化学分析计量
化學分析計量
화학분석계량
CHEMICAL ANALYSIS AND METERAGE
2015年
1期
14-17
,共4页
辛晓东%李伟%胡芳%赵清华%王明泉%孙韶华%贾瑞宝
辛曉東%李偉%鬍芳%趙清華%王明泉%孫韶華%賈瑞寶
신효동%리위%호방%조청화%왕명천%손소화%가서보
高效液相色谱法%电感耦合等离子体质谱法%硒%形态分析
高效液相色譜法%電感耦閤等離子體質譜法%硒%形態分析
고효액상색보법%전감우합등리자체질보법%서%형태분석
high performance liquid chromatography%inductively coupled plasma mass spectrometry%selenium%speciation analysis
采用高效液相色谱法(HPLC)分离水中硒两种常见形态Se(Ⅳ),Se(Ⅵ),通过电感耦合等离子体质谱系统进行检测鉴定,由此建立了水中硒形态的分析方法。以0.15 mmol/L EDTA(钾)–0.1 mmol/L四丁基氢氧化铵–0.15 mmol/L乙酸铵–5%甲醇为流动相,调节流动相pH值至6~7,两种不同形态的硒可在4 min内得到有效分离。测定Se(Ⅳ),Se(Ⅵ),的线性范围为2~100μg/L,线性相关系数(r2)不低于0.999,Se(Ⅳ)和Se(Ⅵ)的检出限分别为0.01,0.05μg/L。分别以水源水、管网水等为基体进行加标回收试验,Se(Ⅳ)和Se(Ⅵ),的回收率分别为102.3%~106.2%,104.7%~108.3%,测定结果的相对标准偏差分别为6.4%~9.6%,4.4%~7.3%(n=5)。该方法灵敏度高,具有良好的精密度和准确度,可用于环境水体中元素硒形态分析。
採用高效液相色譜法(HPLC)分離水中硒兩種常見形態Se(Ⅳ),Se(Ⅵ),通過電感耦閤等離子體質譜繫統進行檢測鑒定,由此建立瞭水中硒形態的分析方法。以0.15 mmol/L EDTA(鉀)–0.1 mmol/L四丁基氫氧化銨–0.15 mmol/L乙痠銨–5%甲醇為流動相,調節流動相pH值至6~7,兩種不同形態的硒可在4 min內得到有效分離。測定Se(Ⅳ),Se(Ⅵ),的線性範圍為2~100μg/L,線性相關繫數(r2)不低于0.999,Se(Ⅳ)和Se(Ⅵ)的檢齣限分彆為0.01,0.05μg/L。分彆以水源水、管網水等為基體進行加標迴收試驗,Se(Ⅳ)和Se(Ⅵ),的迴收率分彆為102.3%~106.2%,104.7%~108.3%,測定結果的相對標準偏差分彆為6.4%~9.6%,4.4%~7.3%(n=5)。該方法靈敏度高,具有良好的精密度和準確度,可用于環境水體中元素硒形態分析。
채용고효액상색보법(HPLC)분리수중서량충상견형태Se(Ⅳ),Se(Ⅵ),통과전감우합등리자체질보계통진행검측감정,유차건립료수중서형태적분석방법。이0.15 mmol/L EDTA(갑)–0.1 mmol/L사정기경양화안–0.15 mmol/L을산안–5%갑순위류동상,조절류동상pH치지6~7,량충불동형태적서가재4 min내득도유효분리。측정Se(Ⅳ),Se(Ⅵ),적선성범위위2~100μg/L,선성상관계수(r2)불저우0.999,Se(Ⅳ)화Se(Ⅵ)적검출한분별위0.01,0.05μg/L。분별이수원수、관망수등위기체진행가표회수시험,Se(Ⅳ)화Se(Ⅵ),적회수솔분별위102.3%~106.2%,104.7%~108.3%,측정결과적상대표준편차분별위6.4%~9.6%,4.4%~7.3%(n=5)。해방법령민도고,구유량호적정밀도화준학도,가용우배경수체중원소서형태분석。
The method for determination of different species of selenium in water samples by high performance liquid chromatography (HPLC)–inductively coupled plasma mass spectrometry (ICP–MS) was established. The results showed that Se( Ⅳ ) and Se( Ⅵ ) could be separated within 4 min by using 0.15 mmol/L EDTA–K,0.1 mmol/L tetrabutyl ammonium hydroxide(TBAOH),0.15 mmol/L ammonium acetate and 5%methanol as mobile phase under pH 6–7. The detection linear range of Se(Ⅳ) and Se(Ⅵ) was 2–100μg/L with correlation coefficient (r2) of 0.999. The detection limits of Se( Ⅳ ) and Se( Ⅵ ) were 0.01, 0.05μg/L, the recoveries were 102.3%–106.2%,104.7%–108.3%, and the relative standard deviations were 6.4%–9.6%,4.4%–7.3%(n=5), respectively. The proposed method shows good accuracy, precision and sensitivity, which can be used for analyzing species of selenium in environment water.