最新安捷伦1100系列微盘液相系统提供快速样品分析的完整方案

安捷伦公司最新推出的1100系列微盘液相系统,在高效液相色谱系统上配以微盘进样装置和快速样品分析系统,将分析效率提高近10倍,且保持较短的保留时间和优异的分析精度。该系统在Agilent1100系列高效液相色谱基础上,配以最新Agilent1100系列微盘自动进样器。进样系统具有最大的灵活性和快速进样的循环方式。进样速率与标准1100系列自动进样器同样高。多重进样功能允许用户在一个样品正在分析的同时,准备另一个样品。多种样品盘包括384位微量托盘和深孔盘,可供用户灵活选择,一次完成700多个样品分析。对热不稳定样品还可选用温控组件。该系统…     

进样阀(I)

高效液相色谱进样阀（或进样器）的作用是将一定量的样品送入色谱仪。样品在流动相的带动下进入色谱柱系统完成分离过程。现代高效液相色谱仪对于进样阀的要求如下：（１）耐高压,因为高效液相色谱通常要在３５．０ＭＰａ或更高的压力下工作;（２）进样量精确;（３）进样重复性好;（４）方便、适用,且可根据需要选择不同的进样量;（５）价格低廉;（６）保证在色谱柱中心进样,操作时不产生流量或压力波动。到目前为止,液相色谱进样阀共有３种形式：１．手动注射进样器;２．手动进样阀;３．自动进样器。从原理上讲,自动进样器是在…     

高效液相色谱仪自动进样器校准方法及不确定度评定

建立高效液相色谱仪自动进样器的校准方法,并对其测量不确定度进行评定。参考欧洲医药管理局《质量控制文件》提供的方法对液相色谱仪自动进样器的进样体积误差、进样残留和进样重复性建立校准方法,经评定得进样体积误差的相对扩展不确定度为1.8%。高效液相色谱仪自动进样器校准方法及不确定度评定方法的建立,为高效液相色谱仪自动进样器的校准提供依据。     

岛津C－R2A全自动高效液相色谱分析程序的设计

 利用Ｃ－Ｒ２Ａ色谱处理机的编程功能，实现了液相色谱法（主机为ＬＣ－４Ａ和ＳＩＬ－２ＡＳ自动进样器）全自动分析，即通过程序实现按设定的样品顺序、进样量、重复次数对样品进行测定，每个样品分析完后，进行数据处理。     

岛津C－R2A全自动高效液相色谱分析程序的设计

利用Ｃ－Ｒ２Ａ色谱处理机的编程功能，实现了液相色谱法（主机为ＬＣ－４Ａ和ＳＩＬ－２ＡＳ自动进样器）全自动分析，即通过程序实现按设定的样品顺序、进样量、重复次数对样品进行测定，每个样品分析完后，进行数据处理，并打印出结果表     

新型全二维微柱液相色谱分离平台的构建

采用自动进样器和一套二元梯度泵构建了以阳离子交换色谱-反相色谱(SCX-RPLC)为分离模式的新型全二维微柱液相色谱分离平台.在第一维分离中,通过自动进样器将不同浓度的盐溶液以台阶梯度输送至SCX柱上,实现肽段的分级洗脱.洗脱下的肽段经C8预柱富集、除盐后,进入第二维C18 RPLC柱上,通过线性梯度实现进一步的分离.采用该平台分离了5种标准蛋白的酶解产物,系统峰容量可达1 467.结果表明,该平台可以自动完成进样、除盐、分离及检测.     

气相色谱仪的两种液体样品自动进样器的兼容设计与研制

设计和构建了多轴多模式、闭环伺服控制系统的研发平台,实现了用于气相色谱仪的不同结构的两种液体自动进样器的并行设计与研制。基于兼容与互换的思路,开发出一体化嵌入式控制驱动模块,采用相同的直流电机、编码器,电气与机械接口统一标准,实现了上述组件在两种机型间的直接代换。研制的标准型110个样品位和平台型40个样品位两种液体自动进样器,与气相色谱仪联机,采用1μL手动进样针,对于0.5μL十六烷-异辛烷标准液体样品,6个不同瓶位连续6次进样测试,重复进样的信号峰面积RSD分别为1.1%和1.5%,取0.1,0.3,0.5,0.7和0.9μL进样,峰面积与进样量的线性相关系数为0.9947。     

烷类特种气体分析装置的研制及其应用

研制烷类特种气体分析专用的多维气相色谱仪，特制的热导检测器，具有手动－自动功能。设计了输气－配气装置和多维气相色谱流程。以微机控制，可按编辑程序清洗系统。检查本底，自动进样，显示或打印谱图和分析结果。可检测多种烷类特种气体组份及其中氧，氮，一氧化碳和甲烷等痕量杂质。     

