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Electrolyzer-Powered Flame Ionization Detector

机译:电解动力火焰电离探测器

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We describe here a novel water electrolyzer-powered flame ionization detector (EFID), characterized by enhanced portability, reduced cost of operation and improved safety of operation and storage. A conventional FID operates with a hydrogen diffusion flame, which has a central flow of pure hydrogen and column effluents, surrounded by a much higher coaxial flow of pure air. In contrast, the EFID is based on the combustion of a premixed (unseparated), hydrogen and oxygen, stoichiometric gas mixture. This premixed gas mixture is provided by a simple water electrolyzer with low power arid water consumption, without separation, compression, or pressure stabilization of the hydrogen and oxygen. The EFID is very similar to FID with two minor modifications: (a) The flame tip must have a narrow hole (4250/μm) to prevent flame flashbacks. (b) The entire detector structure is maintained above 100 ℃ to prevent water condensation due to the lack of diluting air. The EFID sensitivity is similar to that of the FID, and up to twice improved detectivity is demonstrated with the EFID. The flame chemical ionization yield of the EFID linearly increases with the electrolysis current The EFID response is linear over almost o orders of magnitude. The response is selective to carbon compounds where the response in aliphatic compounds is ~30% lower than with aromatic compounds, and no observable difference for N-, S-, P-, and Cl-containing compounds. The use of splitless solvent injections with a megabore column (0.53 mm i.d.) quenches the flame. This flame extinction is eliminated by the use of a miniature air pump during the solvent elution time. Typical electrolyzer operating parameters are current of 1.5 A, 12 mL/day water consumption and 4 W electrolyzer power requirements. Thus, a relatively small size water electrolyzer can provide the total gas consumption of the EFID for up to 40 days before water replenishing is required. This EFID can also be operated either as an EFID or as an FID, simply by replacing the gas sources.
机译:我们在此介绍一种新颖的水电解动力火焰离子化检测器(EFID),其特点是便携性强,降低了操作成本并提高了操作和存储的安全性。常规的FID使用氢扩散火焰运行,氢扩散火焰的中心是纯氢气和塔流出物,周围是更高的同轴纯空气流。相反,EFID基于预混合(未分离)的氢和氧,化学计量气体混合物的燃烧。这种预混合的气体混合物是由简单的水电解槽提供的,该电解槽具有低功率和低水消耗量,而没有氢,氧的分离,压缩或压力稳定作用。 EFID与FID非常相似,但有两个小修改:(a)火焰尖端必须有一个狭窄的孔(4250 /μm),以防止火焰回火。 (b)整个探测器结构保持在100℃以上,以防止由于缺乏稀释空气而导致水凝结。 EFID灵敏度与FID相似,并且EFID的探测灵敏度提高了两倍。 EFID的火焰化学电离产率随电解电流线性增加。EFID响应在几乎一个数量级上呈线性。该反应对碳化合物具有选择性,其中脂族化合物的反应比芳族化合物低约30%,而含N,S,P和Cl的化合物无明显差异。使用兆流色谱柱(内径0.53毫米)的不分流溶剂进样可熄灭火焰。在溶剂洗脱期间,通过使用微型气泵消除了这种火焰的消失。电解槽的典型运行参数为1.5 A的电流,12 mL /天的耗水量和4 W的电解槽功率要求。因此,在需要补充水之前,相对较小尺寸的水电解槽可以提供EFID的总气体消耗长达40天。只需更换气源,该EFID也可以作为EFID或FID进行操作。

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