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矿化水中的待测阴离子分离后,由经过外标标定的积分仪测定峰面积来定量。通过线性回归评价这些数据。收集在表3中的再现数据表明,在所研究的这种浓度中,HCO3-可能引起Cl-测...
矿化水中的待测阴离子分离后, 由经过外标标定的积分仪测定峰面积来定量。通过线性回归评价这些数据。收集在表3 中的再现数据表明,在所研究的这种浓度中, HCO3-可能引起Cl-测定负误差, 即使Br-和NO 3-的保留时间稍微长一点, 这些阴离子的定量也是可能的。
表 3 待测阴离子含量再现性与HCO3-浓度的关系
正如图1的色谱指出那样, 通过实际水样的稀释使Cl-分离过程中基体干扰降至最小。色谱是在AS一4A 阴离子分离柱上注入50µL实际矿化水( A );等体积的Milli-Q水稀释的矿化水( B );标准阴离子溶液( C ) 后分别测得的。
稀释使能够干扰Cl-定量的附加峰消失了。完全分离的所有四种阴离子峰与阴离子标准峰具有相同的保留时间。
根据溶解于实际样品中总的矿物盐浓度, 等分注入各稀释样。用比较阴离子的保留时间来识别每一种阴离子。从表4所示的数据看,显然当矿化水被稀释10倍时, 所有四种阴离子都得到很好的分离, 且它们的保留时间接近阴离子标准的保留时间。
表 4 各种稀释矿化水样品阴离子保留时间的比较
虽然在这样的稀释样品中可以识别上述各阴离子, 但在低浓度下存在于原样品中离子的定量还可能有一些问题。在实验部分所描述的工作条件下确定的检测极限大约是:Cl- 0.02mg/L;Br- 0.01mg/L;NO 3- 0.05 m g/ L;SO 42- 0.05mg /L。数次注入不同浓度阴离子的溶液,积分仪仍能对色谱峰识别和积分的最低溶液被认为是检测限。
研究了由于氢氧化铁沉淀作用可能引起的对样品稳定性的干扰, 对添加了浓度1 ~15 m g / L Fe3+的混合阴离子标准溶液样品,色谱分析有时超过30天,在上述条件下没有观察到检测离子组成的变化。
致谢
该工作得到了斯洛维尼亚研究团体的支持,在此表示感谢。 展开
表 3 待测阴离子含量再现性与HCO3-浓度的关系
正如图1的色谱指出那样, 通过实际水样的稀释使Cl-分离过程中基体干扰降至最小。色谱是在AS一4A 阴离子分离柱上注入50µL实际矿化水( A );等体积的Milli-Q水稀释的矿化水( B );标准阴离子溶液( C ) 后分别测得的。
稀释使能够干扰Cl-定量的附加峰消失了。完全分离的所有四种阴离子峰与阴离子标准峰具有相同的保留时间。
根据溶解于实际样品中总的矿物盐浓度, 等分注入各稀释样。用比较阴离子的保留时间来识别每一种阴离子。从表4所示的数据看,显然当矿化水被稀释10倍时, 所有四种阴离子都得到很好的分离, 且它们的保留时间接近阴离子标准的保留时间。
表 4 各种稀释矿化水样品阴离子保留时间的比较
虽然在这样的稀释样品中可以识别上述各阴离子, 但在低浓度下存在于原样品中离子的定量还可能有一些问题。在实验部分所描述的工作条件下确定的检测极限大约是:Cl- 0.02mg/L;Br- 0.01mg/L;NO 3- 0.05 m g/ L;SO 42- 0.05mg /L。数次注入不同浓度阴离子的溶液,积分仪仍能对色谱峰识别和积分的最低溶液被认为是检测限。
研究了由于氢氧化铁沉淀作用可能引起的对样品稳定性的干扰, 对添加了浓度1 ~15 m g / L Fe3+的混合阴离子标准溶液样品,色谱分析有时超过30天,在上述条件下没有观察到检测离子组成的变化。
致谢
该工作得到了斯洛维尼亚研究团体的支持,在此表示感谢。 展开
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The KuangHuaShui after being tested anion separation by after external standard calibration of integral instrument to quantitative determination of peak area. Through the linear regression evaluation of these data. Collect the reappearance in table 3 data shows that the concentration in the study, HCO3 - may cause Cl - determination, even negative error Br - and NO 3 - of retention time slightly longer, the anion quantitative also is possible.
