分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2015年
2期
187-192
,共6页
张晗%王佳妮%朱永官%张娴
張晗%王佳妮%硃永官%張嫻
장함%왕가니%주영관%장한
土壤%无机磷酸盐%磷酸银%氧同位素
土壤%無機燐痠鹽%燐痠銀%氧同位素
토양%무궤린산염%린산은%양동위소
Soil%Inorganic phosphate%Silver phosphate%Oxygen isotope composition
土壤磷酸盐氧同位素在生物地球化学研究领域中具有重要的应用,土壤成分复杂,氧同位素来源多样,可靠的样品富集和纯化技术是磷酸盐氧同位素研究的前提保障。本研究以土壤无机磷酸盐氧同位素为研究对象,采用多步沉淀法对土壤中无机磷酸盐进行提取,并转化成Ag3 PO4沉淀分离,用于磷酸盐氧同位素测试。以氨水重结晶方法对Ag3 PO4进行纯化,通过XRD和元素分析验证了产品纯度。结果表明,通过H2 O2漂洗去除有机质后,辅助氨水重结晶可有效去除Ag3 PO4中夹杂的Ag2 O和Ag单质等无机杂质,未产生同位素分馏,采用标准KH2 PO4对方法全流程安全性进行验证。对3种不同利用类型的土壤中磷酸盐进行分析,结果表明,方法的平行性良好,不同类型土壤磷酸盐氧同位素差异显著,δ18 Op 值在15.2‰~19.5‰之间,可用于土壤磷溯源研究。
土壤燐痠鹽氧同位素在生物地毬化學研究領域中具有重要的應用,土壤成分複雜,氧同位素來源多樣,可靠的樣品富集和純化技術是燐痠鹽氧同位素研究的前提保障。本研究以土壤無機燐痠鹽氧同位素為研究對象,採用多步沉澱法對土壤中無機燐痠鹽進行提取,併轉化成Ag3 PO4沉澱分離,用于燐痠鹽氧同位素測試。以氨水重結晶方法對Ag3 PO4進行純化,通過XRD和元素分析驗證瞭產品純度。結果錶明,通過H2 O2漂洗去除有機質後,輔助氨水重結晶可有效去除Ag3 PO4中夾雜的Ag2 O和Ag單質等無機雜質,未產生同位素分餾,採用標準KH2 PO4對方法全流程安全性進行驗證。對3種不同利用類型的土壤中燐痠鹽進行分析,結果錶明,方法的平行性良好,不同類型土壤燐痠鹽氧同位素差異顯著,δ18 Op 值在15.2‰~19.5‰之間,可用于土壤燐溯源研究。
토양린산염양동위소재생물지구화학연구영역중구유중요적응용,토양성분복잡,양동위소래원다양,가고적양품부집화순화기술시린산염양동위소연구적전제보장。본연구이토양무궤린산염양동위소위연구대상,채용다보침정법대토양중무궤린산염진행제취,병전화성Ag3 PO4침정분리,용우린산염양동위소측시。이안수중결정방법대Ag3 PO4진행순화,통과XRD화원소분석험증료산품순도。결과표명,통과H2 O2표세거제유궤질후,보조안수중결정가유효거제Ag3 PO4중협잡적Ag2 O화Ag단질등무궤잡질,미산생동위소분류,채용표준KH2 PO4대방법전류정안전성진행험증。대3충불동이용류형적토양중린산염진행분석,결과표명,방법적평행성량호,불동류형토양린산염양동위소차이현저,δ18 Op 치재15.2‰~19.5‰지간,가용우토양린소원연구。
Analytical technique on oxygen isotope composition of phosphate in soil has important applications in biogeochemical research. As the composition of the soil is complex with multiple oxygen sources, a liable phosphate enrichment and purification technology is important for phosphate oxygen isotope research. Here we presented a protocol on the analysis of the δ18 Op of inorganic phosphate in soil, and phosphate was purified with multiple mineral precipitations and finally precipitated as silver phosphate. The efficiency of NH4 OH purification method was examined and the purity of the product was verified through XRD and element analysis. The result showed that treatment of the Ag3 PO4 sample by recrystallizing with ammonia could remove the impurity efficiently without significantly modifying oxygen isotope compositions. The validity of sample processing and reliability of isotope analyses were confirmed by processing a KH2 PO4 standard in parallel with soil P sample. The analytical result of three soil types indicated that this method provided good precision of 0. 2‰. The differences of δ18 Op between three soils groups are significant ( From 15. 2‰ to 19. 5‰) and can be used to tracing P sources.