Trace 1300气相色谱仪故障排查与期间核查
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摘要
使用赛默飞Trace 1300气相色谱仪进行环境样品分析过程中,出现了FID信号变弱、点火困难的现象,严重影响检测数据的准确性,干扰正常分析工作。从样品性质、仪器方法的设置、气路系统以及检测系统进行故障排查,确定故障原因为FID喷嘴堵塞,点火线圈锈蚀严重。对维修好后的气相色谱仪进行期间核查,核查结果:基线噪声为0.066 pA,基线漂移(30 min)为0.321 pA,FID检测限为0.094 1 ng/s,定性重复性为0.062%,定量重复性为1.41%,均满足技术指标要求。
In the running process of Thermo Fisher Trace 1300 gas chromatography FID signal became weak and ignition was difficulties,which seriously affected the accuracy of the detection results and interfered with the normal analysis. Troubleshooting work was carried out mainly from sample properties,instrument method setting,gas system and detection system. Causes of trouble were FID nozzle clogging,and serious corrosion in ignition coil. Period verification was carried out after maintaining the gas chromatography. Baseline noise was 0.066 pA,baseline drift(30 min) was 0.321 pA,FID detection limit was 0.094 1 ng/s,the qualitative repeatability was 0.062% and quantitative repeatability was 1.41%,which could meet requirements of technical indexes.
In the running process of Thermo Fisher Trace 1300 gas chromatography FID signal became weak and ignition was difficulties,which seriously affected the accuracy of the detection results and interfered with the normal analysis. Troubleshooting work was carried out mainly from sample properties,instrument method setting,gas system and detection system. Causes of trouble were FID nozzle clogging,and serious corrosion in ignition coil. Period verification was carried out after maintaining the gas chromatography. Baseline noise was 0.066 pA,baseline drift(30 min) was 0.321 pA,FID detection limit was 0.094 1 ng/s,the qualitative repeatability was 0.062% and quantitative repeatability was 1.41%,which could meet requirements of technical indexes.
引文
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[2]何风香.简述气相色谱分析仪的原理组成及使用[J].黑龙江科学,2013(9):134.
[3]孙银红,俞孝冬.毛细管气相色谱法分析丙烯酸中的阻聚剂甲氧酚和吩噻嗪[J].化学分析计量,2012,21(3):92–94.
[4]韦兰春.色谱法在精细化学品分析中的应用研究[D].南京大学,2016.
[5]董振霖,杨春光,肖珊珊,等.气相色谱和气相色谱–质谱法测定食品中乙草胺残留[J].分析化学,2009(5):698–702.
[6]杨君,王建华,刘靖靖,颜冬云.气相色谱–负化学离子源质谱法在食品安全分析中的应用[J].化学分析计量,2012,21(5):97–100.
[7]张利飞,黄业茹,史双昕等.土壤中多环芳烃和酞酸酯类有机污染物气相色谱–质谱测定方法中的质量控制与质量保证[J].色谱,2010(5):465–469.
[8]张泽楷,张明时.恒温–气相色谱法同时测定司法鉴定中的安定和三唑仑[J].分析试验室,2008(增刊1):380–382.
[9]宋光林.司法案件中轻质矿物油的鉴定[D].贵州大学,2007.
[10]祝波,赵鲁青,陈安珍,等.顶空采样–毛细管气相色谱法分析格列美脲原料药中的溶剂残留[J].色谱,2009(6):755–759.
[11]赵翠丽.气相色谱法在药物残留溶剂测定中的应用研究[D].河北医科大学,2016.
[12]周民锋,徐小平,顾海东,等.衍生气相色谱法在环境监测中的应用[J].中国环境监测,2014(2):108–114.
[13]郑明辉,吴嘉嘉.全二维气相色谱技术在痕量污染物分析中的应用进展[J].色谱,2011(4):281–282.
[14]戴坤富,杨志国,曾茹萍.理化实验室标准物质期间核查的方法与实例[J].理化检验:化学分册,2012,48(12):1 482–1 484.
[15]薛青松,薛腾,蒋金刚.6850气相色谱仪FID检测器静电计故障排除一例[J].分析仪器,2012(2):83–84.
[16]施敏敏.环境监测站如何切实开展仪器设备的期间核查[J].干旱环境监测,2013,27(4):184–187.
[17]沈才忠.测量设备的期间核查及判定[J].中国计量,2007(5):41–42.
[18]刘存成.实验室”期间核查”的初步探讨[J].现代测量与实验室管理,2003(1):45–46.
[19]朱浩.谈谈检测实验室的期间核查及方法[J].计量与测试技术,2006,33(3):10–11.
[20]JJG 700–2016气相色谱仪检定规程[S].