Research Progress of Selenium-enriched Land Resources and Evaluation Methods
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摘要: 硒是重要的生命必需元素，开发富硒农产品是提升我国人体硒摄入水平的安全有效途径，富硒土地资源评价与利用规划是土地质量地球化学调查成果服务于特色农产品发展与脱贫攻坚的重要切入点。本文评述了近年来在土壤和作物硒含量、土壤硒成因来源、土壤硒赋存形态及其生物有效性影响因素、土壤-作物系统硒吸收运移、硒与重金属镉等元素之间的相互作用等调查研究成果。针对我国土壤硒背景值约0.20mg/kg，远低于世界土壤背景值0.40mg/kg，整体上处于低硒水平的实际情况，认为采用0.40mg/kg Se作为富硒土壤标准具有较强的科学依据；多数情况下土壤硒主要来源于成土地质背景，部分地区与人为活动密切有关；富硒土壤可分为地质高背景、次生富集作用、人为输入及其多种作用的叠加成因，元素地球化学性质决定了硒与镉等重金属元素共生的普遍性；土壤硒成因来源以及pH、Eh、有机质、铁铝氧化物等土壤理化条件决定了硒和重金属赋存形态与生物有效性，进而影响到富硒土地的可利用性，成为制定富硒土壤地方标准的理论基础与考虑因素；不同作物种类对硒吸收富集能力不同，筛选适应当地农田生态环境、富硒低镉的农作物具有实际意义；现有的部分富硒农产品标准未充分考虑人体补硒目的，并存在标准间协调性差等问题，急需加强富硒农产品标准的制定。本文提出，富硒土地资源评价不仅需要考虑土壤硒和重金属含量，而且需综合土壤硒成因来源及其生物有效性、土壤-作物系统硒迁移累积、硒与重金属镉等元素之间的相互作用机制，以及当地气候、土壤和景观条件下作物种植的适宜性，依据富硒土地资源可利用性进行分类分区、科学规划和合理种植管理。同时建议，为满足富硒土地资源调查评价与可利用性分析、富硒农产品健康效应研究的需要，需要加强土壤和作物硒含量及其形态的提取分离与分析测试方法技术研究与应用。要点
(1) 成因、形态、吸收迁移机理等是富硒土地资源评价的科学基础。
(2) 土壤硒有效性、环境质量、作物种植适宜性是富硒土地资源可利用性的关键要素。
(3) 急需加强富硒农产品标准的制定，完善土壤和作物硒形态分析测试技术。
HIGHLIGHTS(1) The origin, species, uptake and transport mechanism were bases for selenium-enriched land resource assessment.
(2) Bio-availability, soil environmental quality and plantation suitability were the key factors for the ultilization of selenium-enriched land resources.
(3) It was urgent to enhance research on selenium-enriched agricultural product standards and speciation analysis methods.
Abstract:BACKGROUNDSelenium is an important, essential element of life. The development of selenium-enriched agricultural products is a safe and effective way to increase the level of human selenium intake in China. The evaluation and utilization planning of selenium-enriched land resources are important aspects of land quality geochemical surveys, to serve the development of characteristic agricultural products and to overcome poverty.OBJECTIVESTo improve the methodology for selenium-enriched land assessment and to develop more effective and safe land-use planning methods.METHODSThe research results on selenium content in soil and crops, the origin of soil selenium, the soil selenium occurrence and its bioavailability factors, the