光度法测定生铁和铸铁中磷

利用氟化钠-氯化亚锡还原钼蓝光度法测定磷是钢铁中直接快速测磷的方法。在酸性介质中,磷酸与钼酸铵生成磷钼杂多酸,再用氯化亚锡还原,形成钼蓝。当无铁基存在时,色泽呈纯蓝色,形成的磷钼杂多蓝很稳定;当有铁基存在时,特别是分析含磷量较高的试样时,因发色后的磷钼蓝色泽极不稳定,颜色由深蓝色向     

结晶型磷一多磷钼酸铵的制及其离子交换性能的研究

本文叙述了弗晶型磷－多磷钼酸铵的制备方法，研究了磷－多磷钼酸铵的化学组成，测定了该经合物的离子交换性能，说明多磷酸根部分取代磷酸根所生成的结晶型磷－多磷钼酸铵对铯离子具有良好的离子交换选择性和较高的离子交换容量，是一类新的结晶型无机离子交换剂。     

粒状十二磷钼酸铵结晶的合成及对Cs^＋的交换性能研究

用焦磷酸根在酸性钼酸铵溶液中缓慢水解释放出磷酸根，控制磷钼酸铵（ＡＭＰ）的结晶速度，合成了适合于柱操作的ＡＭＰ粒状结晶。结晶结构分析和化学组成分析确认其为十二磷钼酸铵。在１ｍｏｌ／ＬＨＮＯ３中对Ｃｓ＋的静态交换容量为０．６３ｍｍｏｌ／ｇ，分配系数为３５０ｍｌ／ｇ。在模拟中国裂变废液中，动态交换容量为０．５５ｍｍｏｌ／ｇ。经２×１０６Ｇｙ剂量γ辐照后，交换容量未发生变化。     

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。     

碳素锰及硅锰合金中磷量的快速测定

钢铁中都含有磷,它是由冶炼原料及燃料带入,而磷的存在使钢冷脆并降低钢的冲击性及韧性。碳素锰及硅锰铁是钢铁的冶炼原料之一,因此准确测定其中磷的含量对钢铁生产有着重要的意义。 目前碳素锰及硅锰铁中磷的测定,国家标准方法采用硝酸和氢氟酸分解试样,加入高氯酸冒烟使磷氧化为正磷酸,使之生成磷钼酸铵沉淀,用中和滴定法测定磷量,或者将磷氧化为正磷酸后,以亚硫酸氢钠将铁还原,加入钼酸铵及硫酸肼使之反应,然后用钼蓝光度法测定磷量。有用抗坏血酸还原磷铋钼蓝比色法,也有用磷钒钼黄光度法。这些方法虽然准确度高,但分析周期长,成本高,较难适应生产的需要。为适应生产发展,提高分析速度,在文献[1～4]的基础上,将试样溶解完全后,不经分离,直接用氟化钠-氯化亚锡钼蓝吸光度法快速测定碳素锰及硅锰铁中的磷量。方法简便,稳定性较好,可满足于生产检验。本法测量范围0.10％～0.46％,相对标准偏差小于35％。     

磷在酸碱滴定法中的计量系数

采用磷钼酸铵容量法验证了磷在酸碱滴定法中的计量系数，实验结果表明，磷的计量系数可根据具体实验条件选用不同的数值。     

磷在酸碱滴定法中的计量系数

采用磷钼酸铵容量法验证了磷在酸碱滴定法中的计量系数,实验结果表明,磷的计量系数可根据具体实验条件选用不同的数值。     

镁及镁合金中微量磷的测定方法研究

磷与钼酸铵形成磷钼杂多酸络幌物,用乙酸丁酯萃取分离,用SnCl2还原反萃取后借磷钼蓝光度法测定镁及镁合金中微量磷。在波长700 nm处工作曲线线性范围0~1.5μg/mL,相关系数为0.9995,络合物表观摩尔吸光系数ε=1.45×104L.mol-1.cm-1,相对标准偏差在1.40%~3.10%之间,加标回收率在99.3%~101.0%之间,本法与ICP法相对照结果比较满意。     

微波消解-磷钼蓝分光光度法测定钨矿石中的磷含量

针对钨矿石中的微量元素磷,采用混合酸快速微波消解结合磷钼蓝分光光度法进行测定。经选择优化样品的微波消解和实验测定条件,结果表明:HCl+HNO3+HF的混合酸微波消解后的样品,在硫酸介质中,有钼酸铵存在时,用抗坏血酸将磷还原成磷钼蓝络合物,在825nm处比色测定。方法的加标回收率为98.9%~101.6%,结果准确可靠。硅在熔样过程中挥发除去不会干扰测定,砷会干扰实验,可在酸介质中加入碘化钾,使砷还原至低价而不干扰磷的测定。     

