Thermal analysis of fluidised bed combustion residues containing limestone scavenger

A method has been developed using thermoanalytical techniques for the analysis of residues from coal-burning fluidised bed plant where limestone is used as a sulphur scavenger. This completely eliminates the need for lengthy wet chemical analyses and allows the derivation of parameters necessary for efficient plant operation, such as limestone addition rate, calcium utilisation efficiency and calcium to sulphur mole ratio. The method also gives values for the unburned carbon content and the ratio of coal ash to limestone derivatives in the sample.     

火花放电原子发射光谱测定球墨铸铁的方法研究

球墨铸铁塑性韧性好,成本低,广泛用于汽车、化工、风电等设备的制造;火花放电原子发射光谱分析方便、快捷,广泛用于冶金产品的成分检测,由于球墨铸铁的非白口化状态,其制品无法直接进行光谱分析。通过对球墨铸铁制品试样进行淬火热处理,改变它的表面组织为半白口化状态,结构致密,从而可以进行光谱分析,激发后,被激发的样品表面出现有黑晕的正常激发点,可以读取准确的数据,大大提高了检测速度和效率。对硅、磷、锰、镁的分析精密度RSD分别为 0.006%、0.025%、0.00%、0.10%。硅、磷、锰、镁的光谱分析结果与化学分析法的结果的差值均小于允许临界差。大大提高了检测速度和效率。     

高频红外碳硫分析仪测定含碳化硅耐火材料中碳化硅含量

采用对试样进行灼烧预处理的方法,除去游离碳,用锡粒、纯铁、钨粒作为助熔剂,并以钢铁标准样品校正仪器,高频燃烧红外吸收法测定含碳化硅耐火材料中的碳化硅含量,测定结果的相对标准偏差为1.07%(n=6),该法与化学法的测定结果较接近,精密度和准确度均满足化学分析的要求。     

X射线荧光光谱法快速测定FeSiB非晶合金薄带中硅、硼、铁

提出了以自制的标准样品,采用单点法绘制校准曲线,利用X射线荧光光谱仪测定FeSiB非晶薄带样品中硅、硼和铁的含量。对于4个FeSiB非晶合金薄带样品中硅、硼和铁进行了10次测定,其分析结果的相对标准偏差分别为0.4%~0.5%、1.3%~4.2%和0.2%~0.4%。方法的分析结果与火花源原子发射光谱法、化学重量法和电感耦合等离子体原子发射光谱(ICP-AES)法的测定值吻合较好。方法快速、简便,薄带样品无需制样,适用于FeSiB非晶合金薄带的快速成分分析。     

Contribution a l'etude du dosage par radioactivation du sourfre et du phosphore en tres faibles concentrations dans les metaux de tres haute purete (Aluminium,magnesium, cuivre,fer, nickel)

The chemical separation of sulphur and phosphorus from pure iron and nickel, is described. Sulphur has been determined first by irradiation in fast neutrons, then by irradiation in mixed fast and thermal neutrons. The two methods gave two different results; so, we were led to point out the same phenomenon asJ. Le Hericy had already pointed out for the determination of sulphur in copper. We found that the abnormal amounts of sulphur came from external contamination with chlorine since sulphur is then produced by the³⁵Cl(n, p)³⁵S reaction. The diffusion of³⁵S atoms (produced on the edge of the samples) explains that the concentration of sulphur decreases from the edge to the middle of the sample. We prepared samples of iron and nickel, artificially covered with ammonium chloride, and we studied the apparent concentration of sulphur as a function of the depth in these samples. Our experiences pointed out that the contamination in sulphur yielded by the (n, p) reaction, reaches very quickly the middle of the samples. This phenomenon limits the determination of sulphur by the³⁴S(n, γ)³⁵S reaction, in nickel and iron.      

Verification of certified sulphur values in steel reference materials by isotope-dilution mass spectrometry, and characterization of sulphur present on the solid samples

Sulphur in a number of steel reference materials has been determined by isotope-dilution mass spectrometry, utilizing both open-beaker and sealed-tube dissolution techniques. It is confirmed that the sulphur present in most samples can be completely converted into sulphate by the conventional open-beaker dissolution technique. The results on reference materials are in good agreement with the certified values for BCS samples and the recent or revised certified values for JSS and NBS samples. It is found that the sulphur concentration in the vicinity of the surface of the sample chips is higher than the average and that a significant amount of elemental sulphur is present on most chip samples. The ratio of elemental sulphur to average sulphur content tends to vary in proportion to the manganese content when this is less than 1%.     

