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海洋沉积物中有机碳、无机碳连续测定法——过硫酸钾-非水溶液滴定法

SEQUENTIAL DETERMINATION OF ORGANIC C AND INORGANIC C IN MARINE SEDIMENTS BY PERSULFATE-NONAQUEOUS TITRATIONS

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【作者】 李亮歌; 许金树;

【Author】 Li Liangge and Xu Jinshu (Fujian Institute of Oceanology)

【机构】 福建海洋研究所; 福建海洋研究所;

【摘要】 <正> 1961年,Wilsion提出以过硫酸盐氧化法测定有机碳,引起了人们的关注。首先Menzel等经过改进用于测定海水中溶解的和颗粒有机碳。后来Mills等和Froelich等又应用于海洋沉积物中有机碳的测定。但都需要分离碳酸盐。操作繁琐,费时较长。 我们设计了一种新的双球反应器,并以Ag2SO4为催化剂,结合非水溶液滴定法测定沉积物样品所产生的二氧化碳。

【Abstract】 This paper presents the titrimetry of persulfate-nonaqueous solution with sequential determination of the organic and the inorganic C contents in marine sediments. In a particularly designed paired-ball reactor, the inorganic and organic C contents of a sample was determined separately, yet simultaneously. The carbonates need not be separated beforehand. The Ag2SO4 was used as a catalyst and the time of oxidization was shortened considerably.The optimal conditions have been found. That is, the carbonates of samples are reactivated initially with 3M H3PO4, the inorganic C content is obtained, and then the K2S2O8 (oxidizer) and Ag2SO4 added to the reactor. The reactionary temperature is controlled within 120-130℃ and the organic C content is determined.This method, which is more accurate, simple and rapid, has been successfully applied to the analysis of samples of Oceanic sediments with excellent precision of less than ±0.02%.

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