流动注射HG-AFS法同时测定化探样品中的砷和汞

建立了流动注射HG-AFS测定痕量砷和汞的分析方法。把砷和汞放入20%的王水介质中,它们被硫脲-抗坏血酸预还原,待测量溶液澄清之后,将溶液与硼氢化钾一起导入反应器,产生的氢化物载气导入原子化器中测定,测定结果符合国家标准。本法改进了流动注射HG-AFS法测定砷、汞的分析方法。     

Amphiphilic sodium alginate-vinyl acetate microparticles for drug delivery

To overcome the fast or burst release of hydrophilic drugs from hydrophilic alginate-based carriers,hydrophobic molecule(vinyl acetate,VAc)was grafted on alginate(Alg),which was further used to prepare drug carriers.Amphiphilic Alg-g-PVAc hydrogel beads were firstly prepared by emulsification/internal gelation technique for the loading of bovine serum albumin(BSA).Then,chitosan was coated on the surface of beads to form novel amphiphilic Alg-g-PVAc/chitosan(Alg-g-PVAc/CS)microcapsules.The BSA-loading amphiphilic Alg-g-PVAc/chitosan(Alg-g-PVAc/CS)microcapsules display similar morphology and size to the hydrophilic alginate/chitosan(AC)microcapsules.However,the drug loading and loading efficiency of BSA in Alg-g-PVAc/CS microcapsules are higher,and the release rate of BSA from Alg-g-PVAc/CS microcapsules is slower.The results demonstrate that the introduction of hydrophobic PVAc on alginate can effectively help retard the release of BSA,and the higher degree of substitution is,the slower the release rate is.In addition,the complex membrane can also be adjusted to delay the release of BSA.As a whole,amphiphilic sodium alginate-vinyl acetate/CS microparticles could be developed for macromolecular drug delivery.     

过氧化钠碱熔-电感耦合等离子体发射光谱法测定钛铁矿中的高含量钛

钛矿资源主要类型为钛铁矿岩矿、钛铁矿砂矿、金红石矿。钛铁矿属于难熔矿物,一般不溶于硝酸、盐酸或王水。对于高品位钛铁矿,即使采用盐酸-硝酸-氢氟酸-高氯酸混合酸溶解样品,钛元素也易水解形成难溶的偏钛酸析出,常给分析带来很大困难。容量法和分光光度法等传统方法测定钛存在操作流程长、步骤多、效率低等不足。因此,选择合适前处理方法的同时将大型仪器分析方法结合起来,有利于提高钛铁矿分析的准确度和测试效率。本文建立了以2.0g过氧化钠为熔剂,使用刚玉坩埚在700℃熔融样品15min,热水浸取后盐酸酸化,用电感耦合等离子体发射光谱（ICP-OES）测定钛铁矿中的高含量钛元素的方法。实验中采用全程空白试液稀释定容标准溶液消除了钠基体影响,通过优化熔融温度和时间使样品分解完全,考察了过氧化钠用量来降低待测溶液中盐分以保证测定的稳定性,通过选择合适的分析谱线并采用背景扣除法消除光谱干扰。本方法检出限为0.0035%,测试范围为0.0066%～62.50%（均以TiO₂含量计）;经钛铁矿国家标准物质（GBW07839、GBW07841）验证,相对标准偏差（RSD,n=12）为1.1%～2.1%,相对误差为-1.69%～1.11%。本方法应用于实际样品分析,相对标准偏差（RSD,n=12）均小于4%,TiO₂分析结果与国家标准方法（硫酸铁铵容量法）一致。本方法有效解决了钛铁矿分解不完全及高含量的钛易水解的问题,实现ICP-OES对不同类型钛铁矿样品中钛元素的定量分析。     

