CN104062368A - Vapor headspace enrichment detection method for trace amount of volatile organic pollutants in seawater - Google Patents
Vapor headspace enrichment detection method for trace amount of volatile organic pollutants in seawater Download PDFInfo
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Abstract
The invention relates to a headspace gas chromatography detection technology, particularly discloses a vapor headspace enrichment detection method for a trace amount of volatile organic pollutants in seawater, and belongs to the technical field of water environment detection. The method sequentially comprises the four steps of water sample collection and storage, primary enrichment condensation, secondary enrichment condensation and headspace gas chromatography detection. According to the method, water vapor is used as sweeping gas, water is used as an absorbent, a water sample is secondarily distilled and condensed, and the condensed sample is enriched for headspace gas chromatography detection; a vapor headspace enrichment method is adopted, so that the using amount of an organic solvent in a process of enriching the volatile organic pollutants in the seawater is effectively reduced, and the interference of other components to a target object is prevented; an extraction process of the enrichment method is simple and convenient, the introduction of other solvents is avoided, the method is environment-friendly, low in limit of detection and high in recovery rate and reproducibility, and the requirements of detection of a trace amount of volatile organic pollutants in the seawater can be met.
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 analysis science man's attention.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 cleaner, and organic less water sample need to fill guard column between injection port and chromatographic column, is subject to water sample matrix interference larger.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 desolventizing time, cause volatile matter loss in sample, reduce that non-volatile matter disturbs and volatile component and reduce the advantages such as extract causes altogether noise in single-minded collection sample, thereby make the analysis of the VOCs of trace in sample there is higher sensitivity and analysis speed faster.Puffing and trapping (P & T) belongs to the one of dynamic head space, is VOCs enrichment method in the comparatively effectively 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 has reached reduced levels, the trace compound obtaining by the method is difficult to meet the requirement of qualitative identification conventionally, and this just need to carry out to water sample the enrichment of higher multiple.Puffing and trapping easily produces steam and disturbs in the time purging, operate more complicated, and equipment price costliness, analysis cost is higher.Static Headspace extraction has particular advantages aspect volatile organic matter analysis in water, as sample direct injected does not need pre-treatment, use poisonous organic solvent few, method is quick, easy, highly sensitive, analysis time is short, but that the subject matter existing remains detection limit is higher.We have also utilized automatic Headspace Gas Chromatography eight kinds of benzene homologues in seawater, detection is limited to 2 μ g/L, when actual marine site seawater sample is analyzed, all do not detect benzene homologues, detect like this level, need the enrichment of water sample with bulk mass, could meet the detection demand of ultratrace pollutant in seawater.
In water body, the research of VOCs mainly lays particular emphasis on fresh water aspect at present, relatively less as for the research of VOCs in seawater, and along with coming into operation in a large number of coastal industrial chemicals base, the demand that coastal ocean Environmental security is measured fast for multiple VOCs is simultaneously increasingly sharpened.Therefore, be badly in need of a kind of enrichment detecting method to Determination of Trace Volatile organic contaminant in water sample fast and accurately.
