CN101625343A - Fast analysis method for quantifying dichloroacetonitrile in drinking water - Google Patents
Fast analysis method for quantifying dichloroacetonitrile in drinking water Download PDFInfo
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Abstract
The invention relates to a fast analysis method for quantifying dichloroacetonitrile in drinking water, comprising the following steps of sample pretreatment, instrument condition control and operation measurement; the sample pretreatment comprises the following steps: selecting an optimal chlorination terminator and an extracting agent in a water sample, adopting ascorbic acid and/or ammonium chloride as the chlorination terminator, and adopting methyl tertiary butyl ether or ethyl acetate as the extracting agent; the instrument condition control comprises the steps: determining the temperature-rising program and column head pressure, and determining optimal sample injection quantity and the optimal temperature of a sample injection port. The method adopts a small volume liquid-liquid extracting method to extract DCAN in the water sample, saves the use quantity of the water samples, salt (anhydrous sodium sulfate) and the extracting agent (methyl tertiary butyl ether), reduces sample-measuring cost, adopts GC/MS measurement, determines the instruction parameter condition, can avoid the phenomenon of peak escaping, tailing and the like of DCAN, guarantees normal peak escaping thereof, and can obtain higher detection limit and smaller relative standard deviation (RSD).
Description
Technical field
The invention belongs to municipal plumbing and field of environment engineering, relate to water quality detection, analytical technology.
Background technology
To (the Disinfection by-products of DBPs in the potable water, DBPs) research starts from 1974, discovers, when using chlorine as sanitizer, not only can cause the reaction on the sense of smell and the sense of taste, also can produce class particular compound a---THMs[5].1976, EPA (USEPA) investigation found that chloroform and other THMs are prevalent in the chlorination potable water afterwards [6].In the same year, American National cancer association discovers that chloroform has carcinogenesis [7] to animal.Therefore, the research to DBPs in the potable water begins to cause people's attention.The nineties, the main object of DBPs research is removed outside the THMs, mainly is halogen acetic acid (HAAs), and its " three cause " effect is strong, and the unit carcinogenic risk is far above haloform [8].After 2000, relevant discovering, those new discoveries and the DBPs that is not included into regulation are far longer than DBPs such as THMs to the harm that human body produced.Thereby, appearance along with various organic and inorganic halogenation DBPs (Halo-DBPs), research to DBPs not only is confined on THMs and the HAAs two big class materials, but expansion is to the broad research of Halo-DBPs, as bromate, chlorate, halogenated aldehyde, chlorinated phenol and halogenated furan ketone (it is represented as 3-chloro-4-dichloromethyl-5-hydroxyl-2 (5 hydrogen) furanone, is called for short MX) etc.
On July 1st, 2007, new " drinking water sanitary standard " (the GB 5749-2006) of the formal execution of China, identical with foreign standard, restriction to DBPs content such as THMs in the potable water is more and more stricter, many drinking water supply units have to change sterilization process, traditional disinfection way based on chlorine is replaced with disinfection way based on chloramines, and often and ozone or chlorine dioxide coupling.Along with multiple sanitizer separately or unite use, increasing DBPs is detected in potable water, there be more than 600 kind of DBPs to be in the news at present approximately, wherein with nitrogenous DBPs (nitrogenous disinfectionby-products, N-DBPs) toxicity maximum, distribution range is the widest, becomes the focus of current DBPs research gradually.
Halogen acetonitrile (HANs) is the class among the N-DBPs, wherein, and two chloroacetonitriles (DCAN, molecular formula: CHCl
2CN) be the highest a kind of of content among the HANs, need form mechanism and control method research it.Before formation mechanism of carrying out DCAN and control method research, need set up convenient, DCAN assay method effectively and fast.At present, domestic mensuration about DCAN in the potable water is actually rare, also use gas phase-electronics to capture detecting device (GC-ECD) abroad mostly and measure DCAN, GC-ECD can be preferably the quantitative concentration of DCAN in potable water, but have big defective, promptly form in the Mechanism Study process at DCAN, need to determine the generative process of DCAN, molecular structure between DCAN precursor substance and other accessory substance, thereby the generation rule of searching DCAN are so that controlled.Yet GE-ECD does not have qualitative function, and it is qualitative to need mass spectrum (MS) to carry out, thereby this patent has been developed the DCAN method in a kind of employing gas phase-mass spectrometry (GC-MS) technology fast measuring potable water.
List of references:
[1] Chu Wenhai, Gao Naiyun. the nitrogenous DBPs halogenated nitromethane of potable water progress [J]. water supply and drainage, 2008,34 (7): 34-36.
