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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

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

  • 摘要: 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。

     

    Abstract:
    BACKGROUND The Xianghualing mining area in Hunan Province is an important part of the east-west tectonic-magmatic-metallogenic belt in the Nanling area.The ore-forming geological conditions in the mining area are superior, and it is famous for its many types of deposits and complex types of minerals.The tin-lead-zinc deposit in the Xianghualing mining area is a very important polymetallic deposit in the Nanling metallogenic belt.The ore types are mainly cassiterite sulfide tin ore, tin-lead-zinc ore and sulfide lead-zinc ore.Tin, lead and zinc are very important nonferrous metal elements.The abundance and variation characteristics of these three elements can reflect the regional metallogenic conditions, indicate the existence of deposits or mineralization, and are the important basis for studying the metallogenic model, deepening the understanding of the genesis of the deposit, and identifying the metallogenic control factors.Therefore, it is very necessary to accurately determine the content of tin, lead and zinc in the tin, lead and zinc deposits in the Xianghualing mining area, and it is important to study the regional metallogenic conditions The geological characteristics of the deposit, the occurrence state of elements, mineral processing and comprehensive utilization of non-ferrous metal minerals are of great significance.However, the average grades of tin, lead and zinc in the deposit are percentage contents and tin itself is a refractory element.Conventional open acid dissolution or closed acid dissolution in the dissolution of high content of tin, lead and zinc in the ore will have the disadvantages of incomplete digestion and easy precipitation of the solution, resulting in serious low determination results.However, alkali fusion is more capable of decomposing minerals than acid dissolution.As long as the appropriate alkali fusion reagent, temperature and time are optimized, some high content of inorganic elements, even insoluble elements, can be completely decomposed, which is an ideal method of mineral decomposition pretreatment.
    OBJECTIVES To rapidly and accurately determine the concentrations of tin, lead and zinc in high contents of tin, lead and zinc samples of a tin-lead-zinc deposit in the Xianghualing mining area, Hunan Province.
    METHODS Inductively coupled plasma-optical emission spectrometry (ICP-OES) with alkali fusion was used to determine the levels of tin, lead and zinc.The selection of alkali fusion reagent, reagent dosage, alkali fusion temperature and time as well as the plasma excitation conditions, element spectral lines, button background position and other instrumental determination conditions were optimized.The effects of three kinds of fluxes: sodium hydroxide, anhydrous sodium carbonate and sodium peroxide were compared.
    RESULTS The measured value of tin was greatly affected by the alkali flux.Under the flux of sodium hydroxide or anhydrous sodium carbonate, the measured value of tin was low, while the measured value of tin was consistent with the standard value under the flux of sodium peroxide.Based on the comparison of the effects of various fluxes on the analysis results, sodium peroxide was selected as the flux, melting at a constant temperature of 750℃ for 20 minutes, and acidification with 20mL of hydrochloric acid after 30mL of boiling water extraction to ensure the complete decomposition of the sample.The calibration series was prepared with blank alkali melt solution as the medium, so that the calibration series matched the sample matrix and eliminated the influence of matrix interference.The national first-class geochemical reference materials were used for method quality evaluation, and the results showed that the absolute value of the logarithmic difference between the measured value and the certified value of the reference material was less than 0.04.The detection limits of the method for tin, lead and zinc were 13.60μg/g, 36.45μg/g and 53.83μg/g, respectively.The precision of the method was better than 8%.The determination range of the calibration curve was between 0 to 100μg/mL.
    CONCLUSIONS Due to the use of alkali fusion method and blank alkali fusion solution as the standard preparation medium, this method is suitable for the determination of high contents of tin, lead and zinc in cassiterite-sulfide type tin ores, tin-lead-zinc ores, and sulfide type lead-zinc ores, and it has good application prospects.At present, this method has been successfully applied to the analysis of actual samples in the Xianghualing mining area, Hunan Province, with satisfactory results.

     

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