CN106124666A - The assay method of 55 kinds of volatile organic contaminants in a kind of surface water - Google Patents
The assay method of 55 kinds of volatile organic contaminants in a kind of surface water Download PDFInfo
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- CN106124666A CN106124666A CN201610692162.5A CN201610692162A CN106124666A CN 106124666 A CN106124666 A CN 106124666A CN 201610692162 A CN201610692162 A CN 201610692162A CN 106124666 A CN106124666 A CN 106124666A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G01N2030/025—Gas chromatography
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Abstract
The present invention is applicable to the technical field of Environmental safety supervision, discloses the assay method of 55 kinds of volatile organic contaminants in a kind of surface water, comprises the steps: sample pretreatment, instrument parameter setting, Criterion curve and inner mark method ration.The assay method of 55 kinds of volatile organic contaminants in a kind of surface water of the present invention, after a certain amount of surface water methanol is extracted, add matrix correction liquid, after head space processes, with combined gas chromatography mass spectrometry, in surface water 55 kinds of volatile organic contaminants are carried out qualitative and quantitative analysis, the method is easy and simple to handle, accuracy is high, highly sensitive, interference is few, reproducible, in 40～800 μ g/L concentration ranges, 55 kinds of volatile organic contaminant curve linears are good, correlation coefficient is all more than 0.999, the monitoring of volatile organic contaminant in surface water had stronger practicality, can be used for the risk assessment to surface water pollution situation, there is important environment protection significance.
Description
[technical field]
The present invention relates to the technical field of Environmental safety supervision, particularly to 55 kinds of organic dirts of volatility in a kind of surface water
The assay method of dye thing.
[background technology]
Along with expanding economy, environmental problem is constantly deteriorating, such as the discharge of vehicle exhaust, industrial wastewater, the row of waste gas
Putting, cause environment to be subject to serious threat, environment is the area of space that people depend on for existence, directly influence people health and
Life, therefore strengthens environment protection and has necessity and importance.
And water is the source of all life, be the necessary element of people's daily life, be all life depend on for existence important
Resource, is also the important element maintaining human normal life state.Surface water, refers to be present in earth's crust surface, is exposed to air
Water, be river, glacier, lake, the general name of the four kinds of water bodys in marsh, also known as " terrestrial water ".It is the important of human lives's water
One of source, the key component of Ye Shi various countries water resource.Along with the deterioration of environment, surface water also receives serious dirt
, there is potential safety hazard in dye, occurs that owing to refer to the surface water of degree of being contaminated the disease even phenomenon of death are the most increasingly
Seriously, quote for a long time and human body can be produced serious harm, it is therefore necessary to strengthen the inspecting force to surface water, find in time
Problem, solves problem, has great importance the improvement of environment and the healthy living of people simultaneously, it is therefore necessary to propose one
Plant the assay method of 55 kinds of volatile organic contaminants in surface water.
[summary of the invention]
It is an object of the invention to overcome above-mentioned the deficiencies in the prior art, it is provided that in a kind of surface water, 55 kinds of volatility are organic
The assay method of pollutant, it aims to solve the problem that in prior art that problem of environmental pollution is serious, and surface water is contaminated, and to there is safety the most hidden
Suffer from, and current surface water quality detection is complex, the technical problem that accuracy is relatively low.
For achieving the above object, the mensuration side of 55 kinds of volatile organic contaminants during the present invention proposes a kind of surface water
Method, comprises the steps:
Step one, sample pretreatment: accurately draw a certain amount of surface water with gas-tight syringe, be placed in 10mL top
In empty bottle, after extracting with methanol, it is placed in agitator vibration, after vibration completely, obtains sample liquid, stand, then with clean 1000
μ L syringe accurately draws 500 μ L sample liquid supernatant in 20mL ml headspace bottle, and adds a certain amount of matrix correction liquid, preparation
Become liquid to be measured, and gland seals to be measured；
Step 2, instrument parameter are arranged: head-space sampler and gas chromatograph-mass spectrometer (GC-MS) carry out the setting of parameter；
Step 3, Criterion curve: take the ml headspace bottle of 5 20mL, in each ml headspace bottle, all fill the methanol of 10mL5%
55 kinds of volatile organic contaminants are made series concentration and are respectively 40 μ g/L, 80 μ g/L, 200 μ by solution and 3.6g sodium chloride
G/L, 400 μ g/L, the mixed standard solution of 800 μ g/L, by head-space sampler headspace sampling, and pass through gas chromatography-mass spectrum
Combined instrument uses SIM mode to gather, and obtains standard curve；
Step 4, inner mark method ration: add a certain amount of internal standard substance in the liquid to be measured in step one, be placed in headspace sampling
Device carries out head space process, then uses gas chromatography/mass spectrometry internal standard substance by gas chromatograph-mass spectrometer (GC-MS)
With peak area (or peak height) and the relative correction factor of liquid component to be measured, then automatically calculated by the standard curve in step 3
Obtain measured matter content in soil pattern.
