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摘要: LA-ICP-MS分析矿物元素含量时激光能量密度会影响样品的剥蚀速率，从而影响测试过程的信号强度。激光能量密度变化对测试数据精确度的影响，以及不同天然矿物对激光能量密度的响应尚需进一步明确。本文测定了不同莫氏硬度天然矿物可稳定剥蚀的最小激光能量密度，评估了193nm ArF准分子激光系统中能量密度对地质标准样品（NIST SRM614、USGS BCR-2G、USGS GSC-1G）和天然矿物测试数据质量的影响。研究结果表明：①稳定剥蚀石英和萤石所需的最小激光能量密度为4~5J/cm2，低于前人的报道值（10J/cm2），而稳定剥蚀其他矿物（如滑石、磷灰石、刚玉等）所需的最小能量密度一般在1~2J/cm2；②不同激光能量密度剥蚀条件下，标准样品中大部分微量元素测试结果与推荐值的相对误差小于20%，相对标准偏差（RSD）小于10%，而天然矿物中含量>1μg/g的大部分微量元素测试数据的RSD小于20%；③在一定范围内，激光能量密度越大，数据平均相对误差越小，整体质量更好。Abstract:
BACKGROUNDLaser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) is a frequent instrument for the analysis of trace element content. When LA-ICP-MS is used to analyze the element content of minerals, the laser energy density will affect the denudation rate of the sample and thus affect the signal intensity during the analysis. OBJECTIVESTo further clarify the impact of laser energy density changes on the quality of test data and the response of different natural minerals to laser energy density. METHODSThe element content data of standard samples and nature minerals with different Mohs hardness under different laser energy densities were determined using LA-ICP-MS. Then authors analyzed the relative error (RE) between the test data and the reference values of the standard samples, average of the relative error of elements with RE within the limits of -20%-10% in the same standard sample, and the relative standard deviation of the standard samples and nature minerals test results to evaluate the effect of laser energy density on the test results. RESULTSThe minimum laser energy density required to stabilize ablated quartz and fluorite was 4-5J/cm2, which was lower than the previously reported value (10J/cm2), whereas stable denudation of other minerals such as talc, apatite, and corundum require the minimum energy density of generally 1-2J/cm2. Under the different condition of laser energy density, the relative error of most trace elements in standard samples between analytical results and recommended values was less than 20% and the relative standard deviation was less than 10%. The relative standard deviation of most trace element test data was less than 20% for natural minerals with most element contents >1μg/g. Within a certain range, the greater the laser energy density, the smaller the average relative error of the data, and the better the overall quality. CONCLUSIONSQuartz and fluorite require higher laser energy density for stable ablation than other minerals. Within the appropriate range, laser energy density has little effect on the quality of the individual element data, but it affects the overall quality of the data. -
Key words:
- LA-ICP-MS /
- laser energy density /
- standard samples /
- natural minerals /
- data quality
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图 2 不同能量密度下天然矿物中部分主微量元素测试数据的相对标准偏差(RSD)与该元素含量的趋势图(主量元素的含量大于0.01%，微量元素的含量大于0.1μg/g)
Figure 2.
图 5 不同激光能量密度下标准样品中部分主微量元素测试数据相对标准偏差(RSD)分布图(主量元素的含量大于0.01%，微量元素的含量大于0.1μg/g)
Figure 5.
表 1 LA-ICP-MS微量元素分析工作参数
Table 1. Equipment parameters for LA-ICP-MS trace elemental analysis
ICP-MS工作参数 设定值 激光工作参数 设定值 射频功率 1350W 波长 193nm 等离子体流量 15L/min 能量密度 以实测为准 辅助气流量 0.92L/min 载气 He 检测器 Dual(脉冲和模拟计数) 剥蚀方式 点剥蚀 扫描模式 跳峰 剥蚀束斑大小 60μm 单位质量扫描时间 8ms 剥蚀频率 8Hz 获取模式 时间分辨率分析 脉冲数 320 
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表 2 不同莫氏硬度矿物可稳定剥蚀的最小激光能量密度
Table 2. Minimum laser energy density for stable ablation of different Mohs hardness minerals
矿物 莫氏硬度 可产生稳定信号的最小激光能量密度(J/cm2) 石英 7 5 萤石 4 4 刚玉 9 2 黄玉 8 2 钠长石 6 2 钠铁闪石 5.5~6 2 透闪石 5~6 2 磷灰石 5 2 白云母 2.5~4 2 方解石 3 1 石膏 2 1 滑石 1 1
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