磷酸根分析仪校准方法

为了解决磷酸根分析仪统一量值溯源的问题,通过分析磷酸根分析仪工作原理,探讨了其计量特性和校准方法。提出了校准项目和技术指标:示值误差(±2.0%FS)、测量重复性(≤3%)、零点漂移(≤1.0%FS)、示值稳定性(≤1.0%FS)。该校准方法可以用于准确评价磷酸根分析仪的性能。     

FIA-6000全自动流动注射分析仪通过新产品鉴定

不久前，北京市技术创新服务中心受北京市工业促进局委托，在北京主持召开了北京吉天仪器有限公司研制的“FIA-6000全自动流动注射分析仪”新产品鉴定会。与会专家听取了研制单位所做的工作总结报告、技术总结报告、工艺审查报告、质量检验报告、检测报告、查新报告、用户使用报告，审查了所有技术文件资料，观看了产品的现场演示。专家委员会经过认真讨论，一致认为：     

通过金属有机小分子水凝胶选择性形成实现磷酸根的可视识别

利用磷酸根和钳型三联吡啶锌络合物的金属中心锌离子具有选择性配位的能力,通过金属有机水凝胶的选择性形成实现了对磷酸根的可视识别.在此基础上,利用一系列实验对这类金属有机水凝胶的热稳定性、流变性质、外观样貌进行了详细表征和分析之后提出了对磷酸根选择性识别的可能机理.     

CG-3型自动测谱分析仪投入批量生产

CG-3型自动测谱分析仪是在北京有色金属研究总院研制成功的“CG-2型脉冲扫描自动测谱分析装置”科研成果的基础上,同吉林省图门市分析仪器厂合作,     

固相萃取–离子色谱法测定人尿液中钙、镁、氟、磷酸根离子

建立固相萃取–离子色谱法测定人尿液中钙、镁两种阳离子和氟、磷酸根两种阴离子。采用C₁₈固相萃取柱去除样品中杂质以消除干扰,以CS12 A型阳离子交换柱为分离柱,以甲基磺酸溶液为淋洗液,等度洗脱,测定钙、镁离子;以AS15型阴离子交换柱为分离柱,以KOH溶液为淋洗液,梯度洗脱,测定氟、磷酸根离子。钙、镁离子的质量浓度在0.25～10 mg/L范围内,氟、磷酸根离子的质量浓度分别在0.002 5～0.05 mg/L、1.25～50 mg/L范围内与色谱峰面积具有良好的线性关系,相关系数均大于0.999 0,方法检出限为0.002～0.2 mg/L。样品加标回收率为86.0%～99.5%,测定结果的相对标准偏差为0.12%～5.50%(n=6)。该方法操作简便,灵敏度高。     

中国红参中碳、氢、氮元素和蛋白含量的自动分析

人参为五加科植物人参(Panax ginseng C.A.Mey.)的干燥根。红参则是鲜人参洗净后经高温蒸气加热后干燥而制得的产品。有关人参中皂甙、氨基酸、多肽、挥发油、微量元素等成分的研究国内外均有大量的报道。但关于红参中碳、氢、氮元素的研究以及自动定量方法国内外尚未见报道。 1.仪器:1106型元素自动分析仪(意大利)其配套设备包括B-5000型记录仪,微处理机和电子天平。 2.人参样品:1号红参由吉林省抚松县参茸公司提供。2号红参由抚松县漫江参场提供。3号红参为抚松县参场提供。4号红参由延边地区提供。5号红参由集安县新开河参场提供。上述样品均为6年生。     

一种新的磷酸根离子敏感电极研究

一种新的磷酸根离子敏感电极研究肖丹，俞汝勤，李军，袁孔铨（湖南大学化学化工系，长沙，４１００８２）关键词磷酸根，离子选择电极，磷酸二氢根磷酸根离子浓度的测定在化学化工、环境保护、生命科学和临床医学等领域有着重要的意义。对磷酸根离子敏感电极的研究和探索...     

