ELEMENTAL CONCENTRATIONS IN NINE NEW JAPANESE ROCK REFERENCE SAMPLES

Twenty-eight major, minor and trace elements in nine new rock reference samples of Geological Survey of Japan (GSJ), JA-2, JA-3 JB-1a, JG-1a, JG-2, JG-3, JF-1, JF-2 and JP-1 have been determined using atomic absorption spectrometry, flame emission spectrometry and wet chemical techniques.     

气化—离子色谱法测定岩石中的氯

氯的化学性质活泼,在酸性介质中具有挥发性,由碱性物质吸收,样品在密封的气化吸收器中经处理后用离子色说测定,无污染,操作简单,精度与准确度高,该法用于多种样品的分析,获得较满意的结果。     

DETERMINATION OF PHOSPHOROUS IN FIFTY-NINE GEOCHEMICAL REFERENCE SAMPLES BY EXTRACTIVE SPECTROPHOTOMETRY

A digestion procedure with sequential use of HF-HCl and HNO₃-HClO₄ involving yellow vanadium molybdophosphate complex and its extraction into isobutylmethylketone (IBMK) has been employed for estimation of phosphorus in 59 geochemical reference samples. The agreement between the results obtained from IBMK-extraction and the recommended values has been found to be better than those available from the usual procedures (i.e., estimation in the aqueous phase).     

氧氢碳稳定同位素综合分析研究及标准样品的测定

利用已有的一套真空装置(BrF_5法氧同位素分析装置),通过活动小系统交替上的方式进行了水的CO_2—H_2O平衡法,碳酸盐的18O、13C测试磷酸法,水的氧同位素分析金属锌法以及矿物结构水、包体水的同位素组成分析。对上述方法都用国际标准(V-SMOW、GISP、SLAP的δ18O值和NBS-18、NBS-19的δ18O与δ13C测定结果)检验了试验水平。其测定值与世界各实验室的平均值或推荐值在实验误差范围内基本上是吻合的。实践证明,应用一个真空实验装置进行氧氢碳稳定同位素多种方法综合测试是可行的。     

DETERMINATION OF BROMINE AND IODINE IN FOUR MARINE SEDIMENT REFERENCE SAMPLES BY ENERGY-DISPERSIVE X-RAY FLUORESCENCE SPECTROMETRY

The concentrations of bromine and iodine in the USGS marine mud MAG-1, the NRCC marine sediments BCSS-1 and MESS-1, and the NBS estuarine sediment SRM 1646 have been determined by energy-dispersive x-ray fluorescence spectrometry. Matrix and intermediate thickness effects were overcome by standard additions to constant weights of each sample. 3-sigma detection limits are 6 ppm Br and 24 ppm I. There is a need for many more analysts to report their results before "usable values'can be established for these elements in marine sediment reference malterials.     

5－Br－PADAP分光光度法测定岩矿中的微量铌

２－［（５－溴－２－吡啶）偶氮］５－二乙氨基苯酚（简称５－Ｂｒ－ＰＡＤＡＰ）是一种高灵敏度显色剂，它与Ｎｂ（Ｖ）、酒石酸形成蓝色的三元络合物。其最大吸收峰为６１０ｎｍ，表观摩尔吸光系数为５．９×１０￣４Ｌ·ｍｏｌ￣（－１）·ｃｍ￣（－１），络合物在２５ｍｌ溶液中，ρ（Ｎｂ＿２Ｏ＿５）／（μｇ·ｍｌ￣（－１））为０－１．６符合比尔定律。络合物可稳定２４ｈ以上。以ＥＤＴＡ－Ｃａ消除共存离子的干扰，本法的选择性较好，准确度高，且简便、快速。适用于各种岩矿中微量Ｎｂ的测定。     

密闭溶样-活性炭吸附-化学光谱法测定化探样品中的痕量铂

通过对介质酸度、缓冲剂、活性炭用量进行试验，建立针对化探样品中痕量铂的测定方法。经过化探标样考核，表明该方法快速准确、劳动强度低。     

DETERMINATION OF MERCURY IN ONE HUNDRED AND EIGHTEEN GEOCHEMICAL REFERENCE SAMPLES BY COLD VAPOR ATOMIC ABSORPTION SPECTROMETRY

The mercury content of 118 geochemical reference samples have been determined by combustion followed by cold vapor atomic absorption spectrometry. The negative interference from volatile halogen and sulfur was eliminated by a packing of sodium carbonate in the combustion tube and addition of magnesium oxide to the samples. A comparison with published data show clearly the need for much more data on most reference samples.     

