CN101949906A - 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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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 the 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 branch technical field.
Background technology
The purge and trap method is a kind of sample pre-treatments technology of maturation, few because of the sample size demand, bioaccumulation efficiency is high, matrix disturb little, realize online monitoring and other advantages easily, delivered first in the relevant purge and trap chromatography determination water since the volatile organic matter paper from Bellar in 1974 and Lichtenber, be subjected to the attention of environmental science and analytical chemistry circle always.U.S. EPA 601,602 waits a plurality of standard methods all kinds of volatile organic matters in the water that all adopted the purge and trap technical measurement, and especially along with being extensive use of of commercialization purge and trap instrument, the effect of purge and trap method 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), volatile constituent " purging " from matrix is come out, volatile constituent enters drip catcher with air-flow subsequently, contain adsorbent in the drip catcher or adopt the method for cryotrap to capture, at last extract is carried out the high temperature desorption analysis, this method almost can all extract volatile organic matter quantitatively, and the extraction efficiency height improves sensitivity by concentration process greatly.
The target compound of this method is a volatile organic matter in different liquids or the solid matrix.According to the regulation of the World Health Organization (WHO), volatile organic matter is defined as boiling point at 50 ℃-250 ℃ compound, and saturated vapor pressure surpasses 133.32Pa under the room temperature, at room temperature is present in an airborne type organic with vapor form.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 ℃.
Though 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 can't purge boiling point to gas phase and capture at semi-volatile organic matter more than 250 ℃ or involatile organism under the normal pressure from sample, so it can only analyze boiling point at the volatile organic matter below 250 ℃.
Be higher than 260 ℃ of organic compounds that are lower than 400 ℃ for temperature and be called semi-volatile organic matter, the organic compound that is higher than 400 ℃ is called the involatile organism, for the present general pre-treating method of this two compounds is the organic solvent extraction technology, 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 the EPA 3510 methods employing liquid-liquid extraction method extraction 1L water sample need use the organic reagent of 180mL, and three extractions of branch under the soda acid neutrallty condition, remove moisture with the anhydrous sodium sulfate after curing then, 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 the Solid-Phase Extraction replacement liquid-liquid extraction technology extraction water sample, advantage is that the use amount of organic reagent reduces, extraction process also is a concentration process, but Solid-Phase Extraction need be through overaging, drip washing, last sample, four steps of wash-out, wherein going up the sample step needs the time longer, and whole process need be used organic reagent, various device, vessel and more time equally.In sum, for the nonvolatile organic compound in the 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, introduces easily and disturbs, need the time long, secondary pollution is arranged.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, and provide the 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 the sample, the abstraction technique of abandoning tradition organic solvent.
Purpose of the present invention is realized that by following technical measures wherein said raw material umber is the repetition umber except that specified otherwise.
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 in the water sample; Purge gas is connected with the purging bottle by the purge gas inlet, purges bottle and is connected with drip catcher by the purge gas outlet, and drip catcher is connected with pump by pressure controller.
Take out the well heater put into drip catcher after the drip catcher captured gas, the chromatogram carrier gas is resolved behind the object by transfer line by drip catcher and is connected with chromatogram injection port in the column oven, 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 the water sample may further comprise the steps:
(a) the purging bottle that sample will be housed is put into sample heating device.
(b) outlet is connected successively with purge gas with drip catcher, pressure controller, pump, purge gas inlet, and keeps airtight nothing to leak.
(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 the bottle at 3kpa～95kpa, preferred 5kpa～90kpa, preferred again 20kpa～60kpa purge gas enters the sample of sample purging bottle from the purge gas inlet, enters drip catcher by purge gas after sample steam is taken out of and captures.
(e) drip catcher after the captured gas is moved in the rapid heater, 260 ℃～450 ℃ of temperature, preferred 300 ℃～400 ℃, the chromatogram carrier gas resolves the target compound in the drip catcher get off, enter chromatographic column through transfer line by the chromatogram injection port in the 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, and it is little to introduce the possibility of disturbing.
4. treatment step is simple, and the cycle is short, realizes robotization easily.
Under different negative pressure in the enriched sample 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 half volatilization and the involatile organism that under different negative pressure state, is gaseous state in the enriched sample by decompression, also extracted a lot of impurity (as macromolecular protein, sugar, soil ulmin, fat etc.) influence analysis in one step of back when having avoided traditional solid-phase microextraction directly extracting head to be put into sample extracting, because impurity disturbs and 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 synoptic diagram is analysed in the pyrolysis of drip catcher of the present invention.
1. sample heating device 2. purges bottle, 3. drip catcher, 4. pressure controller, 5. pump, 6. purge gas, 7. purge gas inlet, 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 carried out concrete description; be necessary to be pointed out that at this present embodiment only is used for the present invention is further specified; 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.
The acenaphthylene content of measuring in the water with the decompression purge and trap is example:
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 in the water sample, purge gas 6 is connected with purging bottle 2 by purge gas inlet 7, purge bottle and be connected with drip catcher 3 by purge gas outlet 8, drip catcher 3 passes through pressure controller 4 and is connected with pump 5.