Summary of the invention
The present invention overcomes the deficiency of existing analytical approach, and the steam head space enrichment detecting method of Determination of Trace Volatile organic contaminant in a kind of seawater is fast and accurately provided, 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. enrichment condensation for the first time, 3. enrichment condensation for the second time 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, put into the insulation can of ice bag and deposit after sample collection, takes back laboratory and puts into the water sample storeroom of 4 DEG C and deposit, and completes detection in 7d;
2. enrichment condensation for the first time: 1L sample adds in sample evaporation bottle, sample is heated and steam distillation, volatile constituent is discharged together with water vapor simultaneously, then carry out condensation, in sample evaporation bottle, place in advance redistilled water as absorbing agent, reclaim condensed fluid to double evaporation-cooling bottle, stop collecting until condensed fluid to time within the scope of 120-150mL;
3. enrichment condensation for the second time: 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, in receiving bottle, placing in advance redistilled water seals as absorbing agent, finally in receiving bottle, collect condensed fluid to 8-10mL, after temperature returns to room temperature, carry out head space gas chromatography;
4. headspace gas chromatography detects: get the 10mL water sample of collecting after time condensation in the head space bottle of 20mL specification, add 2.00g sodium chloride, by head space bottle cap sealing; Sodium chloride is dissolved in vortex vibration, 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-electron capture testing conditions setting or gas chromatography-hydrogen flameionization testing conditions, qualitative with retention time, external standard method is quantitative.The present invention is taking 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, has effectively reduced the organic solvent use amount in volatile organic contaminant process in enriching seawater, prevents the interference of other compositions to object.Enrichment method leaching process of the present invention is easy, does not introduce other solvents, environmental protection, and 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, enrichment condensation for the first time mainly comprises with the gathering-device that enrichment condensation for the second time adopts 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 of vertically placing; 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, and the liquid outlet of the second serpentine condenser is connected to the bottom of receiving bottle by conduit.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 and be provided with out gas branch pipe, top one side of collector tube is provided with feed liquor interface, collector tube feed liquor interface with go out between gas branch pipe, to be provided with one and to control the glass knob being communicated with by rotation, the part that collector tube is positioned at below glass knob is made up of outer tube and long duct two parts of being located at outer tube inside, the top of outer tube and long duct is connected, 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 has set up the method for Determination of Trace Volatile organic contaminant in a kind of novel dynamic head space enrichment detection seawater based on gaseous extraction, the method is using water vapor as purge gas, add adsorbent as absorbing medium simultaneously, improve concentration effect, at utmost reduced 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, uses absorbing agent in receiving bottle, has avoided to greatest extent the passage of VOCs.This system is further applied in the compartment analysis of the headspace GC of ultratrace volatile organic contaminant in seawater, 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, thereby obtain information 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 the absorbing agent of water as volatile constituent, concentration effect is good, has effectively reduced 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 does not need expensive gas chromatography-mass spectrum or miscellaneous equipment in the extra large trace organic pollutant in water of detection, and method can be carried out qualitative and quantitative measurement simultaneously, and operation is simple, consuming cost is low, can express-analysis sea trace organic pollutant in water.
Brief description of the drawings
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, 7, the 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 that the present invention is made and/or change all will fall into protection domain of the present invention.
In the present invention, if not refer in particular to, all part, number percents are unit of weight, and equipment and the raw material etc. adopting 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 of vertically placing; 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, and the liquid outlet of the second serpentine condenser is connected to the bottom of receiving bottle 8 by conduit.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 and be provided with out gas branch pipe 45, top one side of collector tube is provided with feed liquor interface 42, collector tube feed liquor interface with go out between gas branch pipe, to be provided with one and to control the glass knob 43 being communicated with by rotation, the part that collector tube is positioned at below glass knob is made up of outer tube 46 and long duct 44 two parts of being located at outer tube inside, the top of outer tube and long duct is connected, 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 operation bidirectional, effectively enrichment, by the rotation of glass knob being controlled to shorten the time of double evaporation-cooling liquid collecting, be specially: glass knob forwards to while making position that long duct is communicated with collector tube top, the liquid being entered by feed liquor interface 42 enters the bottom of double evaporation-cooling bottle by long duct, in the time that liquid collection is complete, close upper glass knob, make long duct and collector tube closed upper part, then open the heating arrangement of double evaporation-cooling bottle bottom, make steam enter the second straight cold finger 6 and carry out time condensation through outer tube and from going out gas branch pipe 45.
