微型反应器液相产物中C1￣C5烃分析系统及方法研究

本文介绍了一个适于终沸点为４００℃或更高的微型反应器液相产物中Ｃ１￣Ｃ５烃全组成分析的专用分析系统和分析方法。系统由六通阀、顶柱和分析柱组成，所有组件均置于同一色谱炉内，采用ＦＩＤ检测外标法定量。分析结果相对标准偏差小于１０％。半年来的应用结果表明，该系统及方法具有操作简便，定量结果准确，适用范围宽，连续运行周期长等特点，可以用于各类宽镏分样品中Ｃ１￣Ｃ５烃的全组成分析。     

C2H5C60H的加成产物的结构和光谱性质的最子化学研究

用ＩＮＤＯ系列方法对Ｃ２Ｈ５Ｃ６０Ｈ的１，２－加成和１，４－加成两种产物异构体的结构进行了理论研究，结果表明，１，２－Ｃ２Ｈ５Ｃ６０Ｈ具有Ｃ５对称性，１，４－Ｃ２Ｈ５Ｃ６０Ｈ没有任何对称性，１，２－Ｃ２Ｈ５Ｃ６０Ｈ的总能量比１，４－Ｃ２Ｈ５Ｃ６０Ｈ的低，以此优化构型为基础，计算了两处产物异构体的电子吸收光谱，讨论了其光谱红炱的原因，同时对产物的ＮＭＲ谱进行了探讨。     

C5烃中双环戊二烯过氧化物的分光光度测定

本报道了Ｃ５烃中双环戊二烯过氧化物（ＰＤＣＰＤ）快速准确的分析方法。在ＨＯＣ２Ｈ４ＯＣＨ３－Ｈ２Ｏ介质中，ＰＤＣＰＤ与ＫＩ反应生成Ｉ３＾－而Ｉ３＾－与ＰＤＣＰＤ的量成正比，在λｍａｘ＝３５２ｎｍ处可进行ＰＤＣＰＤ的光度测定，测定下限为３．２×１０＾－５ｍｏｌ／Ｌ，ＳＤ＝０．３４，ＲＳＤ＝１．４０％。     

气相色谱法分析低碳烷烃氧化脱氢芳构化产物

本文提供了一个简单有效的分析低碳烃氧化转化产物、包括Ｈ２、ＣＯｘ（ｘ＝１，２）和Ｃ１～Ｃ９烃的全组成分析方法，实验结果表明，该方法具有操作简单、定量结果准确性高、分析重复性好、以及连续运行周期长等特点，可满足课题基础研究的需要。     

离子色谱法测定矿物药中可溶性砷（Ⅲ）和砷（Ⅴ）

离子色谱法测定了矿物药雄黄，雌黄在盐酸配制的人工胃液中可溶性砷和砷。对淋洗液的组成及流速进行了选择。以流速为１．０ｍＬ／ｍｉｎ的３．５ｍｍｏｌ／Ｌ Ｎａ２ＣＯ３淋洗液在ＹＳＣ－４Ａ阴离子交换柱上分离，ＹＳ－Ｚ柱抑制，ＨＬＣ－６０１离子色谱仪电导检知器检测。     

羰基硫对FT合成气液相产物的影响

在５２４Ｋ，２．３１ＭＰａ，１８４５ｈ＾－１，Ｈ２／ＣＯ＝２．１的条件下考察了合成气中ＣＯＳ对下合成催化剂活性及产物分布的影响，结果表明，随着催化剂中硫含量的增加，尾气中ＣＯ２，ＣＨ４，含量减少，ＣＯ含量增加，催化剂中毒后，甲烷选择明显提高，Ｃ５重量百分含量降低，气态Ｃ２～Ｃ４烃增加了产物向低碳烃方向移动。油相和水相的产物分析结果表明，催化剂中毒后，气物中含氧化合物增加，液态烃中烯烃减少，正构烷烃     

茯苓菌核多糖的分离和结构分析

分别用０．９％ＮａＣｌ不溶液，热水，０．５ｍｏｌ／Ｌ ＮａＯＨ水溶液和８８％甲酸从新鲜茯苓菌核体中提取出５种多糖：ＰＣ１，ＰＣ２，ＰＣ２－Ａ，ＰＣ３和ＰＣ４．用ＩＲ，ＨＰＬＣ，ＧＣ，＾１ＨＮＭＲ和＾１３Ｃ ＮＭＲ等方法分析了它们的组成和结构。结果表明，ＰＣ１，ＰＣ２和ＰＣ２－Ａ由Ｄ－葡萄糖，Ｄ－木糖，Ｄ－甘露糖和Ｄ－半乳糖组成，ＰＣ１和ＰＣ２－Ａ含葡萄糖醛酸，其葡萄糖含量随提取过程的进行逐渐增加。     

