CN101949906B - Decompressed purge-and-trap processing equipment for non-volatile organic compound in water sample and processing method thereof - Google Patents
Decompressed purge-and-trap processing equipment for non-volatile organic compound in water sample and processing method thereof Download PDFInfo
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- CN101949906B CN101949906B CN2010102475651A CN201010247565A CN101949906B CN 101949906 B CN101949906 B CN 101949906B CN 2010102475651 A CN2010102475651 A CN 2010102475651A CN 201010247565 A CN201010247565 A CN 201010247565A CN 101949906 B CN101949906 B CN 101949906B
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Abstract
The invention discloses decompressed purge-and-trap processing equipment for a non-volatile organic compound in a water sample and a processing method thereof. The invention is characterized in that the equipment is formed by sequentially connecting a sample heater (1), a purge bottle (2), a trapper (3), a pressure controller (4) and a pump (5), wherein purge gas (6) is connected with the purge bottle (2) through a purge gas inlet (7); the purge bottle is connected with the trapper (3) through a purge gas outlet (8); the trapper (3) is connected with the pump (5) through the pressure controller (4); the gas trapped by the trapper (3) is taken out and then placed into a heater (13) of the trapper; chromatographic carrier gas (14) is connected with a chromatographic injection port (12) in a column oven (11) through the trapper (3) and a transmission pipeline (15); and the chromatographic injection port is connected with a chromatographic detector (9) through a chromatographic column (10). The processing method comprises the following steps: forming a negative pressure environment around a test sample under the action of the pump, and increasing the vapor pressure of the non-volatile organic compound under the negative pressure environment; purging the bottom of the sample by utilizing inert gas so that the target compound can be trapped by the trapper after being blown out from the sample; and finally, resolving the target compound at high temperature and then carrying out chromatographic analysis.
Description
Technical field
The present invention relates to decompression purge and trap treating apparatus and the disposal route thereof of nonvolatile organic compound in a kind of water sample, particularly decompression purge and trap mode captures, and the sample treatment of mode wash-out nonvolatile organic compound is analysed in pyrolysis.Belong to chromatogram minute technical field.
Background technology
The purge and trap method is a kind of Sample Pretreatment Technique of maturation, because the sample size demand is few, bioaccumulation efficiency is high, matrix disturb little, easily realize the advantage such as on-line monitoring, delivered first in relevant purge and trap chromatography determination water since the volatile organic matter paper from Bellar in 1974 and Lichtenber, be subject to the attention of environmental science and analytical chemistry circle always.U.S. EPA 601,602, wait a plurality of standard methods all to adopt the purge and trap technology to measure all kinds of volatile organic matters in water, and especially along with being widely used of commercialization purge and trap instrument, the effect of Puffing and trapping in analysis technical field is more and more important.
Its principle is constantly to pass through testing sample with continuous inert gas (being generally high pure nitrogen or helium), " purging " out from matrix with volatile constituent, volatile constituent enters drip catcher with air-flow subsequently, contain adsorbent in drip catcher or adopt the method for cryotrap to capture, finally extract is carried out the high temperature desorption analysis, this method almost can all extract volatile organic matter quantitatively, and extraction efficiency is high, by concentration process, sensitivity is improved greatly.
The target compound of this method is volatile organic matter in different liquids or solid matrix.According to the regulation of the World Health Organization (WHO), volatile organic matter is defined as boiling point at the compound of 50 ℃-250 ℃, and under room temperature, saturated vapor pressure surpasses 133.32Pa, at room temperature with vapor form, is present in an airborne type organic.Be defined as temperature when the 293.15K according to the ECDirective1999/13/EC of European Union, vapour pressure is more than or equal to the organic compound of 0.01kpa.According to the EU of European Union " Paint Directive " 2004/42/EC is defined as the compound that boiling point is less than or equal to 250 ℃.