[2]Krasner，S.W.，et?al.，Occurrence?of?a?New?Generation?of?Disinfection?Byproducts[J].Environ.Sci.Technol.，2006.40(23)：7175-7185.
[3]Mohamadin，A.M.，Possible?role?of?hydroxyl?radicals?in?the?oxidation?of?dichloroacetonitrile?byFenton-like?reaction[J].Journal?of?Inorganic?Biochemistry，2001.84(1-2)：97-105.
[4]Muellner，M.G.，et?al.，Haloacetonitriles?vs.Regulated?Haloacetic?Acids：AreNitrogen-Containing?DBPs?More?Toxic[J].Environ.Sci.Technol.，2007.41(2)：645-651.
[5]Bellar?T?A，Lichtenberg?J?J，Kroner?R?C.Determining?volatile?organics?at?microgram-per-litrelevels?by?gas?chromatography[J].Journal?of?American?Water?Works?Association，1974，66：703-706.
[6]Kopfler?F?C，Melton?R?G，Lingg?R?D，et?al.In?identification?and?analysis?of?organic?pollutants?inwater[R].New?York，USA：Ann?Arbor?Science?Publishers，1976.
[7]National?cancer?institute?report?on?carcinogenesis?bioassay?of?chloroform，carcinogenesisprogram[R].Bethesda，USA：Division?of?cancer?cause?and?prevention，1976.
[8]Rodriguez?M?J，Serodes?J，Danielle?R.Formation?and?fate?of?haloacetic?acids(HAAs)within?thewater?treatment?plant[J].Water?Research，2007，41(18)：4222-4232.
Summary of the invention
The object of the present invention is to provide the rapid analysis of DBPs two chloroacetonitriles in a kind of potable water.
For achieving the above object, solution of the present invention is:
The present invention includes sample pretreatment, three parts are measured in instrument condition optimization and operation.
Sample pretreatment comprises choosing of optimal chlorination reaction terminating agent and extractant in the water sample again.
Instrument condition control comprises again that heating schedule and column cap press determines, the determining of best sample size and injection port optimum temperature.
Operation is measured and to be comprised determining of the determining of working curve, detectability and determination limit again.
Further, described heating schedule and column cap are pressed determines to comprise:
By adjusting initial temperature, retention time and heating rate, contrast DCAN appearance time, and peak height and peak area, the following heating schedule of final acquisition: initial temperature is 30.0 ℃, keep 2.0min, speed with 7.0 ℃/min is warming up to 72.0 ℃ again, can overcome the conditions of streaking at DCAN peak, guarantees that DCAN normally goes out the peak;
Use above-mentioned heating schedule, the column cap that changes in the instrument parameter is pressed, and finally obtains column cap and presses the Shi Jieke in 60～75kPa scope to guarantee that DCAN normally goes out the peak.
Get the water sample of 20mL after ascorbic acid or ammonium chloride dechlorination and place glass test tube, the pH of regulator solution adds the 4.0g anhydrous sodium sulfate in 4.0～6.0 scopes, and the 1.0min that manually vibrates makes anhydrous sodium sulfate fully dissolve, and the water sample liquid level rises to some extent; Afterwards, add the 2.0mL methyl tert-butyl ether, and manual thermal agitation 5.0min, leave standstill 10.0min, get upper strata extractant methyl tert-butyl ether (MTBE) solution, carry out GC/MS and measure;
When GC/MS measured, the concrete parameter of instrument was:
Carrier gas: high-purity helium; Carrier gas flux control mode: pressure control; Column cap is pressed: 60～75kPa; Sample size: 3.0 μ L; Input mode: no split sampling; Data acquisition, analysis: GCMS solution software workstation; Injector temperature: 100～120 ℃; Mass Spectrometer Method actuator temperature: 250 ℃; Ion gun: electron impact ion source; Electron energy: 70eV; Detecting pattern: select ion detection; Molten heating schedule: initial temperature is 30 ℃, keeps 2.0min, and the speed with 7.00 ℃/min is warming up to 72.00 ℃ again; DCAN appearance time: 5.57min.This method recovery is between 83.5%～117.2%; Detection limit is below 0.5 μ g/L; Relative standard deviation is less than 10.0%.
Owing to adopt such scheme, the invention has the beneficial effects as follows::
(1) this method adopts the DCAN in small size liquid-liquid extraction method (Fig. 3) the extraction water sample, the use amount of having saved water sample, salt (anhydrous sodium sulfate) and extractant (methyl tert-butyl ether).Extraction in the past generally will be used 200mL water sample and a large amount of salt and extractants, and the test sample cost is than higher.