soil-crop system selenium absorption and transport, and the interaction between selenium and heavy metal cadmium were reviewed in this article.RESULTSThe geochemical background of selenium in top soils in China was 0.2mg/kg, significantly lower than the average in world soils (0.4mg/kg). Generally, the soils had a low selenium level, and it was believed that the use of 0.40mg/kg selenium as a selenium-enriched soil standard had a strong scientific basis. Selenium in soils was mostly from a geological setting, however, in some cases anthropogenic activities may be an important source of soil selenium. The genetic mechanism of selenium-enriched soils can be categorized as high geological background, weathering accumulation and anthropogenic input as well as a multi-factor combination. The association of selenium with cadmium and other heavy metals was pervasive because of similar geochemical behavior and geological origin. The species and bio-availability of selenium in soils were mainly controlled by its source and soil physic-chemical properties such as pH, Eh, and contents of organic matter, iron oxides and aluminum oxides. In turn, these factors affect the availability of selenium-enriched land and became the theoretical basis and considerations for formulating local standards for selenium-enriched soil. The accumulation ability of selenium varied greatly between crop cultivars. Selection native crop types with higher selenium accumulation ability and low accumulation with Cd as well as other toxic metals was of practical meaning. Some existing selenium-enriched agricultural product standards did not fully consider the purpose of human selenium supplementation, and there were problems such as poor coordination between standards. It was urgent to strengthen the formulation of selenium-enriched agricultural product standards.CONCLUSIONSSelenium-enriched land suitability assessment, local selenium-enriched soil standard establishment and selenium-enriched crop plantation planning should consider the concentration of selenium and heavy metals in soils, their source and genesis, bio-availability and influencing