地质样品卤族元素分析进展

何焘; 汪在聪; 胡兆初

doi:10.3799/dqkx.2021.117

地质样品卤族元素分析进展

doi: 10.3799/dqkx.2021.117

1.
中国地质大学地质过程与矿产资源国家重点实验室, 湖北武汉 430078
2.
中国地质大学地球科学学院, 湖北武汉 430074

基金项目:

国家自然科学基金面上项目 41873029

详细信息

作者简介:
何焘(1992-), 男, 博士后, 主要从事分析地球化学研究.ORCID: 0000-0002-1074-2089.E-mail: taohe1992@sina.com

中图分类号: P599
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- 被引次数: 14
出版历程
- 收稿日期: 2021-06-18
- 刊出日期: 2021-12-15

Advances in Analysis for Halogens in Geological Materials

1.
State Key Laboratory of Geological Processes and Mineral Resources, China University of Geosciences, Wuhan 430078, China
2.
School of Earth Sciences, China University of Geosciences, Wuhan 430074, China

摘要

摘要: 地质样品中卤素是反演与流体和挥发分相关的地质过程的重要示踪元素.由于卤素含量低和强挥发性，准确测定地质样品中卤素一直是分析地球化学的难点.近年来，针对地质样品卤素的样品前处理技术的开发开展了大量工作.高温热解法、碱熔（溶）法、酸性消解法和碱性提取法能够满足土壤、沉积物和岩石中高含量卤素的分析要求.针对低含量卤素，仅有中子活化法和稀有气体质谱法能够准确定量.随着分析地球化学的发展，地质样品卤素分析技术逐渐向更高效的消解方法、更简便的操作以及更高灵敏度和高精度的分析方向改进.总结了近年来国内外在地质样品卤素分析方面所取得的成果，对比了各类方法的优缺点，展望了地质样品卤素分析方法的发展前景.
- 卤族元素 /
- 地质样品 /
- 样品前处理 /
- 分析方法 /
- 地球化学
Abstract: Halogen in geological materials is the key tracer for the fluid/volatile related geological processes. Due to low concentration of halogens and high volatility, it is a challenge for the analysis of halogens in geological materials. Many studies on sample preparation for the analysis of halogens in geological materials have been reported in the last decade. Pyrohydrolysis, alkali fusion, acid digestion and alkali extraction are suitable for the high concentrations of halogens in soils, sediments and most of rocks. Only neutron activation analysis and noble gas technique can be utilized to analyze the low concentrations of halogens in geological materials. With the development of earth science and the analytical geochemistry, the future analysis of halogens will be more effective, more convenients and with higher sensitivity and precision are the future of the analysis of halogens. In this study, we reviewed the development of analysis techniques for halogens and compares the advantages and drawbacks between different methods. Finally, a perspective of the development of analytical method for halogens in geological materials are given.
- halogen /
- geological material /
- sample preparation /
- analytical method /
- geochemistry

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硅化蚀变作用是指岩石在热液作用下，产生含有石英、玉髓、蛋白石、似碧玉等蚀变矿物的过程，是岩石矿物蚀变中一种重要的矿化蚀变类型，且石英脉和硅化带等硅化信息也常作为野外重要的找矿标志(于正军等，2010).很多金矿的形成与硅化蚀变密切相关，一般硅化越强，矿化越显著(肖晋等，1989).

岩石在发生硅化作用后形成的蚀变矿物，其主要成分为SiO₂，由此岩石在发生硅化蚀变作用前后SiO₂含量会发生巨大的变化，而且蚀变程度越强，岩石所含SiO₂含量越高.这就使得发生硅化作用的岩石在SiO₂含量方面成为一种异常，偏离相对均一的地质体背景，所以依据SiO₂含量可以用来辅助对硅化信息的提取.

自从先进星载热发射和反射辐射仪(advanced spaceborne thermal emission and reflection radiometer，ASTER)传感器问世以来，国内外诸多学者针对造岩矿物在ASTER热红外波段的发射光谱特征与SiO₂含量的关系做了大量研究，Ninomiya(2002)实现了从定性到定量的突破；Lyon(1965)测得25个火成岩样品(酸性-超基性)的发射率光谱及其SiO₂含量，结果表明随着SiO₂含量的增加，发射率吸收位置会向短波方向偏移.在国内，杨长保和朱群(2009)从USGS、JPL和JHU 3个岩石矿物光谱库中选择62个火成岩样本，并利用SPSS软件进行多元逐步回归分析从而得出了定量反演SiO₂含量的回归方程.在硅化信息提取研究方面，利用遥感可见光-近红外数据对其进行提取的技术方法已日趋成熟，杨波等(2005)利用Landsat/TM数据建立了矿化信息定量提取模型，对鹰嘴山金矿区的硅化信息进行了提取.

