CN104062368B - The steam head space enrichment detecting method of Determination of Trace Volatile organic contaminant in a kind of seawater - Google Patents
The steam head space enrichment detecting method of Determination of Trace Volatile organic contaminant in a kind of seawater Download PDFInfo
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Abstract
The present invention relates to a kind of headspace gas chromatography detection technique, specifically the steam head space enrichment detecting method of Determination of Trace Volatile organic contaminant in a kind of seawater, belongs to water environment detection technique field.The method comprise successively 1. water sampling and preservation, 2. first time enrichment condensation, 3. second time enrichment condensation and 4. headspace gas chromatography detect four steps, the present invention take water vapor as sweep gas, simultaneously using water as absorbing agent, water sample is through second distillation condensation, the sample that enrichment is concentrated, detects in order to headspace gas chromatography.The present invention adopts the method for steam head space enrichment, effectively reduces the organic solvent use amount in enriching seawater in volatile organic contaminant process, prevents other compositions to the interference of object.Enrichment method leaching process of the present invention is easy, and do not introduce other solvents, environmental protection, detection limit is low, and the recovery is high, and reappearance is better, can meet Determination of Trace Volatile organic contaminant testing requirement in seawater.
Description
Technical field
The present invention relates to a kind of headspace gas chromatography detection technique, specifically the steam head space enrichment detecting method of Determination of Trace Volatile organic contaminant in a kind of seawater, belongs to water environment detection technique field.
Background technology
In recent years, along with the progressively raising of analytical technology, the detection of volatile organic trace compounds is more and more subject to the attention of analysis science man.For the analysis of trace VOCs, pretreatment technology is very crucial.Pre-treating method mainly comprises liquid-liquid extraction (LLE), direct aqueous injection (DAI), Solid-Phase Extraction (SPE), solid-phase microextraction (SPME), membrane extraction (ME), headspace technique (HS) etc.Direct aqueous injection technology is only applicable to relatively cleaner, and organic less water sample, needs to fill guard column between injection port and chromatographic column, larger by water sample matrix interference.Solid-phase microextraction (SPME) extracting head easy damaged, poor reproducibility, the extraction selectivity of object is single.Headspace extraction method is compared with the pre-treating method such as liquid-liquid extraction method, solid-liquid extraction, have and can avoid causing when desolventizing the loss of volatile matter in sample, reduce non-volatile matter interference and volatile component and reduce the advantages such as noise that extract altogether causes in single-minded collection sample, thus make the analysis of the VOCs of trace in sample have higher sensitivity and analysis speed faster.Puffing and trapping (P & T) belongs to the one of Dynamic headspace, is VOCs enrichment method in the comparatively effective water of generally acknowledging at present.By P & t-gc-ms quantitative limit can reach 0.01 μ g/L, does not introduce solvent, matrix interference is little in analytic process.Although its quantitative limit reaches reduced levels, the trace compound obtained by the method is difficult to the requirement meeting qualitative recognition usually, and this just needs enrichment water sample being carried out to higher multiple.Puffing and trapping easily produces steam interference when purging, operate more complicated, and equipment price is expensive, analysis cost is higher.Static Headspace extraction has particular advantages in volatile organic matter analysis in water, as sample direct injected does not need pre-treatment, use toxic organic solvents few, method is quick, easy, highly sensitive, analysis time is short, but the subject matter existed to remain detection limit higher.We also utilize eight kinds of benzene homologues in automatic Headspace Gas Chromatography seawater, detection is limited to 2 μ g/L, when actual marine site seawater sample is analyzed, all do not detect benzene homologues, detect level like this, need the enrichment of water sample with bulk mass, the detection demand of ultratrace pollutant in seawater could be met.
In current water body, the research of VOCs mainly lays particular emphasis on fresh water aspect, and the research as VOCs in seawater is relatively less, and along with coming into operation in a large number of coastal industrial chemicals base, coastal ocean Environmental security is increasingly sharpened for the demand of the quick Simultaneously test of multiple VOCs.Therefore, be badly in need of a kind of fast and accurately to the enrichment detecting method of Determination of Trace Volatile organic contaminant in water sample.