As preferably, the uptake of the surface water in described step one is 5mL, and described methanol is chromatographic grade first
Alcohol, consumption is 2.5mL.
As preferably, the agitator in described step one is constant temperature oscillator, and speed setting is 135rpm, duration of oscillation
For 35min.
As preferably, the 20mL ml headspace bottle in described step one, before adding sample liquid supernatant, adds in advance
9.5mL deionized water and 3.6g sodium chloride, described sodium chloride is top grade pure sodium chloride.
As preferably, the concentration of the matrix correction liquid in described step one is 200 μ g/mL, and addition is 20 μ L.
As preferably, in described step 3, methanol solution is hplc grade methanol solution, and sodium chloride is top grade pure sodium chloride.
As preferably, the described internal standard substance in step 4 is that in step 3, concentration is that 55 kinds of volatility of 200 μ g/L have
Organic pollutants mixed standard solution, addition is 20 μ L.
Beneficial effects of the present invention: compared with prior art, in a kind of surface water that the present invention provides, 55 kinds of volatility have
The assay method of organic pollutants, after being extracted by a certain amount of surface water methanol, adds matrix correction liquid, through head space
After process, with GC-MS, in surface water 55 kinds of volatile organic contaminants are carried out qualitative, quantitative and divide
Analysis, the method is easy and simple to handle, accuracy is high, highly sensitive, interference is few, can be used for the risk assessment to surface water pollution situation,
There is important environment protection significance.
Inventive feature and advantage will be described in detail by embodiment.
[detailed description of the invention]
For making the object, technical solutions and advantages of the present invention of greater clarity, below by embodiment, the present invention is entered
Row further describes.However, it should be understood that specific embodiment described herein is only in order to explain the present invention, and need not
In limiting the scope of the present invention.Additionally, in the following description, eliminate the description to known features and technology, so that avoid need not
Idea of the invention is obscured in strategic point.
The embodiment of the present invention provides the assay method of 55 kinds of volatile organic contaminants in a kind of surface water, including walking as follows
Rapid:
Step one, sample pretreatment: accurately draw a certain amount of surface water with gas-tight syringe, be placed in 10mL top
In empty bottle, after extracting with methanol, it is placed in agitator vibration, after vibration completely, obtains sample liquid, stand, then with clean 1000
μ L syringe accurately draws 500 μ L sample liquid supernatant in 20mL ml headspace bottle, and adds a certain amount of matrix correction liquid, preparation
Become liquid to be measured, and gland seals to be measured.
Wherein, the uptake of surface water is 5mL, and described methanol is hplc grade methanol, and consumption is 2.5mL, vibration
Device is constant temperature oscillator, and speed setting is 135rpm, and duration of oscillation is 35min.
Further, 20mL ml headspace bottle, before adding sample liquid supernatant, adds 9.5mL deionized water and 3.6g in advance
Sodium chloride, described sodium chloride is top grade pure sodium chloride.
Further, the concentration of matrix correction liquid is 200 μ g/mL, and addition is 20 μ L.
Step 2, instrument parameter are arranged: head-space sampler and gas chromatograph-mass spectrometer (GC-MS) carry out the setting of parameter.
