中国地质学会岩矿测试技术专业委员会、国家地质实验测试中心主办

碱熔-电感耦合等离子体发射光谱法测定湖南香花岭矿区锡铅锌矿床中的锡铅锌

肖细炼, 夏金龙, 李小丹, 卢友月, 杨小丽, 杨红梅. 碱熔-电感耦合等离子体发射光谱法测定湖南香花岭矿区锡铅锌矿床中的锡铅锌[J]. 岩矿测试, 2023, 42(1): 125-135. doi: 10.15898/j.cnki.11-2131/td.202107290087
引用本文: 肖细炼, 夏金龙, 李小丹, 卢友月, 杨小丽, 杨红梅. 碱熔-电感耦合等离子体发射光谱法测定湖南香花岭矿区锡铅锌矿床中的锡铅锌[J]. 岩矿测试, 2023, 42(1): 125-135. doi: 10.15898/j.cnki.11-2131/td.202107290087
XIAO Xilian, XIA Jinlong, LI Xiaodan, LU Youyue, YANG Xiaoli, YANG Hongmei. Determination of Tin, Lead and Zinc in a Tin-Lead-Zinc Deposit in Xianghualing Mining Area, Hunan Province by Inductively Coupled Plasma-Optical Emission Spectrometry with Alkali Fusion[J]. Rock and Mineral Analysis, 2023, 42(1): 125-135. doi: 10.15898/j.cnki.11-2131/td.202107290087
Citation: XIAO Xilian, XIA Jinlong, LI Xiaodan, LU Youyue, YANG Xiaoli, YANG Hongmei. Determination of Tin, Lead and Zinc in a Tin-Lead-Zinc Deposit in Xianghualing Mining Area, Hunan Province by Inductively Coupled Plasma-Optical Emission Spectrometry with Alkali Fusion[J]. Rock and Mineral Analysis, 2023, 42(1): 125-135. doi: 10.15898/j.cnki.11-2131/td.202107290087

碱熔-电感耦合等离子体发射光谱法测定湖南香花岭矿区锡铅锌矿床中的锡铅锌

  • 基金项目:
    中国地质调查局花岗岩成岩成矿地质研究中心开放基金项目(PMGR202012);中国地质调查局地质调查项目(DD20221777,DD20190154)
详细信息
    作者简介: 肖细炼,硕士,高级工程师,主要从事地球化学分析方面的研究工作。E-mail: xiaoxilianezhou@126.com
  • 中图分类号: O657.31

Determination of Tin, Lead and Zinc in a Tin-Lead-Zinc Deposit in Xianghualing Mining Area, Hunan Province by Inductively Coupled Plasma-Optical Emission Spectrometry with Alkali Fusion

  • 湖南香花岭矿区是南岭地区东西向构造-岩浆-成矿带的重要组成部分,矿区内成矿地质条件非常优越,以矿床类型多、矿产种类复杂而著称,其中锡铅锌矿床是该矿区南岭成矿带非常重要的多金属矿床,赋存的矿石类型主要以锡石-硫化物型锡矿石、锡铅锌矿石、硫化物型铅锌矿石为主,为了进一步研究区域成矿条件、矿床地质特征、元素赋存状态及有色金属矿产综合利用,准确测定锡、铅、锌有色金属元素的含量非常必要。湖南香花岭矿区锡铅锌矿床中锡、铅、锌元素的平均品位都为百分含量,且锡本身是一种难分解元素,因此,常规的酸溶很难将高含量的锡、铅、锌元素分解完全。针对香花岭矿区锡铅锌矿床样品的特殊性,本文建立了碱熔-电感耦合等离子体发射光谱同时测定湖南香花岭矿区锡铅锌矿床中锡铅锌的分析方法:①优化了碱熔试剂选择、试剂用量、碱熔温度、碱熔时间等实验前处理及等离子体激发条件、元素谱线、扣背景位置等仪器测定条件,在比较氢氧化钠、无水碳酸钠和过氧化钠3种熔剂对分析结果影响的基础上,选择以4.0g过氧化钠作为熔剂,在750℃下恒温熔融试样20min,约30mL沸水浸提后加入20mL浓盐酸酸化,保证样品分解完全;②以空白碱熔酸化溶液为介质配制校准系列,使得校准系列与试样基体匹配,消除了基体干扰影响。③采用国家一级地球化学标准物质进行方法质量评估,结果表明标准物质测定值与标准值的对数差值的绝对值(Δlgw) < 0.04,锡、铅、锌的方法检出限分别为13.60、36.45、53.83μg/g,方法精密度(RSD)均优于8%,校准曲线测定范围为0~100μg/mL。由于采用碱熔方法和以空白碱熔酸化溶液作为标准配制介质,使得该方法适用于锡石-硫化物型锡矿石、锡铅锌矿石、硫化物型铅锌矿石中高含量锡铅锌测定。

  • 加载中
  • 图 1  过氧化钠用量对测定结果的影响

    Figure 1. 

