method is impeded by extraneous source carbon contamination, unsteady graphitization yield and isotope fractionation.
OBJECTIVESTo reduce the requirement of the traditional on-line method on the long-term statical vacuum performance of the sample preparation line, solve the problem of CH₄ produced in the Zn-TiH₂/Fe sealed tube method, while improving the stability of graphitization, and control carbon contamination.
METHODS¹⁴C sample preparation vacuum system and graphite preparation method based on Zn/Fe flame sealing method was established. The effects on the beam current and values of graphite (prepared from OXⅡ and blank samples) between the Zn/Fe on-line method and the Zn/Fe flame sealed tube method were compared. The precision of the Zn/Fe flame sealed tube method was checked with OXⅡ as the unknown sample. Two 'in-house' blank standards IHEG-Cal and IHEG-Coal were used to evaluate the chemical procedure background of both methods. The other 'known-value' reference materials of IAEA C2, C3, C5, C7, C8 and C9 were used to validate the accuracy of the Zn/Fe flame sealed tube method.
RESULTSZn/Fe on-line method can obviously overcome the air leakage, which yields a lower chemical process background (0.24-0.32pMC) and higher ultimate radiocarbon age (47000-48000ya) observed in Zn/Fe flame sealed tube method with long-term stable beam current output. It was demonstrated that Zn/Fe sealed tube method was more suitable for graphite target preparation than Zn/Fe on-line method. The results illustrated that the Zn/Fe flame sealed tube method had good reproducibility (RSD=0.35%, n=20, OXⅡ), and high accuracy for a variety of natural samples ranging from dead carbon samples to modern carbon samples (linear fitting formula y=0.9969x+0.0013, R²=1) with a low background (radiocarbon age of blank 46296±271ya for inorganic carbon and 48341±356ya for organic carbon).
CONCLUSIONSThe graphite sample preparation vacuum system and the Zn/Fe flame sealing method have the characteristics of excellent graphite quality, low chemical procedure background, high accuracy and high precision, and meet the sample preparation requirements of high-precision and low-background ¹⁴C-AMS determination for graphite.
- ¹⁴C-Accelerator Mass Spectrometry,
- graphite target preparation,
- Zn/Fe on-line method,
- Zn/Fe flame sealed tube method

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