In sample evaporation bottle, add sample, in double evaporation-cooling bottle and receiving bottle, add respectively ultrapure water as absorbing medium.In sample evaporation bottle, sample, through heating and steam distillation, causes VOCs to discharge together with water vapor simultaneously, first passes through straight cold finger, then passes through serpentine condenser, through time condensation, opens the piston of collector tube side, reclaims condensed fluid to double evaporation-cooling bottle.After condensation has been collected for the first time, closure piston, heating double evaporation-cooling bottle, VOCs in double evaporation-cooling bottle is discharged together with water vapor simultaneously, again carry 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 steam enrichment headspace gas chromatography of trace chlorobenzene class organic contaminant detects
The secondary enrichment condensation process that completes water sample in the device shown in Fig. 1, 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, put into the insulation can of ice bag and deposit after sample collection, takes back laboratory and puts into the water sample storeroom of 4 DEG C and deposit, and completes detection in 7d;
(2) enrichment condensation for the first time: 1L water sample adds in sample evaporation bottle (2L flask), water sample is through 200 DEG C of heating of electric furnace and steam distillation, cause volatile constituent to discharge together with water vapor simultaneously, through condensation, in double evaporation-cooling bottle (250mL flask), place in advance 1ml water as absorption liquid, reclaim condensed fluid to double evaporation-cooling bottle, treat that condensed fluid stops collecting to 150mL;
(3) enrichment condensation for the second time: the 150mL condensed fluid that above-mentioned steps is collected is through 200 DEG C of heating of electric furnace and steam distillation, volatile constituent is discharged together with water vapor simultaneously, through condensation, in receiving bottle, place in advance 1ml water as absorption liquid, finally in receiving bottle, collect condensed fluid to 10mL, head space gas chromatography is carried out in sealing after temperature returns to room temperature;
(4) headspace gas chromatography detects: get the 10mL water sample of collecting after time condensation in the head space bottle of 20mL specification, add 2.00g sodium chloride, by head space bottle cap sealing; Sodium chloride, 60 DEG C of equilibrium temperatures, equilibration time 30min, headspace gas chromatography sample introduction, sampling volume 800 μ L are dissolved in vortex vibration; Detect according to the gas chromatography-electron capture testing conditions setting, chromatographic condition is: 220 DEG C of injector temperatures; 300 DEG C of electron capture detector temperature; 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 external standard standard measure, according to the concentration of calculated by peak area chlorobenzene compound;
(5) Specification Curve of Increasing
Get respectively appropriate chlorobenzene compound standard reserving solution, be diluted to 1L with urnormal, obtaining 6 mark-on scope concentration 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 operation liquid of pentachlorobenzene, hexachloro-benzene 0.0001～0.005 μ g/L, then operates according to above-mentioned (2), the (3) and (4) requirement of step, according to the corresponding relation drawing standard curve of the chlorobenzene compound concentration adding and peak area; Adopt external standard method, record in seawater in 11 Chlorobenzens content and be and do not detect; The mark-on seawater recovery 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 mark-on concentration of table 1 and Precision Experiment result (n=6)
In embodiment 2 seawater, the steam 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, put into the insulation can of ice bag and deposit after sample collection, takes back laboratory and puts into the water sample storeroom of 4 DEG C and deposit, and completes detection in 7d;
(2) enrichment condensation for the first time: 1L water sample adds in 2L sample evaporation bottle, water sample is through 200 DEG C of heating of electric furnace and steam distillation, cause volatile constituent to discharge and condensation together with water vapor simultaneously, in double evaporation-cooling bottle (250mL flask), place in advance 1ml water as absorption liquid, reclaim condensed fluid to double evaporation-cooling bottle, treat that condensed fluid stops collecting to 150mL;
(3) enrichment condensation for the second time: the 150mL condensed fluid that above-mentioned steps is collected is through 200 DEG C of heating of electric furnace and steam distillation, volatile constituent is discharged together with water vapor simultaneously, condensation, receiving bottle is placed 1ml water in advance as absorption liquid, finally in receiving bottle, collect condensed fluid to 10mL, head space gas chromatography is carried out in sealing after returning to room temperature;
