CN109839421A - The method quickly detected for the direct mass spectrography of semi-volatile organic matter in liquid - Google Patents
The method quickly detected for the direct mass spectrography of semi-volatile organic matter in liquid Download PDFInfo
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- CN109839421A CN109839421A CN201711203610.1A CN201711203610A CN109839421A CN 109839421 A CN109839421 A CN 109839421A CN 201711203610 A CN201711203610 A CN 201711203610A CN 109839421 A CN109839421 A CN 109839421A
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Abstract
The invention discloses a kind of methods quickly detected for the direct mass spectrography of semi-volatile organic matter in liquid.This method utilizes ultrasonic atomizatio principle, and fluid sample is made to be atomized into aerosol state, and the semi-volatile organic matter in liquid enters mass spectrometer under the purging effect of carrier gas and carries out quick analysis detection.Device used by this method includes the sample cell of a both ends open, and sample cell is equipped with fluid sample import and carrier gas inlet.Sample cell upper end with a conical device is closed is connected, a sample is equipped at the top of the conical device and is exported, dimethyl silicone polymer (PDMS) laminar film is posted in bottom, uses metal grid mesh as supporting.Sample cell lower end is screwed on ultrasonic atomizatio head, and ultrasonic atomizatio head is connected with external power, is inside placed with ultrasonic atomizatio piece.The device uses two PDMS laminar films, successively alternately closely pastes and is fixed on metal grid mesh.The use of PDMS film can greatly reduce the moisture content into mass spectrometer, avoid the vacuum environment of mass spectrometer impaired.
Description
Technical field
The invention belongs to the method for sampling fields of on-line mass spectroscopy analysis, and it is straight to be related to semi-volatile organic matter in a kind of pair of liquid
Connect the method that mass spectrography quickly detects.This method makes liquid form aerosol shape by ultrasonic atomizatio principle, therein partly to wave
Hair property organic matter enters mass spectrometer under the purging effect of carrier gas and carries out analysis detection, while dexterously combining PDMS laminar film
Dehumidifying avoids a large amount of steam from entering mass spectrometer, destroys instrument vacuum.Realize the direct of semi-volatile organic matter in liquid
Mass spectrography efficiently quickly detects.
Background technique
Semi-volatile organic matter (SVOCs) be a kind of boiling point in 170-350 DEG C, vapour pressure 13.3~10-5Within the scope of Pa
Organic compound, be mutually prevalent in big gas and water and soil environment with gas phase or particle.SVOCs is from a wealth of sources, most of
With bio-toxicity, some even also have carcinogenic, teratogenesis and mutagenic effect, fatal damage can be caused to human body;They
Saturated vapor force down, biological degradability it is poor, ecological environment can be made to be seriously damaged.Therefore the analysis to SVOCs in environment
Detection is of great significance for toxicological analysis, environmental protection and human health.
Detection for SVOCs in environment, general standard method is (such as: US Gov Env Protection Agency in the world at present
(EPA) the EPA Method 524.2 that recommends, 525.2,601~612, TO-1~TO-17 and China's standard GB/T/T
17130-1997, HJ/T 400-2007, HJ 605-2011 etc.), it is all to be connected using gas-chromatography (GC) or gaschromatographic mass spectrometry
Usage (GC-MS) is detected, although the method for this off-line analysis is accurate, time-consuming, at high cost, does not reflect organic
The change in time and space and dynamic process of pollutant are unable to satisfy the quick detection of a large amount of environmental samples.On-line monitoring technique can be fast
Speed obtains the qualitative and quantitative result of determinand, reflects the dynamic change of environmental contaminants in real time, in the environment the inspection of SVOCs
It surveys and is gradually had been favored by people in research field.Wherein on-line monitoring mass-spectrometric technique can directly obtain the molecule of determinand
The advantages such as amount information, has universality good, and resolution ratio and high sensitivity, qualitative ability is strong, and analysis speed is fast are that neck is tested in analysis
A kind of analysis method being most widely used in domain is widely recognized in on-line monitoring field, is developed rapidly, analysis
As a result have become a kind of the recognized standard.
However, semi-volatile organic matter boiling point is higher, vapour pressure is lower, and Mass Spectrometer Method response when direct injected is lower,
The mode for mostly using Thermal desorption is thus detected to it, discharges the Semi-volatile organism in fluid sample, but Thermal desorption is not suitable for
The compound analysis of thermally labile detects.In addition, heating temperature may destroy this original state of sample when higher, while generating one
A little interfering substances.On the other hand, there are some potential safety problemss for high-temperature heating.
Therefore, the present invention, using ultrasonic energy by fluid sample high-efficient atomizing, makes liquid by the way of ultrasonic atomizatio
Sample forms aerosol shape, under the purging effect of carrier gas, carries out quick analysis detection into mass spectrometer.