沉积岩中有机碳的测定

引言在沉积岩的形成和变化过程中,特别是在成岩过程中,有机质在促进各种元素的迁移、富集和使它们从一种矿物转变为另一种矿物上,有着很大的作用。近年来,有机地球化学的研究,不仅在可燃性有机岩方面有很大的进展,而且在沉积非金属和金属矿床,特别是在稀有分散元素和放射性元素矿床的研究中,也得到了极大的重视和发展。在一般沉积岩中常或多或少的含有有机质,但目前还没有直接测定其总含量的简便完善的方法。由于碳是有机质的主要组成元素,因此普通采用岩石中的有机碳含量作为有机质总含量的标志。由于工作的需要,我们对测定有机碳的湿烧法进行了试验研究,并在测定方法上作了一些改进。现将该方法报导如下,请批评指正。     

硫酸银催化容量法快速测定土壤中的有机碳

在硫酸溶液中，以Ag2SO4为摧化剂，加入过量K2Cr2O7标准溶液氧化土壤中的有机碳，然后用FeSO4标准溶液滴定剩余的K2Cr2O7标准溶液，返滴定法测定有机碳含量。实验测得S为0．0186(n＝15)，RSD％为3．60(X^-＝0．518％)；到定土境和水系沉积物等国家标准物质中有机碳的含量，相对误差小于11．5％。     

DETERMINATION OF TWELVE TRACE ELEMENTS IN TWENTY-SEVEN AND TEN MAJOR ELEMENTS IN TWENTY-THREE GEOCHEMICAL REFERENCE SAMPLES BY X-RAY FLUORESCENCE SPECTROMETRY

This study reports the results of twelve trace elements in twenty-seven International geochemical reference samples (IGRS) (15 from Japan, 7 from South Africa, 4 from France and 1 from U.S.A.). Similarly, ten major elements were also determined in twenty-three GRS (15 from Japan, 5 from South Africa, 2 from France and 1 from U.S.A.). Whenever possible, the results are compared with literature values for these GRS.     

高压密闭罐溶样-氢化物原子荧光法测定环境样品中的硒

使用浓HNO3 HF混合液和浓HNO3液分别在高压密闭罐中消解土壤、沉积物、岩石和植物样品,6 mol/L HCL加热还原样品后用氢化物发生-原子荧光光谱法(HG-AFS)测定样品中的硒.使用该法对土壤标准参考物质GSS-4、GSS-5、GSS-6、GSS-7和植物标准GSV-1、GSV-3进行了分析,硒的测定结果与推荐值一致.加标回收实验的回收率在98.0%～101.4%,平均为99.8%.实测样品中的硒与中子活化分析(NAA)和氢化物-多接受杯质谱计(HG-MC-ICP- MS)的分析结果基本一致,表明该法平行样的重现性好,分析速度快,提高了硒分析的准确度和分析精度.     

巯基棉富集-氢化物发生原子荧光法测定地质样品的总硒含量

地球化学标准参考物质和不同的地质样品均分别采用消解方式A(硝酸、高氯酸混合液)、B(硝酸、高氯酸、氢氟酸混合液)体系消解,样品预先用巯基棉(TCF)吸附装置分离富集,通过氢化物发生原子荧光光谱法(HG-AFS)测试.实验优化了Se(Ⅵ) 到 Se(Ⅳ)的还原效果、仪器条件、TCF吸附条件.两种消解体系所测得结果有很好的一致性,相关系数为0.9986.对于含硒量为0.04 μg/g样品,方法的相对标准偏差为10.2%.A、B体系标准加入法的回收率分别为96%～106%和99%～104%.     

DETERMINATION OF FLUORINE, CHLORINE, BROMINE AND IODINE IN SEVEN GEOCHEMICAL REFERENCE SAMPLES

The concentrations of fluorine, chlorine, bromine and iodine of seven geochemical reference samples have been determined. Analytical techniques were neutron activation analysis for chlorine, bromine and iodine and ion-selective potentiometry for fluorine. After irradiation of the samples, these halogens were separated from the matrix elements by pyrohydrolysis in presence of vanadium (V) oxide. This extraction allows to measure the four halogens in the same sample.     