Table 3 to be measured anion content reproducibility and HCO3 - concentration relationship
As figure 1 chromatographic says that, through the actual watery dilution make Cl - separation process matrix interference down to a minimum. Chromatography is in AS A 4A anion separation column 50 infuse on KuangHuaShui apms L actual (A); As the volume of water dilute Milli - Q KuangHuaShui (B); Standard anion solution (C) measured respectively after.
Dilution enables to interference Cl - quantitative additional peak disappeared. Completely detached all four anion peak and anionic standard peak with the same retention time.
According to actual samples of total soluble in mineral salt concentration, inject the diluted sample quintiles. Using comparative anion of retention time to identify each kind of anion. From table 4 shows data to see KuangHuaShui be diluted, obviously, when 10 times, all four anion are very good separation, and their retention time of retention time close to anionic standards.
Table 4 various dilution of retention time of KuangHuaShui sample anion comparison
Although in this dilution samples can identify the foregoing anion, but in low concentration is the original sample XiaCun ions in quantitative may also have some problems. Described in the LABS section of the working conditions determined the detection limit is about: Cl - 0.02 mg/L; Br - 0.01 mg/L; NO 3-0.05 m g/L; SO 42-0.05 mg/L. Several injection of different concentrations anion, integral meter can still solution of chromatographic peak of recognition and integral minimum solution is considered detection limit.
Study the hydrogen ferric oxide precipitation role due to sample may cause the stability of added concentration of interference, 1 ~ 15 m g/L Fe3 + mix of anionic standard solution samples, chromatographic analysis sometimes more than 30 days, in the above conditions did not observe the changes to the test of ions.
thanks
This work got Slovenia research organizations support in this to say thank you.
Table 3 to be measured anion content reproducibility and HCO3 - concentration relationship
As figure 1 chromatographic says that, through the actual watery dilution make Cl - separation process matrix interference down to a minimum. Chromatography is in AS A 4A anion separation column 50 infuse on KuangHuaShui apms L actual (A); As the volume of water dilute Milli - Q KuangHuaShui (B); Standard anion solution (C) measured respectively after.
Dilution enables to interference Cl - quantitative additional peak disappeared. Completely detached all four anion peak and anionic standard peak with the same retention time.
According to actual samples of total soluble in mineral salt concentration, inject the diluted sample quintiles. Using comparative anion of retention time to identify each kind of anion. From table 4 shows data to see KuangHuaShui be diluted, obviously, when 10 times, all four anion are very good separation, and their retention time of retention time close to anionic standards.
Table 4 various dilution of retention time of KuangHuaShui sample anion comparison
Although in this dilution samples can identify the foregoing anion, but in low concentration is the original sample XiaCun ions in quantitative may also have some problems. Described in the LABS section of the working conditions determined the detection limit is about: Cl - 0.02 mg/L; Br - 0.01 mg/L; NO 3-0.05 m g/L; SO 42-0.05 mg/L. Several injection of different concentrations anion, integral meter can still solution of chromatographic peak of recognition and integral minimum solution is considered detection limit.
Study the hydrogen ferric oxide precipitation role due to sample may cause the stability of added concentration of interference, 1 ~ 15 m g/L Fe3 + mix of anionic standard solution samples, chromatographic analysis sometimes more than 30 days, in the above conditions did not observe the changes to the test of ions.
thanks
This work got Slovenia research organizations support in this to say thank you.
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