液相色谱仪自动进样器样品室温度的校准

液相色谱仪自动进样器样品室的温度对于液相色谱样品的储存与测试有直接影响。为了保证其准确性与溯源性，结合其温控原理和布局结构提出相关的校准项目、校准方法、技术指标及校准设备。同时，针对不同测量方式的校准设备，对有线温度测量方式与无线温度测量方式进行对比。通过分析其结构适应性和实际测量结果得出，有线温度测量方式虽然具备易于获得且成本较低的优势，但其适用范围较小，且可能导致缠绕、牵扯、样品室无法正常闭合、探头位置不易控制等情况，测量结果也显示其会影响样品室温度均匀性的测量。而无线温度测量方式由于其没有线的约束，能适用于各类自动进样器，从实际测量操作和测量结果上看也优于有线测量方式，更适合用于液相色谱仪自动进样器样品室温度的校准。     

离子色谱法快速测定牛奶中SCN~–

建立了离子色谱快速测定牛奶中SCN–的方法。采用东曹IC–2010型号离子色谱仪及TSKgel Super IC–Anion HS型阴离子快速分离柱;淋洗液为5.0 mmol/L Na2CO3溶液,流量为1.5 m L/min,柱温为40℃,进样体积为20μL,样品经乙腈去蛋白,经TOYOPAK ODS小柱除掉脂肪后,经IC–2010自动进样器自动稀释2倍后进样分析。硫氰酸根测定结果的相对标准偏差为0.94%(n=5),加标回收率为97.0%~102.8%。该方法可用于鲜奶中硫氰酸根的检测。     

Improving splitless injection with electronic pressure programming

An experimental injection port has been designed for split or splitless sample introduction in capillary gas chromatography; the inlet uses electronic pressure control, in order that the column head pressure may be set from the GC keyboard, and the inlet may be used in the constant flow or constant pressure modes. Alternatively, the column head pressure may be programmed up or down during a GC run in a manner analogous to even temperature programming. Using electronic pressure control, a method was developed which used high column head pressures (high column flow rates) at the time of injection, followed by rapid reduction of the pressure to that required for optimum GC separation. In this way, high flow rates could be used at the time of splitless injection to reduce sample discrimination, while lower flow rates could be used for the separation. Using this method, up to 5 μl of a test sample could be injected in the splitless mode with no discrimination; in another experiment, 2.3 times as much sample was introduced into the column by using electronic pressure programming. Some GC peak broadening was observed in the first experiment.     

Low-Cost Detection of Methane Gas in Rice Cultivation by Gas Chromatography-Flame Ionization Detector Based on Manual Injection and Split Pattern

Rice cultivation is one of the most significant human-created sources of methane gas. How to accurately measure the methane concentration produced by rice cultivation has become a major problem. The price of the automatic gas sampler used as a national standard for methane detection (HJ 38-2017) is higher than that of gas chromatography, which greatly increases the difficulty of methane detection in the laboratory. This study established a novel methane detection method based on manual injection and split pattern by changing the parameters of the national standard method without adding any additional automatic gas samplers. The standard curve and correlation coefficient obtained from the parallel determination of methane standard gas were y = 2.4192x + 0.1294 and 0.9998, respectively. Relative standard deviation (RSD, <2.82%), recycle rate (99.67–102.02%), limit of detection (LOD, 0.0567 ppm) and limit of quantification (LOQ, 0.189 ppm) of this manual injection method are satisfying, demonstrating that a gas chromatography-flame ionization detector (GC-FID), based on manual injection at a split ratio (SR) of 5:1, could be an effective and accurate method for methane detection. Methane gases produced by three kinds of low-methane rice treated with oxantel pamoate acid, fumaric acid and alcohol, were also collected and detected using the proposed manual injection approach Good peak shapes were obtained, indicating that this approach could also be used for quantification of methane concentration.     

变压器油中溶解气体分析专用气相色谱仪的检定与校准

为解决检定变压器油中溶解气体分析专用气相色谱仪时遇到样品进样量计算不准,检测器对甲烷气体标准物质无响应,专用软件分析方法不能更改等问题,建立变压器油中溶解气体分析专用气相色谱仪的检定与校准方法。当进样模式为一次进样双柱分流时,按分流比计算分流到检测器的样品体积,其它进样模式按进样体积计算进样量;因色谱软件禁止积分导致CH_4在热导检测器上无响应时,应采用有证标准物质中的H_2或O_2进行检定与校准。以7890B型专用气相色谱仪为例,详细说明了变压器油中溶解气体分析专用气相色谱仪的检定与校准流程。该法为检定人员检定该类专用仪器时提供了参考。     

Quantitative analysis of phthalates using a pyrolyzer gas chromatography/mass spectrometry method

A pyrolyzer gas chromatography/mass spectrometry (GC/MS) method eliminates toxic solvents that burden our environment and can address the crucial problem of the solvent extraction GC/MS method. The purpose of this study is to establish an efficient quantitative analysis method for 10 phthalates that are regulated by the several governments. A change of concentrations over time for phthalates and internal standards was measured to verify the feasibility of using an auto sampler that facilitates analyzing multiple samples. Both standards maintained constant concentrations over the appropriate time for analysis. A certified reference material under the auspices of the Korea Research Institute of Standards and Science was used to verify the calibration curve obtained by the pyrolyzer GC/MS method, and a deviation was considered similar to the solvent extraction GC/MS method. Then, the limit of detection and limit of quantitation values were confirmed for various consumer products. To verify the reliability of the method, a comparative test with several accredited testing institutes was conducted, and the results were within the standard deviations of the results provided by the institutes. These results indicate that the pyrolyzer GC/MS method can be used in not only screening but also in accurate quantitative analysis.     

