基体差异对电感耦合等离子体质谱法测定过程中Ba氧化物产率的影响及其对Eu测定结果校正的研究

电感耦合等离子体质谱（ICP-MS） 测定地质样品中稀土元素的过程中,尤其对于高Ba基体的地质样品,由Ba形成 的氧化物和氢氧化物离子对Eu元素会产生质谱峰的重叠干扰,严重影响Eu测定结果的准确度和精确度。通过标准溶液的 条件实验,测定Ba干扰项相对Ba总量的比例（干扰率） 并进行相应的Eu扣除,是一种解决干扰导致Eu测定结果偏高的思 路。然而该干扰率在不同基质溶液中是否一致,且随着Ba含量变化是否稳定目前尚不明确。本文通过对不同基体溶液中Ba 对Eu干扰率的测定（低分辨模式测定）,发现随着溶液中Ba浓度的变化,同一基体溶液中该干扰率较为恒定,而不同基体 溶液中干扰率有明显的差别。这说明在对Eu测定结果进行干扰扣除时,需要利用匹配的基体溶液来获取准确的Ba干扰 率。应用这种方法扣除得到的Eu结果与质谱的高分辨模式（R=10000） 下的测定结果较为一致,数据的重现性也较为理 想。因此,利用基体匹配的方式来进行Ba对Eu的数学扣除是一种可行的方法。     

电感耦合等离子体质谱法(ICP-MS)测定水系沉积物中的铌钽锆铪

建立电感耦合等离子体质谱法(ICP-MS)测定水系沉积物中铌、钽、锆、铪四种元素的分析方法。将样品与氢氧化钠、过氧化钠混合物放入高温炉中,熔融分解完全,用热水提取,过滤后弃去滤液,将滤纸及沉淀用酒石酸-盐酸溶液溶解,稀释至刻度测定。方法检出限(3s)为:LD(Nb)=0.08μg/g,LD(Ta)=0.04μg/g,LD(Zr)=0.5μg/g,LD(Hf)=0.04μg/g,精密度(RSD%,n=6)为:0.84%~4.21%。该测定方法具有灵敏度高、精密度好、分析速度快、线性范围宽、操作性强等优势。采用该方法对国家一级标准物质进行测定表明,其结果与标准值吻合。此方法已在实际地质调查样品分析中得到应用。     

激光剥蚀等离子体质谱分析中激光剥蚀参数对信号响应的影响

探讨了激光剥蚀等离子体质谱固体微区分析中激光剥蚀参数对元素分析信号灵敏度及稳定性的影响。这些参数包括激光功率、脉冲频率、剥蚀孔经、散焦距离、剥蚀方式等。讨论了优化的激光剥蚀等离子体质谱信号采集及数据处理方式。在全质量范围内选用具有代表性的元素作为研究对象,建立了激光剥蚀的一般性特征规律和266nm紫外激光系统的最佳操作条件。在选定的激光剥蚀参数下,大多数被测元素的检出限为22.8~457ng/g,能够满足固体微区分析的要求。     

氢化物发生-原子荧光光谱法测定地球化学样品中痕量碲

采用焙烧富集分离地球化学样品中痕量Te,并用氢化物发生原子荧光光谱法测定。通过实验确定出方法的最佳实验条件,在此条件下获得的检出限为0.005μg/g,线性范围0.025~10μg/g,精密度(RSD,n=8)为5.03%~9.24%。方法已用于国家一级地球化学标准物质中痕量Te的测定,结果与标准值基本相符。     

辽河盆地冷家油田沙河街组三段储层岩相古地理

辽河盆地在沙河街组三段早期水体较深,主要形成扇三角洲及盆底扇;沙三晚期水体较浅,发育湖泊砂体.依据沉积相分布规律,沙三早、中、晚3个时期可进一步分别划分出湖泊扩张和收缩阶段.盆地西部凹陷的冷家油田为东陡西缓的箕状洼陷.研究区内沙三段的古地理格局是决定相分布的关键因素,河流和湖泊能量相对强弱决定扇体沉积的规模.受相对湖平面变化的影响,纵向扇三角洲主要形成于湖泊扩张时期,并且有相带窄、过渡快、以粗碎屑沉积为主的特点.扇体沉积中主要发育前缘分流河道充填沉积,但位于河口前缘或侧缘的滩坝及前三角洲中的盆底扇局部也较发育.     