Summary of the invention
It quickly detects the purpose of the present invention is to provide a kind of for the direct mass spectrography of semi-volatile organic matter in liquid
Method, to achieve the above object, technical scheme is as follows:
Device used includes the sample cell of a both ends open, the upper end with a conical device is closed is connected, under
End with a ultrasonic atomizatio head is closed is connected.It is equipped with fluid sample import at the sample cell lower end, it is close in fluid sample import
Close one silicagel pad of connection, the inlet as sampling needle.It is equipped with carrier gas inlet close to sample cell upper end, for introducing carrier gas.
The top of conical device is equipped with sample export, which passes through the injection port phase of a threeway and mass spectrometer
Even.2 layers or more of metal grid mesh is fixed in the lower part of conical device, and PDMS laminar film is equipped between adjacent metal grid mesh, uses
In a large amount of steam that removal ultrasonic atomizatio generates, a large amount of steam is avoided to destroy the vacuum condition of mass spectrometer system.PDMS laminar film
Edge and the inner wall of conical device mutually amplexiform.The first metal grid mesh is fixed in the bottom of conical device, first metal gate
The first PDMS laminar film is fixed in the upper surface of net, and the upper surface of the PDMS laminar film is equipped with the second metal grid mesh, second metal
The 2nd PDMS laminar film is fixed in the upper surface of aperture plate, and the upper surface of the 2nd PDMS laminar film sets third metal grid mesh, the third
Metal grid mesh is fixed in conical device.Gas enters conical device from conical device lower open end, after PDMS laminar film
It is flowed out from sample export.
Ultrasonic atomizatio head includes a ultrasonic output circuit and ultrasonic atomizatio piece;Ultrasonic atomizatio head is connected with external power.Sample
The height setting in product pond is greater than the atomization height of fluid sample, liquid sample volume of the atomization of fluid sample highly by injecting
It is codetermined with the power of the ultrasonic atomization generator used, determination should be debugged before use
Then this method opens external power, to ultrasonic atomizatio in use, introduce clean carrier gas at carrier gas inlet first
After head preheating 1 minute or more, the liquid sample of certain volume is injected from the silicagel pad of fluid sample import, is opened immediately
The data of mass spectrometer acquire;Fluid sample is atomized into rapidly aerosol shape after entering sample cell, under the carrier band of carrier gas from
Sample export at the top of conical device overflows, and the injection port through mass spectrometer enters mass spectrometer and carries out direct mass spectral analysis inspection
It surveys.
Advantages of the present invention
1) this method is easy to operate, efficiently quickly
2) this method is applied widely, is suitable for any fluid sample
3) this method uses ultrasonic atomizatio, and energy applying mode is mild, small to the destructiveness of sample, and guarantee detects sample
Basis characteristic.
Detailed description of the invention
Fig. 1 is the schematic diagram of the method quickly detected for the direct mass spectrography of semi-volatile organic matter in liquid.
Wherein: 1- sample cell;2- conical device;3- ultrasonic atomizatio head;The 2nd PDMS laminar film of 4-1-, the first PDMS of 4-2-
Laminar film, 5-1- third metal grid mesh, the second metal grid mesh of 5-2-, the first metal grid mesh of 5-3-;6- ultrasonic atomizatio piece;7- dispatch from foreign news agency
Source;8- silicagel pad;9- mass spectrometer;A- fluid sample import;B- carrier gas inlet;C- sample export
Specific embodiment
Device used includes three parts: a upper and lower ends opening, is highly the sample cell of 20cm, a lower ending opening
Conical device and a ultrasonic atomizatio head with closed conical cavity.
The upper open end of the sample cell and lower open end of conical device is closed is connected, lower open end and ultrasonic atomizatio head are closed
It is connected.Ultrasonic atomizatio head includes ultrasonic output circuit and ultrasonic atomizatio piece, and ultrasonic atomizatio head is connected with external power.Close to sample
The sample cell side wall surface of pond lower end is equipped with fluid sample import, and the sample cell side wall surface close to sample cell upper end is equipped with carrier gas
Entrance;Fluid sample entrance is equipped with sealed silicon rubber mat, the inlet as sampling needle.
The top of conical device is equipped with sample export, and sample export passes through the injection port phase of a threeway and mass spectrometer
Even, the third interface emptying of threeway;3 layers of metal grid mesh are fixed in conical device, are set respectively between adjacent metal grid mesh
There is PDMS laminar film, a total of 2 layers of PDMS laminar film, the edge of PDMS laminar film and the inner wall of conical device are affixed
It connects.The first metal grid mesh is fixed in the bottom of conical device, and the first PDMS laminar film is fixed in the upper surface of first metal grid mesh, should
The upper surface of PDMS laminar film is equipped with the second metal grid mesh, and the 2nd PDMS laminar film is fixed in the upper surface of second metal grid mesh,
The upper surface of 2nd PDMS laminar film sets third metal grid mesh, which is fixed in conical device.Gas from
Conical device lower open end enters, and flows out through after PDMS laminar film from sample export.PDMS laminar film is for removing ultrasonic mist
Change a large amount of steam that head generates, a large amount of steam is avoided to destroy the vacuum condition of mass spectrometer system.