用ICP－MS准确测定岩石样品中的40余种微量元素

本文建立了一种用ＨＦ＋ＨＮＯ３，密封溶解样品、以ＵＳＧＳ标准岩石样品ＢＣＲ－１作参考标准、外加质量监控样品测定岩石样品中微量元素的ＩＣＰ－ＭＳ分析方法。该方法具有简单、准确、测定元素多的特点。用该方法对ＵＳＧＳ和ＡＧＳＯ的标准岩石样品中４０余种微量元素进行测定，结果表明，除个别元素的分析结果与推荐值偏差接近或略大于１０％外，绝大多数元素的分析结果与推荐值偏差在５％以内。     

DETERMINATION OF RARE EARTH ELEMENTS IN SIXTEEN SILICATE REFERENCE SAMPLES BY ICP-MS AFTER TM ADDITION AND ION EXCHANGE SEPARATION

This study reports the results of thirteen rare earth elements (REE) in sixteen geochemical reference samples. The analytical procedure involved dissolution of a whole rock or mineral separate, spiking with Tm, and separation of the REE using a simple ion-exchange chromatography procedure. The resulting REE solutions were analysed by ICP-MS. The results are compared with literature values. The agreement between our data and recommended or ID-TIMS values is very favorable. The precision of the technique is better than 5% (2) for all the REE.     

岩石样品中某些微量元素的X射线荧光光谱测定

本文研究了以粉末样品直接压片,铑靶X光管的康普顿散射线作内标和背景的扣除,测定地质样品中微量铌、锆、钇、铷、锶、铀、铜和锌等元素的X射线光谱分析方法。本法具有制备样品简便快速、扣除背景简易准确以及能较好地克服基体效应、方法检测限较低(<2ppm)等优点。方法的精密度与准确度符合分析误差要求。因而本法是测定岩石样品中微量元素的一种简便快速且又较为准确的分析方法。     

INSTRUMENTAL DETERMINATION OF INDIUM IN GEOCHEMICAL REFERENCE SAMPLES BY EPICADMIUM NEUTRON ACTIVATION ANALYSIS AND KO -STANDARDIZATION

The determination of indium in geological materials is difficult by usual analytical techniques because of their lack of sensitivity. Neutron activation analysis with special irradiation and counting conditions allows to determine indium ultra-traces with a quantitative detection limit about a few parts per billion. The method developed is fast and very sensitive and has been tested successfully for several American and French geochemical standards.     

内蒙古达里湖全新世有机碳氮同位素记录与环境演变

内蒙古中东部的达里湖为一水文封闭型湖泊,位于现今东亚夏季风的北部边缘区,对区域环境变化十分敏感.本文对达里湖沉积中心提取的岩芯(DL04沉积岩芯)顶部8.5m沉积物进行了有机地球化学分析.15个全岩样品有机质的放射性碳测年结果表明:岩芯顶部8.5m涵盖了过去大约11500年.按约50年分辨率分析的225个总有机碳(TOC)、总氮(TN)含量、总有机碳/总氮(C/N)原子比值数据以及221个有机碳和有机氮稳定同位素(δ13C和δ13C)数据,详细揭示了全新世东亚夏季风边缘区的水文和生态变化历史.在距今11500 ～ 9800日历年(ca1.aB.P.)期间,所有地球化学指标均呈逐渐增大趋势,指示入湖河流逐渐增强,达里湖开始扩张,水生植物生产率逐渐升高;在9800 ～ 7700cal.aB.P.期间,TOC和TN含量以及C/N比值维持稳定高值,δ13C和δ15N值较小,指示湖泊维持高湖面状态,陆源输入和浮游植物生产率较高;在7700～ 5900cal.aB.P.期间,C/N比值和δ15N维持低值,TOC和TN含量呈现更高值,并且波动变化,δ13C值逐渐增大,表明湖面维持高水平,湖水显著变暖,浮游植物生产率显著升高,流域植被大幅度扩张;在5900 ～ 4850cal.aB.P.期间,TOC和TN含量,C/N比值以及δ13C值显著减小,δ15N值显著增大,暗示地表径流显著减弱,达里湖湖面显著下降,湖泊生产率快速下降;从4850cal.a B.P.开始,TOC和TN含量以及C/N比值呈逐渐减小趋势,δ13C和δ15N值呈逐渐增大趋势,表明湖面逐渐下降,湖水盐度、碱度升高,湖水可能变冷,湖泊生产率逐渐下降,流域植被收缩.全新世东亚夏季风边缘区水文和生态环境的变化可能直接或间接受北半球夏季太阳辐射量和区域季风降水强度的共同控制.