(2) the main gas phase/electronics that adopts captures detecting device (GC/ECD) mensuration DCAN in the former studies, this method adopts GC/MS to measure, and determined detailed instrument parameter condition, can avoid DCAN to go out phenomenons such as peak hangover, guarantee that it normally goes out the peak, and can obtain higher detection limit (MDL) and less relative standard deviation (RSD).
Description of drawings
Fig. 1 is two chloroacetonitriles (DCAN) molecular formula synoptic diagram.
Fig. 2 is a check and analysis schematic flow sheet of the present invention.
Fig. 3 is the extracting operation process flow diagram of check and analysis flow process of the present invention.
Fig. 4 is the standard working curve figure of DCAN.
Fig. 5 is the DCAN total ions chromatogram.
Embodiment
The present invention is further illustrated below in conjunction with the accompanying drawing illustrated embodiment.
The present invention includes sample pretreatment, three parts are measured in instrument condition optimization and operation.
Sample pretreatment comprises choosing of optimal chlorination reaction terminating agent and extractant in the water sample again.
Instrument condition optimization comprises determining of best sample size and injection port optimum temperature again.
Operation is measured and to be comprised determining of the determining of working curve, detectability and determination limit again.
1 sample pretreatment
1.1 terminator is chosen
Test method
Usually chlorine residue and also has the chlorine residue of high level in the potable water after the sterilization in the test water sample that research DBPs generates between 0.05～4.0mg/L, needs to add the reductibility terminator and comes cancellation to have chlorine residue than strong oxidizing property, stops chlorination reaction progress.For avoiding of the influence of chlorination terminator as far as possible to DCAN stability.Need to investigate the influence of chlorination reaction terminator commonly used to DCAN stability.Prepare the water sample of a plurality of same concentration DCAN, choose one of them water sample through gas phase/GC-MS (GC/MS, model: Tianjin, island QP2010) record peak area M immediately sweeping entirely under (SCAN) pattern, in addition, in other DCAN water sample, add a certain amount of terminator commonly used respectively, ascorbic acid, sodium thiosulfate, sodium sulphite, ammonium chloride etc. are (in the DBPs correlative study, the above-mentioned several chlorination reaction terminators of main use), the pH of regulator solution (avoids the DCAN hydrolysis) in 4.0～6.0 scopes, measure the corresponding peak area N of DCAN behind the lucifuge reaction 24h, the peak area M contrast that this peak area N is measured when not adding terminator immediately, i.e. M/N * 100%.The corresponding M/N of the sort of terminator * 100% is big more, and which kind of is more little to the interference of DCAN.It is comparatively suitable as the chlorination terminator to draw ascorbic acid and ammonium chloride.
1.2 choosing of extractant
Test method
At first water sample is crossed 0.45 μ m miillpore filter, added the 4g anhydrous sodium sulfate again in the test tube that is placed with the 20mL water sample, the 1min that manually vibrates makes anhydrous sodium sulfate fully dissolve, and the water sample liquid level rises to some extent.Afterwards, add 2mL extractant and manual thermal agitation 5min, leave standstill 10min, get upper strata extractant solution, carry out GC/MS and measure.Two kinds of extractants have been used in this test, contrast both effect of extracting, and promptly the high person of the recovery is excellent.Draw extractant methyl tert-butyl ether (MTBE) effect of extracting of DCAN is better than ethyl acetate (ETAC).Fig. 3 is an operational flowchart.
2 instrument condition optimizations
2.1 what heating schedule and column cap were pressed determines
By adjusting initial temperature, retention time and heating rate, contrast DCAN appearance time, and peak height and peak area, the following heating schedule of final acquisition: initial temperature is 30.0 ℃, keep 2.0min, speed with 7.0 ℃/min is warming up to 72.0 ℃ again, can overcome the conditions of streaking at DCAN peak, guarantees that DCAN normally goes out the peak.
Use above-mentioned heating schedule, the column cap that changes in the instrument parameter is pressed, and finally obtains column cap and presses the Shi Jieke in 60～75kPa scope to guarantee that DCAN normally goes out the peak.
2.2 determining of best sample size
Control Other Instruments condition is constant, and the GC/MS detecting pattern is that full scan detects (SCAN), and sample size is set at the peak area that 1,2,3,4 and 5 μ L (for sample size, instrument can only carry out integer and set) investigate tie substance respectively.It is 3 μ L that contrast has drawn best sample size, and gained DCAN peak area is too small during less than 3 μ L, causes quantity of solvent too much during greater than 3 μ L, pollutes the ion gun among the MS.
