CN105866287A - Gas chromatography detection method for chlorination by-product dichloro-acetamide - Google Patents
Gas chromatography detection method for chlorination by-product dichloro-acetamide Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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Abstract
The invention relates to a gas chromatography detection method for chlorination by-product dichloro-acetamide. Liquid-liquid extraction-gas chromatography-micro-electronics capture detectors are combined for use. The method comprises the specific steps that a to-be-tested sample solution is subjected to liquid-liquid extraction concentration and other pretreatment; gas chromatography-micro-electronics capture detectors are used for analysis to obtain a gas chromatogram of a to-be-tested sample, a standard curve is drawn for standard solutions of different concentrations on the basis of peak areas and standard solution concentrations, a linear relation between the peak area and the standard solution concentrations, and adding standard recovery is worked out; finally, a signal curve integral function is used for performing area integral on the absorption peak of the sample, and the content of dichloro-acetamide can be worked out by contrast of a standard curve. The method is simple, efficient, high in sensitivity, wide in linear range, good in repeatability, high in yield, accurate in instrumental analysis result, clear in spectrum analysis, capable of rapidly determining the content of dichloro-acetamide in water, and capable of effectively guiding daily production practice.
Description
Technical field
The invention belongs to the detection technique field of water pollutant, be specifically related to a kind of chlorine disinfection by-product two
The gas-chromatography detection method of chloroacetamide.
Background technology
Nitrogenous disinfection byproducts dichloro acetamide (DCAcAm) is widely present in employing and disappears through chlorine or chloramines
In the drinking water of poison.In recent years, due to its cytotoxicity, genotoxicity and " three cause property teratogenesis,
Carcinogenic, mutagenesis " all it is higher than traditional carbon containing disinfection byproduct (DBP) (C-DBPs) such as haloform (THMs)
With halogen acetic acid (HANs), and cause the extensive concern of people.But the content that dichloro acetamide is in water
Low, detection technique requires height, therefore, finds a kind of simplicity, highly sensitive detection method seems particularly
Important.
At present, the detection application of dichloro acetamide is most is exactly gas phase-mass spectrometry method (GC-MS), but
The method still has a disadvantage in that the detection of the method limits higher (the most about 290ng/l) and causes in water
The precision of the dichloro acetamide concentration quantitative detection of nanogram level is the highest, and the concentration for Gamma Magnitude is having
Body application needs first to concentrate at a relatively high multiple could accurately detect, cause the concentration of sample in detection pre-
Process step is relatively complicated.
Therefore, those skilled in the art need a kind of simplicity of offer badly, quick, efficient, accuracy of detection is high
The method of chlorine disinfection by-product dichloro acetamide in detection water.
Summary of the invention
For above-mentioned deficiency of the prior art, the invention provides a kind of chlorine disinfection by-product dichloroacetyl
The gas-chromatography detection method of amine, the method is simple, efficient, highly sensitive, range of linearity width, reappears
Property good, the response rate is high.
For achieving the above object, present invention employs techniques below scheme:
The gas-chromatography detection method of a kind of chlorine disinfection by-product dichloro acetamide, comprises the following steps:
S1, sampling and sample preparation pour water sample into palm fibre after the Kynoar membrane filtration of 0.45 μm
In color vial, water sample frozen water under conditions of pH is 5 is preserved；
S2, the liquid-liquid extraction of sample take 100ml water sample addition 10g anhydrous sodium sulfate and carry out sufficiently
Stirring makes it be completely dissolved, and obtains the water sample of pretreatment；
Add 10ml organic solvent to pretreated water sample, rock mixing, place into gyrate shaker
Upper vibration, is subsequently poured in separatory funnel standing and is substantially layered to appearance, collect the extract on upper strata；
The extract collected is put in nitrogen vaporizer and is concentrated by S3, concentration constant volume, treats volume
When being gradually reduced to close to 1ml, addition anhydrous sodium sulfate dehydration constant volume, to 1ml, pours 1.5ml chromatograph into
In the sample bottle analyzed；
The detection of S4, gas chromatography is by the sample equipped with testing sample of constant volume
Product bottle is put on the specimen holder of gas chromatograph, uses hand sampling or the extraction of head space automatic fine sample introduction needle
Organic solvent blank sample in sample and S2, carries out detecting and recording collection of illustrative plates through microelectronics acquisition detector；
S5, appearance time determine the dichloro acetamide standard solution of variable concentrations by step S4
Requirement carry out operation and obtain gas chromatogram, determine the appearance time of standard substance；Water sample to be measured is passed through
After step S1-S4, gained collection of illustrative plates contrasts with standard substance gas chromatogram, and determine testing sample goes out peak
Time；Draw standard curve according to the gas chromatogram corresponding to variable concentrations standard solution, obtain face, peak
Amass the linear relationship between concentration of standard solution, calculate recovery of standard addition；In described standard solution,
Solute is dichloro acetamide, and solvent is organic solvent in S2；
S6, result are characterized in experiment gained sample collection of illustrative plates and find the peak that appearance time is corresponding, and right
Absworption peak carries out area integral calculating, can be calculated dichloro in testing sample accordingly according to standard curve
The content of acetamide.