Summary of the invention
The present invention overcomes the deficiency of existing analytical approach, provides the steam head space enrichment detecting method of Determination of Trace Volatile organic contaminant in a kind of seawater fast and accurately, to realize the quantitative and qualitative determination of Determination of Trace Volatile organic contaminant in water sample.
The technical solution adopted for the present invention to solve the technical problems is:
A steam head space enrichment detecting method for Determination of Trace Volatile organic contaminant in seawater, the method comprise successively 1. water sampling and preservation, 2. first time enrichment condensation, 3. second time enrichment condensation and 4. headspace gas chromatography detect four steps, wherein
1. water sampling and preservation: water sample is preserved in brown ground glass stoppered bottle, and with tetrafluoroethene sealing, be placed with after sample collection in the insulation can of ice bag and deposit, take back the water sample storeroom putting into 4 DEG C in laboratory and deposit, in 7d, complete detection;
2. first time enrichment condensation: 1L sample adds in sample evaporation bottle, sample is heated and steam distillation, volatile constituent is discharged together with water vapor simultaneously, then condensation is carried out, redistilled water is placed in advance as absorbing agent in sample evaporation bottle, reclaim condensed fluid to double evaporation-cooling bottle, stop time within the scope of liquid to be condensed to 120-150mL collecting;
3. second time enrichment condensation: the condensed fluid that above-mentioned steps is collected is through heating and steam distillation, volatile constituent is discharged together with water vapor simultaneously, condensation, place redistilled water in receiving bottle in advance to seal as absorbing agent, finally in receiving bottle, collect condensed fluid within the scope of 8-10mL, after temperature return to room temperature, carry out head space gas chromatography;
4. headspace gas chromatography detects: the 10mL water sample collected after getting time condensation, in the ml headspace bottle of 20mL specification, adds 2.00g sodium chloride, by head space bottle cap sealing; Vortex oscillation dissolves sodium chloride, within the scope of equilibrium temperature to 40 DEG C-60 DEG C, and equilibration time 30min, headspace gas chromatography sample introduction, sampling volume 800 μ L; Detect according to the gas chromatography set-electron capture detection conditioned disjunction gas chromatography-hydrogen flameionization testing conditions, qualitative with retention time, quantified by external standard method.The present invention take water vapor as sweep gas, and simultaneously using water as absorbing agent, water sample is through second distillation condensation, and the sample that enrichment is concentrated, detects in order to headspace gas chromatography.The present invention adopts the method for steam head space enrichment, effectively reduces the organic solvent use amount in enriching seawater in volatile organic contaminant process, prevents other compositions to the interference of object.Enrichment method leaching process of the present invention is easy, and do not introduce other solvents, environmental protection, detection limit is low, and the recovery is high, and reappearance is better, can meet Determination of Trace Volatile organic contaminant testing requirement in seawater.
As preferably, the gathering-device that first time enrichment condensation adopts with second time enrichment condensation mainly comprises the sample evaporation bottle, double evaporation-cooling bottle and the receiving bottle that are connected successively, the top of described sample evaporation bottle connects straight cold finger by bend pipe, and the other end of this straight cold finger is connected with a serpentine condenser vertically placed; The top of double evaporation-cooling bottle is connected with the collector tube with T-valve function, the liquid outlet of serpentine condenser is connected with the feed liquor interface of collector tube, the gas branch pipe that goes out of collector tube is connected with the second straight cold finger, the other end of the second straight cold finger is connected with the second serpentine condenser, the liquid outlet of the second serpentine condenser by tubes connection to the bottom of receiving bottle.Adopt this gathering-device, concentration effect is good, simple to operate, time saving and energy saving.
As preferably, described collector tube is the straight tube that top has glass stopper, side is provided with out gas branch pipe, the side, top of collector tube is provided with feed liquor interface, collector tube feed liquor interface with go out to be provided with between gas branch pipe one by rotating the glass knob controlling to be communicated with, the part that collector tube is positioned at below glass knob is made up of outer tube and the long duct two parts being located at outer tube inside, outer tube is connected with the top of long duct, long duct is communicated with collector tube top, and outer tube and collector tube closed upper part, the described gas branch pipe that goes out is arranged on outer tube.
As preferably, the bottom of sample evaporation bottle and double evaporation-cooling bottle is respectively equipped with heating arrangement.
