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UHPLC-ICPMS online bromide and iodide species determination analysis method

A technology of ICP-MS and analytical method, which is applied in the field of instrumental analysis, can solve problems such as the lack of established standard analytical methods, and achieve the effects of high recovery rate of standard addition, rapid separation and accurate determination, and low detection limit

Active Publication Date: 2017-08-29
SHANGHAI NORMAL UNIVERSITY
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Problems solved by technology

Applying HPLC and ICP-MS online technology to determine the content of bromine and iodine species in environmental samples, there is no standard analysis method established yet

Method used

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  • UHPLC-ICPMS online bromide and iodide species determination analysis method
  • UHPLC-ICPMS online bromide and iodide species determination analysis method

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specific Embodiment approach

[0021] As shown in Figure 1, the present invention discloses an analysis method for online determination of bromine and iodine species by UHPLC-ICPMS. Specifically, UHPLC is used as a separator and ICPMS is used as a detector to analyze bromine and iodine species. The analysis method is short in time, low in detection limit and high in precision, and can be used for the determination of bromine and iodine species in environmental and other samples. Include the following steps:

[0022] Step 1: Select UHPLC and ICP-MS instruments; the UHPLC and ICP-MS instruments are Flexar FX-15 high performance liquid chromatograph and NexION-350D inductively coupled plasma mass spectrometer from PerkinElmer, USA, respectively.

[0023] Step 2: Perform ICP-MS instrument parameter optimization; ICP-MS instrument parameter optimization uses indium (115) as an internal standard element.

[0024] Step 3: configure the UHPLC separation column and guard column, and optimize the separation conditio...

Embodiment

[0032] As shown in Figure 2, a UHPLC-ICPMS analysis method for online determination of bromine and iodine species is applied to snowfall samples, and it consists of the following steps:

[0033] Step 1: The selected UHPLC and ICP-MS instruments are Flexar FX-15 high performance liquid chromatograph and NexION-350D inductively coupled plasma mass spectrometer from PerkinElmer, USA, respectively.

[0034] Step 2: Use the standard solution of indium (115) to optimize the parameters of the ICP-MS instrument.

[0035]Step 3: The UHPLC instrument is equipped with a Dionex IonPac AS14 separation column (4mm×250mm) and an AG14 guard column (4mm×50mm); the separation condition is 50mM L -1 ammonium nitrate (NH 4 NO 3 ) solution mobile phase, pH 8.70 and flow rate 1.2mL / min, and quantitative loop 50μL, injection volume 50μL, no column temperature and column pressure 700psi.

[0036] Step 4: Connect the pipelines of UHPLC and ICP-MS, and use leak detection.

[0037] Step 5: Use a 0.4...

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Abstract

The invention relates to a UHPLC-ICPMS online bromide and iodide species determination analysis method. The method uses HPLC and ICPMS technologies in a combined way, and comprises the following steps of selecting UHPLC and an ICP-MS instrument; performing ICP-MS instrument parameter optimization; configuring a separation column and a protection column of the UHPLC; optimizing the separation conditions; connecting a pipeline of the UHPLC and the ICP-MS instrument; performing leakage inspection; performing pretreatment on the sample to be tested; determining the separation time through an experiment chromatography separation diagram; measuring the standard curve, the detection limit and the precision; performing sign adding recovery and practical sample determination. The method has the advantages that the separation time is short; the linear relationship is good; the detection limit is low; the sign adding recovery rate is high; the precision is high. The method can be used for the trace analysis of the bromide and iodide species in samples of environment and the like; the fast separation and accurate determination can be realized; the accurate determination of the sample can be completed in 5 minutes.

Description

technical field [0001] The invention belongs to the technical field of instrument analysis, and relates to an analysis method for online determination of bromine and iodine species by UHPLC-ICPMS. Background technique [0002] The contents of bromine, iodine and their species in environmental samples are very low, and it is of great practical significance to quickly and accurately determine bromine, iodine and their species in samples at ppb and ppt levels. With the rapid development of analytical instruments and coupled technologies, especially the development of ICP-MS technology and its combination with separation technologies such as HPLC and IC, it provides a favorable tool for the determination of bromine and iodine species in environmental samples. The online combination technology of HPLC / IC and ICP-MS is an important research topic in recent years, and it has been successfully used for the determination of elemental forms, but rapid separation and accurate determina...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 高运川殷美雪杨超马瑾
Owner SHANGHAI NORMAL UNIVERSITY
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