Although the purge and trap disposal route be a kind of not with an organic solvent, do not use quick, the green disposal route of large-scale extraction equipment, but because purge and trap under normal pressure can't purge boiling point to gas phase and capture at the semi-volatile organic matter more than 250 ℃ or involatile organism from sample, so it can only analyze boiling point at the volatile organic matter below 250 ℃.
Be called semi-volatile organic matter for temperature higher than 260 ℃ of organic compounds lower than 400 ℃, be called the involatile organism higher than the organic compounds of 400 ℃, the organic solvent extraction technology for the present general pre-treating method of this two compounds, this technology is by nonvolatile organic compound in the organic reagent extraction water, as the pre-treating method of liquid-liquid extraction (EPA3510) and Solid-Phase Extraction (EPA3535).
For example the semi-volatile organic matter in EPA 3510 methods employing liquid-liquid extraction method extraction 1L water samples need use the organic reagent of 180mL, and minute three extractions under the soda acid neutrallty condition, then remove moisture with the anhydrous sodium sulfate after curing, blow concentrated extraction solvent to 1mL by Rotary Evaporators or nitrogen again, whole process also needs to use various instruments, glassware and reagent.For another example with the nonvolatile organic compound in Solid-Phase Extraction replacement liquid-liquid extraction technology extraction water sample, advantage is that the use amount of organic reagent reduces, extraction process is also concentration process, but Solid-Phase Extraction need to be through overaging, drip washing, loading, four steps of wash-out, wherein the loading step needs the time longer, and whole process need to be used organic reagent, various device, vessel and more time equally.In sum, for the nonvolatile organic compound in water sample, the characteristics of at present general organic reagent pretreatment technology are to need to use organic reagent, need to use multiple instrument, reagent and analysis vessel, intermediate steps is many, easily introduces and disturbs, need the time long, secondary pollution is arranged.
Summary of the invention
The objective of the invention is for the deficiencies in the prior art, and provide decompression purge and trap treating apparatus and the disposal route thereof of nonvolatile organic compound in a kind of analysis water-like, be characterized in not using organic reagent, do not use large-scale pre-treatment instrument, the purge and trap method that automaticity is high is applied to the analysis of the nonvolatile organic compound in sample, the abstraction technique of abandoning tradition organic solvent.
Purpose of the present invention realizes by following technical measures, and wherein said raw material umber except specified otherwise, is the repetition umber.
In water sample, the decompression purge and trap treating apparatus of nonvolatile organic compound is connected to form by sample heating device, purging bottle, drip catcher, pressure controller and pump successively; Purge gas is connected with the purging bottle by the purge gas entrance, purges bottle and exports with drip catcher and be connected by purge gas, and drip catcher is connected with pump by pressure controller.
Take out the well heater of putting into drip catcher after the drip catcher captured gas, the chromatogram carrier gas is connected with the chromatogram injection port in column oven by transfer line after resolving object by drip catcher, and the chromatogram injection port is connected with chromatographic detector by chromatographic column.
The decompression purge and trap disposal route of nonvolatile organic compound in water sample comprises the following steps:
The purging bottle that (a) sample will be housed is put into sample heating device.
(b) drip catcher, pressure controller, pump, purge gas inlet and purge gas are connected successively and connect, and keep airtight without leaking.
(c) sample is heated to 40 ℃～100 ℃, drip catcher remains on room temperature.
(d) open pump and keep to purge range of negative pressure in bottle at 3kpa～95kpa, preferred 5kpa～90kpa, preferred 20kpa～60kpa purge gas enters the sample of sample purging bottle from the purge gas entrance again, enters drip catcher by purge gas after sample steam is taken out of and captures.
(e) drip catcher after captured gas is moved in rapid heater, 260 ℃～450 ℃ of temperature, preferred 300 ℃～400 ℃, the chromatogram carrier gas resolves the target compound in drip catcher get off, enter chromatographic column through transfer line by the chromatogram injection port in column oven and separate, then by the chromatographic detector analysis.
