热导法快速测定石油焦中氮含量

应用Leco CHN-2000元素分析仪(热导法)测定了石油焦中氮的含量,对仪器工作条件、试样制备,特别是试样的粒度及试样的燃烧条件进行了系统试验并作了较详细的叙述.按所选定的条件对同一石油焦样品连续分析8次,测得仪器及方法的相对标准偏差为0.40%,一次测定的分析速度为5 min.用高纯度的EDTA(酸型)作基准物质制备工作曲线,按此方法及凯氏定氮法分别测定了同一批样品中氮量,所得测定值用t-检验法作检验,结果表明两方法间无显著差异.     

鲍鱼多糖Hal-A的热分析研究

采用热重、热重-红外谱联用及差示扫描量热法，对鲍鱼多糖进行热分析研究 ，结果表明鲍鱼多糖在空气和氮气氛中，230 ～ 340 ℃之间发生剧烈的分解反应 。氮气氛中，是吸热的分解过程；而空气氛中，是放热氧化反应，并且在453 ℃左 右，有另一个急剧的氧化裂解过程。与淀粉、肝素、甲壳素和半乳糖的热分析比较 ，含有硫酸酯的鲍鱼多糖和肝素热稳定性较低，含氨基的甲壳素最高，这反映出不 同基团对多糖热稳定性的影响。     

BTF变色对其热安定性和与PVB等相容性的影响

通过光照制备了一定量的变色苯并三呋咱氧化物（BTF）,再分别采用差热（DTA）,差示扫描量热（DSC）,真空安定性试验（VST）等热分析方法,对变色前后的BTF进行了热安定性研究及与聚乙烯醇缩丁醛（PVB）等接触材料的相容性研究,并通过热重－红外等仪器分析手段,初步探讨了BTF与PVB之间的作用机理。     

热重分析仪

<正>热重分析仪是一种利用热重法检测物质温度―质量变化关系的仪器。热重法是在程序温控下测定物质的质量随温度(或时间)的变化关系。当被测物质在加热过程中有升华、汽化、分解出气体或失去结晶水时,被测的物质质量就会发生变化。这时热重曲线就不是直线而是有所下降。通过分析热重曲线,可以知道被测物质在多少度时产生变化,并且根据失重量可以计算失去了多少物质。热重法的重要特点是定量性强,能准确地测定物质的质量变化及变化的速率,可以说,只要物质受热时发生重量的变化,就可以用热重法来研究其变化过程。     

用煤标准样品校准-脉冲熔融样品-热导法测定炼钢用增碳剂中的氮含量

提出了用煤标准样品校准仪器,脉冲加热样品融熔-热导法测定炼钢用增碳剂中氮含量。试验结果表明:①增碳剂样品须粉碎至粒径为0.180mm并在空气干燥的条件下制备;②根据所用氧氮测定仪的工作性能,选取样品的称样量在3.0~7.0mg之间,并与校准样品的称样量基本保持一致;所称取样品包裹于锡囊中进行分析;③由于存在样品基体对测定氮的影响,应使测定样品与校准仪器的标准样品在成分形态方面尽可能保持相似;用煤标准样品对仪器进行校准更为合理;④按本方法所得测定值与国家标准方法的测定结果一致,符合标准方法中要求的精密度。     

《热分析仪器》

《热分析仪器》是“分析仪器使用与维护丛书”之分册。该书系统介绍了各类热分析与量热仪的原理、基本结构、元件和单元；各类热分析与量热仪及标志仪器性能的各项指标，表征实验数据质量的各项参数；影响实验结果的各种因素和各项标准实验方法；若干应用实例；以及仪器常见的故障处理等内容。     

氧弹式量热法测燃烧热实验的改进

本文讨论了氧弹式量热计的改进方法 ,并对仪器装置和实验原理进行了分析 ,最后给出了仪器改进前后部分实验结果的比较 ,从中可以看出 ,实验准确度有较大的提高。     

抑制剂对大肠杆菌作用的透射电镜及微量热法研究

用透射电镜对大肠杆菌以及大肠杆菌受到３种不同抑制剂抑制时的形态进行了观察，结果发现不同的抑制剂对大肠杆菌的不同抑制作用表现在大肠杆菌的微观形态发生了不同的变化，同时结合微量热的方法，测试了３种不同抑制剂作用下大肠杆菌的生长代谢热谱，热谱曲线的分析结果与透射电镜观察结果吻合。     