In embodiments of the present invention, the parameter of head-space sampler arranges specific as follows:
Transfer tube temperature: 130 DEG C
Sampling system temperature: 130 DEG C
Sample heating temperature: 80 DEG C
Sample heating time: 45min
Hunting speed: FAST
Pressing time: 10s
Fill sampling ring time: 10s
Sampling volume: 1mL
The parameter of gas chromatograph-mass spectrometer (GC-MS) arranges specific as follows:
Injector temperature: 150 DEG C
Input mode: shunting (split ratio 10:1)
Carrier gas: helium (purity 99.999%)
Chromatographic column: Rtx-5MS (30m × 0.25mm × 0.25 μm)
Column temperature is arranged: 40 DEG C (5min) 6 DEG C/min140 DEG C (0min) 5 DEG C/min210 DEG C (0min) 20 DEG C/min230 DEG C
(2min)
Carrier gas control model: constant linear velocity
Linear velocity: 36.1cm/sec
Ion source temperature: 200 DEG C
Chromatography-mass spectroscopy interface temperature: 235 DEG C
Solvent mute time: 3min
Acquisition time: 3.5～35min
Acquisition mode: SIM pattern
Select ion: as shown in table 1
The selection ion of table 1 object
Step 3, Criterion curve: take the ml headspace bottle of 5 20mL, in each ml headspace bottle, all fill the methanol of 10mL5%
55 kinds of volatile organic contaminants are made series concentration and are respectively 40 μ g/L, 80 μ g/L, 200 μ by solution and 3.6g sodium chloride
G/L, 400 μ g/L, the mixed standard solution of 800 μ g/L, by head-space sampler headspace sampling, and pass through gas chromatography-mass spectrum
Combined instrument uses SIM mode to gather, and obtains standard curve.
Wherein, methanol solution is hplc grade methanol solution, and sodium chloride is top grade pure sodium chloride.
Step 4, inner mark method ration: add a certain amount of internal standard substance in the liquid to be measured in step one, be placed in headspace sampling
Device carries out head space process, then uses gas chromatography/mass spectrometry internal standard substance by gas chromatograph-mass spectrometer (GC-MS)
With peak area (or peak height) and the relative correction factor of liquid component to be measured, then automatically calculated by the standard curve in step 3
Obtain measured matter content in soil pattern.
Wherein, internal standard substance is that in step 3, concentration is 55 kinds of volatile organic contaminant mixed standard solutions of 200 μ g/L,
Addition is 20 μ L.
The assay method of 55 kinds of volatile organic contaminants in this kind of surface water, by by a certain amount of earth's surface water sample
After product extract with methanol, add matrix correction liquid, after head space processes, with GC-MS to surface water
In 55 kinds of volatile organic contaminants carry out qualitative and quantitative analysis, the method is easy and simple to handle, accuracy is high, highly sensitive, interference
Few, reproducible, in 40～800 μ g/L concentration ranges, 55 kinds of volatile organic contaminant curve linears are good, correlation coefficient
All more than 0.999, the monitoring of volatile organic contaminant in surface water is had stronger practicality, can be used for surface water
The risk assessment of pollution situation, has important environment protection significance.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention
Any amendment, equivalent or the improvement etc. made within god and principle, should be included within the scope of the present invention.
Claims (7)
1. the assay method of 55 kinds of volatile organic contaminants in a surface water, it is characterised in that: comprise the steps:
Step one, sample pretreatment: accurately draw a certain amount of surface water with gas-tight syringe, be placed in 10mL ml headspace bottle
In, after extracting with methanol, it is placed in agitator vibration, after vibration completely, obtains sample liquid, stand, then with 1000 clean μ L notes
Emitter accurately draws 500 μ L sample liquid supernatant in 20mL ml headspace bottle, and adds a certain amount of matrix correction liquid, is prepared as treating
Survey liquid, and gland seals to be measured；
Step 2, instrument parameter are arranged: head-space sampler and gas chromatograph-mass spectrometer (GC-MS) carry out the setting of parameter；
Step 3, Criterion curve: take the ml headspace bottle of 5 20mL, in each ml headspace bottle, all fill the methanol solution of 10mL5%
With 3.6g sodium chloride, 55 kinds of volatile organic contaminants are made series concentration be respectively 40 μ g/L, 80 μ g/L, 200 μ g/L,
400 μ g/L, the mixed standard solution of 800 μ g/L, by head-space sampler headspace sampling, and pass through gas chromatography-mass spectrography
Instrument uses SIM mode to gather, and obtains standard curve；
Step 4, inner mark method ration: add a certain amount of internal standard substance in the liquid to be measured in step one, be placed in head-space sampler
Carry out head space process, then use gas chromatography/mass spectrometry internal standard substance by gas chromatograph-mass spectrometer (GC-MS) and treat
Survey peak area (or peak height) and the relative correction factor of liquid component, be then calculated automatically from by the standard curve in step 3
Measured matter content in soil pattern.