The present invention compares with traditional solid phase micro-extraction method with traditional purge and trap method, traditional organic reagent extracting process, has following beneficial effect:
1., expand the range of application of purge and trap, contained the analysis of volatile organic matter and nonvolatile organic compound.
2. can realize that zero of organic solvent uses, and does not produce secondary pollution.
3. do not use large-scale process instrumentation, manual operations is few, introduces the possibility of disturbing little.
4. treatment step is simple, and the cycle is short, easily realizes robotization.
Under different negative pressure in enriched sample the process of different vapour pressure components be an extraction and the combined process that purifies, both unite two into one, and are simple and convenient.
6. purge by decompression half volatilization and the involatile organism that is gaseous state under different negative pressure state in enriched sample, also extracted the analysis in a step after a lot of impurity (as macromolecular protein, sugar, soil ulmin, fat etc.) impact when having avoided traditional solid-phase microextraction directly extracting head to be put into sample extracting, because impurity disturbs and the factor such as matrix effect makes the qualitative, quantitative of sample inaccurate.
Description of drawings
The present invention is further described below in conjunction with drawings and Examples.
Fig. 1 is the reduce pressure principle schematic of purge and trap of the present invention.
Fig. 2 is to be that schematic diagram is analysed in the pyrolysis of drip catcher of the present invention.
1. sample heating device, 2. purge bottle, 3. drip catcher, 4. pressure controller, 5. pump, 6. purge gas, 7. purge gas entrance, 8. purge gas outlet, 9. chromatographic detector, 10. chromatographic column, 11. column oven, 12. chromatogram injection ports, the well heater of 13. drip catchers, 14. chromatogram carrier gas, 15. transfer lines
Embodiment
Below by embodiment, the present invention is specifically described; be necessary to be pointed out that at this present embodiment only is used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make some nonessential improvement and adjustment according to foregoing.
Measure acenaphthylene content in water as example take the decompression purge and trap:
In water sample, the decompression purge and trap treating apparatus of nonvolatile organic compound is connected to form by sample heating device 1, purging bottle 2, drip catcher 3, pressure controller 4 and pump 5 successively, purge gas 6 is connected with purging bottle 2 by purge gas entrance 7, the purging bottle exports 8 by purge gas and is connected with drip catcher 3, and drip catcher 3 is connected with pump 5 by pressure controller 4.
Take out the well heater 13 of putting into drip catcher after drip catcher 3 captured gas, chromatogram carrier gas 14 is connected with the chromatogram injection port 12 in column oven 11 by transfer line 15 after resolving object by drip catcher 3, and the chromatogram injection port is connected with chromatographic detector 9 by chromatographic column 10.
The decompression purge and trap disposal route of acenaphthylene in water sample:
1, standard solution preparation
(1) compound concentration is the acenaphthylene mixed standard solution of 0.2 μ g/L, 2.0 μ g/L, 20.0 μ g/L and 200.0 μ g/L, and the acenaphthylene boiling point is 275 ℃, and vapour pressure is 1.3 * 10
-4～1.3 * 10
-3Between kpa.
(2) above-mentioned standard is respectively got 10mL water and be added in 20mL head space bottle, and the sealing top empty bottle.
2, gas circuit connects
Head space bottle, drip catcher, pressure controller, pump, purge gas pipeline after sample heating device, sealing are connected shown in successively.
3, purge and trap method
The sample heating-up temperature is made as 40 ℃, by pump and pressure controller, the pressure of whole closed system is controlled at 90kpa, material for trapping adopts polyacrylate (PA) the solid-phase microextraction pin of 85 μ m thickness, the drip catcher temperature is room temperature, decompression purge gas flow 1L/min, purge and trap time 30min, 300 ℃ of resolution temperatures, resolve time 10min.
