High-sensitivity testing method capable of simultaneously implementing measurement of multiple negative ions
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A test method and anion technology, applied in the field of ion chromatography analysis, can solve the problems of low sensitivity, high detection limit, and many interferences, and achieve the effect of wide range of measurement objects and low detection limit
Inactive Publication Date: 2013-05-01
TONGJI UNIV
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Conductometric detectors are versatile, but have low sensitivity and high detection limits, especially for easily polarizable anions such as Br - , I - , S 2 o 3 2- etc.), because these ions are prone to redox reactions, the detection sensitivity is low and there are many interferences
The amperometric detector is based on the current change when the target ion undergoes a redox reaction on the electrode surface, and has a high sensitivity. - , NO 3 - , SO 4 2- Plasma
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Embodiment 1
[0011] 1. Sample preparation
[0012] Prepare Cl - , NO 2 - 、Br - , NO 3 - , SO 4 2- , I - , S 2 o 3 2- mixed solution of Cl - The concentration is 2μM, and the concentration of other ions is 1μM, with 9mM:1mM Na 2 CO 3 in NaHCO 3 The mixed solution is the eluent.
[0013] 2. Sample analysis
[0014] Use a 10mL syringe to draw 10mL of the above solution and inject it into a Dionex IC-1500 ion chromatograph. The anion guard column and analytical column are DIONEX IonPac AG9-HC (4mm i.d.×50mm) and DIONEX IonPac AS9-HC (4mm i.d.×250mm) respectively. , the eluent is 9mM:1mM Na 2 CO 3 with NaHCO 3 The mixed solution, the flow rate is 0.9ml / min, the injection quantitative loop is a PEEK tube with an outer diameter of 1 / 16 in, an inner diameter of 0.030 in, and a length of 7m. The suppressor is DIONEX ASRS 300, and the suppressing current is 88mA. The temperature is 28-32°C.
[0015] This embodiment analyzes spectrogram as attached figure 1 As shown, the peak ti...
Embodiment 2
[0018] Prepare a series of concentrations containing Cl - , NO 2 - 、Br - , NO 3 - , SO 4 2- , I - , S 2 o 3 2- The mixed solution, the ion concentration in each solution is as shown in Table 1,
[0019] Table 1 Concentration of a series of mixed solutions
[0020] Mixed standard solution serial number Cl - μM NO 2 - μM Br - μM NO 3 - μM SO 4 2- μM I - μM S 2 o 3 2- μM Ⅰ 0.2 0.1 0.1 0.1 0.1 0.1 0.1 Ⅱ 2 1 1 1 1 1 1 Ⅲ 4 2 2 2 2 2 2 Ⅳ 10 5 5 5 5 5 5 Ⅴ 20 10 10 10 10 10 10 Ⅵ 50 50 50 50 50 50 50
[0021] The above-mentioned 6 kinds of mixed solutions were injected into Dionex IC-1500 ion chromatograph in sequence, and the models of anion guard column and analytical column were DIONEX IonPac AG9-HC (4mm i.d.×50mm) and DIONEX IonPac AS9-HC (4mm i.d.×250mm) respectively. , the eluent is 9mM:1mM Na 2 CO 3 with NaHCO 3 The mixed solution, the injection qu...
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Abstract
The invention relates to a high-sensitivity testing method capable of simultaneously implementing measurement of multiple negative ions. The analysis objects not only comprise Cl<->, NO2<->, NO3<-> and SO4<2->, but also comprise easily polarized ions Br<->, I<-> and S2O3<2->. A negative ion analysis column AS9-HC and a protection column AG9-HC are adopted together, the washing solution comprises Na2CO3 and NaHCO3 in a concentration ratio of 9mm: 1mm, the flow rate of the washing solution is 0.9 to 1.1ml / min, the detector is an electrical conductivity detector, the current of a suppressor is 88mA, the temperature of the columns and the temperature of a detection cell are 28 to 32 DEG C, and the used quantitative ring is a polyether-ether-ketone (PEEK) tube with inside diameter of 0.030in, outside diameter of 1 / 16in and length of 7m. The lower detection limits of the ions are low and reach nano scale, namely the lower detection limit of Cl<-> is 0.61 nanometer, the lower detection limit of the NO2<-> is 0.94 nanometer, the lower detection limit of the NO3<-> is 0.93 nanometer, the lower detection limit of the SO4<2-> is 0.81 nanometer, the lower detection limit of the Br<-> is 0.90 nanometer, the lower detection limit of the I<-> is 2.48 nanometers and the lower detection limit of the S2O3<2-> is 1.84 nanometers. The method is simple and convenient for operation, and can be used for implementing high-sensitivity measurement of multiple negative ions indoors or outdoors.
Description
technical field [0001] The invention belongs to the technical field of ion chromatography analysis, and in particular relates to a high-sensitivity test method capable of simultaneously realizing the determination of multiple anions in water. It can be used indoor or in the field to treat various anions (Cl - , NO 2 - , NO 3 - , SO 4 2- 、Br - , I - , S 2 o 3 2- ) analysis. Background technique [0002] In nature, hot spring water, seawater, groundwater, industrial wastewater and other water bodies contain different types and concentrations of anions, including the more stable Cl - , NO 2 - , NO 3 - , SO 4 2- and Br, which is easily polarized and prone to redox reactions - , I - , S 2 o 3 2- , the classic wet chemical analysis can only be determined separately by different chemical methods, and has the disadvantages of much interference, long time, and low sensitivity. [0003] Ion chromatography is suitable for the simultaneous analysis of multiple an...
Claims
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