Preferably, in step S1, add in Brown Glass Brown glass bottles and jars only and ensure that water sample pH is the buffer of 5, institute
State buffer and use 0.2M sodium acetate and the mixed solution of 0.3M acetic acid.
Preferably, in S2, organic solvent is ethyl acetate or methyl tertiary butyl ether(MTBE).
Preferably, in step S2, the temperature of gyrate shaker is set to 25 DEG C, and frequency of vibration is set to 100
Rev/min.
Preferably, in step S3, set bath temperature as 37 DEG C, nitrogen pressure 0.3Mpa.
Preferably, in step S4, gas chromatograph uses Agilent HP-5 capillary gas chromatography
Post；Injector temperature is set to 235 DEG C；Microelectronics acquisition detector temperature is 260 DEG C；Carrier gas is high-purity
Nitrogen, flow velocity is 2ml/min, and make-up gas flow is 50ml/min；Sampling volume is 2ml；Sample introduction side
Formula is Splitless injecting samples, and after sample introduction 0.75min, split ratio is 10:1；Gas chromatographic column heating schedule is such as
Under, initial temperature is located at 80 DEG C and keeps 5min, is warming up to 150 DEG C with the speed of 30 DEG C/min, keeps
1min, total run time 8.333min.
Preferably, in step S5, the Concentraton gradient of joined standard solution is respectively 50,100,300,
1200μg/L。
Preferably, in step S5, the calculating formula of recovery of standard addition isWherein, R is
The response rate, Cs represents the concentration adding standard solution；C represents instrument concentrations.
The beneficial effects of the present invention is:
1), the present invention uses liquid-liquid extraction-gas chromatography to measure nitrogenous in water disappearing
The concentration of toxic byproduct dichloro acetamide, first carries out liquid-liquid extraction enrichment etc. by testing sample solution
Pre-treatment；Then, pass through gas chromatogram---microelectronics acquisition detector is analyzed, to obtain testing sample
Gas chromatogram, and the standard solution for variable concentrations draws mark with peak area and concentration of standard solution
Directrix curve, obtains the linear relationship between peak area and concentration of standard solution, calculates recovery of standard addition；
Finally, the signal curve integrating function utilizing instrument to carry carries out area integral to the absworption peak of sample, right
Sighting target directrix curve can calculate the content of dichloro acetamide.The method is simple to operate, efficient, has
High sensitivity and the gratifying response rate and repeatability.
2), the detection method that provides of the present invention, under contrasting through atlas analysis and production practices: micro-electricity
Sub-acquisition detector has higher selectivity, susceptiveness；Gas chromatography energy
Enough overcome the shortcoming of GC-MS in background technology, it is not necessary to concentrate at a relatively high multiple, only need to concentrate 100
Can accurately detect the concentration of dichloro acetamide again, through overtesting gained, the detection limit of the method is reduced to
50ng/l, the response rate reach more than 90%, repeatability is high.The more important thing is, the installation cost of gas phase instrument
With low compared with GC-MS, being more suitable for great majority does not has the labs of enough business models to detect.Separately
Outward, the liquid-liquid extraction method intending in sample concentration using is more convenient than conventional solid phase extraction, efficiently, save.
Therefore, liquid-liquid extraction-gas chromatography shows in detection dichloroacetyl amine content
Go out preferable superiority.
Accompanying drawing explanation
Fig. 1 is dichloro acetamide canonical plotting.
Fig. 2 is the gas chromatogram of dichloro acetamide standard solution (100 μ g/L).
Fig. 3 is the gas chromatogram comparison figure of embodiment four testing samples of V-type spent filter backwash water.
Detailed description of the invention
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the present invention is carried out clear,
It is fully described by.Following example are only used for clearly illustrating technical scheme, and can not
Limit the scope of the invention with this.
