Volatile phase profiling of mainstream smoke by glass capillary gas-chromatographic techniques

A heated injection system for a microprocessor-controlled GC has been developed for the (GC)² analysis of the volatile phase of whole smoke of a cigarette. Effects of injection port temperature and the presence of a Cambridge filter pad are demonstrated. Chromatograms are shown for smoke samples with and without a Cambridge Filter with the sample valve oven at 25°, 165° and 205°C. The use of a flame ionization and a nitrogen-phosphorous detector is illustrated.     

A photometric detector driven by beta radiation

It was recently found that typical Chromatographic carrier gases such as argon or nitrogen could be used in a modified flame photometric detector for general or selective determination of eluted molecules. The detector was powered not by a flame but by a radioactively stimulated, mild discharge. The luminescence arose from the second positive system of nitrogen (in argon), and various emissions from aroyl-containing molecules (in nitrogen).This study describes experiments that take away not only the flame but also the discharge: The energy that produces the luminescence is derived solely from the beta decay of⁶³Ni. Because of this low power input, the sensitivity of the present beta-driven photometric detector (-PD) is limited to about 25 ppm of nitrogen (in argon), and to about 5 pg/s for benzaldehyde and other well-responding aroyl compounds (in nitrogen). In accordance with mechanisms postulated earlier, other types of molecules do not produce significant responses in the absence of an electrical field.Material taken from doctoral thesis     

Highly sensitive determination of haloperidol in human serum by capillary gas chromatography using a surface ionization detector

A method has been developed for highly sensitive determination of haloperidol in human serum involving a simple extraction procedure followed by gas chromatographic separation. Target components were separated from the extracting solvents with a Van den Berg type solventless sample injector before introduction Into a DB-1 capillary separation column. A surface ionization detector (SID), which has highly selective sensitivity for Substituted amines, was employed for quantitation using bromperidol as an internal standard. Chloroform proved to be the best extracting solvent, yielding a quantitative detection limit of 5 ng/ml (S/N = 2). Comparison of the response to target compounds obtained by the SID, FTD (flame thermionic detector), and FID (flame ionization detector) showed the SID to be superior.     

Luminol chemiluminescence HPLC reaction detector for amino acids and other ligands

A detector for HPLC is based on suppression of chemiluminescence from the Cu(II)-luminol-peroxide reaction. Analytes which complex Cu(II) reduce the free Cu(II) concentration and thus the observed chemiluminescence intensity. The degree of chemiluminescence suppression is a measure of the analyte concentrations. Detection limits are in the range of 1 pmole-1 nmole for amino acids (both primary and secondary without derivatization), CN^–, amines, catecholamines, catechol, and aminoglycoside antibiotics. The detection approach is demonstrated with an ion-exchange separation of amino acids, a reverse phase separation of catecholamines, and an ion-pair separation of the three components of gentamicin C in commercial gentamicin sulfate.     

Electrochemical detector with a 20 nl volume for micro-columns liquid chromatography

Summary A flow-through two electrode wall-jet cell with a platinum measuring electrode and a cell volume of 20 nl has been designed and evaluated. It has been used to detect phenols by reversed phase liquid chromatography using short micro bore columns. The linear dynamic range between the measured current and the concentration is greater than 10³ (1.5×10^–7–5×10^–4 mol/l) and the minimum analyzable amount was found to be 10 pg for pyrocatechol. A negligible broadening in the detector permits the use of micro columns down to 0.5 mm internal diameter, packed with 5 m particles, without any substantial distortion of eluted zones.Presented at the 14th International Symposium on Chromatography London, September, 1982     

Electron capture detector response to low electron affinity aromatic hydrocarbons using positive ion stabilization and alkyl chloride sensitization

The electron capture detector (ECD) response to numerous aromatic hydrocarbons of low electron affinity (EA) is shown to be detrimentally affected by two processes which compete with and typically overwhelm the electron capture reactions of these molecules. It is shown that the effects of these two undesired reactions can be eliminated by the permanent addition of trimethylamine and one of several alkyl monochlorides to the detector make-up gas. These modifications of the detector gas result in greatly increased sensitivity, increased linearity, and increased reproducibility of response. A kinetic model for the ECD responses of low EA resonance capture molecules is developed which appears to explain these improvements.     

用二维色谱技术测定聚合反应气体组成

介绍一种无阀切换的二维气相色谱分析方法。采用两根不同性质的色谱柱并联连接，样品分别经两根色谱柱分离后汇合在一起进入同一检测器。一次进样可同时测定Ｈ２、Ｏ２、Ｎ２及Ｃ１～Ｃ３的组分。     

Sequential optimisation of the separation of a complex mixture of plastics additives by HPLC with a quaternary gradient and a dual detection system

Summary The separation of two families of plastics additives (phenolic antioxidants and UV absorbers) has been achieved by high performance liquid chromatography with a quaternary gradient. A methodology of separation based on a sequential optimization is described. After a preliminary study of the effects of solvents on retention of compounds, the mobile phase is first chosen for each class of additives (Irganox and Tinuvin), then for the mixture of all the compounds and the separation is finally optimized. The importance of the column phase ratio is also reported. The use of two detectors, UV absorbance and light-scattering, enables all the compounds to be detected. The performance of the detectors has been compared and the effects of the nebulization temperature on the detection of low molecular mass compounds is reported.     

Ion pair generation rates near planar3H and63Ni electron capture detector foils

The ion-pair generation rate (ionization topography) in plasmas from⁶³Ni and particularly Ti³H₄ foils, as used in electron capture detectors, was measured at room temperature using large, parallel plates of low backscattering ability in nitrogen gas of varying density. For one atmosphere pressure, the fall-off of ion pair formation as calculated from the exponential region equalsN ₀·e ^–0.19d for⁶³Ni andN ₀·e ^–1.4d for³H (whereN ₀ is the initial ionization rate immediately adjacent to the foil andd is the distance from the foil in mm). The experimentally measured half ranges (distances from the foil within which 50% of all possible ion pairs are created) are 2.7 mm for⁶³Ni and 0.27 mm for³H. The half ranges calculated from the exponential region where there is less interference from electron backscattering, are 3.7 and 0.5 mm, respectively. The latter values are considered closer to the true, unimpeded ionization topography near planar⁶³Ni and³H foils.Material taken from doctoral thesis     

溶液酸度在线检测装置的研制

研制了酸度在线检测装置，并应用于溶液酸度在线检测，溶液酸度在线检测装置，设有防污过滤器，自动采样器，蠕动泵，小型管道ｐＨ传感器和控制电路等，其特点为防污除油，随机自动采样，定时检测，全部管道化，可单独使用和计算机控制系统联网，适用于溶液酸在线分析，测定精度〈ｐＨ０．０５。