吸热型碳氢燃料热沉的测定研究

改进并重新组装了自行研制的高温热导型流动热量计 ,利用电标定法测定了该仪器在 70 0℃和 80 0℃的热量常数。为检验仪器的可靠性 ,本仪器测定了氮气的热沉 ,结果表明实验值与用氮气的热容公式计算所得的计算值基本吻合。对自制的吸热型碳氢燃料 (FRA)和作为模型化合物的正庚烷的热沉进行了测定 ,发现在 70 0℃时两者的热沉值比较接近 ,分别为 3 0 7MJ kg和 3 2 3MJ kg。在 80 0℃时 ,两者都具有较高的热沉值 ,分别达到 5 6 9MJ kg和 6 6 0MJ kg ,该热沉值能够满足超高音速飞行器的热管理要求。     

DSC程序设定升(降)温速率偏离的简易修正方法

通过对程序设定的不同升、降温速率下差示扫描量热法(DSC)图谱的数值分析，发现在试样发生相变时实际过程的升(降)温速率偏离仪器程序设定的线性速率现象；从热流的定义出发，提出了对DSC相变热流数据作升(降)温速率偏离线性的简易修正方法。     

电感耦合等离子体质谱(ICP-MS)法测定地球化学样品中的痕量金

采用王水体系对地球化学样品进行水浴消解,聚氨酯泡塑吸附富集,硫脲解脱,电感耦合等离子体质谱(ICP-MS)法测定地球化学样品中的金元素。采用调谐液调节ICP-MS仪器至最佳化,以GAu-11b为标准,单点校正直接测定。对痕量金标准物质(GAu-12、GAu-13、GAu-11b、GAu-10a、GAu-2b、GAu-7b、GAu-8a)的分析结果与标准值相一致,方法相对标准偏差(RSD,n=12)为4.8%~6.7%。方法检出限为0.015ng/g,加标回收率为85.5%~100%。与常规石墨炉原子吸收光谱法测定方法相比较,ICP-MS法操作简单快捷、试剂用量少、信背比高,有利于大批量地球化学样品快速测定。     

连续流动分析法测定土壤中的挥发酚

建立了连续流动分析仪测定土壤中挥发酚含量的方法。称取5 g左右的土壤样品,以磷酸调节p H值为4,加入适量水并进行蒸馏,馏出液用连续流动分析仪测定挥发酚含量。在4.96~200μg/L范围内,挥发酚的质量浓度与相对峰高线性相关,线性方程为y=235.31x+51.6,相关系数r~2=0.999 8,挥发酚的检出限为1.24μg/L。取2种土壤样品分别进行6次平行测定,测定结果的相对标准偏差分别为1.52%,1.56%。对2种挥发酚标准样品进行测试,相对误差分别为1.90%,2.08%,加标回收率在87.8%~95.5%之间。该方法适合大批量样品的连续分析,且无需使用三氯甲烷,与传统方法相比更安全环保。     

Portable Analyzer for Rapid Analysis of Total Protein, Fat and Lactose Contents in Raw Milk Measured by Non-dispersive Short-wave Near-infrared Spectrometry

A novel portable analyzer for raw milk quality control during the material purchase at dairy plants was developed, by which the percentages(mass fraction) of main components including total protein, fat, and lactose of an unhomogenized milk sample could be determinated in 1 min with the help of non-dispersive short-wave near-infrared (NDSWNIR) spectrometry in a wavelength range from 600 nm to 1100 nm and multivariate calibration. The analyzer was designed with a single-beam optical system, which comprised a temperature control module, a multi-channel narrow-band light source(16 wavelengths), a glass absorption cell with 15 mm sample thickness, a silicon photodiode detector, several compound lenses and a recorder module. A total of 80 raw milk samples were collected at a dairy farm twice a month for 4 months. The samples were scanned with a common UV-Vis-NIR spectrometer and analyzed according to China GB standard methods. The uninformative variables elimination(UVE) method was carried out on the spectrum data and the percentages of main components of all the samples to choose the peak emitting wavelength of each channel of the light source. Another 90 raw milk samples were collected from the same dairy farm thrice a month for 3 months. The samples were analyzed according to China GB standard methods and with the proposed analyzer. The percentages of the main components and the NDSWNIR absorption data of the samples were used for the construction and validation of the multivariate calibration model with partial least squares(PLS) method. The root-mean-square errors of prediction(RMSEP) of total protein, fat and lactose were 0.201, 0.172 and 0.247 and the coefficients of correlation(R) were 0.932, 0.981 and 0.933, respectively.     

一次消解土壤样品测定汞、砷和硒

建立了测定土壤中3种挥发性元素(汞、砷、硒)的一次消解方法,确定以程序控温石墨自动消解仪+王水-氢氟酸-硼酸络合敞开体系为最佳消解体系,采用氢化物发生-原子荧光光谱法(HG-AFS)分别测定同一消解液中汞、砷、硒的含量.采用国家标物中心有证标准物质土壤环境样品GSS-1~GSS-8进行了方法验证,结果均符合标准偏差的允许范围.此消解方法相比于现行标准方法,避免了针对各元素的分次处理,简化了消解步骤,节省了前处理时间,减少了试剂消耗,提高了实验效率,适用性广、灵敏度高、检出限低,尤其适合批量样品的微量/痕量元素分析,可作为一种大规模土壤样品中重金属污染监测和治理的快捷方法.     