Quantitative micro-analysis of metal ions in subcellular compartments of cultured dopaminergic cells by combination of three ion beam techniques

Quantification of the trace element content of subcellular compartments is a challenging task because of the lack of analytical quantitative techniques with adequate spatial resolution and sensitivity. Ion beam micro-analysis, using MeV protons or alpha particles, offers a unique combination of analytical methods that can be used with micrometric resolution for the determination of chemical element distributions. This work illustrates how the association of three ion beam analytical methods, PIXE (particle induced X-ray emission), BS (backscattering spectrometry), and STIM (scanning transmission ion spectrometry), allows quantitative determination of the trace element content of single cells. PIXE is used for trace element detection while BS enables beam-current normalization, and STIM local mass determination. These methods were applied to freeze-dried cells, following a specific cryogenic protocol for sample preparation which preserves biological structures and chemical distributions in the cells. We investigated how iron accumulates into dopaminergic cells cultured in vitro. We found that the iron content increases in dopaminergic cells exposed to an excess iron, with marked accumulation within distal ends, suggesting interaction between iron and dopamine within neurotransmitter vesicles. Increased iron content of dopaminergic neurons is suspected to promote neurodegeneration in Parkinson’s disease.     

高频燃烧-红外吸收法测定碳酸锶中的硫

采用HIR-944B红外碳硫分析仪快速测定碳酸锶中的硫。对测定条件如助熔剂加入量、样品加入方式、参考物质的选择进行了探讨。确定的助熔剂最佳配比为0.5 g纯铁+0.3 g锡粒+1.5 g钨粒。样品平铺于混合助熔剂的中间层,最上部覆盖薄铝片压紧,以有证石灰石为参考物质。该方法测定结果的相对标准偏差为1.85%、2.12%(n=5),加标回收率为96%、98%。     

地外样品研究中电子探针元素面扫描分析技术的应用

由于月壤等地外样品十分珍贵,在实验室研究中优先使用原位、微区、无损的元素分析方法。电子探针元素面扫描是地外样品研究中常用的分析方法之一。该方法可获取样品整体或者感兴趣区域的多种元素分布数据,应用于矿物相识别与含量估算,锆石等定年矿物的快速定位,矿物环带、出溶、反应边结构等特殊岩相和矿物接触关系等分析和研究。本研究中以嫦娥五号月壤、月球陨石、火星陨石研究为例,介绍了目前元素面扫描的应用方法。此外,本文还对比、分析了电子探针面扫描技术与其它面扫描技术的优缺点和适用范围。未来十年,我国将实施一系列月球、火星、小行星等天体采样返回任务。电子探针元素面扫描分析未来将在这些地外样品研究中广泛使用。同时,建议行星科学家围绕所关心的科学问题,合理搭配多种分析方法以实现各种技术优势互补和样品科学价值最大化,服务我国月球与深空探测任务科学产出和行星科学发展。     

硅钼酸盐光度法测定硅铁中硅的含量

用HNO3、HF溶样,草酸遮蔽干扰离子,钼酸铵与硅酸反应生成硅钼杂多酸,加入硫酸亚铁铵后形成硅钼蓝,在660nm波长处比色。硅铁标准样品中硅含量测定结果的相对标准偏差为0.27%~0.28%,该方法测定结果与高氯酸脱水重量法的测定结果相当。     

The determination of sulphur by combustion in iron,steel and associated materials

The sprinciples of combustion techniques suitable for the determination of sulphur in irons, steels, slags, etc. and their application to a range of materials are outlined. Conditions which give a 100% yield by high-frequency induction heating are established. Deposition of sulphur trioxide on the walls of the delivery train is obviated by heating electrically, giving total sulphur absorption in hydrogen peroxide. Good results for BCS irons, steels, slags and iron ores are given but the presence of fluorine causes a positive interference, unless the alkalimetric titration is replaced by an iodimetric procedure. Resistance heating is still used for lime and solid fuels.     

进口氧化皮化学特性及X射线荧光光谱分析

采用玻璃片法熔融进口氧化皮样品,并应用X射线荧光光谱法测定其中全铁和硅、铝、磷、钙、镁、钛、砷、铅等15种杂质元素的含量.根据氧化皮成分含量范围,利用多个铁矿石标准样品、部分标准样品添加基准物质Fe2O3配制系列校准物质,建立工作曲线.结果表明,该方法能准确、快速地对氧化皮进行分析,测量值与经典方法或标准值比较没有显著性差异.     

