冶金分析
冶金分析
야금분석
METALLURGICAL ANALYSIS
2015年
6期
40-43
,共4页
磷酸氢二铵%钛白粉%电感耦合等离子体原子发射光谱法(ICP-AES)%铜%钒
燐痠氫二銨%鈦白粉%電感耦閤等離子體原子髮射光譜法(ICP-AES)%銅%釩
린산경이안%태백분%전감우합등리자체원자발사광보법(ICP-AES)%동%범
diammonium hydrogen phosphate%titanium dioxide%inductively coupled plasma atomic emission spec-trometry(ICP-AES)%copper%vanadium
针对钛白粉样品中钛基体对电感耦合等离子体原子发射光谱法( ICP-AES)测定痕量铜和钒有干扰,提出了利用磷酸氢二铵[(NH4)2HPO4]沉淀分离钛基体后ICP-AES测定钛白粉产品中痕量铜和钒的方法。对溶样方式、(NH4)2HPO4沉淀钛的条件和ICP-AES的测定条件进行研究,结果表明：对于0.1 g钛白粉样品,在H2 SO4和( NH4)2 SO4介质中,用沸水浴加热3~5 min,可使钛与(NH4)2HPO4形成的Ti(HPO4)2沉淀完全,在实验确定的仪器工作条件下以Cu 324.7 mm和V 292.4 nm进行测定,结果稳定。铜和钒的检出限分别为0.001μg/mL 和0.0007μg/mL。应用实验方法对钛白粉实际样品中铜和钒进行测定,相对标准偏差(RSD,n=6)不大于1.2%,加标回收率在90%~117%之间。方法可以用于钛白粉的日常分析。
針對鈦白粉樣品中鈦基體對電感耦閤等離子體原子髮射光譜法( ICP-AES)測定痕量銅和釩有榦擾,提齣瞭利用燐痠氫二銨[(NH4)2HPO4]沉澱分離鈦基體後ICP-AES測定鈦白粉產品中痕量銅和釩的方法。對溶樣方式、(NH4)2HPO4沉澱鈦的條件和ICP-AES的測定條件進行研究,結果錶明：對于0.1 g鈦白粉樣品,在H2 SO4和( NH4)2 SO4介質中,用沸水浴加熱3~5 min,可使鈦與(NH4)2HPO4形成的Ti(HPO4)2沉澱完全,在實驗確定的儀器工作條件下以Cu 324.7 mm和V 292.4 nm進行測定,結果穩定。銅和釩的檢齣限分彆為0.001μg/mL 和0.0007μg/mL。應用實驗方法對鈦白粉實際樣品中銅和釩進行測定,相對標準偏差(RSD,n=6)不大于1.2%,加標迴收率在90%~117%之間。方法可以用于鈦白粉的日常分析。
침대태백분양품중태기체대전감우합등리자체원자발사광보법( ICP-AES)측정흔량동화범유간우,제출료이용린산경이안[(NH4)2HPO4]침정분리태기체후ICP-AES측정태백분산품중흔량동화범적방법。대용양방식、(NH4)2HPO4침정태적조건화ICP-AES적측정조건진행연구,결과표명：대우0.1 g태백분양품,재H2 SO4화( NH4)2 SO4개질중,용비수욕가열3~5 min,가사태여(NH4)2HPO4형성적Ti(HPO4)2침정완전,재실험학정적의기공작조건하이Cu 324.7 mm화V 292.4 nm진행측정,결과은정。동화범적검출한분별위0.001μg/mL 화0.0007μg/mL。응용실험방법대태백분실제양품중동화범진행측정,상대표준편차(RSD,n=6)불대우1.2%,가표회수솔재90%~117%지간。방법가이용우태백분적일상분석。
The determination of trace copper and vanadium in titanium dioxide sample by inductively coupled plas-ma atomic emission spectrometry ( ICP-AES) was interfered with the titanium matrix. The titanium matrix was pre-cipitated and separated by diammonium hydrogen phosphate [(NH4)2HPO4]. Then, the content of trace copper and vanadium in titanium dioxide sample was determined by ICP-AES. The sample dissolution method, the precipi-tation conditions of titanium with (NH4)2HPO4 and the determination conditions of ICP-AES were investigated. The results showed that the titanium in 0. 1 g of titanium dioxide sample could be fully react with (NH4)2HPO4 to form Ti(HPO4)2 precipitate in ammonium sulfate and sulfuric acid medium after heating in boiling bath for 3-5 min. The determination results were stable under the selected instrumental conditions with Cu 327. 4 nm and V 292. 4 nm as analytical spectral line. The detection limit of copper and vanadium was 0. 001 μg/mL and 0. 000 7μg/mL, respectively. The proposed method was applied to determination of copper and vanadium in titanium diox-ide actual samples. The relative standard deviation (RSD) was not more than 1. 2%, and the recoveries were be-tween 90% and 117%. The proposed method was applicable for the routine analysis of titanium dioxide.