The present invention establishes a kind of method that novel Dynamic headspace enrichment based on gaseous extraction detects Determination of Trace Volatile organic contaminant in seawater, the method is using water vapor as purge gas, add adsorbent as absorbing medium simultaneously, namely improve concentration effect, at utmost reduce again the interference that additional substance may bring.The aqueous solution that in condenser pipe stream, condensation is got off plays the effect of enrichment VOCs, meanwhile, in receiving bottle, uses absorbing agent, avoids the passage of VOCs to greatest extent.This system is applied in the compartment analysis of the headspace GC of ultratrace volatile organic contaminant in seawater further, there is analysis speed fast, highly sensitive, reagent consumes low, the advantages such as universality is strong, improve 1-2 the order of magnitude than the detection limit of direct headspace GC, thus obtain the information of abundanter, reliable trace constituent.
Beneficial effect of the present invention: second distillation condensation enrichment process of the present invention, concentration effect is good, simple to operate; Adopt water as the absorbing agent of volatile constituent, concentration effect is good, significantly reduces the interference of other impurity to enriched composition; Employing headspace gas chromatography detects, and has higher sensitivity and degree of accuracy; Compared with existing measuring technology, the present invention is detecting the gas chromatography-mass spectrum or miscellaneous equipment that do not need costliness in extra large trace organic pollutant in water, and method can carry out qualitative and quantitative measurement simultaneously, and operation is simple, consuming cost is low, can express-analysis sea trace organic pollutant in water.
Accompanying drawing explanation
Fig. 1 is the main TV structure schematic diagram of the gathering-device of Determination of Trace Volatile organic contaminant in steam head space enriching seawater of the present invention;
Fig. 2 is the structural representation of collector tube of the present invention;
In figure: 1, sample evaporation bottle, 2, straight cold finger, 3, serpentine condenser, 4, collector tube, 41, glass stopper, 42, feed liquor interface, 43, glass knob, 44, long duct, 45, go out gas branch pipe, 46, outer tube, 5, double evaporation-cooling bottle, 6, the second straight cold finger, the 7, second serpentine condenser, 8, receiving bottle.
Embodiment
Below by specific embodiment, and by reference to the accompanying drawings, technical scheme of the present invention is described in further detail.Should be appreciated that enforcement of the present invention is not limited to the following examples, any pro forma accommodation make the present invention and/or change all will fall into scope.
In the present invention, if not refer in particular to, all parts, number percent are unit of weight, and the equipment adopted and raw material etc. all can be buied from market or this area is conventional.Method in following embodiment, if no special instructions, is the conventional method of this area.
The gathering-device of Determination of Trace Volatile organic contaminant in a kind of steam head space enriching seawater as depicted in figs. 1 and 2, this device mainly comprises the sample evaporation bottle 1, double evaporation-cooling bottle 5 and the receiving bottle 8 that connect successively, the top of described sample evaporation bottle connects straight cold finger 2 by bend pipe, and the other end of this straight cold finger is connected with a serpentine condenser 3 vertically placed; The top of double evaporation-cooling bottle is connected with the collector tube 4 with T-valve function, the liquid outlet of serpentine condenser is connected with the feed liquor interface of collector tube, the gas branch pipe that goes out of collector tube is connected with the second straight cold finger 6, the other end of the second straight cold finger is connected with the second serpentine condenser 7, the liquid outlet of the second serpentine condenser by tubes connection to the bottom of receiving bottle 8.The bottom of sample evaporation bottle and double evaporation-cooling bottle is respectively equipped with heating arrangement.