factors, transport and accumulation in soil-crop system, the synergistic or antagonistic effects between selenium and other chemicals such as cadmium, as well as plantation suitability of crop cultivars under local climate, soil conditions and landscape. According to the availability of selenium-enriched land resources, classification, zoning, scientific planning and reasonable planting management are carried out. In order to meet the needs of investigation and evaluation of selenium-enriched land resources, availability analysis, and research on the health effects of selenium-enriched agricultural products, it is recommended to strengthen the research and application of extraction, separation, analysis, and determination methods for soil and crop selenium content and species.
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以沉积岩为主要容矿岩石的卡林型金矿是目前世界上储量最大的金矿类型之一，其中的金以“不可见金”或颗粒极细状(纳米级)存在是该类型金矿最重要的特点之一。主要载金矿物有黄铁矿、毒砂和黏土矿物，尤以黄铁矿最为重要。氧化矿石中主要载金矿物是褐铁矿和黏土矿，自然金粒度很细，大多为次显微金[1]。国内外对该类型金矿载金矿物开展了较系统的电子探针分析，结合X射线光电子能谱对黄铁矿和毒砂进行了表面元素的定性和定量分析，对探讨矿床的成矿条件、成矿过程及成矿机理具有重要的依据和信息[2-4]。
甘肃省陇南赵家庄金矿是近年来在西秦岭南部地区发现的此类型金矿之一，该地区卡林型金矿又有与国内外同类型矿床不同的特点，受构造破碎带控制。从已研究的资料来看，前人对该地区金的成矿模式与机理研究较多，积累了很多含矿层位、控矿构造、地球化学等成果，但是对含金矿物的组分和赋存状态研究较少，加之该地区的矿山开采较少，限制了矿石的综合开发利用。故本文应用偏光显微镜与电子探针相结合的手段，对该地区含金矿物的含量、矿物种类、赋存状态及其嵌布特征进行研究，并利用电子探针进行微粒金定性和定量测定，拟为研究矿床的成因、成矿过程和成矿机理提供依据，也为金矿床的选矿提供理论指导，具有重要的经济意义。
1. 地质背景
研究区地处西秦岭褶皱带南秦岭被动陆缘褶皱带南侧，位于扬子板块西北缘的次一级大地构造单元，夹持于文县—康县大断裂和枫相—铜钱区域韧性剪切带之间，碧口古陆西北缘大断裂通过本区，区域构造线呈NEE向展布[2, 5-6]。
研究区东西长8 km，南北宽7 km，面积约55 km2，主要包括昌河坝、馍馍山及巩家山三个矿段。
地层主要为古生界中泥盆统三河口群，由老至新依次为桥头组(Dq)、屯寨组下、中、上段(Dt1、Dt2、Dt3)和羊汤寨组下岩段(Dy1)，岩性为含碳微粒灰岩、中厚层灰岩夹绢云石英千枚岩、含碳千枚岩及含铁石英岩、片理化不等粒斜长石英砂岩、中基性火山岩、含白云质灰岩、绢云石英灰质片岩等。矿化产于屯寨组，含矿岩性以片岩、千枚岩、板岩为主，个别为石英碳酸盐化韧性变形含碳白云母构造片岩。
区内断裂构造发育(图 1)，总体构造形态表现为一北西倾斜的单斜构造，受韧性剪切带及F5断裂的影响，局部表现为背斜，按照走向大致可划分为近东西向和北东向两组，其中东西向F5断裂为主要的导矿断裂，其旁侧的次级断裂为主要的控矿断裂，如F2、F6及F9等。
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图 1 赵家庄金矿区域地质简图1—全新统；2—更新统；3—石炭系—泥盆系益洼沟组；4—泥盆系羊汤寨组上岩段；5—泥盆系羊汤寨组下岩段；6—泥盆系屯寨组上岩段；7—泥盆系屯寨组中岩段；8—泥盆系屯寨组下岩段；9—泥盆系桥头组；10—寒武—震旦系临江组；11—震旦系关家沟组上岩段；12—震旦系关家沟组中岩段；13—震旦系关家沟组下岩性段；14—长城系白杨岩组下岩段；15—花岗闪长斑岩；16—黑云母闪长岩脉；17—石英脉；18—逆断层；19—性质不明断层；20—韧性剪切带。Figure 1. Regional geology sketch map of Zhaojiazhuang gold deposit区域上岩浆活动强烈，研究区内主要以规模较小的岩脉产出，在巩家山、馍馍山及昌河坝矿段均发育有长10余米、宽2~5 m不等的花岗斑岩脉及闪长玢岩脉，且在部分见矿钻孔中发现了花岗斑岩，发育粗粒-细粒黄铁矿，部分钻孔花岗斑岩具有金异常，由此可见区内岩浆活动与金矿化关系密切。
