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引用本文:孙 萱,宋金明,于 颖,孙玲玲.元素分析仪快速测定海洋沉积物TOC和TN的条件优化[J].海洋科学,2014,38(7):14-19.
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元素分析仪快速测定海洋沉积物TOC和TN的条件优化
孙 萱1, 宋金明1, 于 颖1, 孙玲玲1
中国科学院 海洋研究所
摘要:
报道了在优化样品前处理、燃烧温度、最小加氧量和最佳称样量的基础上, 综合构建优化了直接固体进样varioMACRO cube 元素分析仪同时测定海洋沉积物样品中总有机碳(TOC)和总氮(TN)的条件, 即准确称取20~30 mg 沉积物样品用1 mol/L 盐酸除去无机碳后, 直接进样在燃烧管温度960 ℃, 次级燃烧管温度830 ℃, 还原管温度900 ℃, 氦气压力0.12 MPa, 流量600 mL/min, 氧气压力0. 20 MPa, 加氧量22.5 mL 仪器条件下, 用标准曲线法峰面积获取TOC 和TN 浓度。结果表明, 海洋沉积物中TOC 和TN 测定的检出限分别为0.0508%和0.0146%, 回收率分别为97.7%~100.9%和97.2%~101.1%, 对4个实际外海沉积物样测定总有机碳和总氮结果的相对标准偏差(RSD)为0.83%~3.06% 和1.33%~3.49%(n=12)。该方法操作简便快速、灵敏度高, 具有较好的精密度和准确度, 可准确可靠地用于海洋沉积物中总有机碳和总氮含量的测定。
关键词:  总有机碳  总氮  海洋沉积物  元素分析仪
DOI:10.11759/hykx20130801001
分类号:
基金项目:中国科学院仪器设备功能开发技术创新项目(yg2012055)
A rapid method for determing the total organic carbon and total nitrogen in marine sediments with an Elemental Analyzer
Abstract:
A method fordeterming the total organic carbon (TOC) and total nitrogen (TN) in marine sediment samples by simultaneously injecting solid sample into vario MACRO cube elemental analyzer was reported. The determination conditions were optimized by sample pretreatment, combustion temperature, the oxygen volume and sample weight et al.. Twenty (20)-30mg accurately weighed sediment samples with 1mol/L hydrochloric acid to remove inorganic carbon were injected directlyto the elemental analyzer. The concentrations of TOC and TN were calculated by standard curves with combustion tube temperatureat 960℃, post combustion tube temperature at 830 ℃, reduction tube temperature at 900℃, helium pressure 0.12 MPa, flow 600 mL/min, oxygen pressure 0.20 MPa, and oxygen volume 22.5 mL. The detection limits of TOC and TN were 0.0508% and 0.0146%, and the recoveries were 97.7%~100.9% and 97.2%~101.1%, respectively. The RSDs of TOC and TN in four marine sediment samples (n=12) were 0.83%~3.06% and 1.33%~3.49%,respectively. The method was simple, fast, sensitive, precise, and accurate, and is suitable for analysis of TOC and TN in marine sediment samples.
Key words:  total organic carbon  total nitrogen  marine sediments  elemental analyzer
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