高镁磷尾矿中钙、镁、磷赋存状态研究

选择了贵州省重要磷矿生产基地—瓮福磷矿浮选尾矿为代表,对其中钙、镁、磷的矿物学重要特征进行了比较系统的研究,获得了一些重要结论,从而为高镁磷尾矿的综合利用、白云石与胶磷矿的分离等提供理论依据,对实现磷尾矿资源的二次利用、指导开发者设计科学合理的矿石选冶工艺流程都有十分重要的意义。按照元素赋存形态分析的方法,选用了化学成分、化学物相、电子能谱、扫描电子显微镜、X射线粉晶衍射分析方法等多种手段系统、全面地测定了磷尾矿结构、形貌的重要特征,获得了钙、镁、磷赋存状态的重要结论,发现了尾矿及其原矿的异同性:磷尾矿中含量最高的组分及其含量分别是:氧化钙34.11%,氧化镁17.65%,五氧化二磷5.30%;镁主要以白云石的形式赋存,并有少量以磷酸盐、硅酸盐形式存在,其在各相占的比例分别为99.80%、0.10%、0.10%;磷主要以磷灰石的形式赋存(占97.08%),并有少量以铁氧化物(1.04%)、独居石(0.19%)、磷钇矿(1.83%)形式存在;钙主要以白云石的形式赋存(占96.95%),并有少量以方解石(1.11%)、磷酸盐(1.94%)形式存在。贵州瓮福地区高镁磷尾矿中的镁、磷、钙主要赋存形式分别为白云石、磷灰石、白云石。     

电感耦合等离子体原子发射光谱法(ICP-AES)测定铜磁铁矿中铜、锰、铝、钙、镁、钛和磷的含量

通过样品处理、干扰实验、方法检出限、准确度和精密度实验,确定了最佳实验条件,建立了电感耦合等离子体-原子发射光谱法(ICP-AES)测定铜磁铁矿中铜、锰、铝、钙、镁、钛和磷含量的方法。试料经盐酸、硝酸、氢氟酸、高氯酸分解,用盐酸溶解盐类,过滤,采用电感耦合等离子体原子发射光谱法同时测定滤液中铜、锰、铝、钙、镁、钛和磷的含量。方法检出限为锰、钛和磷小于0.00085%,其它元素小于0.0054%,分析结果与分光光度法、X射线荧光光谱法(XRF)和原子吸收光谱法(AAS)分析结果一致,8个实验室对5个水平样品进行协同实验给出了方法的精密度。     

冠心病患者血清钙、镁、磷变化的临床分析

为探讨冠心病患者血清钙、镁、磷的变化及其与冠心病的关系,对62例冠心病患者进行了血清钙、镁、磷含量的测定,并与41例健康人测定结果进行了对比分析。结果表明,冠心病组与健康对照组比较,血清钙离子和镁离子的含量均有显著性差异（P〈0．01）,磷无显著性差异（P〉0．05）。提示冠心病患者有血清离子含量的异常改变,主要表现为血清钙离子和镁离子含量的降低。     

电沉积非晶态镍磷合金的研究

本文用电化学方法, X射线衍射及电子能谱方法研究了阴极恒电位沉积非晶态镍磷合金镀层,实验结果表明,影响镍磷合金非晶结构的主要因素是镀层中的磷含量,当磷含量大于9%时,镀层具有良好的非晶结构,镀层中镍和磷主要以元素态形式存在,磷的析出具有诱导共析特点。     

X射线荧光光谱法测定白云石中12种元素的含量

采用X射线荧光光谱法测定白云石中钠、镁、铝、硅、磷、硫、钾、钙、锰、铁、钛、锌等12种元素的含量。样品以四硼酸锂和偏硼酸锂为熔剂和溴化锂为脱模剂于1 050℃熔融,样片用于X射线荧光光谱分析。以GBW 07114、GBW 07216A、GBW 07217A、YSBC 11703-1995、YSBC28722-1993、YSBC 28723-1993等标准物质为基础制作工作曲线。优化了各元素的基体校正数学模型。对白云石样品重复测定11次,测得其相对标准偏差(n=11)在0.2%~7.3%之间。方法用于白云石标准样品的分析,所得结果与认定值相符。     