Determination of sulphur content in drill core samples by backscattered beta-particles and gamma-ray absorption

A relatively simple method of sulphur determination in drill cores of calcium carbonate matrix is described. The method is based on the combination of measurements of backscattered beta-particles and transmitted low energy gamma-radiation intensities. The transmitted gamma-radiation measurement corrects the errors of sulphur determination caused by the varying strontium sulphate and silicon dioxide content. The method has been tested on 170 samples. It was estimated that the standard deviation of sulphur determination does not exceed 2.5% of sulphur. The apparatus for routine absorption measurement is also described.     

LA-ICP-MS, IC and DPASV-DPCSV determination of metallic impurities in solar-grade silicon

Stringent specifications are laid down for the silicon used for solar cells. The present work deals with the application of different techniques to the simultaneous determination of most common metallic impurities like iron, copper, nickel, zinc, lead and cadmium, in industrial process control. Laser ablation inductively coupled plasma mass spectrometry is quite expensive in apparatus, but it directly performs the analysis of solid silicon with very good sensitivity, even if coupled to considerable standard deviation, probably due to the material defects. Both ion chromatography and voltammetry need sample pre-treatment, but they are characterized by cheap and simple apparatus, suitable detection limits, good sensitivity and small standard deviation.     

An investigation into the use of ionizing radiation for the destruction of sulphur mustard

Chemical warfare agents have been stockpiled for almost a decade and their destruction has become an environmental issue that will continue to require attention for many years. There are hundreds of thousands of tonnes yet to be destroyed, and the current chemical or incineration techniques are not without problems. While many researchers are seeking better chemical techniques, we decided to try ionizing radiation to destroy sulphur mustard with the goal of producing non-toxic products. We irradiated a variety of sulphur mustard samples by both a mixed field source (β, γ and neutrons) and a pure gamma source. The mixed field irradiation of wet sulphur mustard for long irradiation times was the most successful at destroying the chemical agent.     

Determination of sulphur and total sulphur dioxide in wines by an ICP-AES method

Sulphur contents of the original sample and the sample free from sulphur dioxide were determined by ICP-AES following nitric acid digestion under high pressure (using PAAR HPA equipment), and the total sulphur content was calculated from the difference between the results obtained. With the aim of preparing a sample free from sulphur dioxide, bound sulphur dioxide was released by sodium hydroxide, then after acidifying by phosphoric acid, boiling was carried out. Relative standard deviations of the results obtained for total sulphur, the sulphur without S(IV) and total sulphur dioxide were lower than 2.5, 3.5 and 5% respectively. Various amounts of sulphur (in the form of Na₂SO₄), added to wine samples, were successfully recovered between 95.5 and 104.9%. Based on comparative analyses performed by a widely accepted classic method, the indirect method developed was found to be adequate for the determination of total sulphur dioxide. The procedure is suitable for serial tests.     

Fast non-destructive determination of iron and sulphur in coal by means of neutron radiative capture

The possibility of determination of iron and sulphur in large-scale samples of coal /20–50 kg/, based on process /n, /, was evaluated. The spectral lines of the doublet 7631 keV and 7645 keV were used for the determination of iron, while the line at 5421 keV was used for the determination of sulphur. The neutron source was²⁵²Cf /total neutron emission at 2.5×10⁷ s^–1/ located additionally in D₂O moderator. A Ge/Li/ detector was used for gamma radiation detection. The calibration dependencies of the analyzer were linear. In exposure times of up to 1 h, the detection limits of 0.34% and 0.64% and accuracies of 0.25% and 0.4% have been achieved in case of iron and sulphur, respectively.     

空气-乙炔火焰原子吸收法测定硫铁矿中的砷

研究了空气-乙炔火焰原子吸收法测定硫铁矿中砷的方法,讨论了其测试条件和共存元素的干扰,样品采用酸浸溶解、直接上机测定。结果表明,该法具有操作简单、快速、火焰温度较高等优点,线性回归方程及相关系数分别为:A=0.003 20 C 0.009 77,r=0.999 3。     

化学反应-顶空气相色谱法测定气相二氧化硅表面硅羟基

建立了一种基于化学反应-顶空气相色谱测定气相二氧化硅表面硅羟基含量的新方法.实验取气相二氧化硅放入顶空瓶中于105℃烘箱中加热2 h去除水分,将甲苯稀释的格氏试剂注入密闭的顶空瓶中,格氏试剂与气相二氧化硅表面硅羟基快速反应产生甲烷(CH4),甲烷量与气相二氧化硅表面硅羟基含量成正比.经过气相色谱-氢火焰离子化检测器测定...