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本文采用惰性气氛脉冲加热色谱法测定了无氧铜中微量氧,测定灵敏度可以到达1ppm。并重点对试样制备、降低空白、熔池选择等条件进行了试验。该方法空白低,灵敏度高,操作简便,实用于炉前控制快速分析。 1.仪器及分析条件:采用自制的脉冲加热气相色谱仪,脉冲加热电流可达1000A。色谱条件为:氩载气流量120毫升/分,载气压力0.3公斤/厘米~2,色谱柱φ4(内径)×1500毫米,色谱担体上试601型碳分子筛40—60目,柱温40℃,热导池桥电流90毫安(采用恒热丝电流)。 2.试样制备:试样(φ7.5×9毫米)先用丙酮洗涤,干燥;待称重后,投到20毫升1N的沸腾盐酸中漂洗20秒,迅速在流水中冲洗和用无水乙醇洗涤二次,立即加到密闭进样器中用人流量氩冲洗
In this paper, the determination of trace oxygen in oxygen-free copper by inert gas pulse heating chromatography, the determination of sensitivity can reach 1ppm. And focus on the sample preparation, reduce the blank, the choice of pool conditions were tested. The method has the advantages of low blankness, high sensitivity, easy operation and practical application in rapid analysis of furnace front control. 1. Instruments and analysis conditions: homemade pulse heating gas chromatograph, pulse heating current up to 1000A. The chromatographic conditions were as follows: argon carrier gas flow rate 120 ml / min, carrier gas pressure 0.3 kg / cm ~ 2, column φ4 (inner diameter) × 1500 mm, , Thermal conductivity tank bridge current 90 mA (with constant hot wire current). 2. Sample Preparation: The sample (φ7.5 × 9 mm) was first washed with acetone and dried; to be weighed, poured into 20 ml of 1N boiling hydrochloric acid for 20 seconds, rinsed rapidly in running water, Ethanol twice, immediately added to a closed sampler rinse with flow of argon