围岩蚀变较发育，常见有黄铁矿化、硅化、碳酸盐化、赤铁矿化、褐铁矿化、高岭土化、绢云母化等，多沿断裂或构造裂隙面呈带状分布。其中，硅化、黄铁矿化、褐铁矿化、碳酸盐化与金矿化呈正相关；高岭土化、绢云母化与金矿化关系不明显。
研究区分别在昌河坝、馍馍山、巩家山三个地段圈定出金矿(化)体数十条，矿体一般长68~85 m，厚度1.03~7.51 m，金品位3.04~8.04 g/t。矿体产状与地产产状一致，走向近东西向，矿体顶底板以结晶灰岩为主。
2. 实验部分
2.1 样品的采集
电子探针分析技术是微束分析中的常规测试技术之一。电子探针因其分析区域小、绝对及相对灵敏度高、分析元素范围广等优点，为地质科学研究提供了重要的研究手段，目前已经成为地学领域中矿物学、岩石学、矿床学及相关学科的重要研究工具[7]。本次研究的样品均是采自赵家庄金矿的钻孔中矿石样品，电子探针和能谱分析样品均为含有黄铁矿的金矿石，样品的显微照片如图 2所示。
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图 2 矿石矿物特征a—平行构造片理排列的他形粒状黄铁矿；b—重结晶黄铁矿；c—次生草莓状黄铁矿；d—重结晶的黄铁矿包裹的黄铜矿。Figure 2. Characteristics of ore minerals2.2 测量仪器与测量条件
本次研究共分析166点，黄铁矿的电子探针分析在长安大学电子探针实验室完成，仪器型号为JXA-8100电子探针分析仪(日本电子公司)，在几百到上千的放大倍数下重点寻找粒径小的金银矿物、硫化物矿物，同时对其成分进行测定，补缺显微镜的局限性，更准确地探讨其赋存状态。仪器分析条件为：加速电压15 kV(硫化物)；束流1×10-8 A；束斑直径5 μm；检出角40°；校正ZAF；温度25℃，湿度55%~60%。分析方法依据国家标准GB/T 15617—2002《硅酸盐矿物的电子探针定量分析方法》和GB/T 15246—2002《硫化物矿物的电子探针定量分析方法》。
3. 结果与讨论
3.1 主要载金矿物及成分特征
通过大量岩石光薄片的镜下观察，初步判断金银矿物的赋存状态，为下一步电子探针分析做准备。对样品进行显微镜下鉴定，根据矿物组成，矿石中金属矿物成分主要为黄铁矿、褐铁矿，少量黄铜矿及自然金，含量约2%；非金属矿物主要有石英、方解石、白云母，少量碳质成分等，含量约95%。
金属矿物中含金矿物主要为黄铁矿。黄铁矿具有三种成因：第一种为早期的破碎黄铁矿(图 2a)，主要分布于变形带中，粒径小于0.02 mm，大多数以碎粒结构为主，分布比较均匀；第二种为变形后重结晶的黄铁矿(图 2b)，粒径0.1~0.25 mm，全部呈重结晶结构，具有半自形特征，其中可见包裹的黄铜矿，粒径0.02 mm；第三种为次生黄铁矿(图 2c)，具有生物结构，以草莓状集合体为主，粒径小于0.002 mm。其中第一种及第三种黄铁矿与成矿作用密切，是金矿物的主要载体。黄铜矿(图 2d)较少，主要被粗粒黄铁矿包裹，粒径0.02 mm，他形粒状结构，包裹黄铁矿平行片理分布。
通过对赵家庄金矿载金矿物开展较为系统的显微照相和电子探针分析，矿石中金属矿物主要为黄铁矿、黄铜矿、毒砂，其次为闪锌矿、方铅矿，并见有少量银金矿。电子探针分析结果表明，赵家庄金矿自然金主要呈“不可见”超显微包裹金形式存在，载金矿物主要为黄铁矿(图 3a)，其次为黄铜矿(图 3b)、闪锌矿(图 3c)。自然金具有较高的成色，颜色为红黄色，包裹于脉石矿物中，粒径0.005 mm；裂隙金显微微细粒嵌布在黄铁矿、黄铜矿、绢云母、石英晶隙及裂隙中，主要赋存于黄铁矿、黄铜矿中，少量赋存于绢云母等黏土矿物之中。
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图 3 载金矿物特征a—黄铁矿；b—黄铜矿；c—闪锌矿(2, 3探针点)；d—毒砂(2探针点)。Figure 3. Characteristics of gold-bearing minerals赵家庄金矿主要载金矿物黄铁矿和黄铜矿中Au、Fe、S、Cu、As等元素的电子探针波谱分析结果列于表 1，数据表明赵家庄金矿各类载金矿物中除了主含量元素外，还有一些微量元素。