The instrument and equipment that the embodiment of the present invention is used mainly has the 7890B that Agilent company of the U.S. produces
(KS501, IKA) that gas chromatograph (being equipped with microelectronics acquisition detector) and Germany produce rotates
Agitator, dichloro acetamide standard substance (DCAcAm) come from Alfa Aesar company of Germany.
Embodiment 1～4
The dichloroacetyl amine content produced after detecting certain water factory's V-type filter back washing draining chlorination
S1, sampling and sample preparation gather the anti-of water factory's V-type filter tank with the sampling bottle clean through ultrasonic cleaning
Flush discharge.Take according to backwash technique feature that gas rushes the stage, air water rushes the stage, water washes beginning rank open respectively
Section and water rush the backwash draining of ending phase, and it is 1., 2., 3. and 4. (the most right that sampling numbering is respectively
Answer embodiment 1, embodiment 2, embodiment 3, embodiment 4)；By water sample through 0.45 μm after static 2 hours
Kynoar membrane filtration trapped particles, will filter after water sample pour in Brown Glass Brown glass bottles and jars only, with joining in advance
Make buffer (0.2M sodium acetate and the acetic acid of 0.3M) regulation water sample pH value to about 5.0,
Vial being put in frozen water (0 DEG C) and preserves, under this state, dichloro acetamide can stable existence；Examination
Take 200ml water sample before testing beginning to add liquor natrii hypochloritis's (containing effective chlorine 5%) of 55 μ l and carry out disinfection,
Under room temperature condition, it is placed on shady place and makes it fully react more than 24h.
After S2, the liquid-liquid extraction of sample take 100ml sterilization, water sample addition 10g anhydrous sodium sulfate is carried out
Sufficiently stirring makes it be completely dissolved, and obtains the water sample of pretreatment；
In the water sample of pretreatment, add 10ml ethyl acetate, first firmly rock 1min with hands and make it complete
Mixing, places into the 5min (temperature: 25 DEG C, frequency of vibration: 100 revs/min) that vibrates on gyrate shaker,
Finally pour static 5min in separatory funnel into and significantly layering occurs, be collected from below upper strata liquid level 1cm
Extract；
The extract of the about 20ml collected is put in nitrogen vaporizer and is carried out by S3, concentration constant volume
Concentrate, setting bath temperature: 37 DEG C, nitrogen pressure 0.3Mpa, observe residual body at set intervals
Long-pending, when volume is close to 1ml, finally it is separately added into anhydrous sodium sulfate dehydration constant volume to 1ml, embodiment
4 water samples of 1～4 are poured in the sample bottle of 1.5ml chromatography respectively.
The sample of constant volume is put into gas phase color by the detection of S4, gas chromatography
On the specimen holder of the instrument of spectrum, set instrument working condition: chromatographic column is as Agilent HP-5 Capillary Gas
Phase chromatographic column, specification is 30m × 0.32mm × 0.25 μm, flow: 2.001ml/min；Injection port: temperature
Spend 235 DEG C, pressure 10.040psi, flow 64.88ml/min, heat insulation purge flow rate 3.0ml/min；Micro-
Electron capture detector temperature is 260 DEG C, tail wind drift amount 58.00ml/min；Carrier gas is high pure nitrogen, stream
Speed is 2ml/min, and make-up gas flow is 50ml/min；Sampling volume is 2ml；Input mode be regardless of
Flowing to sample, after 0.75min, split ratio is 10:1；Gas chromatographic column heating schedule is: initial temperature is
80 DEG C keep 5min, are then warming up to 150 DEG C with 30 DEG C/min, keep 1min, total run time
8.333min；Head space automatic fine sample introduction needle extraction numbering is used to be respectively sample 1., 2., 3. and 4.
Carry out detecting and recording collection of illustrative plates with blank sample (ethyl acetate).
S5, appearance time are determined and are carried out by the requirement of step S4 by dichloro acetamide standard solution
Operation obtains gas chromatogram, determines the appearance time of standard substance；Water sample to be measured by embodiment 1～4
The collection of illustrative plates obtained after step S1～S4 contrasts with standard substance gas chromatogram, determines and treats test sample
Product appearance time；According to corresponding to variable concentrations standard solution gas chromatogram draw standard curve (as
Shown in Fig. 1, do joined Concentraton gradient during standard curve and be respectively 50,100,300,1200 μ g/L；Its
In gas chromatogram corresponding to 100 μ g/L standard solution as shown in Figure 2), thus obtain peak area with
Linear relationship between concentration of standard solution, calculates recovery of standard addition；In described standard solution, solute
For dichloro acetamide, solvent is ethyl acetate；As shown in table 1 below, according to this method standard solution institute
Obtain sample appearance time and be about 5.63min；Through comparing embodiment 1～the appearance time of 4 four water samples
Be respectively as follows: 5.631,5.633,5.633,5.636min；Recovery of standard addition is 90%～111%.