Described collector tube is the straight tube that top has glass stopper 41, side is provided with out gas branch pipe 45, the side, top of collector tube is provided with feed liquor interface 42, collector tube feed liquor interface with go out to be provided with between gas branch pipe one by rotating the glass knob 43 controlling to be communicated with, the part that collector tube is positioned at below glass knob is made up of outer tube 46 and long duct 44 two parts being located at outer tube inside, outer tube is connected with the top of long duct, long duct is communicated with collector tube top, and outer tube and collector tube closed upper part, the described gas branch pipe that goes out is arranged on outer tube.The lower end of outer tube is connected with double evaporation-cooling bottle.The special construction of collector tube, make device of the present invention can realize the quick of volatile organic contaminant without the need to operation bidirectional, effective enrichment, by controlling to the rotation of glass knob the time shortening double evaporation-cooling liquid collecting, be specially: when glass knob forwards the position that long duct is communicated with collector tube top to, the liquid entered by feed liquor interface 42 enters the bottom of double evaporation-cooling bottle by long duct, when liquid collection is complete, shut glass knob, make long duct and collector tube closed upper part, then the heating arrangement bottom double evaporation-cooling bottle is opened, make steam through outer tube and enter the second straight cold finger 6 carry out time condensation from going out gas branch pipe 45.
Add sample in sample evaporation bottle, in double evaporation-cooling bottle and receiving bottle, add ultrapure water respectively as absorbing medium.In sample evaporation bottle, sample is through heating and steam distillation, causes VOCs to discharge together with water vapor simultaneously, first through straight cold finger, then through serpentine condenser, through time condensation, opens the piston of collector tube side, reclaims condensed fluid to double evaporation-cooling bottle.After first time, condensation collected, closure piston, has heated double evaporation-cooling bottle, VOCs in double evaporation-cooling bottle is discharged together with water vapor simultaneously, again carries out collecting condensed fluid with aforementioned similar operations, finally in receiving bottle, collect condensed fluid, sealing, to carry out next step detection operation.
In embodiment 1 seawater, the vapor enrichment headspace gas chromatography of trace chlorobenzene class organic contaminant detects
In the device shown in Fig. 1, complete the secondary enrichment condensation process of water sample, concrete method of operating is as follows:
(1) water sampling and preservation: water sample is preserved in brown ground glass stoppered bottle, and with tetrafluoroethene sealing, be placed with after sample collection in the insulation can of ice bag and deposit, take back the water sample storeroom putting into 4 DEG C in laboratory and deposit, in 7d, complete detection;
(2) first time enrichment condensation: 1L water sample adds in sample evaporation bottle (2L flask), water sample is through the heating of 200 DEG C, electric furnace and steam distillation, cause volatile constituent to discharge together with water vapor simultaneously, through condensation, 1ml water is placed in advance as absorbing liquid in double evaporation-cooling bottle (250mL flask), reclaim condensed fluid to double evaporation-cooling bottle, liquid to be condensed stops collecting to 150mL;
(3) second time enrichment condensation: the 150mL condensed fluid that above-mentioned steps is collected is through the heating of 200 DEG C, electric furnace and steam distillation, volatile constituent is discharged together with water vapor simultaneously, through condensation, 1ml water is placed in advance as absorbing liquid in receiving bottle, finally in receiving bottle, collect condensed fluid to 10mL, sealing, carries out head space gas chromatography after temperature return to room temperature;
(4) headspace gas chromatography detects: the 10mL water sample collected after getting time condensation, in the ml headspace bottle of 20mL specification, adds 2.00g sodium chloride, by head space bottle cap sealing; Vortex oscillation dissolves sodium chloride, equilibrium temperature 60 DEG C, equilibration time 30min, headspace gas chromatography sample introduction, sampling volume 800 μ L; Detect according to the gas chromatography set-electron capture detection condition, chromatographic condition is: injector temperature 220 DEG C; Electron capture detector temperature 300 DEG C; Carrier gas is high pure nitrogen, and flow velocity is 1mL/min; Sampling volume is 800 μ L; DB-35 capillary gas chromatographic column heating schedule is: 40 DEG C keep 4min, 10 DEG C/min is warming up to 160 DEG C, keep 1min, 10 DEG C/min is warming up to 220 DEG C, keep 5min, qualitative with retention time, drawing standard working curve, with quantified by external standard method, according to the concentration of calculated by peak area chlorobenzene compound;
(5) Specification Curve of Increasing
Get appropriate chlorobenzene compound standard reserving solution respectively, 1L is diluted to urnormal, obtaining 6 mark-on range of concentrations is dichloro-benzenes 0.016 ~ 0.80 μ g/L, trichloro-benzenes 0.00176 ~ 0.088 μ g/L, tetrachlorobenzene 0.0004 ~ 0.02 μ g/L, the standard working solution of pentachlorobenzene, hexachloro-benzene 0.0001 ~ 0.005 μ g/L, then operates according to the requirement of above-mentioned (2), (3) and (4) step, according to the corresponding relation drawing standard curve of the chlorobenzene compound concentration added and peak area; Adopt external standard method, to record in seawater Chlorobenzens content in 11 and be and do not detect; Mark-on seawater recoveries is at 75-95%, RSD≤15%, and concrete data, in table 1, meet the requirement of analytical approach to the recovery.