N,N'-双(膦酰基苯基次甲基)-2-咪唑啉酮及2,3-哌嗪二酮的合成

许多天然存在和人工合成的氨基磷酸因具有抗菌、除草、植物生长调节等多方面的生物活性，从而使这一领域的研究十分活跃［’］。而２一咪哩琳酮和２，３一派嗓Ｍ酮也是具有除草、杀菌等多种生物活性的化合物Ｉ’］，因此我们设计将ａ一氨基磷酸引入到２一眯吃财酮及２，３服喀二酮的结构中，设计并合成了Ｉｌｌ、Ｗ两类新化合物，以期找到高生物活性的化合物。１实验部分ＢｒｕｋｅｒＡＣ．Ｐ２００型核磁共振仪，ＴＭＳ为内标，溶剂ＣＤＣ１３；ＶＧＺＡＢ－ＨＳ型质谱仪；Ｙａｎａｃｏ．ＣＨＮＣＯＲＤＥＲＭＴ－３型元素自动分析仪；硅胶…     

微波消解试样-催化动力学光度法测定腌菜中亚硝酸根

腌菜试样用稀磷酸及过氧化氢置于PTFE罐中,在微波炉先后在400 W及500 W消解2 min及4 min,所得试样溶液于100 mL容量瓶中定容供光度测定.在稀磷酸介质中偶氮胂Ⅰ溶液与溴酸钾溶液的氧化褪色反应因亚硝酸根的存在而催化加速.有及没有亚硝酸根存在的两份相同试液的吸光度A及A0之差△A与亚硝酸根质量浓度在50 μg·L-1以内呈线性关系,其检出限为0.82 μg·L-1用此方法分析3件腌菜试样,测定结果的相对标准偏差(n=6)均小于2%.以此样品为基体,加入亚硝酸根标准溶液进行回收试验,测得的回收率在98.0%～102.0%之间.     

HCA-3B型微机数显自动分析仪测定锰磷硅的不确定度评定

讨论了使用HCA-3B型数显自动分析仪测定锰,磷,硅时不确定度的估算。     

Direct determination of total mercury in phosphate rock using alkaline fusion digestion

The aim of this work was to develop a new method to determine the mercury (Hg) concentrations in phosphate rock using a dedicated analytical instrument (the DMA80 Tricell by Milestone) that employs an integrated sequence of thermal decomposition followed by catalyst conversion, amalgamation and atomic absorption spectrophotometry. However, this instrument underestimates Hg concentrations when phosphorite and apatite rocks are investigated with a classic thermal decomposition treatment that complies with US EPA method 7473.     

再论中国分析仪器的十大关系

再次论述了我国分析仪器振兴、发展和赶超国际先进水平所必须注重的十大关系，可供分析仪器的制造者、使用者和有关的领导者参考。     

Autonomous microfluidic system for phosphate detection

Miniaturization of analytical devices through the advent of microfluidics and micro total analysis systems is an important step forward for applications such as medical diagnostics and environmental monitoring. The development of field-deployable instruments requires that the entire system, including all necessary peripheral components, be miniaturized and packaged in a portable device. A sensor for long-term monitoring of phosphate levels has been developed that incorporates sampling, reagent and waste storage, detection, and wireless communication into a complete, miniaturized system. The device employs a low-power detection and communication system, so the entire instrument can operate autonomously for 7 days on a single rechargeable, 12 V battery. In addition, integration of a wireless communication device allows the instrument to be controlled and results to be downloaded remotely. This autonomous system has a limit of detection of 0.3 mg/L and a linear dynamic range between 0 and 20 mg/L.     

电感耦合等离子体质谱法测定磷矿石中锰、铜、铅、锌、铬、镉

建立了HNO3-HCl O4-HF混合酸溶样,电感耦合等离子体质谱法同时测定磷矿石中的锰、铜、铅、锌、铬和镉等6个微量重金属元素的有效方法.试验中对仪器的最佳工作参数进行了优化,选择适当的同位素,并用铑作内标元素,有效地抑制了分析信号的漂移.在选定的条件下,对样品进行了精密度和回收率试验,方法相对标准偏差(RSD,n=9)为0.99%~1.98%,加标回收率为98.0%~102.0%.     