4, instrumental analysis condition
Agilent6890N-5973i type gas chromatograph-mass spectrometer, DB-5MS chromatographic column (30m*0.25mm*250 μ m), carrier gas is helium (purity 99.999%), flow rate of carrier gas 1.2mL/min, 300 ℃ of injector temperatures, 320 ℃ of makings interface temperature, heating schedule is 80 ℃ of (2min)-8 ℃/min-320 ℃ (10min), 280 ℃ of ion source temperatures, 150 ℃ of quadrupole rod temperature.
5, sample analysis
Analyze as stated above the acenaphthylene in certain water sample, and carry out simultaneously mark-on and reclaim analysis, the concentration after mark-on is 20 μ g/L.
6, experimental result
The typical curve of acenaphthylene is Y=758277X, and related coefficient is 0.994, detects and is limited to 0.01 μ g/L, detects without acenaphthylene in water sample, and recovery of standard addition is 82.34%.
Embodiment 2
Adopt the device of embodiment 1, analyze benzo in certain water sample [a] anthracene, bend, the method for benzo [a] pyrene, benzo [b] fluoranthene:
1, standard solution preparation
(1) compound concentration is the mixed standard solution of above-mentioned four kinds of palycyclic aromatics of 0.01 μ g/L, 0.1 μ g/L, 1.0 μ g/L, 10.0 μ g/L, and wherein the normal concentration of benzo [b] fluoranthene is for being respectively 0.02 μ g/L, 0.2 μ g/L, 2.0 μ g/L, 20.0 its character of μ g/L in Table 1.
(2) above-mentioned standard is got 10mL water and be added in 20mL head space bottle, and the sealing top empty bottle.
2, gas circuit connects
With embodiment 1.
3, purge and trap method
The sample heating-up temperature is made as 80 ℃, by pump and pressure controller, the pressure of whole closed system is controlled at 20kpa, material for trapping adopts polyacrylate (PA) the solid-phase microextraction pin of 85 μ m thickness, the drip catcher temperature is room temperature, decompression purge gas flow 1L/min, purge and trap time 30min, 340 ℃ of resolution temperatures, resolve time 10min.
4, instrumental analysis condition
Agilent6890N-5973i type gas chromatograph-mass spectrometer, DB-5MS chromatographic column (30m*0.25mm*250 μ m), carrier gas is helium (purity 99.999%), flow rate of carrier gas 1.2mL/min, 340 ℃ of injector temperatures, 320 ℃ of makings interface temperature, heating schedule is 80 ℃ of (2min)-8 ℃/min-320 ℃ (10min), 280 ℃ of ion source temperatures, 150 ℃ of quadrupole rod temperature.
5, experimental result
The experimental result of the decompression purge and trap of four kinds of palycyclic aromatics is in Table 1.Related coefficient is all greater than 0.995, and the range of linearity, at 0.01～20 μ g/L, detects without above-mentioned four kinds of palycyclic aromatics in water sample, and the recovery of standard addition scope is between 103.60%～115.86%.
Adopt the device of embodiment 1, benzo in analysis water-like [k] fluoranthene, benzo (g, h, i) perylene, indeno [method of 1,2,3-cd] perylene, dibenzo (a, h) anthracene:
1, standard solution preparation
(1) compound concentration is the mixed standard solution of above-mentioned four kinds of palycyclic aromatics of 0.01 μ g/L, 0.1 μ g/L, 1.0 μ g/L, 10.0 μ g/L, benzo (g wherein, the normal concentration of h, i) perylene is for being respectively 0.02 μ g/L, 0.2 μ g/L, 2.0 μ g/L, 20.0 its character of μ g/L in Table 2.
(2) above-mentioned standard is got 10mL water and be added in 20mL head space bottle, and the sealing top empty bottle.
2, gas circuit connects
With embodiment 1.