表 1 主要载金矿物元素含量分析结果Table 1. Analytical results of elements in gold-bearing minerals测试对象 点号 含量(%) As S Fe Pb Zn Ag Cu Au 总计 黄铜矿 67-1b3-3 - 25.44 9.98 0.11 - 0.02 62.65 0.11 98.31 71-2b1-4 - 33.56 0.58 0.10 64.21 - - 0.15 98.62 闪锌矿 67-1b1-4 0.05 33.03 3.23 0.09 61.75 - - 0.26 98.42 平均值 0.05 33.30 1.91 0.10 62.98 - - 0.20 98.52 67-1b2-5 0.03 49.45 44.31 0.63 - - 0.04 0.13 94.59 67-1b2-5 0.00 52.95 44.49 0.21 0.01 - 0.08 0.16 97.89 67-1b2-5 0.01 51.91 45.68 0.24 - - 0.00 0.10 97.94 67-1b2-6 0.18 51.03 45.05 0.22 0.02 0.06 0.02 0.12 96.70 67-1b2-6 0.13 51.11 43.48 0.30 0.01 0.09 0.04 0.23 95.39 71-2b1-1 0.06 53.81 45.06 0.21 - - - 0.21 99.35 粗晶黄铁矿
(100~200 μm)71-2b1-3 0.04 55.27 45.15 0.17 0.07 0.00 - 0.18 100.87 71-1b1-3 - 51.03 45.59 0.20 0.01 0.02 0.02 0.12 96.98 71-1b1-4 0.02 50.96 45.49 0.28 0.04 - 0.00 0.13 96.92 67-1b1-2 0.00 53.49 46.34 0.23 0.11 - 0.04 0.11 100.31 67-1b1-3 0.01 53.34 45.81 0.18 0.04 - - 0.14 99.52 67-1b1-4 - 53.18 45.64 0.20 - - - 0.15 99.17 平均值 0.05 52.29 45.17 0.26 0.04 0.04 0.03 0.15 97.97 67-1b4-4 - 53.20 45.94 0.15 0.03 - - 0.22 99.54 67-1b4-4 - 53.00 45.57 0.17 - 0.02 0.01 0.23 99.00 67-1b4-3 - 53.31 45.49 0.24 0.03 0.03 - 0.23 99.33 67-1b4-2 - 52.41 45.69 0.12 0.02 - - 0.11 98.35 67-1b4-1 0.02 53.31 45.93 0.19 0.07 - - 0.14 99.67 67-1b4-1 0.02 52.96 45.95 0.16 - 0.02 0.03 0.19 99.32 细晶黄铁矿
(20~50 μm)67-1b4-1 0.01 53.12 45.71 0.14 - 0.01 - 0.12 99.11 71-2b3-1 0.02 52.68 46.78 0.18 0.02 - 0.03 0.11 99.82 71-2b3-3 - 51.31 46.02 0.24 0.04 0.01 - 0.21 97.84 67-1b1-3 - 53.33 45.91 0.19 - 0.04 - 0.22 99.69 平均值 0.02 52.86 45.90 0.18 0.03 0.02 0.02 0.18 99.17 71-2b2-3 2.99 50.11 44.10 0.20 - 0.03 0.01 0.19 97.62 71-2b2-4 1.10 49.86 45.85 0.21 - 0.01 0.01 0.10 97.14 草莓状黄铁矿
(15~30 μm)71-2b2-4 2.12 50.91 45.40 0.12 0.04 - - 0.14 98.73 71-2b2-5 2.06 51.52 46.15 0.26 0.12 0.03 - 0.15 100.27 平均值 2.07 50.60 45.38 0.20 0.08 0.02 0.01 0.14 98.44 黄铜矿中Au的含量为0.11%，Pb和Ag含量分别为0.11%、0.02%；闪锌矿中Au平均含量为0.20%，As和Pb平均含量分别为0.05%、0.10%；粗晶黄铁矿中Au平均含量为0.15%，As、Pb、Zn、Ag、Cu平均含量分别为0.05%、0.26%、0.04%、0.04%、0.03%；细晶黄铁矿中Au平均含量为0.18%，As、Pb、Zn、Ag、Cu平均含量分别为0.02%、0.18%、0.03%、0.02%、0.02%；草莓黄铁矿中Au平均含量为0.14%，As、Pb、Zn、Ag、Cu平均含量分别为2.07%、0.20%、0.08%、0.02%、0.01%。
