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Method for analyzing content of tonalid in water

A technology of musk tuna and an analysis method, applied in the field of analysis of trace amounts of musk tuna, can solve problems such as lack of uniform standards, and achieve the effects of ensuring consistency, accuracy, and uniform distribution

Inactive Publication Date: 2013-03-13
SHENYANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Unfortunately, there is no unified standard for the determination of trace amounts of musk in water, so it is urgent to develop an efficient, fast and accurate analysis method for musk in water

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 1. Prepare standard solutions

[0021] Weigh the Tuna musk standard substance, dissolve it in analytically pure acetone, and prepare a standard stock solution of 100 micrograms per liter. Pipette 0.2ml, 0.4ml, 0.6ml, 0.8ml, 1.0ml, 1.2ml, 1.4ml standard stock solution, dilute with purified water to a concentration of 200ng / L, 400ng / L, 600ng / L , 800 ng / L, 1000 ng / L, 1200 ng / L, 1400 ng / L series of standard solutions.

[0022] 2. Solid Phase Microextraction

[0023] Carry out solid-phase microextraction to the standard solution, the condition of its solid-phase microextraction is: adopt the polydimethylsilane extraction head of filter membrane thickness 100 microns, measure 5 milliliters of standard solution obtained in step 1, immerse extraction, extraction temperature 35 ℃ , The extraction time is 40 minutes. The gas chromatography desorption temperature is 250°C, and the desorption time is 5 minutes.

[0024] 3. Gas Chromatography-Mass Spectrometry Analysis

[0025]...

Embodiment 2

[0029] 1. Prepare standard solutions

[0030] Weigh the Tuna musk standard substance, dissolve it in analytically pure acetone, and prepare a standard stock solution of 100 micrograms per liter. Pipette 0.3ml, 0.5ml, 0.7ml, 0.9ml, 1.1ml, 1.3ml, 1.5ml standard stock solution, dilute with purified water to a concentration of 300ng / L, 500ng / L, 700ng / L , 900 ng / L, 1100 ng / L, 1300 ng / L, 1500 ng / L series of standard solutions.

[0031] 2. Solid Phase Microextraction

[0032] Carry out solid-phase microextraction to the standard solution, the condition of its solid-phase microextraction is: adopt the polydimethylsilane extraction head of filter membrane thickness 100 microns, measure 7 milliliters of standard solution obtained in step 1, immerse extraction, extraction temperature 35 ℃ , The extraction time is 40 minutes. The gas chromatography desorption temperature is 250°C, and the desorption time is 5 minutes.

[0033] 3. Gas Chromatography-Mass Spectrometry Analysis

[0034]...

Embodiment 3

[0038] 1. Prepare standard solutions

[0039] Weigh the Tuna musk standard substance, dissolve it in analytically pure acetone, and prepare a standard stock solution of 100 micrograms per liter. Pipette 0.25ml, 0.45ml, 0.65ml, 0.85ml, 1.05ml, 1.25ml, 1.45ml standard stock solution, dilute with purified water to a concentration of 250ng / L, 450ng / L, 650ng / L , 850 ng / L, 1050 ng / L, 1250 ng / L, 1450 ng / L series of standard solutions.

[0040] 2. Solid Phase Microextraction

[0041] Carry out solid-phase microextraction to the standard solution, the condition of its solid-phase microextraction is: adopt the polydimethylsilane extraction head of filter film thickness 100 microns, measure 10 milliliters of standard solution obtained in step 1, immerse extraction, extraction temperature 35 ℃ , The extraction time is 40 minutes. The gas chromatography desorption temperature is 250°C, and the desorption time is 5 minutes.

[0042] 3. Gas Chromatography-Mass Spectrometry Analysis

[0...

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Abstract

The invention relates to a method for analyzing content of tonalid in water, which comprises the following steps of: 1. standard solution preparation, wherein the standard solution preparation comprises the steps of weighing standard tonalid, dissolving the standard tonalid into analytical pure acetone, and preparing 100microgramme / L of standard storage solution; 2. sold phase microextraction, wherein the sold phase microextraction is carried out on the standard solution; 3. gas chromatography-mass spectrometry analysis, wherein the gas chromatography-mass spectrometry analysis is carried out on the standard solution processed by the sold phase microextraction so as to obtain peak area and a standard curve of the tonalid content in the standard solution; and 4. sample analysis, wherein the sample analysis comprises the steps of filtering a water sample containing the tonalid by a 0.45 micrometer microfiltration membrane, taking 5-10ml of filtered water sample, repeating the step 2 and analysis operation in the step 3, and obtaining the peak area and the content of the tonalid in the water sample as compared with the standard curve. The method for analyzing content of tonalid in water, can efficiently, rapidly and accurately accomplish the trace quantity measurement on the tonalid in sewage.

Description

technical field [0001] The invention relates to a method for analyzing trace musk musk in sewage, and belongs to the technical field of environmental monitoring. Background technique [0002] Tuna musk 7-Acetyl-1, 1, 3, 4, 4, 6-hexamethyltetralin tonalide, the isomer of Wanshan musk, is a good deodorant, widely used in the essence of soap box washing products , It is also very useful in oily fragrance baths with baths, and the maximum dosage can exceed 10%. [0003] After the chemicals containing musk enter the water body, different from the characteristics of traditional persistent organic pollutants such as "refractory degradation", "bioaccumulation" and "global circulation", musk is highly polar, easily soluble in water and weak Their volatility prevents their "global evaporation" behavior like traditional persistent organic pollutants, which means that the distribution of Tuna musk in the environment will mainly be through water phase transfer and food chain diffusion....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 李海波李英华
Owner SHENYANG UNIV