The chlorobenzene compound recovery of the different spiked levels of table 1 and Precision Experiment result (n=6)
In embodiment 2 seawater, the vapor enrichment headspace gas chromatography of Determination of Trace Benzene organic contaminant detects
(1) water sampling and preservation: water sample is preserved in brown ground glass stoppered bottle, and with tetrafluoroethene sealing, be placed with after sample collection in the insulation can of ice bag and deposit, take back the water sample storeroom putting into 4 DEG C in laboratory and deposit, in 7d, complete detection;
(2) first time enrichment condensation: 1L water sample adds in 2L sample evaporation bottle, water sample is through the heating of 200 DEG C, electric furnace and steam distillation, cause volatile constituent to discharge and condensation together with water vapor simultaneously, 1ml water is placed in advance as absorbing liquid in double evaporation-cooling bottle (250mL flask), reclaim condensed fluid to double evaporation-cooling bottle, liquid to be condensed stops collecting to 150mL;
(3) second time enrichment condensation: the 150mL condensed fluid that above-mentioned steps is collected is through the heating of 200 DEG C, electric furnace and steam distillation, volatile constituent is discharged together with water vapor simultaneously, condensation, receiving bottle places 1ml water in advance as absorbing liquid, finally in receiving bottle, collect condensed fluid to 10mL, sealing, to be restoredly carries out head space gas chromatography to room temperature;
(4) headspace gas chromatography detects: the 10mL water sample collected after getting time condensation, in the ml headspace bottle of 20mL specification, adds 2.00g sodium chloride, by head space bottle cap sealing; Vortex oscillation dissolves sodium chloride, equilibrium temperature 40 DEG C, equilibration time 30min, headspace gas chromatography sample introduction, sampling volume 800 μ L; Detect according to the gas chromatography set-hydrogen flameionization testing conditions, chromatographic condition is: injector temperature 180 DEG C; Flame ionization ditector temperature 200 DEG C; Carrier gas is high pure nitrogen, and flow velocity is 1mL/min; Sampling volume is 800 μ L; Nukol capillary gas chromatographic column heating schedule is: 40 DEG C keep 4min, and 3 DEG C/min is warming up to 120 DEG C, and keep 5min, qualitative with retention time, drawing standard working curve, with quantified by external standard method, according to the concentration of calculated by peak area benzene homologues;
(5) Specification Curve of Increasing
Get appropriate benzene homologues standard reserving solution respectively, 1L is diluted to urnormal, obtaining 6 mark-on range of concentrations is benzene homologues 1.0 ~ 20 μ g/L, standard working solution, then operate according to the requirement of above-mentioned (2), (3) and (4) step, according to the corresponding relation drawing standard curve of the benzene homologues compound concentration added and peak area; Adopt external standard method, to record in seawater benzene homologues content in 6 and be and do not detect; Mark-on seawater recoveries is at 75-95%, RSD≤15%, and concrete data, in table 2, meet the requirement of analytical approach to the recovery.
The benzene homologues recovery of the different spiked levels of table 2 and Precision Experiment result (n=6)
Above-described embodiment is to explanation of the present invention, is not limitation of the invention, anyly all belongs to protection scope of the present invention to the scheme after simple transformation of the present invention.