前人对于SiO₂含量反演及硅化信息提取是分开独立研究，并没有考虑依据二者间的关系.利用SiO₂含量和热红外遥感数据来对硅化信息的提取的研究还尚未见报道.因此，本文选取ASTER热红外数据，对蚀变矿物在ASTER热红外波段的光谱特征进行分析，以SiO₂含量为辅助因子，寻求硅化信息的提取方法.

1. 硅化信息提取方法

1.1 ASTER热红外数据预处理

ASTER热红外数据包含5个波段(波段10~14)，波段范围为8.125~11.650 μm，空间分辨率为90 m，辐射度分辨率≤0.3 k，量化级别为12 bits.

ASTER热红外数据的预处理包括辐射定标、大气校正、几何校正以及发射率反演.笔者基于TIR AtmosCorrect模型对ASTER热红外数据进行大气校正，消除了大气对地物发射率信息的影响；同时在ASTER可见光-近红外波段影像上选取与基准图像相对应的控制点，通过控制点坐标信息找到对应于热红外波段影像上的点，完成了ASTER热红外数据的几何校正.利用发射率归一化法对ASTER热红外波段数据进行了发射率反演(徐州等，2006)，得到了ASTER的10~14波段发射率影像图.

1.2 硅化蚀变矿物热红外波谱特征分析

在研究ASTER热红外数据硅化信息提取方法的过程中，对USGS标准波谱数据库中硅化蚀变矿物石英及蛋白石发射率曲线重采样到ASTER热红外波段，综合分析后，笔者发现石英和蛋白石在9.0 μm处有明显的吸收谷(对应ASTER数据的B₁₂)，在10.65 μm处有明显的发射峰特征(对应ASTER数据的B₁₃)(图 1).

图 1 硅化蚀变矿物ASTER热红外发射率曲线

Fig. 1. The ASTER TIR emissivity spectral of silicification minerals

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1.3 硅化信息提取方法

依据蚀变矿物在ASTER热红外波段的发射率曲线特征，结合Rowan and Mars(2003)针对ASTER热红外数据使用的比值法，笔者发现可以突出硅化信息，对硅化信息按照蚀变强度分为3级进行初步提取.

在对硅化信息初步提取的基础上，依据发生硅化作用的岩石在SiO₂含量大小上明显高于其他地质背景，同时硅化蚀变越强SiO₂含量越高.依据此，可以将SiO₂含量定义为提取硅化信息的辅助因子，对初步提取的硅化信息做进一步纠正，以完善ASTER热红外遥感硅化信息提取方法，方法具体流程如图 2所示.

图 2 ASTER热红外遥感硅化信息提取方法流程

Fig. 2. The procedure of method for ASTER TIR silicification information extraction

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2. 方法应用

为验证提出的ASTER热红外硅化信息提取方法是否具有可行性，笔者选取两处成像于2005年9月15日的ASTER热红外影像，在内蒙古二连浩特市北部区域做实地验证分析.

2.1 研究区地质概况

研究区位于内蒙古二连浩特市北部，地理坐标范围111°45′00″~112°15′00″E，44°10′00″~44°45′00″N.由于研究区地处戈壁荒漠区，植被覆盖度较低，岩石裸露条件较好，所以被选作为低覆盖草原蚀变信息提取方法及地质填图方法研究区.

研究区出露地层以石炭系-二叠系为主，零星发育中、晚奥陶世、早石炭世、晚石炭世和晚侏罗世的地层，多为第四系覆盖.区内褶皱构造和断裂构造同等发育，所显示的构造线方向以NE方向为主.区内岩浆岩分布相对广泛，以华力西期和燕山期的花岗岩类侵入岩石为主.华力西期岩体侵入石炭系宝力高庙组或中、下奥陶统乌宾敖包组中，以二长花岗岩、正长花岗岩、砂砾岩以及黑云母花岗闪长岩为主，华力西晚期的岩体被侏罗纪地层不整合覆盖，或被燕山期花岗岩侵入(图 3).