Table 1 dichloro acetamide standard curve and recovery of standard addition
S6, result characterize the OpenLAB CDS gas chromatograph operation software utilizing apparatus preparation
Graphs integrating function, usable floor area normalization method draws the content of dichloro acetamide: at experiment gained
In sample collection of illustrative plates, (as it is shown on figure 3, the gas chromatogram comparison for embodiment 1～4 four water samples is schemed) is looked for
To the peak that respective appearance time is corresponding, and it is integrated drawing peak area to absworption peak, can be from standard
Curve is calculated corresponding content；Detect after concentrating 100 times due to water sample, calculate
Concentration is 100 times of actual concentrations, and the result of four water samples is as shown in table 2.
The dichloro acetamide assay result produced after certain V-type filter fluorescence method chlorination of table 2
The detection method that the present invention provides, material appearance time and peak steady after chromatographic column, simple to operate,
Result precise and high efficiency, substantial amounts of time and testing cost can be saved.
The above is only the preferred embodiment of the present invention, it is noted that general for the art
For logical technical staff, on the premise of without departing from the technology of the present invention principle, it is also possible to make some improvement
And deformation, these improve and deformation also should be regarded as protection scope of the present invention.
Claims (8)
1. the gas-chromatography detection method of a chlorine disinfection by-product dichloro acetamide, it is characterised in that bag
Include following steps:
S1, sampling and sample preparation pour water sample into palm fibre after the Kynoar membrane filtration of 0.45 μm
In color vial, water sample frozen water under conditions of pH is 5 is preserved；
S2, the liquid-liquid extraction of sample take 100ml water sample addition 10g anhydrous sodium sulfate and carry out sufficiently
Stirring makes it be completely dissolved, and obtains the water sample of pretreatment；
Add 10ml organic solvent to pretreated water sample and rock mixing, place on gyrate shaker
Vibration, is subsequently poured in separatory funnel standing and substantially layering extremely occurs, collect the extract on upper strata；
The extract collected is put in nitrogen vaporizer and is concentrated by S3, concentration constant volume, treats volume
When being gradually reduced to close to 1ml, addition anhydrous sodium sulfate dehydration constant volume, to 1ml, pours chromatography into
In sample bottle；
The detection of S4, gas chromatography is by the sample equipped with testing sample of constant volume
Product bottle is put on the specimen holder of gas chromatograph, uses hand sampling or the extraction of head space automatic fine sample introduction needle
Organic solvent blank sample in sample and S2, carries out detecting and recording collection of illustrative plates through microelectronics acquisition detector；
S5, appearance time determine the dichloro acetamide standard solution of variable concentrations according to step S4
Carry out operation and obtain gas chromatogram, determine the appearance time of standard substance；Water sample to be measured is passed through step
After S1-S4, gained collection of illustrative plates contrasts with standard substance gas chromatogram, determines the appearance time of testing sample；
According to the gas chromatogram corresponding to variable concentrations standard solution, draw peak area and concentration of standard solution it
Between the standard curve of relation, obtain the linear relationship between peak area and concentration of standard solution, calculate and add
The mark response rate；In described standard solution, solute is dichloro acetamide, and solvent is organic solvent in S2；
S6, result are characterized in the sample collection of illustrative plates of experiment gained and find the absorption that appearance time is corresponding
Peak, and be integrated absworption peak area calculating, can be calculated according to standard curve correspondence and treat test sample
The content of dichloro acetamide in product.
The gas chromatogram inspection of a kind of chlorine disinfection by-product dichloro acetamide the most according to claim 1
Survey method, it is characterised in that: in step S1, there was added guarantee water sample pH in Brown Glass Brown glass bottles and jars only is 5
Buffer, described buffer uses 0.2M sodium acetate and the mixed solution of 0.3M acetic acid.
The gas chromatogram inspection of a kind of chlorine disinfection by-product dichloro acetamide the most according to claim 1
Survey method, it is characterised in that: in S2, organic solvent is ethyl acetate or methyl tertiary butyl ether(MTBE).
The gas chromatogram inspection of a kind of chlorine disinfection by-product dichloro acetamide the most according to claim 1
Survey method, it is characterised in that: in step S2, the temperature of gyrate shaker is set to 25 DEG C, frequency of vibration
It is set to 100 revs/min.