多维气相色谱法测定催化裂化气体组成

１引言 催化裂化气体组成测定是炼油厂中重要的分析项目之一,其组成除含有Ｃ１～Ｃ５等轻烃组分外,还含有Ｈ２、Ｏ２、Ｎ２、ＣＯ、ＣＯ２等永久性气体,常规方法是利用３台气相色谱仪,一个样品３次进样,达到全组分分离,操作繁琐且准确度差。本文介绍的多维气相色谱法测定催化裂化气体组成,一个样品只需一次进样就能达到全组分的分离检测,操作简便,且重复性好,准确度高。２实验部分２．１仪器和色谱柱 ＨＰ５８９０Ⅱ型气相色谱仪;ＨＰ３３９６Ⅱ型积分仪（美国惠普公司）。癸二腈（柱１Ａ０．６ｍ×３．２ｍｍｉ．ｄ．：柱１Ｂ …     

浆态床FT合成／固定床ZSM－5改质的合成液体燃料工艺的研究和开发

从合成气制取液体燃料的浆态床ＦＴ合成／固定床２ＳＭ－５改质的反应系统由Ⅰ段鼓泡浆液反应器（内径４０ｍｍ，高４５０Ｏｍｍ）和Ⅱ段固定床ＺＳＭ－５反应器（内径４０ｍｍ，高９００ｍｍ）组成，在温度２５０～２８０℃（Ⅰ段），３００～３４０℃（Ⅱ段），压力１．５～２．５ＭＰａ，空速２．０ＮＬ／ｇＦｅ·ｈ（Ⅰ段），５００～１０００ｈ￣－１（Ⅱ段），Ｈ＿２ＣＯ比０．５～１．５和气速１～２ｃｍ／ｓ范围内，考察了工艺参数对反应性能的影响，１０００ｈ以上的寿命试验的平均结果为：合成气单程转化率６５．１％，产率１００ｇ／Ｎｍ￣３（Ｃｏ＋Ｈ＿２），总烃生产达３５０ｇ／Ｆｅ。使用富ＣＯ合成气时，达１１０ｇ／Ｎｍ￣３（ＣＯ＋Ｈ＿２）。实测的ＦＴ合成反应热为２９３８；５ｋＪ／Ｎｍ￣３（ＣＯ＋Ｈ＿２）。长期运转试验表明，工艺流程合理，设备操作和温度控制可靠。采用的浆液循环回路方法可初步分离蜡中的催化剂。     

〔NH_4（15－C－5）_2〕〔Cd_2（SCN）_5〕配合物的晶体和分子结构

用凝胶法合成了标题化合物［ＮＨ４（１５－Ｃ－５）２］［Ｃｄ２（ＳＣＮ）５］（１５－Ｃ－５＝Ｃ１０Ｈ２０Ｏ５）的晶体，并对其进行了红外光谱、元素分析等各项物理性质的测试，并经Ｘ射线单晶结构分析得到了配合物的全部晶体学数据：Ｍｒ＝９７３．７８，正交晶系，空间群Ｐｎｍａ，晶胞参数ａ＝１０．５０７（１）Ａ，ｂ＝１６．５８４（２）Ａ，ｃ＝２３．４９４（２）Ａ，Ｖ＝４０９３．８（３）Ａ３，Ｚ＝４，Ｄｃ＝２．５８０ｇ／ｃｍ３，μ＝１３．３１ｃｍ（－１），Ｆ（０００）＝１９６８，Ｒ＝０．０７０，Ｒω＝０．０８５。结构分析结果表明，配阳离子是由一个ＮＨ４＋和两个１５－Ｃ－５组成的，ＮＨ４＋没有进入１５－Ｃ－５空腔内，而是位于两个１５－Ｃ－５之间，呈夹心结构；配阴离子是以［Ｃｄ２（ＳＣＮ）５］为单元的阴离子长键，其中一组ＳＣＮ－被四个Ｃｄ离子共享，其余两组ＳＣＮ－被两个Ｃｄ离子共享，呈变形八面体构型。配阳离子［ＮＨ４（１５－Ｃ５）２］＋和配阴离子［Ｃｄ２（ＳＣＮ）５］－间靠静电力结合成配合物晶体。     

Sampling device for a simple,fast calibration technique in gas chromatographic trace analysis of gas phases and vapor phases

In order to accommodate continually changing tasks in the [μl/l]–[nl/m³] ranges of gas chromatographic trace analysis of gas phases and vapor phases, a simple and time-saving calibration technique is presented which renders unnecessary conventional test mixtures of the abovementioned concentration ranges. This new method is based on the simulation of such mixtures at the inlet of the GC unit with the aid of commercially available multiway sampling valves of various volumes by means of partial pressure sampling.     