图 3 研究区地质图

1.湖积层：现代湖积淤泥沉积；2.冲洪积层: 由砂岩及砾石层组成；3.冲洪积层: 由粗砂和砾石层组成；4.阿巴嘎组: 灰紫色、紫褐色气孔状玄武岩及伊丁玄武岩、安山玄武岩；5.宝格达乌拉组：砖红色泥岩夹含砾粗砂岩；6.伊尔丁曼哈组：红色粘土和黄色砂砾岩；7.大磨拐河组：页岩、泥岩、砂岩、砂砾岩及砾岩组成夹褐煤；8.白音高老组：流纹质岩屑晶屑凝灰岩、流纹岩及流纹质溶结凝灰岩等酸性火山岩；9.玛尼吐组：安山岩、粗安岩、石英粗安岩、安山玢岩安山质角砾凝灰岩、英安玢岩及灰黑色及灰紫色玄武岩；10.宝力高庙组二段：灰-灰褐色安山岩、溶解凝灰岩，黄褐色灰绿色流纹质含角砾晶屑凝灰岩、凝灰质砂岩英安岩等中酸性火山岩及火山碎屑岩，含植物化石；11.宝力高庙组二段：(变质)长石砂岩、板岩、砾岩、硬砂岩为主夹中酸性岩屑晶屑凝灰岩、安山玢岩及灰岩透镜体；12.泥鳅河组：为浅海相碎屑岩夹灰岩组合，岩性为灰色、灰绿色、褐灰色(变质)粉砂质泥、砂岩夹灰岩；13.乌宾敖包组：灰褐色、灰绿色板岩、绢云母板岩、分砂质板岩、长石砂岩、变泥岩夹安山玢岩及灰岩透镜体；14.肉红色中细粒正长花岗岩；15.肉红色中细粒云母二长花岗岩；16.肉红色斑状中细粒黑云母二长花岗岩；17.肉红色中细粒-细中粒碱长花岗岩；18.灰绿色角闪花岗闪长岩；19.灰绿-暗灰绿色中细粒闪长岩、石英闪长岩；20.灰、灰白、灰黄色中细粒正长花岗岩、碱长花岗岩局部有闪石碱性花岗岩；21.灰白-灰色斑状中细粒黑云母正长花岗岩；22.肉红色中细粒-细粒二长花岗岩；23.灰白-灰色中细粒黑云母二长花岗岩；24.灰白-灰色斑状中细粒黑云母二长花岗岩及少量花岗闪长岩；25.灰白-灰色花岗闪长岩及少量石英闪长岩、石英二长岩；26.晚侏罗世次粗面斑岩；27.石英脉；28.花岗岩脉；29.碱性花岗斑岩脉；30.闪长岩脉；31.地质界线；32.实测地层不整合界线、火山喷发不整合地质界线；33.实测正断层；34.实测逆断层；35.实测平移断层；36.实测性质不明断层；37.角岩化；38.构造破碎带

Fig. 3. Geological sketch of the research area

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2.2 SiO₂含量反演

陈江和王安建(2007)将ASU波谱库的矿物波谱重采样至ASTER热红外波段，对矿物的波谱进行波段比值处理，选择波段比值与SiO₂含量最大相关系数，进行对数模拟，从而确定了发射率波谱与SiO₂含量的数值关系.其反演公式如下：

$\begin{array}{l} \;\;\;\;\;\;\;{\rm{Si}}{{\rm{O}}_2} = 28.76 \times {\rm{ln(}}6.56 \times {E_{13}} \times {E_{14}}/({E_{10}} \times \\ {\mathit{E}_{12}}){\rm{), }} \end{array}$

(1)

式(1)中，E₁₀、E₁₂、E₁₃和E₁₄对应ASTER热红外波段中心波长处的发射率值.笔者依据公式(1)，在对ASTER热红外数据做完预处理的基础上，利用波段计算工具得出了研究区的SiO₂含量结果(图 4).图 4中含量高值对应于地质图上的红色粘土和黄色砂砾岩，含量低值对应于地质图上的安山岩及粗安岩等.

图 4 研究区SiO₂含量

Fig. 4. The sketch showing the content of SiO₂

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2.3 硅化信息提取

利用比值法(B₁₃/B₁₂)对研究区发射率影像进行处理，得到突出硅化信息的图像.对其进行滤波处理后，统计滤波后图像的均值和标准差，对初步提取的硅化信息按蚀变强度分为3级.硅化信息初步结果如图 5所示.

