分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2015年
9期
1366-1370
,共5页
辉光放电质谱法%镍锌铁氧体%杂质元素%铜粉%归一化
輝光放電質譜法%鎳鋅鐵氧體%雜質元素%銅粉%歸一化
휘광방전질보법%얼자철양체%잡질원소%동분%귀일화
Glow discharge mass spectrometry%Nickel-zinc ferrites%Impurity elements%Copper powder%Normalization
建立了辉光放电质谱( GD-MS)法测定镍锌铁氧体中22种杂质元素( Li, Be, Na, Mg, Si, P, K, Ca, Ti V, Cr, Mn, Co, Ga, Sr, Mo, Ag, Cd, Sn, Sb, W, Pb)的分析方法。以铜粉为导电材质,与镍锌铁氧体粉末混合均匀后压片,考察了样品的制备条件以及辉光放电电流、放电电压、放电气体流量以及预溅射时间等放电参数对分析信号灵敏度和稳定性的影响,通过同位素的选择、质谱中分辨率模式和高分辨率模式的应用消除了质谱干扰,将Fe, Ni, Zn, O和Cu,5种元素的总信号作归一化处理,利用差减法计算获得镍锌铁氧体中杂质元素的含量。研究结果表明,22种待测元素的检出限在0.001~0.29μg/g之间,相对标准偏差为3.5％~18.6％,样品测定结果与采用ICP-MS法分析的分析结果基本一致,表明本方法具有较好的准确度和精密度。
建立瞭輝光放電質譜( GD-MS)法測定鎳鋅鐵氧體中22種雜質元素( Li, Be, Na, Mg, Si, P, K, Ca, Ti V, Cr, Mn, Co, Ga, Sr, Mo, Ag, Cd, Sn, Sb, W, Pb)的分析方法。以銅粉為導電材質,與鎳鋅鐵氧體粉末混閤均勻後壓片,攷察瞭樣品的製備條件以及輝光放電電流、放電電壓、放電氣體流量以及預濺射時間等放電參數對分析信號靈敏度和穩定性的影響,通過同位素的選擇、質譜中分辨率模式和高分辨率模式的應用消除瞭質譜榦擾,將Fe, Ni, Zn, O和Cu,5種元素的總信號作歸一化處理,利用差減法計算穫得鎳鋅鐵氧體中雜質元素的含量。研究結果錶明,22種待測元素的檢齣限在0.001~0.29μg/g之間,相對標準偏差為3.5％~18.6％,樣品測定結果與採用ICP-MS法分析的分析結果基本一緻,錶明本方法具有較好的準確度和精密度。
건립료휘광방전질보( GD-MS)법측정얼자철양체중22충잡질원소( Li, Be, Na, Mg, Si, P, K, Ca, Ti V, Cr, Mn, Co, Ga, Sr, Mo, Ag, Cd, Sn, Sb, W, Pb)적분석방법。이동분위도전재질,여얼자철양체분말혼합균균후압편,고찰료양품적제비조건이급휘광방전전류、방전전압、방전기체류량이급예천사시간등방전삼수대분석신호령민도화은정성적영향,통과동위소적선택、질보중분변솔모식화고분변솔모식적응용소제료질보간우,장Fe, Ni, Zn, O화Cu,5충원소적총신호작귀일화처리,이용차감법계산획득얼자철양체중잡질원소적함량。연구결과표명,22충대측원소적검출한재0.001~0.29μg/g지간,상대표준편차위3.5％~18.6％,양품측정결과여채용ICP-MS법분석적분석결과기본일치,표명본방법구유교호적준학도화정밀도。
A direct current glow discharge mass spectrometry ( GD-MS) for the determination of Li, Be, Na, Mg, Si, P, K, Ca, Ti, V, Cr, Mn, Co, Ga, Sr, Mo, Ag, Cd, Sn, Sb, W and Pb in nickel-zinc ferrites was developed. Copper powder as the conductive medium was evenly mixed with nickel-zinc ferrites powder for tableting, and then the impurity elements in nickel-zinc ferrites were determined by GD-MS. The influence of sample preparation and the glow discharge conditions including discharge current, discharge voltage, discharge gas flow rate and pre-sputter time on discharge stability and analysis sensitivity were investigated. The mass spectrometry interferences of analytes were investigated, as well as appropriate isotopes were selected. Most of the mass spectrometry interferences were avoided by measuring in medium resolution mode and high resolution mode. Total signal of Fe, Ni, Zn, O and Cu normalization was adopted, and the impurity elements in nickel-zinc ferrites were calculate in subtraction. The results showed that the detection limits for the investigated elements were in the range of 0. 001-0. 29 μg/g, the relative standard deviations of each element were within 3 . 5%-18 . 6%. The analysis results were consistent with those obtained by inductively coupled plasma mass spectrometry.