原子吸收法测定血清中的无机磷和钙

本文叙述了用原子吸收法测定同一个少量血清样品中的无机磷和钙。血清用高氨酸沉淀蛋白后,加过量钼酸铵。在pH0.4～1.6范围内,用乙酸丁酯萃取生成的微量磷钼酸,与过量的钼酸铵分离。水相测钙,有机相用稀氨水反萃后测钼,间接分析磷。     

磷的生理功能

磷和钙一样 ,是骨骼和牙齿的主要成分。骨和齿中磷、钙是以磷酸钙的形式存在。磷是细胞核蛋白的主要成分 ,遍布肌肉、神经、血液。肌肉和神经中的磷化物———三磷酸腺苷大分子具有储存和转移能量的作用。碳水化合物、脂肪、蛋白质等被氧化释放出的能量立即转移到三磷酸腺苷分子中 ,它把能量储存起来。当肌肉运动、神经兴奋和传递信息、体内合成新物质、排泄等需要能量的时候 ,三磷酸腺苷便把库存的能量释放出来。血液中的磷以磷酸盐的形式存在 ,可以调节酸碱平衡。磷还以磷脂的形式广泛存在于细胞膜、脑髓、神经组织和肝脏里。例如 ,人脑内…     

波长色散X射线荧光光谱法测定铁矿石中铁硅钙铝磷镁锰钛

采用四硼酸锂熔融—X射线荧光光谱法测定铁矿石中铁、硅、钙、铝、磷、镁、锰和钛，以10个铁矿石标准物质建立校准曲线，用Lachance—Trail校正模式进行回归校正。方法准确、快速、简便。     

白云石添加剂对稻秆灰熔融特性及固钾能力的影响

在管式炉中研究了稻草秸秆的结渣特性与白云石作为添加剂对稻秆燃烧结渣的影响及其机理。采用电感耦合等离子体发射光谱(ICP-OES)和X射线衍射(XRD)表征了稻秆灰分与白云石之间的相互作用。结果表明,当白云石添加质量分数为5%时,对稻秆的结渣特性具有明显的改善。白云石具有较好的固钾能力,在900和1000℃下尤为明显。白云石中富含的Mg和Ca元素能够与稻秆灰分中的SiO_2反应形成高熔点的硅酸盐矿物,包括透辉石、钙镁橄榄石和镁硅钙石。     

人工神经网络及模拟退火算法应用于原子吸收光谱法同时测定钙、磷

试验发现:原子吸收光谱法(AAS)在442.7 Nm波长处测定钙时受到大于0.10 mg·L-1磷共存的干扰,使钙的测定结果偏低,而且此负偏差降低的幅度随磷浓度的增加而增大.试验还发现:当共存磷的量在0.1～6.0 mg·L-1之间时,钙测量值的负偏差幅度与磷浓度之间存在明显的相关性.应用反向传播人工神经网络(BP-ANN)及模拟退火两种计算法对上述非线性干扰效应进行了研究,并提出了在单一波长检测的条件下,钙、磷两元素的原子吸收光谱法同时测定,此法应用于循环水中钙、磷的同时测定.两元素的检测范围依次为0.08～10.0 mg·L-1及0.10～6.0 mg·L-1,测得其回收率分别为100.5%和98.0%.     

INAA and PIXE characterization of heavy metals and rare earth elements emissions from phosphorite handling in harbours

Harbour activities such as loading, unloading and transport of materials may be an important source of Atmospheric Particulate Matter (APM). Depending on the materials, the type of operation and the meteorological conditions, these activities may have an impact on the levels of APM around harbour areas. The aim of this work was to characterize the emissions of dust providing from operations associated with phosphorite handling in harbours. Phosphorite is a non-detrital sedimentary rock which contains high amounts of phosphate bearing minerals and is used for the production of phosphorous based fertilizers. When handled in harbours frequently cause visual and environment impacts due to its physical and chemical characteristics. The techniques Instrumental Neutron Activation Analysis and Particle Induced X-ray Emission were applied as sensitive analytical tools for the determination of heavy metals and rare earth elements in phosphorite and in the APM sampled in the harbour during the unloading operations. Results showed that manipulation of phosphorite during harbour operations resulted in high emissions of particles, principally from the coarse fraction. These emissions were enriched in rare earth elements and heavy metals and were very affected by the provenience of the phosphorite.     