(4) headspace gas chromatography detects: get the 10mL water sample of collecting after time condensation in the head space bottle of 20mL specification, add 2.00g sodium chloride, by head space bottle cap sealing; Sodium chloride, 40 DEG C of equilibrium temperatures, equilibration time 30min, headspace gas chromatography sample introduction, sampling volume 800 μ L are dissolved in vortex vibration; Detect according to the gas chromatography-hydrogen flameionization testing conditions setting, chromatographic condition is: 180 DEG C of injector temperatures; 200 DEG C of flame ionization ditector temperature; 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, keep 5min, and qualitative with retention time, drawing standard working curve, with external standard standard measure, according to the concentration of calculated by peak area benzene homologues;
(5) Specification Curve of Increasing
Get respectively appropriate benzene homologues standard reserving solution, be diluted to 1L with urnormal, obtaining 6 mark-on scope concentration is benzene homologues 1.0～20 μ g/L, standard operation liquid, then operate according to above-mentioned (2), the (3) and (4) requirement of step, according to the corresponding relation drawing standard curve of the benzene homologues compound concentration adding and peak area; Adopt external standard method, record in seawater in 6 benzene homologues content and be and do not detect; The mark-on seawater recovery 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 mark-on concentration 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, any scheme after simple transformation of the present invention is all belonged to protection scope of the present invention.
Claims (4)
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. enrichment condensation for the first time, 3. enrichment condensation for the second time 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, put into the insulation can of ice bag and deposit after sample collection, takes back laboratory and puts into the water sample storeroom of 4 DEG C and deposit, and completes detection in 7d;
2. enrichment condensation for the first time: 1 L sample adds in sample evaporation bottle, sample is heated and steam distillation, volatile constituent is discharged together with water vapor simultaneously, then carry out condensation, in sample evaporation bottle, place in advance redistilled water as absorbing agent, reclaim condensed fluid to double evaporation-cooling bottle, stop collecting until condensed fluid to time within the scope of 120-150 mL;
3. enrichment condensation for the second time: 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, in receiving bottle, placing in advance redistilled water seals as absorbing agent, finally in receiving bottle, collect condensed fluid to 8-10 mL, after temperature returns to room temperature, carry out head space gas chromatography;
4. headspace gas chromatography detects: get the 10 mL water samples of collecting after time condensation in the head space bottle of 20 mL specifications, add 2.00 g sodium chloride, by head space bottle cap sealing; Sodium chloride is dissolved in vortex vibration, 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-electron capture testing conditions setting or gas chromatography-hydrogen flameionization testing conditions, qualitative with retention time, external standard method is quantitative.
2. enrichment detecting method according to claim 1, it is characterized in that: enrichment condensation for the first time mainly comprises with the gathering-device that enrichment condensation for the second time adopts 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 of vertically placing; 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, and the liquid outlet of the second serpentine condenser is connected to the bottom of receiving bottle by conduit.
3. enrichment detecting method according to claim 2, it is characterized in that: described collector tube is that top has glass stopper, side is provided with out the straight tube of gas branch pipe, top one side of collector tube is provided with feed liquor interface, collector tube feed liquor interface with go out between gas branch pipe, to be provided with one and to control the glass knob being communicated with by rotation, the part that collector tube is positioned at below glass knob is made up of outer tube and long duct two parts of being located at outer tube inside, the top of outer tube and long duct is connected, 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.
4. according to the enrichment detecting method described in claim 2 or 3, it 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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| 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 |
| CN109238788A (en) * | 2018-09-29 | 2019-01-18 | 浙江省海洋水产研究所 | Collect the device and method of VOC in water body |
| CN109238788B (en) * | 2018-09-29 | 2021-05-18 | 浙江省海洋水产研究所 | Device and method for collecting VOC in water body |
| 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 |
| CN115184511A (en) * | 2022-08-25 | 2022-10-14 | 宜宾五粮液股份有限公司 | Method for in-situ determination of volatile phenols in white spirit |
| 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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