Claims (2)
1. the steam head space enrichment detecting method of Determination of Trace Volatile organic contaminant in a seawater, it is characterized in that: the method comprise successively 1. water sampling and preservation, 2. first time enrichment condensation, 3. second time enrichment condensation and 4. headspace gas chromatography detect four steps, wherein
1. water sampling and preservation: water sample is preserved in brown ground glass stoppered bottle, and with tetrafluoroethene sealing, be placed with after sample collection in the insulation can of ice bag and deposit, take back the water sample storeroom putting into 4 DEG C in laboratory and deposit, in 7d, complete detection;
2. first time enrichment condensation: 1L sample adds in sample evaporation bottle, sample is heated and steam distillation, volatile constituent is discharged together with water vapor simultaneously, then condensation is carried out, redistilled water is placed in advance as absorbing agent in sample evaporation bottle, reclaim condensed fluid to double evaporation-cooling bottle, stop time within the scope of liquid to be condensed to 120-150mL collecting;
3. second time enrichment condensation: the condensed fluid that above-mentioned steps is collected is through heating and steam distillation, volatile constituent is discharged together with water vapor simultaneously, condensation, place redistilled water in receiving bottle in advance to seal as absorbing agent, finally in receiving bottle, collect condensed fluid within the scope of 8-10mL, after temperature return to room temperature, carry out head space gas chromatography;
4. headspace gas chromatography detects: the 10mL water sample collected after getting time condensation, in the ml headspace bottle of 20mL specification, adds 2.00g sodium chloride, by head space bottle cap sealing; Vortex oscillation dissolves sodium chloride, within the scope of equilibrium temperature to 40 DEG C-60 DEG C, and equilibration time 30min, headspace gas chromatography sample introduction, sampling volume 800 μ L; Detect according to the gas chromatography set-electron capture detection conditioned disjunction gas chromatography-hydrogen flameionization testing conditions, qualitative with retention time, quantified by external standard method;
The gathering-device that first time enrichment condensation adopts with second time enrichment condensation mainly comprises the sample evaporation bottle, double evaporation-cooling bottle and the receiving bottle that are connected successively, the top of described sample evaporation bottle connects straight cold finger by bend pipe, and the other end of this straight cold finger is connected with a serpentine condenser vertically placed; The top of double evaporation-cooling bottle is connected with the collector tube with T-valve function, the liquid outlet of serpentine condenser is connected with the feed liquor interface of collector tube, the gas branch pipe that goes out of collector tube is connected with the second straight cold finger, the other end of the second straight cold finger is connected with the second serpentine condenser, the liquid outlet of the second serpentine condenser by tubes connection to the bottom of receiving bottle; Described collector tube is the straight tube that top has glass stopper, side is provided with out gas branch pipe, the side, top of collector tube is provided with feed liquor interface, collector tube feed liquor interface with go out to be provided with between gas branch pipe one by rotating the glass knob controlling to be communicated with, the part that collector tube is positioned at below glass knob is made up of outer tube and the long duct two parts being located at outer tube inside, outer tube is connected with the top of long duct, long duct is communicated with collector tube top, and outer tube and collector tube closed upper part, the described gas branch pipe that goes out is arranged on outer tube.
2. enrichment detecting method according to claim 1, is characterized in that: the bottom of sample evaporation bottle and double evaporation-cooling bottle is respectively equipped with heating arrangement.
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| CN107192786B (en) * | 2017-07-04 | 2018-05-11 | 国家地质实验测试中心 | The enrichment preparation facilities and its method of gas in a kind of water body |
| CN107817220B (en) * | 2017-11-29 | 2020-11-24 | 长春黄金研究院有限公司 | Method for measuring mass concentration of easily released cyanide in thiocyanate-containing water |
| CN109253897B (en) * | 2018-09-18 | 2020-11-17 | 浙江海洋大学 | On-line monitoring device for emerging marine pollutants |
| CN109459544A (en) * | 2018-09-20 | 2019-03-12 | 北京雪迪龙科技股份有限公司 | The system and method for volatile organic matter in a kind of on-line monitoring water |
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| CN109813819A (en) * | 2019-01-30 | 2019-05-28 | 中国科学院地质与地球物理研究所兰州油气资源研究中心 | A kind of micro volatile organic compounds enrichment and sampling device |
| CN113466319A (en) * | 2021-07-29 | 2021-10-01 | 力合科技（湖南）股份有限公司 | System for monitoring trace thallium in water, using method and method for detecting trace thallium in water |
| CN115184511B (en) * | 2022-08-25 | 2023-09-19 | 宜宾五粮液股份有限公司 | Method for in-situ determination of volatile phenolic substances in white spirit |
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