Gas-mass spectrometry chromatography combined detection method of ammonia nitrogen and isotope content in water sample

A detection method and isotope technology, applied in the detection field, can solve problems such as impracticability, and achieve the effects of high precision and accuracy, wide application range, and good yield

Active Publication Date: 2020-07-10
PEARL RIVER HYDRAULIC RES INST OF PEARL RIVER WATER RESOURCES COMMISSION
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The mass difference between nitrogen isotopes is only 1, and their physical and chemical properties are almost exactly the same, so it is impossible to separate the above isotopes with conventional GC-MS or HPLC-MS

Method used

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  • Gas-mass spectrometry chromatography combined detection method of ammonia nitrogen and isotope content in water sample
  • Gas-mass spectrometry chromatography combined detection method of ammonia nitrogen and isotope content in water sample
  • Gas-mass spectrometry chromatography combined detection method of ammonia nitrogen and isotope content in water sample

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Experimental program
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Effect test

Embodiment 1

[0034] Embodiment 1: Utilize the ammonium sulfate solution of known concentration to evaluate the accuracy of detection method of the present invention

[0035] Step 1: Sampling

[0036] Contain 50 μmol of ( 14 NH 4 ) 2 SO 4 and 50 μmol of ( 15 NH 4 ) 2 SO 4 The mixed solution of 1000mL, accurately pipette 10.0ml sample as the sample solution.

[0037] Step 2: Prepare blank control solution

[0038] Accurately pipette 10.0ml double distilled water as blank control solution.

[0039] Step 3: Add 3ml of neutral formaldehyde to the sample solution prepared in the first step, mix and shake well, react for about 30min, adjust the pH of the obtained product to 9.0 with 6mol / L sodium hydroxide, and then pass through C 18 Solid-phase extraction cartridges were activated with 10ml of methanol (HPLC grade) and 10ml of water in sequence before use. The sample solution to be analyzed is all passed through C 18 After the small column, rinse the analysis sample solution contain...

Embodiment 2

[0053] Embodiment 2: Determination of ammonia nitrogen and isotope content of unknown concentration sample

[0054] The first step, sampling

[0055] Take 10,000ml of 6 water samples located in the river section of Guangzhou River, adjust the pH<2.0 with 6mol / L sulfuric acid to stabilize the content of ammonia nitrogen and its isotopes in the samples, concentrate to 10.0ml with a rotary evaporator in a water bath at 70°C, and filter Remove the precipitate from the solution.

[0056] Step 2: Prepare blank control solution

[0057] Accurately pipette 10,000ml of double distilled water, and concentrate to 10.0ml according to the first step method, as a blank control solution.

[0058] Step 3: Add 3ml of analytically pure neutral formaldehyde to the sample solution prepared in the first step, mix and shake well, react for about 30min, adjust the pH of the obtained product to 9.0 with 6mol / L sodium hydroxide, and use 5ml / L min after C 18 Solid-phase extraction cartridges, solid...

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Abstract

The invention belongs to the field of detection, and discloses a gas-mass spectrometry chromatography combined detection method of ammonia nitrogen and an isotope content in a water sample. Accordingto the method, neutral formaldehyde is added into a to-be-detected water sample for reaction to generate stable imine, and then GC-MS is used for detection. According to the method, the gas is prevented from being used as a detection object, mass spectrum signals are greatly different after <14>NH4<+> and <15>NH4<+> react with neutral formaldehyde so that a conventional gas-mass spectrometry chromatography combined detection method can be used for direct qualitative and quantitative detection. In addition, only an operation pH value needs to be well controlled in an operation process, a good recovery rate is achieved within a time range in the right, the method is simple, and precision and accuracy are high.

Description

technical field [0001] The invention belongs to the field of detection, in particular to a gas-mass spectrometry detection method for ammonia nitrogen and its isotope content in water samples. Background technique [0002] Ammonia nitrogen is one of the main indicators of water eutrophication, and also one of the main indicators for the control of drinking water and surface water in my country. Ammonia nitrogen mainly comes from domestic wastewater. The large discharge of these ammonia nitrogen-containing wastewater increases the nitrogen content in the water body and leads to eutrophication of the water body. Black and smelly. At present, nitrogen isotopes are used to trace the source of nitrogen pollution, nitrogen cycle and fate in the research environment. However, due to the consistent chemical and physical properties of ammonia nitrogen itself and the direct chemical and physical properties of ammonia nitrogen isotopes, it cannot be effectively monitored by convention...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8675Y02A20/20
Inventor 郭伟蒋然
Owner PEARL RIVER HYDRAULIC RES INST OF PEARL RIVER WATER RESOURCES COMMISSION
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