The assay method of 55 kinds of volatile organic contaminants in a kind of surface water the most as claimed in claim 1, it is characterised in that:
The uptake of the surface water in described step one is 5mL, and described methanol is hplc grade methanol, and consumption is 2.5mL.
The assay method of 55 kinds of volatile organic contaminants in a kind of surface water the most as claimed in claim 1, it is characterised in that:
Agitator in described step one is constant temperature oscillator, and speed setting is 135rpm, and duration of oscillation is 35min.
The assay method of 55 kinds of volatile organic contaminants in a kind of surface water the most as claimed in claim 1, it is characterised in that:
20mL ml headspace bottle in described step one, before adding sample liquid supernatant, adds 9.5mL deionized water and 3.6g in advance
Sodium chloride, described sodium chloride is top grade pure sodium chloride.
The assay method of 55 kinds of volatile organic contaminants in a kind of surface water the most as claimed in claim 1, it is characterised in that:
The concentration of the matrix correction liquid in described step one is 200 μ g/mL, and addition is 20 μ L.
The assay method of 55 kinds of volatile organic contaminants in a kind of surface water the most as claimed in claim 1, it is characterised in that:
In described step 3, methanol solution is hplc grade methanol solution, and sodium chloride is top grade pure sodium chloride.
The assay method of 55 kinds of volatile organic contaminants in a kind of surface water the most as claimed in claim 1, it is characterised in that:
The described internal standard substance in step 4 is that in step 3, concentration is that 55 kinds of volatile organic contaminant hybrid standards of 200 μ g/L are molten
Liquid, addition is 20 μ L.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107085062A (en) * | 2017-05-27 | 2017-08-22 | 深圳天祥质量技术服务有限公司 | The method of testing of VOC in water |
| CN109668973A (en) * | 2017-10-17 | 2019-04-23 | 中国石油化工股份有限公司 | The measuring method of gas station underground water pollutant |
| CN110749678A (en) * | 2019-11-08 | 2020-02-04 | 广东优策检验检测技术有限公司 | Method for measuring organic volatile substances in soil by using gas chromatography-mass spectrometry-headspace |
| CN112505282A (en) * | 2020-12-25 | 2021-03-16 | 生态环境部南京环境科学研究所 | Real-time accurate tracing early warning method and system for environmental water pollution |
| CN112697938A (en) * | 2020-12-22 | 2021-04-23 | 北京市劳动保护科学研究所 | Analysis method of tetrahydrothiophene in soil |
| CN114252539A (en) * | 2022-01-07 | 2022-03-29 | 大连理工大学 | Method for comprehensively measuring content of volatile organic compounds in petrochemical wastewater |
-
2016
- 2016-08-18 CN CN201610692162.5A patent/CN106124666A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107085062A (en) * | 2017-05-27 | 2017-08-22 | 深圳天祥质量技术服务有限公司 | The method of testing of VOC in water |
| CN109668973A (en) * | 2017-10-17 | 2019-04-23 | 中国石油化工股份有限公司 | The measuring method of gas station underground water pollutant |
| CN110749678A (en) * | 2019-11-08 | 2020-02-04 | 广东优策检验检测技术有限公司 | Method for measuring organic volatile substances in soil by using gas chromatography-mass spectrometry-headspace |
| CN112697938A (en) * | 2020-12-22 | 2021-04-23 | 北京市劳动保护科学研究所 | Analysis method of tetrahydrothiophene in soil |
| CN112505282A (en) * | 2020-12-25 | 2021-03-16 | 生态环境部南京环境科学研究所 | Real-time accurate tracing early warning method and system for environmental water pollution |
| CN114252539A (en) * | 2022-01-07 | 2022-03-29 | 大连理工大学 | Method for comprehensively measuring content of volatile organic compounds in petrochemical wastewater |
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