分光光度法测定铁合金中的磷

以含磷较低的铁合金作底液,以钼酸铵为显色剂,用磷钼蓝光度法测定铁合金中的磷。磷钼蓝的摩尔吸光系数为7.8×10~5L/(mol·cm),与磷钼黄光度法、氟化钠-氯化亚锡还原磷钼蓝光度法相比,测定灵敏度有不同程度的提高。该方法用于实际样品分析,结果准确、可靠。     

火焰原子吸收法测定土壤中铜铅镉锌

以吡咯烷二硫代氨基甲酸铵为螯合剂,四氯化碳为萃取剂萃取土壤消解液,继而用硝酸-过氧化氢混合液反萃取至水相,然后用火焰原子吸收光谱法测定铜、铅、镉和锌,结果满意。     

A continuous hydride-generation system for direct current plasma atomic-emission spectrometry (DCP-AES) Determination of arsenic and selenium

A continuously operating hydride-generation system has been developed for determination of volatile hydride-forming elements such as arsenic and selenium by d.c. plasma atomic-emission spectrometry. Arsenic and selenium are converted into their hydrides by reduction with sodium borohydride. The hydrides evolved are stripped from the liquid phase in a gas/liquid separator and are continuously fed into the d.c. plasma by a small argon stream. Under optimized operating conditions the detection limits (3s) obtained for arsenic and selenium are 0.3 and 0.5, mug/l., respectively. The precision at the 5 mu/l. level is better than 4% r.s.d. The measurement time, including sample introduction and three replicate measurements with 5-sec integration per sample is about 1 min. The effects of well known interferents such as copper and nickel have been investigated. For minimizing their interference continuous addition of 1, 10-phenanthroline as masking agent has been found useful. The method has been tested by its use for analysing NBS standard reference materials.     

Determination of antimony in lead-zinc concentrates and other smelter products by atomic absorption spectrometry after extraction with di-isopropyl ether and reductive stripping

Several papers have appeared in the literature describing the determination of antimony, where antimony(V) is extracted into the organic phase and the organic solutions directly analyzed by atomic absorption spectrometry (AAS). This paper describes a procedure where antimony from the organic solution is reductively stripped into an aqueous phase and analyzed for antimony by AAS. The advantage of the method for a routine process control laboratory is highlighted.     

Rapid measurement of 241Pu activity at environmental levels using low-level liquid scintillation analysis

A straightforward and rapid method has been developed for the determination of ²⁴¹Pu activities. Pu is chemically separated from the sample, purified and electrodeposited to produce a source for alpha spectrometric determination of ²³⁸Pu and ^239,240Pu. Pu is stripped from the disc with concentrated nitric acid and extracted into tri-octylphosphine oxide (TOPO)/toluene. The organic extract is then mixed directly with commercial liquid scintillation cocktail without any further purification procedures and the sample counted on a Wallac 1220 Quantulus liquid scintillation counter (LSC). ²⁴¹Pu activity is estimated via the ²⁴²Pu yield monitor acquired by alpha spectrometry measurement. Experimental results for the performance testing of a low-level liquid scintillation spectrometer and the data for the evaluation of the method using standard reference materials are presented.     

Species determination of selenium in natural waters

A method is described for the determination in natural waters of selenite, selenate, dimethyl selenide, and dimethyl diselenide. The detection limits are in the parts per trillion range. The volatile methyl species are removed from the sample with a stripping gas. The inorganic forms are selectively reduced to the hydride, and also stripped from the sample. A liquid nitrogen trap is used to collect both the selenides and the generated hydrides. Separation of the methyl species is accomplished by gas chromatography. All the species are detected by an atomic absorption spectrometer equipped with a quartz tube furnace.     

