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Detecting of different arsenic forms in environmental water based on HPLC-ICP-MS hyphenated technology

A technology of HPLC-ICP-MS and ICP-MS, which is applied in the field of water quality environmental monitoring, can solve the problems of unscientific impact on the environment and ecology, strong toxicity and carcinogenicity of arsenic and its compounds, and achieve low and high detection limits. The effect of high sensitivity and stability

Pending Publication Date: 2019-07-12
河北省地质环境监测院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Arsenic and its compounds are highly toxic and carcinogenic. However, it is unscientific to measure the total arsenic content at this stage to indicate the arsenic exposure level or the impact on the environment and ecology.

Method used

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  • Detecting of different arsenic forms in environmental water based on HPLC-ICP-MS hyphenated technology
  • Detecting of different arsenic forms in environmental water based on HPLC-ICP-MS hyphenated technology
  • Detecting of different arsenic forms in environmental water based on HPLC-ICP-MS hyphenated technology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Embodiment 1: Optimization of liquid chromatography separation conditions

[0045] When using HPLC-ICP-MS to analyze the arsenic species in the sample, the selection and optimization of liquid chromatography separation conditions are very critical. The present invention investigates the separation effects of four forms of arsenic, As(III), As(V), DMA and MMA, from the following four aspects.

[0046] 1.1 Selection of chromatographic column

[0047] In water, As(Ⅲ), As(V), DMA and MMA all exist in the form of anions, so they can be separated according to the ion exchange mechanism. For anion exchange columns, under common mobile phase conditions, anions As(Ⅲ), As(V), DMA, MMA interact with ion exchanger groups on the stationary phase of the column, and are eluted in sequence according to the force come out. IonPac AS19 is a conventional anion exchange column capable of separating most anions.

[0048] 1.2 Selection of mobile phase and its concentration and pH value ...

Embodiment 2

[0060] Example 2: Research on Inductively Coupled Plasma Mass Spectrometry (ICP-MS) Analytical Conditions

[0061] The present invention chooses 75 The debugging solution with As concentration of 10 μg / L (contains internal standard elements 89 Y), do experiments on the power of the instrument plasma radio frequency generator (RF), carrier gas flow, cooling gas flow, plasma gas flow, sampling depth and other conditions; the measurement process is monitored at the same time 140 Ce and its double charge 70 and oxide 156, calculated double ion yield and oxide yield.

[0062] 2.1 Effect of plasma RF power

[0063] When the plasma RF power is changed, the intensity count of the element to be detected is detected. The measured data is shown in Table 2, and the RF power is used as the abscissa, the cps is used as the ordinate on the left, and the double charge and oxide yield of Ce are plotted on the right. See Figure 8 . The graph shows that as the RF power increases, the inten...

Embodiment 3

[0080] Example 3: Confirmation of indicators for the determination of arsenic in different forms by HPLC-ICP-MS

[0081] 3.1 Detection limit and linear range of combined method

[0082] Prepare a blank sample and add a small amount of standard water sample to be tested for analysis, measure 7 times continuously, and calculate the detection limit of the method according to 3 times the relative standard deviation of the measurement results. The specific data are shown in Table 6.

[0083] It can be seen from the table that the detection limits of the four forms of arsenic (calculated as As) are: As(Ⅲ), 0.08μg / L; As(V), 0.07μg / L; MMA, 0.06μg / L; DMA, 0.05μg / L. According to the U.S. EPA SW-846, the concentration of 4 times the detection limit is used as the lower limit of determination, and the lower limit of determination is as follows: As(Ⅲ), 0.4 μg / L; As(V), 0.3 μg / L; MMA, 0.3 μg / L; DMA , 0.2 μg / L.

[0084] Table 6 Detection limit data of different forms of arsenic

[0085] ...

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Abstract

The invention provides detecting of different arsenic forms in environmental water based on an HPLC-ICP-MS hyphenated technology. Detecting specifically comprises the steps that (1) a mixed standard solution is collocated, specifically, flowing phase L-aminothiopropionic acid serves as a solvent to collocate an arsenic mixed standard solution; (2) standard curves are drawn, specifically, the mixedstandard solution prepared from the step 1 is taken, the arsenic form concentration is detected by using the HPLC-ICP-MS, and according to the arsenic form concentration in the mixed standard solution and corresponding signal intensity, the standard curves of arsenic forms are drawn; (3) pretreatment is conducted on a sample, specifically, a to-be-detected water sample passes through a 0.45 [mu]mfilter membrane before sampling, a KOH solution is added, the sample is placed in a 4 DEG C low temperature condition after sampling, in experiment, the to-be-detected sample is measured out to a centrifuge tube, a flow phase is added to serve as a to-be-detected sample solution, and meanwhile blank test is carried out; and (4) the sample is detected, specifically, the HPLC-ICP-MS is used for measuring and analyzing the arsenic form concentration in the to-be-detected sample solution, the respective concentration value of the arsenic forms in the to-be-detected sample are calculated and analized according to RSD (relative standard deviation) of signal intensity obtained by calculating and the respective standard curves of the arsenic forms.

Description

technical field [0001] The invention relates to a detection method for different arsenic forms in environmental water, in particular to a detection method for different arsenic forms in environmental water based on HPLC-ICP-MS, and belongs to the field of water quality environmental monitoring. Background technique [0002] Poor water environment quality, severely damaged water ecology, and many environmental hazards are very prominent in some areas of our country, which affect and damage the health of the people and are not conducive to sustainable economic and social development. With the development of environmental science, biomedicine and other disciplines, many scholars have realized that the bioavailability, toxicity, and chemical activity and remigration of heavy metals in the environment are not only related to the total amount of heavy metals, but also to a greater extent. Determined by its form, different forms produce different environmental effects. Specific el...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 李义董会军董建芳赵峰赵俊梅刘亚平毕海超李梓瑶朱蕾李凡
Owner 河北省地质环境监测院
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