地质样品中硫化物形式铁的分离和测定

提出一个利用次氯酸钠氧化铁硫化物碱性磺基水杨酸提取并直接测定碳酸盐相中铁硫化物的方法。结果表明,30%的NaClO溶液浸泡样品40h以上,可以完全释放铁硫化物并形成氢氧化铁胶体。0.1g/mL的碱性磺基水杨酸溶液则较容易地溶解新生成的氢氧化铁胶体,形成黄色的铁-磺基水杨酸络合物,可被分光光度法定量测定。该方法集选择性分离、富集和测定于一体,分析流程简单,结果可靠,适合地质样品中硫化物形式铁的测定。     

碳酸钠浸取一紫外荧光光谱法测定地质样品中痕量铀

地质样品经HF-HNO_3-HCl-HClO_4溶解后,用50 g/L碳酸钠溶液浸取分离,采用紫外荧光光谱法直接测定上清液的铀含量。浸取时间选择30 min,Fe、Zn、Ca、Co、Ni、Cu和Mn等元素留在残渣中不产生干扰。方法精密度(RSD,n=12)为3．37%～7．06%,检出限为0．009μg/g(进样量100μL)。方法参加区域地球化学考核样品的测试,合格率100%,适用于土壤、水系沉积物、岩石及Fe、Zn、Ca、Co、Ni、Cu和Mn含量较高的样品中痕量铀的测定。     

糖蜜酒精废液中钾测定方法的研究

采用四苯硼钠溶液滴定电导-测量法,对糖蜜酒精废液中钾的测定方法进行了研究。该法简便快速,测定周期仅需20m in左右,所需试剂种类和用量少,准确度和精密度与四苯硼钾重量法相当。     

X射线荧光光谱法测定萤石中氟化钙

采用偏磷酸钠作熔剂制备萤石熔融片，用波长色散X射线荧光光谱法测定萤石中的氟化钙。考察了偏磷酸钠作为熔剂和稀释剂对萤石的熔解能力。方法经萤石国家一级标准物质检验，测定结果与标准值相符，10次测定的相对标准偏差（RSD）为0．23％。     

硫氰酸钾-十二烷基磺酸钠分光光度法测定矿石中钼

为使硫氰酸盐分光光度法测定矿石中钼的测定结果更稳定可靠，采用加入阴离子表面活性剂十二烷基磺酸钠的方法，对原实验加以改进。结果表明，采用改进后的方法，即使温度高于30℃时，吸光度值仍可稳定3h以上，且灵敏度有所提高。方法用于国家一级标准物质的测定，结果与标准值相符。     

火焰原子发射光谱法测定碳化钛中微量钠

对火焰原子发射光谱法测定碳化钛中微量钠的条件进行了试验。样品用硝酸-氢氟酸溶解，在0．30mol／L硝酸介质中，以硝酸钾作消电离剂消除钠的电离干扰，饱和硼酸溶液络合试液中过量的氟离子。方法检出限为0．015μg／mL，样品加标回收率为97．6％-105．6％，方法的精密度（RSD，n=6）小于2．5％。     

Development of secondary porosity in the Fairholme carbonate complex (southwest Alberta, Canada)

Because of their economic importance as hydrocarbon reservoirs, the Upper Devonian dolomitized carbonate reefs in southwest Alberta have been the subject of several studies. Still, there is no consensus on the process of matrix dolomitization and furthermore, the process of vug development is not often addressed. The studied outcrops show features of an early diagenetic matrix-selective dolomitization by a Late Devonian seawater-derived fluid. Seepage reflux dolomitization combined with latent reflux is proposed, which best explains most chemical characteristics. The cements in the vugs are precipitated from warm saline, ⁸⁷Sr-enriched fluids and testify to thermogenic sulphate reduction based on the presence of sulphur, CO₂ and H₂S in inclusions, relatively high homogenization temperatures and depleted δ¹³C values, which sets constraints on the timing of vug formation. Secondary porosity may be created by the mixing of formation water with a tectonically and topographically driven fluid and by the dissolution of anhydrite nodules.