    表 1  锡、铅、锌元素分析谱线及扣背景位置

    Table 1.  Analysis spectral line and buckle background position of tin, lead and zinc elements

    元素 分析线波长
    (nm)
    谱线级次 扣背景位置
    Sn 189.989 477 左、右
    Pb 220.353 153 左、右
    Zn 213.856 458 左、右
    下载: 导出CSV

    表 2  氢氧化钠、无水碳酸钠、过氧化钠熔剂对测定结果的影响

    Table 2.  Effect of alkali fluxes such as sodium hydroxide, anhydrous sodium carbonate and sodium peroxide on the results

    标准物质编号 矿石类型 Sn含量(%) Pb含量(%) Zn含量(%) 碱熔试剂
    标准值 测定值 标准值 测定值 标准值 测定值
    GBW07240 钨矿石 0.14±0.03 0.099 0.26±0.01 0.26 0.29±0.02 0.28 氢氧化钠
    GBW07282 锡矿石 1.27±0.01 0.794 2.82±0.06 2.72 0.91±0.03 0.90
    GBW07281 锡矿石 4.47±0.10 2.79 2.72±0.07 2.69 0.74±0.03 0.74
    GBW07240 钨矿石 0.14±0.03 0.082 0.26±0.01 0.25 0.29±0.02 0.27 无水碳酸钠
    GBW07282 锡矿石 1.27±0.01 0.635 2.82±0.06 2.76 0.91±0.03 0.89
    GBW07281 锡矿石 4.47±0.10 2.14 2.72±0.07 2.68 0.74±0.03 0.71
    GBW07240 钨矿石 0.14±0.03 0.14 0.26±0.01 0.26 0.29±0.02 0.29 过氧化钠
    GBW07282 锡矿石 1.27±0.01 1.27 2.82±0.06 2.81 0.91±0.03 0.90
    GBW07281 锡矿石 4.47±0.10 4.44 2.72±0.07 2.70 0.74±0.03 0.73
    下载: 导出CSV

    表 3  空白碱熔酸化介质和去离子水介质的分析比对结果

    Table 3.  Analysis and comparison results of blank alkali fusion acidification medium and deionized water medium

    标准物质编号 元素 标准值(%) 空白碱熔酸化介质 去离子水介质
    测定值(%) 相对误差(%) 测定值(%) 相对误差(%)
    Sn 0.14±0.03 0.15 7.14 0.097 -30.71
    GBW07240 Pb 0.26±0.01 0.25 -3.85 0.19 -26.92
    Zn 0.29±0.02 0.29 1.38 0.23 -20.69
    Sn 1.27±0.01 1.24 -2.36 0.96 -24.41
    GBW07282 Pb 2.82±0.06 2.86 1.42 1.98 -29.79
    Zn 0.91±0.03 0.90 -1.10 0.74 -18.68
    Sn 4.47±0.10 4.53 1.34 3.20 -28.41
    GBW07281 Pb 2.72±0.07 2.64 -2.94 2.11 -22.43
    Zn 0.74±0.03 0.72 -2.70 0.59 -20.27
    下载: 导出CSV

    表 4  方法精密度

    Table 4.  Precision tests of the method

    标准物质
    编号
    Sn Pb Zn
    测定值
    (%)
    RSD
    (%)
    测定值
    (%)
    RSD
    (%)
    测定值
    (%)
    RSD
    (%)
    GBW07240 0.144 5.4 0.261 4.6 0.283 4.5
    GBW07282 1.24 3.1 2.80 2.9 0.908 3.4
    GBW07281 4.45 1.7 2.68 2.9 0.742 3.5
    下载: 导出CSV

    表 5  方法准确度

    Table 5.  Accuracy tests of the method

    元素 项目 GBW07240 GBW07282 GBW07281 GBW07163 GBW07286 GBW07287 GBW(E)070080 GBW07231
    标准值(%) 0.14±0.03 1.27±0.01 4.47±0.10 (0.002) 0.0008±0.0001 (0.00017) - 45.80±0.005
    Sn 平均值(%) 0.15 1.23 4.41 - - - - 45.38
    Δlgw 0.02 0.01 0.01 - - - - 0.00
    标准值(%) 0.26±0.01 2.82±0.06 2.72±0.07 2.17±0.07 1.27±0.07 3.38±0.10 22.96±0.09 2.89±0.03
    Pb 平均值(%) 0.27 2.86 2.75 2.11 1.22 3.31 22.73 2.76
    Δlgw 0.01 0.01 0.00 0.01 0.02 0.01 0.00 0.02
    标准值(%) 0.29±0.02 0.91±0.03 0.74±0.03 4.26±0.15 2.51±0.05 6.20±0.16 16.22±0.06 0.264±0.004
    Zn 平均值(%) 0.31 0.94 0.75 4.23 2.52 6.25 16.29 0.259
    Δlgw 0.03 0.02 0.00 0.00 0.00 0.00 0.00 0.01
    下载: 导出CSV

    表 6  样品分析结果

    Table 6.  Analytical results of the samples

    样品编号 岩性 Sn含量测定值(%) Pb含量测定值(%) Zn含量测定值(%)
    21LZL-05 伟晶岩 0.45 2.09 0.32
    21LZL-08 黑云母花岗岩 0.17 0.58 3.38
    LZL-08 中等风化花岗岩 0.26 2.03 0.79
    XF-03 块状铅锌矿石 0.14 33.42 1.55
    XF-04 磁黄铁矿铅锌矿石 0.25 25.84 17.61
    XF-09 磁黄铁矿多金属硫化物矿石 12.53 0.15 0.21
    下载: 导出CSV
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出版历程
收稿日期:  2021-07-29
修回日期:  2021-12-03
录用日期:  2022-01-28
刊出日期:  2023-01-28

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