Atomic absorption spectrometric determination of calcium and other metallic elements in some animal protein sources

The phosphorus content of some animal protein sources was determined in order to identify the sample with the highest phosphorus content for use as a pilot sample. Varying concentrations of strontium and lanthanum were added to solutions of the ashed pilot sample for the determination of calcium and magnesium using flame atomic absorption spectrophotometry operated on the air-acetylene mode. At least 3000 ppm of strontium or lanthanum was required to completely overcome the interference of phosphate ion, PO(4)(3-), and give peak values for calcium. The presence of strontium or lanthanum did not affect the amount of magnesium obtained from the analyses. Based on this, a procedure is proposed and the results obtained by this procedure for calcium are more enhanced than those obtained without the addition of strontium or lanthanum for the same samples whereas comparable results were obtained for all other elements whether strontium or lanthanum was added or not. The method gives more accurate results and is reproducible. The coefficients of variation calculated using one of the samples were 0.58% for magnesium, 3.12% for zinc; 0.44% for calcium, 11.06% for lead, 22.22% for nickel, 3.53% for manganese and 3.50% for iron at the concentration levels found in that sample. Recoveries of spiked calcium, magnesium and zinc were quantitative. Also, for selected elements, results from the procedure compared well with those from chemical analysis.     

Determination of mineral phosphate species in sedimentary phosphate rock in Mardin, SE Anatolia, Turkey by sequential extraction

The importance of the effect of phosphate rock depends on the chemical form of phosphorus in which this element is combined. The paper presents the results of inorganic and organic forms of phosphorus in the phosphate rock from Mazidag-Derik, Semikan deposit located at Mardin city at SE Anatolia of Turkey. Total phosphorus concentration in the rock is an average 18.5%. The inorganic phosphorus mean % contents were 99.98% for studied sedimentary phosphate rock. Speciation of inorganic phosphorus was carried out using a method based on sequential extractions of the sedimentary phosphate rock each releasing four forms of inorganic phosphorus: loosely sorbed phosphorus, phosphorus bound to aluminium (P-Al), phosphorus bound to calcium (P-Ca) and phosphorus bound to iron (P-Fe). Calcium bound phosphorus is the dominant form of inorganic phosphorus in the studied sedimentary phosphate rock. Aluminium bound phosphorus is the second, iron bound phosphorus is the third most prevailing form. Loosely bound phosphorus is present in the lowest amounts. Analyses of phosphorus forms in sedimentary phosphate rock using a UV spectrophotometric method and ICP-AES are reported here. For the phosphorus the two methods give the same results and the concentrations are in good agreement with the reference values.     

Study of the interaction of mono-, di-, and trisubstituted sodium orthophosphates with thermally activated dolomite

Interaction of dolomite thermally treated at 800°C with solutions of mono-, di-, and trisubstituted sodium phosphate was studied. It was shown that thermally treated dolomite binds 0.75 to 3.0 mmol g^–1 of phosphorus, depending on the nature of a phosphating reagent, and the interaction mostly occurs with magnesium oxide, which enables use of this kind of dolomite as a sorbent of phosphate ions. It was found that the nature of the phosphating reagent affects the chemical and phase composition of the materials obtained, as well as their sorption properties with respect to heavy metal ions. The products formed in acid-free phosphation of dolomite have high sorption capacity, from 1.5 to 6.8 mmol g^–1 for Pb²⁺, Zn²⁺, Cu²⁺, Cd²⁺, Ni²⁺, Sr²⁺, and Co²⁺ ions, which enables their use as effective sorbents for heavy metal ions.urning.     

