海洋沉积物中石英单矿物的化学分离

海洋沉积物中的石英作为陆源物质的标志性矿物,是古环境和古气候演化的信息载体,已成为古环境和古气候演化研究的重要替代指标.提供了改进了的化学分离海洋沉积物中石英单矿物的方法流程.在流程中的不同阶段可有效去掉全样中的生物组分、粘土矿物和长石等,取得海洋沉积物全样的总陆源矿物、石英+长石、石英的相对和绝对含量,通过计算可获得各种组分的通量,通过粒度分析可获得粒度数据.同一样品的17次重复实验表明,含量结果的平均相对误差仅为2.36%;显微镜和X射线衍射分析检查所分离出的石英纯度可达98%以上;激光粒度分析表明,化学试剂对石英的溶蚀作用不明显,不影响粒度分析结果.     

Direct Current Plasma Emission Spectrometric Determination of Major, Minor and Trace Elements in Microwave Oven Acid Leachates of Powdered Whole Coal Samples

Major concentrations of Al₂O₃, Fe₂O₃, MgO, CaO, Na₂O and K₂O, minor levels of TiO₂, P₂O₅ and thirty petrologically, geochemically and environmentally significant trace elements have been determined in microwave oven acid leachates of whole powdered coal samples by direct current plasma‐atomic emission spectrometry (DCP‐AES). A single sample preparation procedure was suitable for all the determinations with no additional dilution step for major elements solution. Dried samples (0.5 g) were treated in low‐pressure PFA digestion vessels with HF/HCl/HNO₃/HClO₄ acids to quantitatively extract the analytes from the bulk material, while leaving the major part of organic matrix as a residue. The major constituents of geological samples, in particular the easily ionised elements (EIEs) such as alkali and alkaline earths, may complicate the instrumental determinations in DCP‐AES because of differential enhancements of elemental emission intensities and stray light interferences. Taking account of these factors, the coal matrix is considered to have very low major oxide totals as compared to many other common geo‐environmental and related materials (rocks, sediments, soil, ashes etc.). The sample size employed here, while yielding a relatively concentrated solution to cover a wide range of elemental determinations, provided a sample matrix that significantly diminished interferences for DCP measurements. The need for closely matching the unknowns and calibrators was eliminated except for overall acidity and an excess quantity of caesium for EIE buffering. Calibration of the spectrometer was accomplished by simple aqueous single element solutions as high concentration calibrators in addition to a reagent blank as a low concentration calibrator. Two point working curves were established to allow for the maximum concentrations of each element expected in the unknowns. The precision of determinations under routine conditions as well as the reproducibility of the leaching and precision of instrumental measurements have been evaluated. Relative standard deviations (RSD) were of 1–2% for those elements whose concentrations in solid samples were well above the limits of quantification. Method detection limits in the buffered solutions were also evaluated. To evaluate the accuracy of the microwave oven‐DCP method a suite of eight certified coal reference materials of differing rank, were analysed with good agreement with the certified and/or available published data. Results are presented for the uncertified major oxides in the AR series reference materials.     

延迟交联凝胶研制及其在广西某铀矿堵漏应用

针对地质钻探小井眼条件下失返性漏失堵漏技术难题,开展了适用于地质钻探堵漏要求的聚合物交联凝胶研究。采用单因素优选法,优选了交联凝胶体系用各种处理剂,并以环保型植物胶GJ为成胶剂,加入交联控制剂N1及交联剂1号等组分,研制了一种延迟交联凝胶。该凝胶在广西某铀矿勘查ZK6-37-1孔堵漏成功应用,解决了2个孔段失返性漏失问题。研究结果表明,该凝胶具有交联时间可控(交联时间10～75 min)以及较高的凝胶强度（承压≥6 MPa）,在解决失返性漏失方面具有广阔的应用前景。     

聚氨酯泡塑富集硫脲解脱-石墨炉原子吸收光谱法测定地质样品中金铂

泡沫塑料常用于富集常规地质样品中的铂族元素,而富集后往往用高温灰化法解脱,此法操作繁琐,温度过高易使铂配合物分解为王水难以提取的不溶性残渣,导致测试结果不稳定、效率低;单独使用20 g/L硫脲溶液解脱,测试结果的重现性差。本文对此方法进行改进,采用50%王水封闭溶解试样,氯化亚锡还原,聚氨酯泡塑富集,20 g/L硫脲-20%盐酸溶液解脱,石墨炉原子吸收光谱法测定金和铂。在盐酸-氯化亚锡体系中,吸附温度为20℃,振荡时间为30 min时,金和铂的回收率均在95%以上,金和铂的检出限分别为0.23 ng/g和0.39 ng/g,精密度(RSD,n=10)分别为1.8%～10.3%和1.3%～13.3%。经国家一级标准物质验证,测定值和标准值基本相符。该方法泡塑解脱时无需高温灰化,用王水多次提取,在100℃沸水浴中即可一次完成,样品处理快捷。与高温灰化法相比,提取温度大为降低,分析流程简单,显著提高了单次测样量,且干扰小、空白值低,可以满足除王水难溶的铂矿种外大部分地质样品快速测定的需要。     