Practical method for the measurement of Alkyl mercaptans in natural gas by multi-dimensional gas chromatography, capillary flow technology, and flame ionization detection

Volatile sulfur compounds such as alkylmercaptans are undesired impurities in natural gas streams. As a result, natural gas treatment and purification services are essential in many industries that utilize natural gas either as a fuel or in a chemical process. While there are many analytical methods that can be employed for the measurement of mercaptans, a simple, practical, and easy-to-implement method is required for remote field deployment. An analytical method, based on multi-dimensional gas chromatography (MDGC), capillary flow technology and flame ionization has been successfully developed for the application described. Results based on the technique showed alkylmercaptans can be accurately measured with a minimum detection limit of 200 ppb (v/v) or better, a linear range of up to 100 ppm (v/v), and a relative standard deviation (n=10) of 1.2% or less were obtained by manual injection with a total sample-to-sample analysis time of less than 15 min.     

快速气相色谱法测定汽车工业废气中芳烃排放量

采用气体直接进样及快速程序升温气相色谱法,能在８０ｓ内快速,简单地测定废气中芳烃等多种组分的含量。在本方法中,芳烃的最低检出浓度为０．１ｍｇ／ｍ６３,该方法允在两周内测定了汽车喷漆车间４８个排气口的５７６个样品,具有简单,快速,灵敏,实用等优点,特别适合于涂装工业气体稀释溶剂样品的测定。     

顶空直接进样气相色谱法测定黏胶剂中的苯系物

目的建立检测黏胶剂中苯系物的方法。方法用顶空直接进样气相色谱法测定黏胶剂中的苯、甲苯、乙苯、对二甲苯、间二甲苯、邻二甲苯以及苯乙烯7种组分,对气相色谱柱、顶空加热温度以及顶空提取时间进行了讨论。结果对苯乙烯等7种被测组分的检测限均小于5mg/kg,7种组分在毛细管柱中能够很好的分离,回收率范围为81%～94%,RSD为5%～10%,具有操作简单、快速等特点。结论能够满足对黏胶剂中苯系物测定的分析要求。     

气相色谱法测定爱迪注射液中的斑蟊素

 研究了斑蟊素在几种萃取体系中的分配行为,测定了它的分配系数。选定二氯甲烷为萃取剂,在相比为1∶10时,只需一次萃取便可以使斑蟊素定量富集。选用OV-17填充柱、外标法定量。方法的分离效果令人满意,检测限低,结果的准确性和精密度良好。     

Analysis of phytosterols and phytostanols in enriched dairy products by Fast gas chromatography with mass spectrometry

A Fast gas chromatography and mass spectrometry method for plant sterols/stanols analysis was developed, using a short capillary gas chromatography column (10 m × 0.1 mm internal diameter × 0.1 μm film thickness) coated with 5% diphenyl‐polysiloxane. A silylated mixture of the main plant sterols/stanols standards (β‐sitosterol, campesterol, stigmasterol, campestanol, sitostanol) was well separated in 1.5 min, with a good peak resolution (>1.4, determined on a critical chromatographic peak pair (β‐sitosterol and sitostanol)), repeatability (<13%), and sensitivity (<0.017 ng/mL). The suitability of this Fast chromatography method was tested on plant sterols/stanols‐enriched dairy products (yogurt and milk), which were subjected to lipid extraction, cold saponification, and silylation prior to injection. The analytical performance (sensitivity < 0.256 ng/mL and repeatability < 10.36%) and significant reduction of the analysis time and consumables demonstrate that Fast gas chromatography‐mass spectrometry method could be also employed for the plant sterols/stanols analysis in functional dairy products.     

提高碘量法测定天然气中硫化氢效率的方法

碘量法是测定管道输送天然气中硫化氢的一种经典方法,而管道输送天然气中硫化氢含量较低,按照GB/T11060.1–2010方法测定,取样量较大,取样时间长,影响工作效率。针对此问题,从两方面对碘量法进行改进:减小天然气取样量进行试验,并与国标规定取样量时的实验结果进行比对,确定最佳取样量;增大取样流量进行试验,并与国标规定取样流量时的实验结果进行比对,确定最佳取样流量。对硫化氢质量浓度为7.2~14.3,14.3~28.7 mg/m~3的天然气样品进行试验测定,结果表明,将天然气取样量减少为20 L,取样时间分别由200,100 min缩短为40 min;将天然气取样流量设定为750 m L/min,取样时间分别由200,100 min缩短为133,67 min。减少取样量或者提高取样流量,均能缩短管输天然气的取样时间,提高检测效率。