载金矿物中存在金的富集点，如闪锌矿中67-1b1-4点Au含量为0.26%；粗晶黄铁矿67-1b2-6点Au含量为0.175%；细晶黄铁矿中67-1b4-3、67-1b4-4点Au含量为0.23%；草莓状黄铁矿中71-2b2-3点Au含量为0.19%。在500倍显微镜下，几乎未发现显微可见金，显示金矿中Au以机械混入的“不可见”显微-超显微包体金形式存在于载金矿物中[8-12]。赵家庄金矿各主要载金矿物中Au含量依次为：闪锌矿＞细晶黄铁矿＞粗晶黄铁矿＞草莓状黄铁矿＞黄铜矿，但由于闪锌矿较少，电子探针点少，数据出现偶然较高的现象，不具有普遍性，总体金含量依次为：细晶黄铁矿＞粗晶黄铁矿＞草莓状黄铁矿＞黄铜矿。
3.2 面扫描分析
根据各脉体及矿物之间的穿切关系，矿石标本、光薄片观察到的矿石组构、矿物组合及其特征，结合前人的数据，赵家庄金矿的成矿作用可分为沉积成岩期、热液期和表生氧化阶段[3]。沉积成岩期主要以少量草莓状黄铁矿为主(图 2b)，零星分布于含矿地层中；热液期黄铁矿大多数以细晶黄铁矿为主，少量为草莓状、粗晶黄铁矿，热液阶段的黄铁矿主要呈自形(图 4a)和半自形的晶型(图 4b)，赋金黄铁矿又以细粒自形为主，莓球状、粗粒以及条带状次之。这些黄铁矿成因复杂，并且可能普遍受到热液蚀变作用影响，产于石英脉裂隙中；表生氧化期主要是沉积成岩期和热液阶段的黄铁矿在表生条件下发生氧化，形成褐铁矿等，可产生金的次生富集[3]。
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图 4 热液期呈自形(a)和半自形(b)黄铁矿Figure 4. Automorphic (a) and subhedral (b) crystal pyrites of hydrothermal stage本次研究主要对赵家庄金矿12件探针片中的粗晶黄铁矿(100~200 μm)、细晶黄铁矿(20~50 μm)、草莓状黄铁矿(15~30 μm)及黄铜矿等主要载金矿物进行了电子探针面扫描图像及元素定量分析。在黄铁矿和黄铜矿等载金矿物中，Fe、S、Cu等主要组成元素较均匀地分布，清楚地显示了黄铁矿中主要组成元素Fe、S以及黄铜矿中Fe、S、Cu的分布状态。在粗晶黄铁矿、细晶黄铁矿以及黄铜矿中均可见到Au的分布，并且Au的含量比其周边非金属矿物要高出许多。但在这些金属硫化物的内部，Au分布并不均匀[3, 13-15]。不同时期的黄铁矿(粗晶黄铁矿、细晶黄铁矿、草莓状黄铁矿)中Au的分布也不均匀，存在差异性，主要表现为在细晶黄铁矿和草莓状黄铁矿中的Au含量有增加趋势，这种现象说明此类黄铁矿为后期构造热液阶段形成，金含量更高[4, 16-17]。
3.3 金的存在形式
显微镜下和电子探针分析显示，研究区矿石中金的存在形式主要有两种：一种为“可见金”，另一种为“不可见金”[6, 18]。其中，可见金(一般扫描电镜下可见，粒度＞0.001 mm)包裹于脉石矿物中，或者以裂隙金的形式嵌布在黄铁矿、黄铜矿、绢云母、石英晶隙及裂隙中，主要赋存于黄铁矿、黄铜矿中，少量赋存于绢云母等黏土矿物之中，颗粒粒径为0.002~0.005 mm。
“不可见金”指的是在一般扫描电镜下不能检出的次显微金(＜0.001 mm)[18]，国内外研究者对此开展了大量工作，大多数学者认为金主要以Au+和Au0的价态存在，少数学者认为金的价态是Au3+和Au-。近年来许多光谱技术及高分辨率分析研究结果都表明，金在含砷黄铁矿中以两种形式存在：Au+和Au0[3, 18-21]，Reich(2005)将美国多个低温热液型和卡林型金矿黄铁矿分析数据投入logAu-logAs图中，总结出一条被称为“溶解度限度线”(CAu=0.02CAs+4×10-5)，并以此来判断含砷黄铁矿中金的存在形式[18]；溶解度线以上的含砷黄铁矿中的金为纳米级自然金(Au0)，溶解度线以下的含砷黄铁矿中的金主要以固溶体(Au+)形式存在。如图 5所示，研究区金矿含砷黄铁矿分析数据点全都位于溶解度线以上，表明含砷黄铁矿中的金主要以纳米级颗粒金形式存在。
综上，研究区金主要有两种存在形式：“可见金”包裹于脉石矿物中，或以裂隙金的形式嵌布在矿物晶隙及裂隙中；“不可见金”以纳米级颗粒金的形式存在于载金矿物中。
4. 结论
通过电子探针面扫描图像及元素定量分析技术，对赵家庄金矿床主要载金矿物黄铁矿的元素含量、形态特征及矿物之间的空间分布关系进行研究，分析显示主要载金矿物为黄铁矿、黄铜矿、毒砂、闪锌矿等，主要载金矿物中Au含量依次为：细晶黄铁矿＞粗晶黄铁矿＞草莓状黄铁矿＞黄铜矿。不同时期的黄铁矿(粗晶黄铁矿、细晶黄铁矿、草莓状黄铁矿)中Au的分布均匀，但也存在差异性，主要表现为在细晶黄铁矿和草莓状黄铁矿中Au的含量有增加趋势，这种现象表明此类黄铁矿的金含量更高，为后期构造热液阶段形成。金主要有两种存在形式，“可见金”包裹于脉石矿物中，或以裂隙金的形式嵌布在矿物晶隙及裂隙中；“不可见金”以纳米级颗粒金的形式存在于载金矿物中。
通过本次研究，为研究矿床成因、成矿过程及成矿机理提供了佐证，且该技术为一些微细矿物分布、组合规律及其与非矿石的关系研究提供了一套方法，同时对后期矿石的选冶提供了技术基础，易于根据含金矿物的特征选择合适的选冶方法。
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