封闭消解-阳离子交换分离-电感耦合等离子体质谱法测定铜铅锌矿石中的铼

阴离子交换树脂已被应用于酸法消解-电感耦合等离子体质谱(ICP-MS)测定铜铅锌矿石等地质样品中铼的分离富集,样品溶液中的ReO_4~-用树脂交换吸附后再用洗脱剂将ReO_4~-选择性洗脱,该方法流程长,影响其稳定性和准确性。本文以基体元素为吸附交换目标,用8 g的732强酸型阳离子交换树脂在2%硝酸介质条件下静态吸附1.5 h,可有效地消除基体元素的影响。用空矿(石英)稀释低含量铼的样品做空白试验,获得方法检出限为0.004μg/g,精密度(RSD)小于6%,加标回收率为96%~104%。本方法应用的732强酸型阳离子交换树脂在适宜酸度条件下,对矿石中除钨、钼以外的金属元素吸附率高达95%以上,降低了样品溶液离子强度和干扰元素浓度,实现了ICP-MS的直接测定,操作方法比阴离子交换吸附法简便。     

Separation of Clay Minerals from Host Sediments Using Cation Exchange Resins

Classic physical and chemical treatments applied to separating clay minerals from the host sediments are often difficult or aggressive for clay minerals. A technique using cation exchange resins (amberlite IRC-50H and amberlite IR-120) is used to separate clay minerals from the host sediments. The technique is based on the exchange of cations in the minerals that may be associated clay minerals in sediments, such as Ca and Mg from dolomite; Ca from calcite, gypsum and francolite with cations carried by resin radicals. The associated minerals such as gypsum, calcite, dolomite and francolite are removed in descending order. Separation of clay minerals using cation exchange resins is less aggressive than that by other classic treatments. The efficiency of amberlite IRC-50H in the removal of associated minerals is greater than that of amberlite IR-120.     

D190型大孔巯基树脂分离富集原子吸收光谱法测定地质样品中微量金和钯

采用D190 型大孔巯基树脂分离富集微量金和钯 ,研究了各种条件对分离富集和测定的影响 ,证明了金和钯在 3 %王水介质中形成氯络阴离子与树脂上的巯基 (-SH)发生螯合作用形成螯合物而迅速地被吸附在树脂上。同时 ,溶液中一些贱金属离子不易与巯基生成螯合物而分离。采用酸性硫脲定量洗脱 ,树脂结构不被破坏 ,可重新使用     

垦西特稠油化学降粘机理的研究

详细研究了胜利油田垦西特稠油中的胶质、沥青质用降粘剂处理前后的红外特征吸收峰和透射电镜照片的变化。由红外光谱数据和透射电镜分析可知,降粘剂分子借助强的形成氢键的能力和渗透、分散作用进入胶质和沥青质片状分子之间,破坏了胶质、沥青质分子平面重叠的聚集体,使聚集结构变得疏松,表明聚集有序性降低是稠油降粘的主要机理。     

Chemistry of marine resources－XIX． The molecule design and synthesis of crow－link type Alkyd resin and its enrichment behaviour For potassium ion in sea water

Ｃｈｅｍｉｓｔｒｙｏｆｍａｒｉｎｅｒｅｓｏｕｒｃｅｓ－ＸＩＸ．Ｔｈｅｍｏｌｅｃｕｌｅｄｅｓｉｇｎａｎｄｓｙｎｔｈｅｓｉｓｏｆｃｒｏｗ－ｌｉｎｋｔｙｐｅａｌｋｙｄｒｅｓｉｎａｎｄｉｔｓｅｎｒｉｃｈｍｅｎｔｂｅｈａｖｉｏｕｒｆｏｒｐｏｔａｓｓｉｕｍｉｏｎ...     