Take out the well heater 13 of putting into drip catcher after drip catcher 3 captured gas, chromatogram carrier gas 14 is resolved behind the objects by transfer line 15 by drip catcher 3 and is connected with chromatogram injection port 12 in the column oven 11, and the chromatogram injection port passes through chromatographic column 10 and is connected with chromatographic detector 9.
The decompression purge and trap disposal route of acenaphthylene in the 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 the kpa.
(2) above-mentioned standard is respectively got 10mL water and be added in the 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 arrangement, the 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 with the pressure control of whole closed system at 90kpa, material for trapping adopts polyacrylate (PA) the solid-phase microextraction pin of 85 μ m thickness, the drip catcher temperature is a room temperature, decompression purge gas flow 1L/min, purge and trap time 30min, 300 ℃ of resolution temperatures are resolved 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 the acenaphthylene in certain water sample as stated above, and carry out mark-on simultaneously and reclaim analysis, the concentration behind the 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 to be limited to 0.01 μ g/L, and no acenaphthylene detects in the 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, wherein the normal concentration of benzo [b] fluoranthene for be respectively 0.02 μ g/L, 0.2 μ g/L, 2.0 μ g/L, 20.0 its character of μ g/L see Table 1.
(2) above-mentioned standard is got 10mL water and be added in the 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 with the pressure control of whole closed system at 20kpa, material for trapping adopts polyacrylate (PA) the solid-phase microextraction pin of 85 μ m thickness, the drip catcher temperature is a room temperature, decompression purge gas flow 1L/min, purge and trap time 30min, 340 ℃ of resolution temperatures are resolved 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 sees Table 1.The facies relationship number average is greater than 0.995, and the range of linearity is at 0.01～20 μ g/L, and no above-mentioned four kinds of palycyclic aromatics detect in the water sample, and the recovery of standard addition scope is between 103.60%～115.86%.
Adopt the device of embodiment 1, benzo in the analysis water-like [k] fluoranthene, benzo (g, h, i) perylene, indeno [1,2,3-cd] perylene, dibenzo (a, h) method of 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, h, i) the normal concentration of perylene for be respectively 0.02 μ g/L, 0.2 μ g/L, 2.0 μ g/L, 20.0 its character of μ g/L see Table 2.
(2) above-mentioned standard is got 10mL water and be added in the 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 with the pressure control of whole closed system at 5kpa, material for trapping adopts polyacrylate (PA) the solid-phase microextraction pin of 85 μ m thickness, the drip catcher temperature is a room temperature, decompression purge gas flow 1L/min, purge and trap time 30min, 400 ℃ of resolution temperatures are resolved 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 sees Table 2.The facies relationship number average is greater than 0.992, and the range of linearity is at 0.01～10.0 μ g/L, and no above-mentioned four kinds of palycyclic aromatics detect in the 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 (7)
1. the decompression purge and trap treating apparatus of nonvolatile organic compound in the water sample, it is characterized in that this device is connected to form by sample heating device (1), purging bottle (2), a drip catcher (3), pressure controller (4) and pump (5) successively, purge gas (6) is connected with purging bottle (2) by purge gas inlet (7), purge bottle and be connected with drip catcher (3) by purge gas outlet (8), drip catcher (3) is connected with pump (5) by pressure controller (4).
2. the decompression purge and trap treating apparatus of nonvolatile organic compound in the water sample according to claim 1, it is characterized in that taking out the well heater (13) of putting into drip catcher after drip catcher (3) captured gas, chromatogram carrier gas (14) is resolved behind the object by transfer line (15) by drip catcher (3) and is connected with chromatogram injection port (12) in the column oven (11), and the chromatogram injection port passes through chromatographic column (10) and is connected with chromatographic detector (9).
3. as the decompression purge and trap disposal route of nonvolatile organic compound in the water sample as described in claims 1 or 2, it is characterized in that this method may further comprise the steps:
(a) the purging bottle (2) that sample will be housed is put into sample heating device (1);
(b) drip catcher (3), pressure controller (4), pump (5), purge gas inlet (7) and purge gas outlet (8) are connected successively, and keep airtight nothing to leak;
(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 the bottle at 3kpa～95kpa, purge gas enters the sample of sample purging bottle (2) from purge gas inlet (7), enters drip catcher (3) by purge gas outlet (8) after sample steam is taken out of and captures;
(e) drip catcher after the captured gas is moved in the rapid heater (13), 260 ℃～450 ℃ of temperature, chromatogram carrier gas (14) resolves the target compound in the drip catcher (3) get off, enter chromatographic column (10) through transfer line (15) by the chromatogram injection port (12) in the column oven (11) and separate, analyze by chromatographic detector (9) then.
4. as the decompression purge and trap disposal route of nonvolatile organic compound in the water sample as described in claims 3, it is characterized in that 40～90 ℃ of sample heating-up temperatures.
5. as the decompression purge and trap disposal route of nonvolatile organic compound in the water sample as described in claims 3, it is characterized in that the sample range of negative pressure is at 5kpa～90kpa.
6. as the decompression purge and trap disposal route of nonvolatile organic compound in the water sample as described in claims 3, it is characterized in that the sample range of negative pressure is at 20kpa～60kpa.
7. as the decompression purge and trap disposal route of nonvolatile organic compound in the water sample as described in claims 3, it is characterized in that the resolution temperature scope is at 300 ℃～400 ℃.
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