Application of copper sulfate pentahydrate as an ammonia removal reagent for the determination of trace impurities in ammonia by gas chromatography

Rapid analysis of trace permanent gas impurities in high purity ammonia gas for the microelectronics industry is described, using a gas chromatograph equipped with a phtoionization detector. Our system incorporates a reactive precolumn in combination with the analytical column to remove the ammonia matrix peak that otherwise would complicate the measurements due to baseline fluctuations and loss of analytes. The performance of 21 precolumn candidate materials was evaluated. Copper sulfate pentahydrate (CuSO₄·5H₂O) was shown to selectively react with ammonia at room temperature and atmospheric column pressures, without affecting the hydrogen, oxygen, nitrogen, methane or carbon monoxide peak areas. To prevent loss of trace carbon dioxide, an additional boron trioxide reactant layer was inserted above the copper sulfate pentahydrate bed in the reactive precolumn. Using the combined materials, calibration curves for carbon dioxide proved to be equivalent in both ammonia and helium matrix gases. These curves were equivalent in both matrix gases. The quantitative performance of the system was also evaluated. Peak repeatabilities, based on eight injections, were in the range of 4.1–8.2% relative standard deviation; and detection limits were 6.9 ppb for H₂, 1.8 ppb for O₂, 1.6 ppb for N₂, 6.4 ppb for CH₄, 13 ppb for CO, and 5.4 ppb for CO₂.     

Direct gas chromatographic analysis of halogenated hydrocarbons at the part-per-trillion level

Large sample volume on-column injection (up to 250 μL) of n-pentane solutions of halogenated hydrocarbons has been employed for the direct measurement of both low-boiling and high-boiling compounds in what is essentially a single run. Two-bonded phase, fused-silica capillary columns are joined in series, through which the low-boiling compounds are first chromatographed and detected with an electron capture detector. High-boiling compounds are then trapped in a section joining the two columns, and subsequently chromatographed in the second column, using the same detector. This procedure permits analysis at the ppt level.     

哌嗪及其共生物的气相色谱分析研究

研究了哌嗪及其共生物的气相色谱分析方法。采用Chromsorb WAW（60～80目）为担体,以氢氧化钾作减尾剂,聚乙二醇（PEG 2万）作固定液,在长 1.5m的玻璃填充柱上哌嗪及其共生物得到良好的分离。除乙二胺外,其他相对误差均小于2％。并且计算了哌嗪及其共生物的得率和原料的转化率。     

气体传感器阵列信号的盲分离研究

本文在使用一个四单元微热板式集成气体传感器阵列测试煤矿中的两种主要易燃易爆气体一氧化碳和甲烷的基础上, 将气体传感器阵列与盲信号分离技术相结合, 讨论了混合气体分析的盲可辨识性, 并使用盲信号分离中的一种主要方法独立分量分析法(ICA)进行了分析和验证.     

GC-MS-SIM quantitation of amantadine in biological samples

Summary A simple, selective and sensitive method for the quantitation of amantadine in biological samples is described. After extraction from biological samples using a two-step procedure, amantadine is quantitatively converted into its isothiocyanate (NCS) derivative by treatment with carbon disulfide and then determined quantitatively using isobaric compounds, p-methoxyphenyl-ethylamine-NCS or N-acetylamantadine as external standards. The applicability of this method is illustrated by determining plasma levels of amantadine for pharmacokinetic studies and levels in dialysate samples of amantadine treated patients who were on dialysis machines.     

GC analysis of gas in halogen lamps using a new sampling device

Summary A new type of gas sampling device was constructed to improve the analysis of the gas in halogen lamps. Low levels of gases such as O₂, CH₄, C₂H₄ and CH₃Br could be determined by the techniques worked out.     

Low temperature sampling techniques for the determination of less volatile compounds in gaseous mixtures

Summary The analysis of trace quantities of the less volatile polar compounds (H₂O, NH₃, HCN, amines, alcohols, esters etc.) is frequently seriously affected by dubious sampling procedures. In the present contribution two different sampling techniques at dry ice temperature (195 K) are described which both claim considerable and predictable efficacy. Depending on whether the matrices of the samples are still gaseous or condensable at 195 K and ambient pressure, a scrubbing technique may be used or condensation in the presence of a suitable solvent with subsequent evaporation of the matrix. Some solvents and solvent mixtures with FP<195 K are compiled. The normally disadvantageous low volatility can be exploited for enrichment. The scrubbing technique enables detection limits of 1 ppb(V/V) to be achieved, the condensation technique 1 ppm(m/m). Simple checking methods for both techniques are described. Thermodynamic considerations for ideal mixtures enable the calculation of upper limits for possible deviations. Examples are presented.Presented at the 14th International Symposium on Chromatography London, September, 1982