Determination of arsenic, cadmium, cobalt, chromium, lead, molybdenum, nickel, and selenium in fertilizers by microwave digestion and inductively coupled plasma-optical emission spectrometry detection: collaborative study

There is increasing regulatory interest in the non-nutritive metals content of fertilizer materials, but at present there is no consensus analytical method for acid digestion and instrument detection of those elements in fertilizer matrixes. This lack of method standardization has resulted in unacceptable variability of results between fertilizer laboratories performing metals analysis. A method has been developed using microwave digestion with nitric acid at 200 degrees C, followed by inductively coupled plasma-optical emission spectrometry instrument detection, for the elements arsenic, cadmium, cobalt, chromium, molybdenum, nickel, lead, and selenium. The method has been collaboratively studied, and statistical results are here reported. Fourteen collaborators were sent 62 sample materials in a blind duplicate design. Materials represented a broad cross section of fertilizer types, including phosphate ore, manufactured phosphate products, N-P-K blends, organic fertilizers, and micro-nutrient materials. As much as possible within the limit of the number of samples, materials were selected from different regions of the United States and the world. Limit of detection (LOD) was determined using synthetic fertilizers consisting of reagent grade chemicals with near zero levels of the non-nutritive elements, analyzed blindly. Samples with high iron content caused the most variability between laboratories. Most samples reasonably above LOD gave HorRat values within the range 0.5 to 2.0, indicating acceptable method performance according to AOAC guidelines for analyses in the mg/kg range. The method is recommended for AOAC Official First Action status.     

Purification of Solid-Phase Synthesized Peptides on the Coil Planet Centrifuge

Abstract

The analytical flow-through coil planet centrifuge, an instrument for countercurrent chromatography, performs the preparative purification of synthetic peptides. Various two-phase solvent systems have been tried with either phase mobile to purify many synthesized peptides. A series of N-terminal fragment peptides of cholecystokinin octapeptide (CCK 26–33) were synthesized by solid-phase techniques and purified on the coil planet centrifuge. The peptides were sulfated and chromatographed again. For hydrophobic peptides, purification is effected in solvent systems with a mobile aqueous phase. The n-butanol, acetic acid and water system (4:1:5 by volume) with the lower phase mobile was utilized. For sulfated peptides, the neutral system, 0.2 M ammonium acetate and n-butanol was generally applied.     

Performance characteristics of an ion chromatographic method for the quantitation of citrate and phosphate in pharmaceutical solutions

The performance of an ion chromatographic method for measuring citrate and phosphate in pharmaceutical solutions is evaluated. Performance characteristics examined include accuracy, precision, specificity, response linearity, robustness, and the ability to meet system suitability criteria. In general, the method is found to be robust within reasonable deviations from its specified operating conditions. Analytical accuracy is typically 100 +/- 3%, and short-term precision is not more than 1.5% relative standard deviation. The instrument response is linear over a range of 50% to 150% of the standard preparation target concentrations (12 mg/L for phosphate and 20 mg/L for citrate), and the results obtained using a single-point standard versus a calibration curve are essentially equivalent. A small analytical bias is observed and ascribed to the relative purity of the differing salts, used as raw materials in tested finished products and as reference standards in the analytical method. The assay is specific in that no phosphate or citrate peaks are observed in a variety of method-related solutions and matrix blanks (with and without autoclaving). The assay with manual preparation of the eluents is sensitive to the composition of the eluent in the sense that the eluent must be effectively degassed and protected from CO(2) ingress during use. In order for the assay to perform effectively, extensive system equilibration and conditioning is required. However, a properly conditioned and equilibrated system can be used to test a number of samples via chromatographic runs that include many (> 50) injections.     

Correction of a calibration scale for the rapid visual semiquantitative determination of phosphate ions in agricultural samples

A procedure was developed of fabricating a colored calibration scale for determining phosphate ions in aqueous solutions. The procedure is suitable for correcting hue steps depending on the analytical range of phosphate ions. A rapid procedure was proposed for visual testing in a blister cell with a bulk mixture of dry reagents. A test effect was observed immediately after the cell was opened and several drops of a test solution were added. Mixture compositions were developed for the visual determination of phosphate ions in a concentration range of 0.5–80 mg/L by the formation and reduction of phosphomolybdic acid using auxiliary reagents.     

便携式CO2红外线分析仪的应用和检定

便携式CO2红外线分析仪用于检测室内二氧化碳的浓度,主要介绍该仪器的工作原理、应用、检定方法以及常见故障分析。