过程能力指数在化探样品分析质量评估中的应用

过程能力指数(C_PK)是衡量工序能力满足产品质量标准要求程度的量值,C_PK越大,产品质量越高,同时考虑到生产加工的经济性,通常将C_PK控制在一个可以接受的水平。本研究首次将工业生产常用的过程能力指数方法运用于地矿实验室分析质量评估,通过计算西藏1:20万罗拉木等两个图幅化探样品中插入的西藏地区沉积物成分分析标准物质(GBW 07320、GBW 07325、GBW 07328)共114个检测项目的过程能力指数,综合评价样品分析数据的整体质量。结果表明,所有检测项目的C_PK均大于C_PK允许值,Na₂O、MgO、Al₂O₃、SiO₂等63个检测项目的C_PK>1.33,Cu、Li、Be、W等47个项目的C_PK>0.67,Th、Ag、Cr、Hg等4个项目的C_PK<0.67。对于过程能力较差的检测项目应列入质量改进计划,如通过能力验证试验、选择合适的标准物质、仪器期间核查、标准化操作、分析技术改进等措施提高分析数据的准确度和稳定性。过程能力指数的应用为化探样品分析测试质量评价提供了一种简便快捷、科学合理的质量评价方法,可为不同检测项目分析方案的合理选择提供依据,同时有效降低实验室经济成本。     

P507萃淋树脂分离-电感耦合等离子体质谱法快速测定化探样品中的银

应用电感耦合等离子体质谱法(ICP-MS)测定化探样品中低含量的Ag时,常受到Zr、Nb氧化物离子91Zr16O和93Nb16O的严重干扰,使得低含量Ag结果误差较大.本文报道了一个简易的测定化探样品中Ag的新方法,将用于ICP-MS测定常规微量元素的溶液通过P507萃淋树脂交换柱,Zr、Nb等干扰元素被P507树脂强烈吸附,而Ag和内标元素Rh通过交换柱,实现了化探样品中待测元素Ag和内标元素Rh与干扰元素Zr、Nb的有效分离,Ag和Rh的回收率达到95％以上,检出限为0.05 μg/g,标准样品的测定结果准确可靠.该方法在测定常规微量元素的基础上,不需要另外称样及处理样品,相对于其他方法,流程简单、快速,适合化探样品Ag的测定,且树脂经氢氟酸处理后可重复使用,降低了实验成本.     

水样中溶解性无机碳同位素测试前处理方法对比研究

水中溶解性无机碳(DIC)的碳同位素前处理方法由传统的BaCl2沉淀法,逐步发展到野外采样后直接通过连续流系统(GasBench-IRMS)测试.当前对于BaCl2沉淀法和连续流测试结果的差异,以及最佳DIC的前处理方法均需要开展深入研究.本文应用BaCl2沉淀法、医用无菌高密度聚乙烯瓶装样、GasBenchⅡ顶空样品瓶野外直接生成CO2气体三种前处理方法,对比研究前处理方法对采自桂林盘龙洞洞穴滴水和地下河水样中DIC碳同位素测试的影响.结果表明,由于BaCl2沉淀法使水样中游离CO2逸出,导致测定的DIC碳同位素值相对于另两种方法均偏正:地下河水样的碳同位素值最大偏正0.26‰;洞穴滴水的碳同位素值最大偏正0.33‰.因为野外水样采集环境的温度、大气压强与实验室内部环境变化较小,没有引起CO2、HCO3的溶解度改变,用医用无菌高密度聚乙烯瓶和GasBenchⅡ顶空样品瓶采集水样的碳同位素测试结果相同;相对而言,利用GasBenchⅡ顶空样品瓶直接产生CO2气体,能够避免外界环境条件变化导致CO2、HCO3-的溶解度发生变化引起碳同位素分馏,是精确测定水中DIC碳同位素最佳的前处理方法.     

硫磷混酸溶矿测定矿样中铝、铬方法研究

硫磷混酸溶矿分解,ICP-AES同时测定不同样品中铝、铬含量.样品分解完全,操作简便,检测快速,结果稳定,准确度高.铝、铬的检出限分别为0.0042μg/ml、0.0036 μg/ml,RSD分别为0.33％、1.33％,回收率在97.8％～104％之间.     

ICP-AES法同时测定地质样品中Cu-Pb-Zn-Sc-Mo

样品经盐酸和硝酸溶解、氢氟酸助溶、高氯酸冒烟排除氢氟酸及盐酸溶解盐类处理后,电感耦合等离子体发射光谱法(ICP-AES)可同时准确测定地质样品中Cu-Pb-Zn-Sc-Mo,方法检出限为Cu(3μg/g)、Pb(2μg/g)、Zn(2μg/g)、Mo(3μg/g)和Sc(1μg/g)。用国家标样及内部控制样品进行验证,相对标准偏差为0.89%².88%。建立的分析方法具有测定范围宽、结果准确、操作简便、适合批量样品测定等优点,分析方法精密度满足《地质矿产实验室测试质量管理规范》的要求。     