The determination of certain major and minor elements in geological samples by inductively coupled plasma atomic emission spectrometry. Some interference problems with the analysis of geological standard reference materials and nutrition supplements

Direct ICP-AES measurements of the digested geological standard reference material samples yielded the wrong information about their composition. The differences between certified and measured concentrations of the samples were due to the complicated sample matrix. The measured concentrations can be successfully corrected by using a multiple linear regression technique. The correction is based on the multiple regression line calculated from the analytical results at synthetic mixtures of matrix elements, where concentrations varied on five levels. There were no significant (P = 0.05) differences between certified and measured concentrations in standard reference materials after the correction. The same method was used in the analysis of nutrition supplements.     

氢氧化钠标准溶液浓度不确定度的评定

评定了按照GB／T601-2002方法配制和标定氢氧化钠标准溶液浓度的不确定度。从仪器、试剂、操作及实验环境方面分析了不确定度来源,对不确定度分量进行了分析、计算、合成。氢氧化钠标准溶液浓度的不确定度主要由标定时消耗体积的读数误差产生。在试剂纯度、仪器精度符合规定时,氢氧化钠标准溶液浓度的相对扩展不确定度为0．14％。     

纳氏试剂测定水中氨氮影响因素的探讨

对国家生活饮用水标准检验方法"GB/T5750—2006"中涉及到的水中氨氮的检测条件进行了探讨,讨论了样品的采集与保存,影响显色、空白值的各项因素,并提出相应的解决办法。对国家标准物质以及实际样品的验证表明,方法的相对误差为0.03%~1.5%,相对标准偏差RSD为0.55%~5.3%,准确度也能满足分析要求,对国家标准方法进行了补充与细化,在实际工作中有参考价值。     

Feasibility of eliminating interferences in graphite furnace atomic absorption spectrometry using analyte transfer to the permanently modified graphite tube surface

A procedure is proposed to avoid spectral and/or non-spectral interferences in graphite furnace atomic absorption spectrometry (GF AAS) by transferring the analyte during the pyrolysis stage from a solid sampling platform to the graphite tube wall that has been coated with a permanent modifier, e.g. by electrodeposition of a platinum-group metal. The direct determination of mercury in solid coal samples was chosen as a model to investigate the feasibility of this idea. The graphite tube surface was coated with palladium and the analyte was transferred from the solid sampling platform to the tube wall at a temperature of 500±50 °C. A characteristic mass of m₀=64 pg Hg was obtained for an atomization temperature of 1300 °C, proposing a quantitative transfer of the analyte to the tube wall. Calibration against aqueous mercury standards was not feasible as this element was lost in part already during the drying stage and could not be trapped quantitatively on the modified graphite tube surface. However, the results for all except one of the coal reference materials were within the 95% confidence interval of the certificate when the slope of a correlation curve between the integrated absorbance, normalized for 1 mg of sample, and the certified value for mercury was used for calibration. A detection limit of 0.025–0.05 μg g⁻¹ Hg in coal, calculated from three times the standard deviation of the investigated coal samples, could be obtained with the proposed method. The spectral interference due to excessive background absorption in the direct determination of mercury in coal could be eliminated completely. It is expected that this analyte transfer can be used in a similar way to eliminate other spectral and/or non-spectral interferences in the GF AAS determination of other volatile analytes.     

The determination of certain major and minor elements in geological samples by inductively coupled plasma atomic emission spectrometry. Some interference problems with the analysis of geological standard reference materials and nutrition supplements

Direct ICP-AES measurements of the digested geological standard reference material samples yielded the wrong information about their composition. The differences between certified and measured concentrations of the samples were due to the complicated sample matrix. The measured concentrations can be successfully corrected by using a multiple linear regression technique. The correction is based on the multiple regression line calculated from the analytical results at synthetic mixtures of matrix elements, where concentrations varied on five levels. There were no significant (P = 0.05) differences between certified and measured concentrations in standard reference materials after the correction. The same method was used in the analysis of nutrition supplements. Received: 25 January 2000 / Revised: 15 March 2000 / Accepted: 31 March 2000     

石墨炉原子吸收法直接测定海水中铅的方法探索

目的探索石墨炉原子吸收法直接测定海水中铅的检测方法。方法用硝酸铵稀释海水样品,用硝酸钯和磷酸二氢铵作为基体改进剂,用石墨炉原子吸收法测定了海水中的铅含量。结果通过加标回收的验证,检测结果准确可靠。结论适合用于海水中铅含量的测定。