贵州织金三甲寒武系戈仲伍组含磷岩系稀土富集规律研究

对贵州织金三甲地区寒武系底部戈仲伍组含磷岩系稀土元素、微量元素和一些常量元素等在剖面上的变化规律进行系统的研究，并结合剖面上小壳动物化石富集特点，认为寒武系底部戈仲伍组中有两个磷和稀土成矿期，稀土含量与磷含量成显著的正相关关系，而与小壳动物化石丰度没有显著相关性。     

Spectral interferences from phosphate matrices in the determination of arsenic, antimony, selenium and tellurium by electrothermal atomic absorption spectrometry

The spectral interferences of phosphorus species originating from the thermal decomposition of calcium phosphate on Sb, As, Se and Te resonance lines, and the influence of increasing amounts of Ce, Ni, W, Pd, Pt, Zr and other elements on non-correctable signals generated by calcium phosphate and on selenium and phosphorus sensitivity have been studied. The results indicate that spectral interference is caused by P₂ absorption and that the extent of interference depends on the wavelength and the spectral band width. The generation of P₂ is masked by large amounts of all the tested reagents. There is a significant reduction in selenium sensitivity in the presence of high concentrations of Ce, Pd and Pt while no decrease in sensitivity is caused by the presence of even 1% nickel and tungsten solutions. All the reagents tested provided enhanced phosphorus sensitivity, thorium being the best.     

The mineral phase in the cuticles of two species of Crustacea consists of magnesium calcite, amorphous calcium carbonate, and amorphous calcium phosphate

The cuticules (shells) of the woodlice Porcellio scaber and Armadillidium vulgare were analysed with respect to their content of inorganic material. It was found that the cuticles consist of crystalline magnesium calcite, amorphous calcium carbonate (ACC), and amorphous calcium phosphate (ACP), besides small amounts of water and an organic matrix. It is concluded that the cuticle, which constitutes a mineralized protective organ, is chemically adapted to the biological requirements by this combination of different materials.     

Rapid determination of magnesium in the presence of calcium and phosphate by titration with cdta

A method is presented for the accurate determination of magnesium in phosphate rock and phosphoric acid down to 0.03% magnesium oxide in the presence of 0–70% phosphorus pentoxide by titration with cyclohexanediaminetetraacetic acid (CDTA). Interference from heavy metals for which inaccurate empirical corrections have previously been made in the combined magnesium and calcium titration are linearly and unequivocally determined and subtracted from the combined titration. Magnesium oxide is determined in less than 20 min after sample digestion for Ca: Mg ratios from 1:9 to 850:1.     

Determination of trace phosphorus in high purity tantalum materials by inductively coupled plasma mass spectrometry subsequent to matrix separation with on-line anion exchange/coprecipitation

An on-line matrix separation/inductively coupled plasma mass spectrometry (ICP-MS) method is proposed for the determination of trace amounts of phosphorus in high purity tantalum metal, tantalum (V) oxide, and tantalum pentaethoxide. In the present method, the matrix tantalum in the sample solution was adsorbed on the anion exchange resin, and phosphorus (phosphate ion) was eluted with the carrier solution of HF and HNO3 mixture. Then, the effluent solution was subsequently mixed with bismuth solution and aqueous ammonia solution to coprecipitate phosphate together with bismuth hydroxide. The precipitate formed was collected on the in-line membrane filter to wash out nitric acid with pure water, and then dissolved with hydrochloric acid. The obtained phosphorus sample solution was introduced directly into the nebulizer of ICP-MS for the determination of phosphorus. Phosphorus was determined at the molecular ion signal of 31P16O+ (m/z 47). The detection limit (3sigma) of phosphorus in the present method was 1.3 ng mL(-1) as the sample solution basis, and the relative standard deviation for 30 ng mL(-1) of phosphorus in the standard solution was 4.3% in the replicate measurements (n=11). The present method was applied to the analysis of high purity tantalum materials. The concentrations of phosphorus in tantalum samples were in fairly good agreement with those obtained by glow discharge mass spectrometry (GDMS).