A chemical enhancement method for the spectrophotometric determination of trace amounts of arsenic

A highly sensitive spectrophotometric method for the determination of 0.03-1.0 microg of arsenic is described. After extraction as AsI(3) into benzene, it is selectively stripped into water. Both the arsenic(III) and iodide present in the aqueous phase are made to react with iodate in acidic medium in the presence of chloride to form the anionic chloro complex, ICl(-)(2). The determination is completed after extraction of ICl(-)(2) species as an ion-pair with Rhodamine 6G into benzene and measuring the absorption of the extract at 535 nm. The coefficient of variation is 1.5% for 10 determinations of 0.5 microg of arsenic. The method has been applied to the determination of arsenic content in plant materials, high purity iron, copper base alloys and inorganic arsenic levels of natural waters.     

Shifting Chemical Equilibria in Flow—Efficient Decarbonylation Driven by Annular Flow Regimes

To efficiently drive chemical reactions, it is often necessary to influence an equilibrium by removing one or more components from the reaction space. Such manipulation is straightforward in open systems, for example, by distillation of a volatile product from the reaction mixture. Herein we describe a unique high‐temperature/high‐pressure gas/liquid continuous‐flow process for the rhodium‐catalyzed decarbonylation of aldehydes. The carbon monoxide released during the reaction is carried with a stream of an inert gas through the center of the tubing, whereas the liquid feed travels as an annular film along the wall of the channel. As a consequence, carbon monoxide is effectively vaporized from the liquid phase into the gas phase and stripped from the reaction mixture, thus driving the equilibrium to the product and preventing poisoning of the catalyst. This approach enables the catalytic decarbonylation of a variety of aldehydes with unprecedented efficiency with a standard coil‐based flow device.     

Vortex‐assisted liquid–liquid microextraction of strontium from water samples using 4′,4″(5″)‐di‐(tert‐butylcyclohexano)‐18‐crown‐6 and tetraphenylborate

A vortex‐assisted liquid–liquid microextraction method was developed for the chromatographic determination of strontium in aqueous samples. In the method, strontium was complexed with 4′,4″(5″)‐di‐(tert‐butylcyclohexano)‐18‐crown‐6 in the presence of tetraphenylborate as the counter anion, which increased the hydrophobicity of the ion‐association complex, resulting in its improved extraction into 1‐octanol. Strontium from the organic phase was stripped with nitric acid back to aqueous solution and determined by ion chromatography. The optimum microextraction conditions were as follows: 2.0 mL aqueous samples with 3 mM tetraphenylborate; 150 μL of 1‐octanol as the extractant phase with 10 mM DtBuCH18C6; vortex extraction time for 10 s; centrifugation at 6000 rpm for 4 min; stripping by 0.1 M nitric acid. Under the optimum conditions, the detection limit for strontium was 0.005 mg/L. The calibration curves showed good linearity over the range between 0.01 and 2.5 mg/L. Intra‐ and interday precisions of the present method were satisfactory with relative standard deviations of 1.7 and 2.1%, respectively.     

液晶研究（Ⅰ）──4＇－酰基－4－羟基－1，1＇－联苯酯类液晶的合成与性质

以４＇－羟基联苯为原料合成了８种新型４＇－酰基－４－羟基联苯酯类化合物．除化合物５＿ｈ外，均为新的近晶相液晶化合物．它们具有较宽的相变温度范围和较高的热稳定性．用偏光显微镜和差热分析仪研究了它们的相行为，讨论了分子结构对液晶相行为的影响．     

Determination of total organic carbon in water in the form of carbamate by means of a simple denuder/electrolytic conductivity flow cell system

A simple and sensitive technique for measuring both volatile organic carbon (VOC) and total organic carbon (TOC) in water is presented. The VOC fraction is stripped by a stream of oxygen and subjected to high-temperature catalytic combustion after removing the carbon dioxide, obtained from inorganic constituents at pH ? 2, with lithium hydroxide. The residual non-volatile organics (NVOC) are converted into carbon dioxide by injecting an aliquot of the stripped sample directly into the combustion tube. The carbon dioxide derived from the VOC/NVOC is preconcentrated from the gas stream by absorption in a stainless-steel capillary tube coated with a 2 M ethanolic solution of 3-methoxypropylamine. The carbamate formed in the liquid film is then eluted with a stream of the absorbent circulating through a microelectrolytic conductivity detector. The change in specific conductance due to the presence of the carbamate in the effluent stream is linearly related to the amount of VOC/NVOC/TOC up to 4.5 μg of carbon. The limit of detection for VOC is 0.5 μg l^?1 and for NVOC it is 100 μg l^?1. A simple determination takes 5 min. The precision was better than 5% (P=95%) for 0.5–4.5 μg of carbon. The method is also suitable for the determination of total carbon and inorganic carbon in water.