3, purge and trap method
The sample heating-up temperature is made as 90 ℃, by pump and pressure controller, the pressure of whole closed system is controlled at 5kpa, material for trapping adopts polyacrylate (PA) the solid-phase microextraction pin of 85 μ m thickness, the drip catcher temperature is room temperature, decompression purge gas flow 1L/min, purge and trap time 30min, 400 ℃ of resolution temperatures, resolve time 10min.
4, instrumental analysis condition
Agilent6890N-5973i type gas chromatograph-mass spectrometer, DB-5MS chromatographic column (30m*0.25mm*250 μ m), carrier gas is helium (purity 99.999%), flow rate of carrier gas 1.2mL/min, 400 ℃ of injector temperatures, 320 ℃ of makings interface temperature, heating schedule is 80 ℃ of (2min)-8 ℃/min-320 ℃ (10min), 280 ℃ of ion source temperatures, 150 ℃ of quadrupole rod temperature.
5, experimental result
The experimental result of the decompression purge and trap of four kinds of palycyclic aromatics is in Table 2.Related coefficient is all greater than 0.992, and the range of linearity, at 0.01～10.0 μ g/L, detects without above-mentioned four kinds of palycyclic aromatics in water sample, and the recovery of standard addition scope is between 64.34%～120.02%.
Table 1 is bent the experimental result that waits four kinds of palycyclic aromatic decompression purge and traps
The experimental result of table 2 palycyclic aromatic decompression purge and trap
Claims (5)
1. the decompression purge and trap disposal route of palycyclic aromatic in a water sample, use the decompression purge and trap device to capture, described decompression purge and trap device is successively by sample heating device (1), purge bottle (2), drip catcher (3), pressure controller (4) and pump (5) connect to form, purge bottle (2) and put into sample heating device (1), purge gas (6) is connected with purging bottle (2) by purge gas entrance (7), the purging bottle exports (8) by purge gas and is connected with drip catcher (3), drip catcher (3) is connected with pump (5) by pressure controller (4), take out the well heater (13) of putting into drip catcher after drip catcher (3) captured gas, chromatogram carrier gas (14) is connected with the chromatogram injection port (12) in column oven (11) by transfer line (15) after resolving object by drip catcher (3), the chromatogram injection port is connected with chromatographic detector (9) by chromatographic column (10), it is characterized in that the method comprises the following steps:
The purging bottle (2) that (a) sample will be housed is put into sample heating device (1);
(b) drip catcher (3), pressure controller (4), pump (5), purge gas inlet (7) are connected (8) with purge gas and connect successively, and keep airtight without leaking;
(c) sample is heated to 40 ℃～100 ℃, drip catcher (3) remains on room temperature;
(d) open pump (5) and keep to purge range of negative pressure in bottle at 3kpa～95kpa, purge gas enters the sample of sample purging bottle (2) from purge gas entrance (7), export (8) by purge gas after sample steam is taken out of and enter drip catcher (3) and capture, polyacrylate (PA) the solid-phase microextraction pin of material for trapping employing 85 μ m thickness;
(e) drip catcher after captured gas is moved in rapid heater (13), 260 ℃～450 ℃ of temperature, chromatogram carrier gas (14) resolves the target compound in drip catcher (3) get off, enter chromatographic column (10) through transfer line (15) by the chromatogram injection port (12) in column oven (11) and separate, then by chromatographic detector (9), analyze.
2. the decompression purge and trap disposal route of palycyclic aromatic in water sample as claimed in claim 1, is characterized in that 40～90 ℃ of sample heating-up temperatures.
3. the decompression purge and trap disposal route of palycyclic aromatic in water sample as claimed in claim 1, is characterized in that the sample range of negative pressure is at 5kpa～90kpa.
4. the decompression purge and trap disposal route of palycyclic aromatic in water sample as claimed in claim 1, is characterized in that the sample range of negative pressure is at 20kpa～60kpa.
5. the decompression purge and trap disposal route of palycyclic aromatic in water sample as claimed in claim 1, is characterized in that the resolution temperature scope is at 300 ℃～400 ℃.
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