图 5 硅化蚀变信息初步结果

Fig. 5. The original silicification information results of study area

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对反演得到的SiO₂含量结果与初步提取的硅化信息结果进行叠加对比分析，将图像中SiO₂含量明显高于周围背景而没有在蚀变结果中得到体现的区域，认定为存在硅化蚀变.由此得到研究区的最终硅化信息结果(图 6).对比分析图 5与图 6，可以明显地发现在区域A~D中，通过引入SiO₂含量这一辅助因子使得在最终得到的结果图中硅化信息得以补充完善.尤其是在区域A与C中，完善的硅化信息在野外实地勘察中得到了实地验证.

图 6 硅化蚀变信息最终结果

Fig. 6. The ultimate silicification information results of study area

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通过实验区野外考察，笔者发现在研究区裸露岩石处硅化蚀变现象十分明显，硅化程度由弱到强，在39个野外硅化采样点中，33个采样点在结果图中得到验证，精度达到86.14%.然而对于初始硅化信息提取结果，其没有考虑SiO₂含量与硅化信息间的关系，这就使得有些野外实际存在的岩石硅化蚀变在结果图中没有被提取出来，提取结果精度为76.92%.总的来说，通过以SiO₂含量为辅助因子对硅化信息纠正，使得硅化信息提取结果精度提高了9.22%.

3. 结论

通过分析硅化蚀变矿物在ASTER热红外波段的波谱特征，利用比值法(B₁₃/B₁₂)得到初步硅化信息结果，结合硅化蚀变与SiO₂含量间的关系对硅化信息进行纠正，完善了提取方法.通过在内蒙古二连浩特市北部区域对方法进行实地应用，笔者发现硅化信息提取结果与野外实地勘察吻合度较高，精度达到86.14%，与未利用SiO₂含量来对硅化信息进行纠正的结果相比，精度提高了9.22%.结果表明，以SiO₂含量为辅助因子的硅化信息提取方法能够实现对野外硅化信息进行较精确的提取，丰富了利用遥感技术对硅化信息提取的手段，对遥感地质找矿工作带来了帮助.

图 1 地球上不同卤素储库的Br/Cl和I/Cl比值与不同矿床类型流体的Br/Cl和I/Cl比值(改自Lecumberri-Sanchez and Bodnar, 2018)

Fig. 1. Characteristic Br/Cl and I/Cl ratios of the different halogen reservoirs on the Earth and fluids in different ore deposit types(revised from Lecimberri-Sanchez and Bodnar, 2018)

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图 2 国内土壤(GSS系列)和沉积物(GSD系列)标准物质和国际岩石标准物质(玄武岩BHVO-2、安山岩AGV-2、花岗岩GS-N和橄榄岩JP-1)中Br (a)和I (b)的测定值

Fig. 2. The measured values of Br (a) and I (b) in reference standard materials including soils (GSS series), sediments (GSD series) and rocks (basalt BHVO-2, andesite AGV-2, granite GS-N and peridotite JP-1)

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图 3 高温热解法装置(改自Chai and Muramatsu, 2007)

Fig. 3. The schematic diagram of pyrohydrolysis (revised from Chai and Muramatsu, 2007)

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图 4 氟化氢铵消解卤素分析方法机理图(改自He et al., 2019)

Fig. 4. The decomposition mechanism of NH₄HF₂ digestion for halogen analysis (revised from He et al., 2019)

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图 5 ⁷⁹Br中子活化过程示意（改自Ruzié-Hamilton et al., 2016)

Fig. 5. The schematic of neutron irradiation for ⁷⁹Br(revised from Ruzié-Hamilton et al., 2016)

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图 6 在电离温度T_ion=7 500 K时，理论计算的各元素的电离程度

Fig. 6. Calculated values for degree of ionization of various elements at T_ion=7 500 K

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表 1 地球各个储库的卤素丰度

Table 1. Abundances of halogens on Earth

储库类型	储库总质量(10²¹ kg)	F(μg/g)	Cl(μg/g)	Br(μg/g)	I(μg/g)
海水	1.4±0.7	1.30±0.07	19 300±970	66±3.3	0.058±0.006
蒸发盐	0.030±0.005	10±10	550 000±50 000	150±100	1±1
海洋沉积物	0.5±0.1	1 000±300	4 000±3 000	40±20	30±15
沉积岩	1.5±0.3	550±100	700±400	4±3	1.5±1.0
地壳卤水	0.06±0.03	20±15	100 000±50 000	600±400	15±10
地壳	26±3	550±100	300±100	0.60±0.25	0.018±0.009
地幔	2 800±800	12±2	5±2	0.013±0.006	0.000 3±0.000 01
原始地幔	4 040	17±6	26±8	76±25	0.007±0.004
注：数据引自Kendrick et al.(2017).