成像光谱矿物填图精度兼与矿物丰度关系初探

成像光谱遥感技术在岩石矿物识别和矿物填图方面发挥着越来越大作用,而成像光谱矿物填图的精度问题一直是研究的焦点。文章利用高光谱数据HyMap对新疆东天山地区的矿物填图结果,通过引入矿物填绘分布强度的概念,探索性的分析了成像光谱矿物填图与填绘矿物丰度的关系。     

<Superscript>226</Superscript>Ra, <Superscript>232</Superscript>Th and <Superscript>40</Superscript>K activities in soils of Cuihua Mountain National Geological Park,China

Gamma activity from the naturally occurring radionuclides namely, ²²⁶Ra, ²³²Th, the primordial radionuclide ⁴⁰K was measured in the soil of Cuihua Mountain National Geological Park, China using γ-ray spectrometry technique. The mean activity of ²²⁶Ra, ²³²Th and ⁴⁰K were found to be 27.2 ± 6.5, 43.9 ± 6.2 and 653.1 ± 127.6 Bq kg⁻¹, respectively. The concentrations of these radionuclides were compared with the typical world values and the average activities of Chinese soil. The radium equivalent activity, the air absorbed dose rate, the annual effective dose rate, and the external hazard index were evaluated and compared with the internationally approved values. All the soil samples have Ra_eq lower than the limit of 370 Bq kg⁻¹ and H _ex less than unity. The overall mean outdoor terrestrial gamma dose rate is 66.3 nGy h⁻¹ and the corresponding outdoor annual effective dose is 0.081 mSv.     

Sulfur isotope measurement of sulfate and sulfide by high-resolution MC-ICP-MS

We have developed a technique for the accurate and precise determination of ³⁴S/³²S isotope ratios (δ³⁴S) in sulfur-bearing minerals using solution and laser ablation multiple-collector inductively coupled plasma mass spectrometry (MC-ICP-MS). We have examined and determined rigorous corrections for analytical difficulties such as instrumental mass bias, unresolved isobaric interferences, blanks, and laser ablation- and matrix-induced isotopic fractionation. Use of high resolution sector-field mass spectrometry removes major isobaric interferences from O₂⁺. Standard-sample bracketing is used to correct for the instrumental mass bias of unknown samples. Background on sulfur masses arising from memory effects and residual oxygen-tailing are typically minor (< 0.2‰, within analytical error), and are mathematically removed by on-peak zero subtraction and by bracketing of samples with standards determined at the same signal intensity (within 20%). Matrix effects are significant (up to 0.7‰) for matrix compositions relevant to many natural sulfur-bearing minerals. For solution analysis, sulfur isotope compositions are best determined using purified (matrix-clean) sulfur standards and sample solutions using the chemical purification protocol we present. For in situ analysis, where the complex matrix cannot be removed prior to analysis, appropriately matrix-matching standards and samples removes matrix artifacts and yields sulfur isotope ratios consistent with conventional techniques using matrix-clean analytes. Our method enables solid samples to be calibrated against aqueous standards; a consideration that is important when certified, isotopically-homogeneous and appropriately matrix-matched solid standards do not exist. Further, bulk and in situ analyses can be performed interchangeably in a single analytical session because the instrumental setup is identical for both. We validated the robustness of our analytical method through multiple isotope analyses of a range of reference materials and have compared these with isotope ratios determined using independent techniques. Long-term reproducibility of S isotope compositions is typically 0.20‰ and 0.45‰ (2σ) for solution and laser analysis, respectively. Our method affords the opportunity to make accurate and relatively precise S isotope measurement for a wide range of sulfur-bearing materials, and is particularly appropriate for geologic samples with complex matrix and for which high-resolution in situ analysis is critical.     

超灵敏加速器质谱计测定^32Si样品制备新技术

介绍了制备元素硅的一种化学方法，它可用于ＡＭＳ装置的离子源。含硅的物质溶解在ＨＦ中，用ＬｉＡｌＨ４把ＳｉＦ４还原成ＳｉＨ４，再将ＳｉＨ４加热分解成元素硅，并且沉淀在石墨盘上，用ＡＭＳ测定ｗ３２Ｓｉ／ｗＳｉ总比值，其灵敏度可达１０＾－１３。     

祁连山夏季地形云综合探测试验

2006年和2007年夏季在祁连山冷龙岭西段开展了地形云云量、云状、大气水汽、风场、雨滴谱和雨强等的综合探测试验,以分析祁连山地形云的特征。结果表明：①祁连山区夏季云量丰富,平均云量在6成以上。西南气流天气背景下总云量多达8成;②祁连山夏季无降水日大气水汽非常少,700 hPa以上层大气相对湿度大多在20%以下;③西南气流背景下祁连山南北侧山谷风的共同作用,气流昼间向山顶辐合,夜间向山谷辐散,当水汽条件充足时,极易抬升形成可以产生降水的地形云;④祁连山降水主要由小于1 mm的雨滴组成。