海洋资源的化学 Ⅻ、O,O_-''''邻苯二酚二乙酸—甲醛树脂的合成及其对低浓溶液中钾离子的吸着性能

本文报导了在多聚磷酸作用下,0,0’-邻苯二酚二乙酸同三聚甲醛缩聚生成具有对钾离子吸着作用的树脂的反应。探讨了摩尔配比、反应温度和反应时间等影响树脂性能的因素。提出了合成0,0’-邻苯二酚二乙酸—甲醛树脂的最宜条件: CH_2O:CDAH_2=1:4(摩尔); (CH_2O+CDAH_2):PPA=1:4(重量); 温度=120—130℃;时间=1小时。树脂产率为84—91％。树脂在380PPm氯化钾水溶液中(相当于海水中的钾离子浓度)对钾离子的吸着容量是28—30毫克钾离子/克(干树脂)[动态法]。富集因数是73—78。     

AG-MP-1M阴离子交换树脂分离-表面热电质谱法测定沉积物中的铅同位素组成

利用新型阴离子交换树脂分离沉积物中的重金属Pb,采用表面热电离质谱法(TIMS)测定了沉积物样品中的Pb同位素组成。新型树脂为大孔径阴离子树脂AG-MP-1M,淋洗液采用低浓度的盐酸,避免了使用难以纯化的氢溴酸,可有效地降低试剂空白。通过对铅同位素标准物质NIST NBS-981的重复测试,方法的精密度(<0.5%,2s)和准确度均达到了应用研究的要求。对5个实际沉积物样品中的铅同位素组成进行测定,获得了理想的分析效果。     

抗高温随钻封堵材料研究进展

钻遇渗透性漏失地层、破碎地层及低承压地层时,通常加入随钻封堵材料以防止钻井液漏失、提高孔壁稳定性和地层承压能力。深井高温地层及高温地热、高温干热岩钻探,遇到上述复杂情况时,需采用抗高温封堵材料。本文介绍了我国近年来抗高温随钻封堵材料研究与应用的进展情况,包括由桥接堵漏材料组成的抗高温随钻堵漏剂、膨胀型聚合物堵漏剂、超低渗透处理剂及弹性石墨等新型抗高温随钻堵漏材料。分析了4种抗高温随钻封堵材料的组分及其堵漏原理,并对抗高温随钻封堵材料的研究方向提出了建议。     

选择用于制作海洋测量传感器的环氧树脂

在制作用于海洋测量的传感器时,经常要使用环氧树脂材料。由于此类传感器与常规物理量测量传感器的工作条件不同,它们大多直接工作在条件比较恶劣的海洋环境之中,所以对其制作材料的选择应是较慎重的。笔者在多年研制传感器的过程中,经常要面临测量、筛选环氧树脂材料的问题。文章介绍我们选用环氧树脂材料时采用的一种简便而实用的方法及部分测量数据。希望能够与各位同行进行探讨,共同提高。     

Determination of Platinum‐Group Elements and Re‐Os Isotopes using ID‐ICP‐MS and N‐TIMS from a Single Digestion after Two‐Stage Column Separation

We report an improved procedure for the determination of the platinum‐group elements (PGE) and Re, and Os isotopes from a single sample aliquot by isotope dilution (ID) using inductively coupled plasma‐mass spectrometry (ICP‐MS) and negative thermal ionisation mass spectrometry (N‐TIMS), respectively. A two‐stage column method was used to purify PGE‐Re from their sample matrix and interfering elements (e.g., Mo, Zr and Hf) after Os had been separated by CCl₄ solvent extraction. The first column separation step used cation exchange resin (AG50W‐X8) to concentrate PGE‐Re and some potential interfering elements (e.g., Mo, Zr and Hf). In the second step, N‐benzoyl‐N‐phenylhydroxylamine (BPHA) extraction resin was used to separate PGE‐Re from the remaining interfering elements, which all remained strongly absorbed to the resin. The method was used to determine the PGE and rhenium, and Os isotope ratios in a range of geochemical reference materials (TDB‐1, WGB‐1, BHVO‐2 and UB‐N). The obtained results agree well with those previously published. This new method enables PGE‐Re abundances and Os isotopic ratios to be determined on the same sample digestion, and circumvents the problems created by sample heterogeneity when comparing PGE and Re‐Os isotope data.