The gas chromatogram inspection of a kind of chlorine disinfection by-product dichloro acetamide the most according to claim 1
Survey method, it is characterised in that: in step S3, setting bath temperature as 37 DEG C, nitrogen pressure is 0.3Mpa.
The gas chromatogram inspection of a kind of chlorine disinfection by-product dichloro acetamide the most according to claim 1
Survey method, it is characterised in that: in step S4, gas chromatograph uses Agilent HP-5 capillary tube
Gas chromatographic column；Injector temperature is set to 235 DEG C；Microelectronics acquisition detector temperature is 260 DEG C；Carry
Gas is high pure nitrogen, and flow velocity is 2ml/min, and make-up gas flow is 50ml/min；Sampling volume is 2ml；
Input mode is Splitless injecting samples, and after sample introduction 0.75min, split ratio is 10:1；Gas chromatographic column heats up
Program is as follows, and initial temperature is located at 80 DEG C and keeps 5min, is warming up to 150 DEG C with the speed of 30 DEG C/min,
Keep 1min, total run time 8.333min.
The gas chromatogram inspection of a kind of chlorine disinfection by-product dichloro acetamide the most according to claim 1
Survey method, it is characterised in that: in step S5, the Concentraton gradient of joined standard solution is respectively 50,100,
300、1200μg/L。
8. according to the gas phase color of a kind of chlorine disinfection by-product dichloro acetamide described in claim 1 or 7
Spectrum detection method, it is characterised in that: in step S5, the calculating formula of recovery of standard addition is
Wherein, Cs represents the concentration adding standard solution；C represents instrument concentrations.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106338559A (en) * | 2016-08-24 | 2017-01-18 | 河海大学 | Gas chromatography detection method of chlorination by-product dichloroacetamide |
| CN106501388A (en) * | 2016-09-22 | 2017-03-15 | 北京万全德众医药生物技术有限公司 | A kind of method of trichloroacetamide in use gas chromatography separation determination eplerenone |
| CN107192782A (en) * | 2017-07-11 | 2017-09-22 | 河海大学 | A kind of method of 8 kinds of DBPs including 4 kinds of halogen acetonitriles of synchronous detection |
| CN108593802A (en) * | 2018-05-25 | 2018-09-28 | 天津大学 | The gas chromatography-electron capture detector detection method of halogenated benzoquinones |
| CN111272927A (en) * | 2020-03-20 | 2020-06-12 | 同济大学 | Method for improving accuracy of haloacetic acid gas chromatography detection |
| CN111948322A (en) * | 2020-07-30 | 2020-11-17 | 河海大学 | Method for detecting organic tin in water body |
| CN114514418A (en) * | 2019-07-18 | 2022-05-17 | 生物技术欧洲股份公司 | Method for determining at least one parameter of a sample composition comprising nucleic acids, such as RNA, and optionally particles |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106338559A (en) * | 2016-08-24 | 2017-01-18 | 河海大学 | Gas chromatography detection method of chlorination by-product dichloroacetamide |
| CN106338559B (en) * | 2016-08-24 | 2019-07-12 | 河海大学 | A kind of gas-chromatography detection method of chlorine disinfection by-product dichloro acetamide |
| CN106501388A (en) * | 2016-09-22 | 2017-03-15 | 北京万全德众医药生物技术有限公司 | A kind of method of trichloroacetamide in use gas chromatography separation determination eplerenone |
| CN107192782A (en) * | 2017-07-11 | 2017-09-22 | 河海大学 | A kind of method of 8 kinds of DBPs including 4 kinds of halogen acetonitriles of synchronous detection |
| CN107192782B (en) * | 2017-07-11 | 2019-10-22 | 河海大学 | A kind of method of 8 kinds of disinfection by-products including 4 kinds of halogen acetonitriles of synchronous detection |
| CN108593802A (en) * | 2018-05-25 | 2018-09-28 | 天津大学 | The gas chromatography-electron capture detector detection method of halogenated benzoquinones |
| CN114514418A (en) * | 2019-07-18 | 2022-05-17 | 生物技术欧洲股份公司 | Method for determining at least one parameter of a sample composition comprising nucleic acids, such as RNA, and optionally particles |
| CN111272927A (en) * | 2020-03-20 | 2020-06-12 | 同济大学 | Method for improving accuracy of haloacetic acid gas chromatography detection |
| CN111948322A (en) * | 2020-07-30 | 2020-11-17 | 河海大学 | Method for detecting organic tin in water body |
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Application publication date: 20160817 |