太白山北坡花粉通量与表土花粉研究

太白山北坡各森林植被带乔木花粉百分比多高于45%,与植被组成类似。高山草甸带捕捉器样品乔木花粉百分比低于15%,与植被组成一致,但表土花粉组合中乔木花粉百分比高于50%,外来花粉数量较多,进行高山带古环境研究应予注意。太白红杉林花粉通量最低,高山灌丛草甸最高。落叶栎林带表土花粉浓度最低,红桦林带最高。表土中松、冷杉属花粉百分比远高于花粉捕捉器,表明其在表土中有较好的保存能力。落叶松属和杜鹃花科花粉在表土及捕捉器中百分比均较低,表明对植被指示性良好。栎属与桦属花粉通量类似,但桦属花粉浓度大于栎属,表明栎属较桦属易于保存。     

Replacement of Dietary Fish Oil with Vegetable Oils Improves the Growth and Flesh Quality of Large Yellow Croaker （Larmichthys crocea）

We investigated the effect of the replacement of dietary fish oil with vegetable oils on the growth and flesh quality of large yellow croaker(Larmichthys crocea). The basal diet(FO) was formulated to contain 66.5% fish meal and 6.4% menhaden fish oil; whereas the other 3 experimental diets were formulated by replacing the fish oil with 50% soybean oil(SO50), 100% soybean oil(SO100) and 100% palm oil(PO100), respectively. The 4 diets were randomly assigned to 4 floating sea cages(3.0 m × 3.0 m × 3.0 m), and each was stocked with 250 fish individuals with an initial average weight of 245.29 g ± 7.45 g. The fish were fed to apparent satiation twice a day at 5:00 and 17:00, respectively, for 12 weeks. Experimental analysis showed that the specific growth rate of fish fed SO50 or PO100 were significantly higher than that of fish fed FO or SO100(P0.05), and crude lipid contents of ventral muscle and viscera were significantly lower in fish fed FO than in those fed the other 3 diets(P0.05). No significant differences in condition factor, viscerosomatic index, hepatosomatic index, gutted yield and colorimetric values of fish among the dietary treatments were observed(P0.05). Compared to FO diet, SO50, SO100 and PO100 diets led to substantial decreases in the liquid loss and water loss from fresh fillets(1 d, 4℃)(P0.05). Similarly, thiobarbituric acid reactive substance(TBARS) values of fillets under different storage conditions(1 d, 4℃; 7 d, 4℃; 4 weeks,-20℃; 8 weeks,-20℃) decreased significantly after partial or complete replacement of fish oil with vegetable oils. These findings indicated that the growth performance and selected flesh quality properties(liquid holding capacity and TBARS value) of large yellow croaker were substantially improved by replacing dietary fish oil with vegetable oils.     

环境植物样品中铜铅锌铁锰的测定

将环境植物样品在４００─５００℃灰化，用硝酸、氢氟酸和高氯酸分解，用盐酸（１＋１）提取，控制２％─３％的盐酸介质，用火焰原子吸收分光光度法测定环境植物样品中的微量铜、铅、锌、铁、锰。该方法简单、快速、可靠。对环境植物标准样品的测定结果理想。     

化探样品中部分元素测定溶矿方法的改进

文章研究了用 1∶1王水分解化探样品中Cu、Pb、Zn、Co、Ni、Fe、Mn等元素新的样品溶解测定方法 ,即王水分解测定法 ,该法的检出限、准确度、精密度均达到 1∶5万化探样品分析要求。此法已用于化探及区域地质普查样品分析 ,并取得了较好效果     

五酸溶样-电感耦合等离子体质谱法同时测定地质样品中的稀土等28种金属元素

电感耦合等离子体质谱法(ICP-MS)测定大批量地质样品中的稀土和钴铪铟锰铌钽铊铬镉镓锗钒锡等金属元素,主要采用三酸或四酸溶解样品.由于地质样品组分复杂,稀土等金属元素含量低,各元素性质差异大,三酸或四酸溶样经常出现易挥发元素如钒铬镉镓锡的测定结果不稳定、镧铈镨钕等稀土元素溶解不完全的问题.本文在盐酸-硝酸-氢氟酸-高...     

电感耦合等离子体质谱法测定地质样品中稀散元素铬镓铟碲铊

采用电感耦合等离子体质谱技术,研究了地质样品中稀散元素铬、镓、铟、碲、铊含量的质谱分析方法。研究确定了最佳测定酸度、干扰元素的校正方法,结果令人满意。方法检出限为0.001 3~0.063μg/g,精密度(RSD,n=11)为2.00%~4.87%,优于其他方法,具有较好的灵敏度。方法快速、简便,结果准确,可用于地质样品中稀散元素铬、镓、铟、碲、铊含量的分析,适用于批量样品的快速测定。