黔西南灰家堡金矿田有机岩相学和地球化学

灰家堡金矿田是黔西南卡林型金矿床的集中产地之一,对其中的水银洞、紫木凼、太平洞和簸箕田4个代表性金矿床进行了有机岩相学和地球化学研究。灰家堡金矿田的矿床中固体沥青主要产于矿石内,与矿化关系密切,产出形态受孔隙、构造裂隙控制;沥青与热液期矿物的共生组合关系表明其形成时间与成矿时间大致一致。矿石中普遍发育有机质包裹体。有机地球化学特征表明,金矿石和围岩中的有机质成熟度均较高,经历了类似的地质作用过程;有机质形成于强还原、中低盐度的沉积环境;有机质来源以海相菌藻类等低等生物为主,有少量陆源高等植物的输入。     

Optical properties of estuarine dissolved organic matter isolated using cross-flow ultrafiltration

Dissolved organic matter(DOM) from freshwater, mid-salinity, and seawater endmember samples in the Jiulong River Estuary, China were fractionated using cross-flow ultrafiltration with a 10-kDa membrane. The colloidal organic matter(COM; 10 kDa–0.22 μm) retentate, low molecular weight(LMW) DOM(10 kDa) permeate, and bulk samples were analyzed using absorption spectroscopy and three-dimensional fluorescence excitation-emission-matrix spectroscopy. The UV-visible spectra of COM were very similar to those obtained for permeate and bulk samples, decreasing monotonically with increasing wavelength. Most of the chromophoric DOM(CDOM, expressed as the absorption coefficient a355) occurred in the LMW fraction, while the percentage of CDOM in the colloidal fraction was substantially higher in the freshwater endmember(13.4% of the total) than in the seawater endmember(6.8%). The bulk CDOM showed a conservative mixing behavior in the estuary, while there was removal of the COM fraction and a concurrent addition of the permeate fraction in the mid-salinity sample, implying that part of the colloidal CDOM was transformed into LMW CDOM. Two humic-like components(C1: 250, 325/402 nm; and C2: 265, 360/458 nm) and one protein-like component(C3: 275/334 nm) were identified using parallel factor analysis. The contributions of the C1, C2, and C3 components of the COM fraction to the bulk sample were 2.5%–8.7%, 4.8%–12.6%, and 7.4%–14.7%, respectively, revealing that fluorescent DOM occurred mainly in the LMW fraction in the Jiulong River Estuary. The C1 and C2 components in the retentate and permeate samples showed conservative mixing behavior, but the intensity ratio of C2/C1 was higher in the retentate than in the permeate fractions for all salinity samples, showing that the humic component was more enriched in the COM than the fulvic component. The intensity ratio of C3/(C1+C2) was much higher in the retentate than in the permeate fraction for mid-salinity and seawater samples, revealing that the protein-like component was relatively more enriched in COM than the humic-like component. The contribution of the protein-like component(C3) to the total fluorescence in the retentate increased from 14% in the freshwater endmember to 72% for the seawater endmember samples, clearly indicating the variation of dominance by the humic-like component compared to the protein-like component during the estuarine mixing process of COM.     

Archaeal diversity and abundance within different layers of summer sea-ice and seawater from Prydz Bay,Antarctica

Fluorescence in-situ hybridization （FISH） and 16S rRNA gene clone library analyses were used to determine the abundance and diversity of archaea in Prydz Bay, Antarctica. Correlation analysis was also performed to assess links between physicochemical parameters and archaeal abundance and diversity within the sea-ice. Samples of sea-ice and seawater were collected during the 26th Chinese National Antarctic Research Expedition. The results of FISH showed that archaea were relatively abundant within the top layer of the sea-ice, and correlation analysis suggested that the concentration of 4NH＋ might be one of the main factors underlying this distribution pattern. However, using 16S rRNA gene libraries, archaea were not detected in the top and middle layers of the sea-ice. All archaeal clones obtained from the bottom layer of the sea-ice were grouped into the Marine Group I Crenarchaeota while the archaeal clones from seawater were assigned to Marine Group I Crenarchaeota, Marine Group II Euryarchaeota, and Marine Group III Euryarchaeota. Overall, the ifndings of this study showed that the diversity of archaea in the sea-ice in Prydz Bay was low.     

“海洋六号”首航科考成果通过验收

正近日,中国大洋协会办公室组织专家对中国大洋23航次报告进行验收。专家组审阅了航次资料和样品测试数据汇交情况,听取了航次首席科学家何高文的汇报,一致同意通过验收,报告评审为优秀。经过近两年的室内研究,项目主要取得了五方面研究成果:获取7000米级下潜区地质和环境资料,提出了"蛟龙"号7000米级海试下潜区方案;揭示了新调查海山的地形地     

川西北天井山古隆起固体沥青地球化学特征及其地质意义

为探究川西北地区天井山古隆起固体沥青地球化学特征、成因和来源及其地质意义,采集研究区寒武系、泥盆系和二叠系20块野外露头沥青样品,通过固体沥青族组成、生物标志化学物、碳同位素等分析测试,结合构造演化史,建立研究区沥青动态演化形成模式.结果表明:天井山古隆起固体沥青是古油藏遭受严重生物降解而形成的,寒武系和泥盆系沥青来源于筇竹寺组烃源岩,二叠系沥青来源于筇竹寺组和二叠系烃源岩的混合.天井山古隆起经历大面积古油藏聚集,沥青封堵保存条件较好的翼部是古油藏的有利勘探目标.该结果为川西北地区天井山构造勘探与开发提供指导,也为类似的构造演化复杂地区沥青形成与油气演化研究提供借鉴.