Then this method opens external power, to ultrasonic atomizatio in use, introduce clean carrier gas at carrier gas inlet first
After head preheating 2 minutes, the liquid sample of 3ml is injected from the silicagel pad of fluid sample import, opens mass spectrometer immediately
Data acquisition;Fluid sample is atomized into rapidly aerosol shape after entering sample cell, from conical device under the carrier band of carrier gas
The sample export at top overflows, and the injection port through mass spectrometer enters mass spectrometer and carries out direct mass spectral analysis detection.
Claims (7)
1. the method quickly detected for the direct mass spectrography of semi-volatile organic matter in liquid, it is characterised in that:
Device used includes the conical device of the sample cell (1) of upper and lower ends opening, lower ending opening with closed conical cavity
(2), the upper open end of sample cell (1) with conical device (2) lower open end is closed is connected, the lower open end and one of sample cell (1)
A ultrasonic atomizatio head (3) is closed to be connected;
Sample cell (1) is equipped with fluid sample import (a) and carrier gas inlet (b);
The top of conical device (2) is equipped with sample export (c), sample export (c) by threeway and mass spectrometer (9) into
Sample mouth is connected;The third interface of threeway is vented;
2 layers or more of metal grid mesh is fixed in the lower part of conical device (2), and PDMS sheet is equipped between adjacent metal grid mesh
Film, the edge of PDMS laminar film and the inner wall of conical device (2) mutually amplexiform, and gas is from conical device (2) lower open end
Into conical device (2), flowed out through after PDMS laminar film from sample export (c).
2. the method according to claim 1 quickly detected for the direct mass spectrography of semi-volatile organic matter in liquid,
It is characterized in that:
Fluid sample import (a) place is equipped with sealed silicon rubber mat (8), the inlet as sampling needle.
3. the method according to claim 1 quickly detected for the direct mass spectrography of semi-volatile organic matter in liquid,
It is characterized in that:
The first metal grid mesh (5-3) is fixed in the bottom of conical device (2), and the upper surface of first metal grid mesh (5-3) fixes
The upper surface of one PDMS laminar film (4-2), the PDMS laminar film (4-2) is equipped with the second metal grid mesh (5-2), second metal gate
The 2nd PDMS laminar film (4-1) is fixed in the upper surface of net (5-2), and the upper surface of the 2nd PDMS laminar film (4-1) sets third gold
Belong to aperture plate (5-1), which is fixed in conical device (2).
4. the method according to claim 1 quickly detected for the direct mass spectrography of semi-volatile organic matter in liquid,
It is characterized in that:
Ultrasonic atomizatio head (3) includes a ultrasonic output circuit and ultrasonic atomizatio piece (6);Ultrasonic atomizatio head (3) and external power (7)
It is connected.
5. the method according to claim 1 quickly detected for the direct mass spectrography of semi-volatile organic matter in liquid,
It is characterized in that:
The height setting of sample cell (1) is greater than the atomization height of its interior fluid sample, and the atomization height of fluid sample is by injecting
Liquid sample volume and the ultrasonic atomizatio head (3) used power codetermine, determination should be debugged before use;Fluid sample into
Mouth (a) is close to the lower end of sample cell (1), upper end of the carrier gas inlet (b) close to sample cell (1).
6. the method according to claim 1 or 3 quickly detected for the direct mass spectrography of semi-volatile organic matter in liquid,
It is characterized by:
PDMS laminar film is used to remove a large amount of steam of ultrasonic atomizatio head (3) generation, and a large amount of steam is avoided to destroy mass spectrometer system
Vacuum condition.
7. the method quickly detected described in -6 for the direct mass spectrography of semi-volatile organic matter in liquid according to claim 1,
It is characterized by:
Then this method opens external power (7), to ultrasonic mist in use, introduce clean carrier gas at carrier gas inlet (b) first
After changing head (3) preheating 1 minute or more, the testing liquid sample of certain volume is injected at the silicagel pad (8) of fluid sample import (a)
Product open the data acquisition of mass spectrometer (9) immediately;Fluid sample enters sample cell (1) and is atomized into aerosol shape rapidly afterwards,
It is overflowed under the carrier band of carrier gas from the sample export (c) at the top of conical device (2), the injection port through mass spectrometer (9) enters matter
Spectrometer device (9) carries out direct mass spectral analysis detection.
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Cited By (1)
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CN113340973A (en) * | 2021-06-08 | 2021-09-03 | 白伟东 | Method and device for rapidly detecting total volatile organic compounds |
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Application publication date: 20190604 |