分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2014年
10期
1544-1548
,共5页
王慕华%钟乃飞%叶明立%黄忠平%朱岩
王慕華%鐘迺飛%葉明立%黃忠平%硃巖
왕모화%종내비%협명립%황충평%주암
阴阳离子%同时分析%多分离模式液相色谱法%直接电导检测
陰暘離子%同時分析%多分離模式液相色譜法%直接電導檢測
음양리자%동시분석%다분리모식액상색보법%직접전도검측
Cations and anions%Simultaneous determination%Multimodal liquid chromatography%Direct conductivity detection
采用基于纳米聚合物-硅胶混合技术,同时具有反相、阴、阳离子交换的多分离模式色谱分离功能的Acclaim Trinity P1色谱柱,直接电导检测,建立了同时分析Li+, NH+4, K+, HCOO-, NO-2, Cl-, NO-3和Br-8种离子的分析方法。通过探讨淋洗液对离子保留的影响,优化得到实验条件如下:淋洗液:25 mmol/L乙酸钠+50%(V/V)乙腈,用冰醋酸调至pH 5.0;柱温:30℃;流速:0.50 mL/min;直接电导检测。8种阴阳离子(Li+, NH+4, K+, HCOO-, NO-2, Cl-, NO-3和Br-)能够同时被分离和检测。化肥样品经稀释溶解过滤后直接进样,结果表明,8种离子的线性范围为0.5~200 mg/L,线性相关系数均大于0.9997,相对标准偏差RSD (n=9)为1.3%~2.5%,检出限(S/N=3)在0.16~1.70 mg/L之间。将本方法用于化肥中阴阳离子的测定,加标回收率为95.8%~103.8%。
採用基于納米聚閤物-硅膠混閤技術,同時具有反相、陰、暘離子交換的多分離模式色譜分離功能的Acclaim Trinity P1色譜柱,直接電導檢測,建立瞭同時分析Li+, NH+4, K+, HCOO-, NO-2, Cl-, NO-3和Br-8種離子的分析方法。通過探討淋洗液對離子保留的影響,優化得到實驗條件如下:淋洗液:25 mmol/L乙痠鈉+50%(V/V)乙腈,用冰醋痠調至pH 5.0;柱溫:30℃;流速:0.50 mL/min;直接電導檢測。8種陰暘離子(Li+, NH+4, K+, HCOO-, NO-2, Cl-, NO-3和Br-)能夠同時被分離和檢測。化肥樣品經稀釋溶解過濾後直接進樣,結果錶明,8種離子的線性範圍為0.5~200 mg/L,線性相關繫數均大于0.9997,相對標準偏差RSD (n=9)為1.3%~2.5%,檢齣限(S/N=3)在0.16~1.70 mg/L之間。將本方法用于化肥中陰暘離子的測定,加標迴收率為95.8%~103.8%。
채용기우납미취합물-규효혼합기술,동시구유반상、음、양리자교환적다분리모식색보분리공능적Acclaim Trinity P1색보주,직접전도검측,건립료동시분석Li+, NH+4, K+, HCOO-, NO-2, Cl-, NO-3화Br-8충리자적분석방법。통과탐토림세액대리자보류적영향,우화득도실험조건여하:림세액:25 mmol/L을산납+50%(V/V)을정,용빙작산조지pH 5.0;주온:30℃;류속:0.50 mL/min;직접전도검측。8충음양리자(Li+, NH+4, K+, HCOO-, NO-2, Cl-, NO-3화Br-)능구동시피분리화검측。화비양품경희석용해과려후직접진양,결과표명,8충리자적선성범위위0.5~200 mg/L,선성상관계수균대우0.9997,상대표준편차RSD (n=9)위1.3%~2.5%,검출한(S/N=3)재0.16~1.70 mg/L지간。장본방법용우화비중음양리자적측정,가표회수솔위95.8%~103.8%。
A new method has been established for simultaneous determination of anions and cations in fertilizer sample by multimodal liquid chromatography with direct conductivity detection. An Acclaim Trinity P1 column based on nanopolymer silica hybrid technology with multimodal separation functional groups reversed-phase/anion-exchange/cation-exchange was used for the analysis. The chromatographic conditions were optimized and the effect ion of eluent on retention was discussed. Eight ions ( Li+, NH+4 , K+, HCOO-, NO-2 , Cl-, NO-3 and Br-) were separated and determined simultaneously by using 25 mmol/L CH3 COONa solution containing 50% acetonitrile at pH=5. 0 as mobile phase. The flow rate was 0. 50 mL/min and the temperature was 30 ℃. Under the optimum conditions, the linear ranges of the method were in the range of 0 . 5-200 mg/L for all the ions with correlation coefficient of 0 . 9997-0 . 9999 . Whereas the detection limits (S/N=3) were in the range of 0. 16-1. 72 mg/L and the relative standard deviations (RSD, n=9) were in the range of 1 . 3-2 . 5%. The method was applied to the determination of anions and cations in the fertilizer samples with satisfied results and the recoveries were in the range of 95 . 8%-103 . 8%.