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表 2 卤素的质谱干扰所需分辨率

Table 2. The resolution to resolve the spectral interferences on halogens

被测元素	干扰离子	所需分辨率(M/ΔM)
¹⁹F⁺	³⁸Ar²⁺	1 116
	¹⁸O¹H⁺	1 160
³⁵Cl⁺	¹⁹F¹⁶O⁺	1 430
	¹⁸O¹⁸O¹H⁺	1 059
³⁷Cl⁺	³⁶Ar¹H⁺	4 680
⁷⁹Br⁺	⁶³Cu¹⁶O⁺	12 790
	⁴¹K³⁸Ar⁺	12 688
	³⁹K⁴⁰Ar⁺	10 184
	⁴⁰Ar³⁸Ar¹H⁺	5 405
⁸¹Br⁺	⁶⁵Cu¹⁶O⁺	12 624
	⁴⁵Sc³⁶Ar⁺	11 286
	⁴¹K⁴⁰Ar⁺	10 217
	⁶³Cu¹⁸O⁺	6 489
	⁴⁰Ar⁴⁰Ar¹H⁺	4 965
¹²⁷I⁺	⁸⁷Sr⁴⁰Ar⁺	3 822
	⁸⁷Rb⁴⁰Ar⁺	3 854
	¹¹¹Cd¹⁶O⁺	23 545

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参考文献(136)

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1. 硅化信息提取方法
1.1 ASTER热红外数据预处理
1.2 硅化蚀变矿物热红外波谱特征分析
1.3 硅化信息提取方法
2. 方法应用
2.1 研究区地质概况
2.2 SiO2含量反演
2.3 硅化信息提取
3. 结论

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地质样品卤族元素分析进展

doi: 10.3799/dqkx.2021.117

作者简介:
何焘(1992-), 男, 博士后, 主要从事分析地球化学研究.ORCID: 0000-0002-1074-2089.E-mail: taohe1992@sina.com

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Advances in Analysis for Halogens in Geological Materials

1. 硅化信息提取方法

1.1 ASTER热红外数据预处理

1.2 硅化蚀变矿物热红外波谱特征分析

1.3 硅化信息提取方法

2. 方法应用

2.1 研究区地质概况

2.2 SiO₂含量反演

2.3 硅化信息提取

3. 结论

期刊类型引用(9)

其他类型引用(5)

计量

目录

1. 硅化信息提取方法

1.1 ASTER热红外数据预处理

1.2 硅化蚀变矿物热红外波谱特征分析

1.3 硅化信息提取方法

2. 方法应用

2.1 研究区地质概况

2.2 SiO₂含量反演

2.3 硅化信息提取

3. 结论

留言板

地质样品卤族元素分析进展

doi: 10.3799/dqkx.2021.117

作者简介: 何焘(1992-), 男, 博士后, 主要从事分析地球化学研究.ORCID: 0000-0002-1074-2089.E-mail: taohe1992@sina.com

计量

出版历程

Advances in Analysis for Halogens in Geological Materials

1. 硅化信息提取方法

1.1 ASTER热红外数据预处理

1.2 硅化蚀变矿物热红外波谱特征分析

1.3 硅化信息提取方法

2. 方法应用

2.1 研究区地质概况

2.2 SiO2含量反演

2.3 硅化信息提取

3. 结论

期刊类型引用(9)

其他类型引用(5)

计量

出版历程

目录

1. 硅化信息提取方法

1.1 ASTER热红外数据预处理

1.2 硅化蚀变矿物热红外波谱特征分析

1.3 硅化信息提取方法

2. 方法应用

2.1 研究区地质概况

2.2 SiO2含量反演

2.3 硅化信息提取

3. 结论

作者简介:
何焘(1992-), 男, 博士后, 主要从事分析地球化学研究.ORCID: 0000-0002-1074-2089.E-mail: taohe1992@sina.com

2.2 SiO₂含量反演

2.2 SiO₂含量反演