冶金分析
冶金分析
야금분석
METALLURGICAL ANALYSIS
2010年
2期
38-41
,共4页
刘月成%王尚芝%李海%杨成全%樊俊莉
劉月成%王尚芝%李海%楊成全%樊俊莉
류월성%왕상지%리해%양성전%번준리
火焰原子吸收光谱法%钙%铜%铁%锰%风化岩石%云冈石窟
火燄原子吸收光譜法%鈣%銅%鐵%錳%風化巖石%雲岡石窟
화염원자흡수광보법%개%동%철%맹%풍화암석%운강석굴
flame atomic absorption spectrometry%calcium%copper%iron%manganese%weathering rock%Yungang Grottoes
采用HF-HNO_3-HClO_4混酸消化样品,HNO_3溶解盐类,火焰原子吸收光谱法直接测定试液中钙、铜、铁、锰的含量.对共存离子的干扰情况进行了考察,发现大量的Si对测定有干扰,在处理样品时通过生成SiF_4除去;磷、铝、钛等元素对钙的化学干扰,通过加入释放剂SrCl_2消除.背景吸收使用氘灯扣除.采用标准曲线法测定,Ca、Cu、Fe、Mn的校准曲线的线性范围分别为0.00~20.00μg/mL、0.00~6.00弘g/mL、0.00~10.00 μg/mL、0.00~6.00μg/mL,检出限分别为0.000 3μg/mL、0.001 3 μg/mL、0.002 6μg/mL、0.006 9 μg/mL.方法用于云冈石窟风化岩石中钙、铜、铁、锰的测定,相对标准偏差分别为2.8%、3.0%、1.4%、2.9%,加标回收率在96%~110%之间.
採用HF-HNO_3-HClO_4混痠消化樣品,HNO_3溶解鹽類,火燄原子吸收光譜法直接測定試液中鈣、銅、鐵、錳的含量.對共存離子的榦擾情況進行瞭攷察,髮現大量的Si對測定有榦擾,在處理樣品時通過生成SiF_4除去;燐、鋁、鈦等元素對鈣的化學榦擾,通過加入釋放劑SrCl_2消除.揹景吸收使用氘燈釦除.採用標準麯線法測定,Ca、Cu、Fe、Mn的校準麯線的線性範圍分彆為0.00~20.00μg/mL、0.00~6.00弘g/mL、0.00~10.00 μg/mL、0.00~6.00μg/mL,檢齣限分彆為0.000 3μg/mL、0.001 3 μg/mL、0.002 6μg/mL、0.006 9 μg/mL.方法用于雲岡石窟風化巖石中鈣、銅、鐵、錳的測定,相對標準偏差分彆為2.8%、3.0%、1.4%、2.9%,加標迴收率在96%~110%之間.
채용HF-HNO_3-HClO_4혼산소화양품,HNO_3용해염류,화염원자흡수광보법직접측정시액중개、동、철、맹적함량.대공존리자적간우정황진행료고찰,발현대량적Si대측정유간우,재처리양품시통과생성SiF_4제거;린、려、태등원소대개적화학간우,통과가입석방제SrCl_2소제.배경흡수사용도등구제.채용표준곡선법측정,Ca、Cu、Fe、Mn적교준곡선적선성범위분별위0.00~20.00μg/mL、0.00~6.00홍g/mL、0.00~10.00 μg/mL、0.00~6.00μg/mL,검출한분별위0.000 3μg/mL、0.001 3 μg/mL、0.002 6μg/mL、0.006 9 μg/mL.방법용우운강석굴풍화암석중개、동、철、맹적측정,상대표준편차분별위2.8%、3.0%、1.4%、2.9%,가표회수솔재96%~110%지간.
The sample was dissolved in mixed acid of HF-HNO_3-HClO_4 while the produced salts were dissolved in HNO_3. The content of calcium, copper, iron and manganese in sample solution was directly determined by flame atomic absorption spectrometry. The interference of coexisting ions was tested. It was found that a mass of silicon could interfere with the determination, but they could be eliminated in form of SiF_4 during sample preparation. The chemical interference from phosphorus, aluminium and titanium could be eliminated by adding SrCl_2. The background absorption was deducted using deuterium lamp. The determination was conducted with standard curve method. The linear range of calcium, copper, iron and manganese was 0-20. 00 μg/mL, 0. 00-6. 00μg/mL, 0. 00-10. 00 μg/mL and 0. 00-6.00 μg/mL, and the detection limit was 0. 000 3 μg/mL, 0. 001 3μg/mL, 0. 002 6 μg/mL and 0. 006 9 μg/mL, respectively. This method was applied to the determination of calcium, copper, iron and manganese in weathering rock of Yungang Grottoes, with the relative standard deviations (RSD) of 2.8%, 3.0%, 1.4% and 2.9%, and the recoveries in the range of 90%-110%.