2.3 determining of injection port optimum temperature
Instrument acquiescence injector temperature is 180 ℃, however the easy decomposes of DCAN, thereby need to reduce injector temperature.Control Other Instruments condition is constant, and injector temperature is set at 90,100,110,120,130,140,150,160 and 170 ℃ respectively, and the peak area under the contrast different temperatures changes, and comparing result is determined 100～120 ℃ of best injector temperatures.
3 operations are measured
3.1 determining of working curve
Hybrid standard liquid: the DCAN hybrid standard product solution of getting 2000mg/L is an amount of, places brown volumetric flask, is mixed with the hybrid standard liquid that mass concentration is 10mg/L with deionized water.
Calibration standard liquid: with organic solvent diluting hybrid standard liquid, be mixed with the calibration standard liquid of 6 mass concentration levels (20,60,80,100,150,200 μ g/L), be used for the production standard working curve.Standard working curve as shown in Figure 4.
3.2DCAN chromatogram and appearance time
Fig. 5 is that the DCAN calibration standard liquid of 200 μ g/L is measured gained through GC/MS, and as seen from Figure 5, the DCAN appearance time is 5.57min.
3.3 determining of detectability and determination limit
Under selected condition, DCAN is in the scope internal linear relation good (r＞0.995) of 20～200 μ g/L, and the method recovery is between 83.5%～117.2%; Detection limit (MDL) is below 0.5 μ g/L; RSD is less than 10.0%.
By above-mentioned introduction, that this method summary is as follows:
Get the water sample of 20mL after ascorbic acid or ammonium chloride dechlorination and place glass test tube, the pH of regulator solution adds the 4.0g anhydrous sodium sulfate in 4.0～6.0 scopes, and the 1.0min that manually vibrates makes anhydrous sodium sulfate fully dissolve, and the water sample liquid level rises to some extent.Afterwards, add 2.0mL methyl tert-butyl ether (MTBE), and manual thermal agitation 5.0min, leave standstill 10.0min, get upper strata extractant MTBE solution, carry out GC/MS and measure.
When GC/MS measured, the concrete parameter of instrument was:
Carrier gas: high-purity helium; Carrier gas flux control mode: pressure control; Column cap is pressed: 65.7kPa (60～75kPa all can); Sample size: 3.0 μ L; Input mode: no split sampling; Data acquisition, analysis: GCMS solution software workstation.Injector temperature: 110 ℃ (100～120 ℃ all can); Mass Spectrometer Method actuator temperature: 250 ℃ (instrument acquiescence numerical value); Ion gun: electron impact ion source (EI) (using always); Electron energy: 70eV (instrument acquiescence numerical value); Detecting pattern: select ion detection (SIM) (using always).Molten heating schedule: initial temperature is 30 ℃, keeps 2.0min, and the speed with 7.00 ℃/min is warming up to 72.00 ℃ again; DCAN appearance time: 5.57min.This method recovery is between 83.5%～117.2%; Detection limit (MDL) is below 0.5 μ g/L; Relative standard deviation (RSD) is less than 10.0% (RSD has been controlled in the detectability critical value of stipulating in the U.S.EPA552.3 of the EPA method (≤20%)).
The above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.The person skilled in the art obviously can easily make various modifications to these embodiment, and needn't pass through performing creative labour being applied in the General Principle of this explanation among other embodiment.Therefore, the invention is not restricted to the embodiment here, those skilled in the art should be within protection scope of the present invention for improvement and modification that the present invention makes according to announcement of the present invention.
Claims (3)
1, a kind of rapid analysis of two chloroacetonitriles comprises: sample pretreatment, and instrument condition control and operation are measured, and it is characterized in that: sample pretreatment comprises choosing of optimal chlorination reaction terminating agent and extractant in the water sample;
Adopt ascorbic acid or ammonium chloride as the chlorination terminator, adopt methyl tert-butyl ether or ethyl acetate as extractant;
The control of described instrument condition comprises that heating schedule and column cap press determines, the determining of best sample size and injection port optimum temperature.
2, method according to claim 1 is characterized in that: described heating schedule and column cap are pressed determines to comprise:
By adjusting initial temperature, retention time and heating rate, contrast DCAN appearance time, and peak height and peak area, the following heating schedule of final acquisition: initial temperature is 30.0 ℃, keep 2.0min, speed with 7.0 ℃/min is warming up to 72.0 ℃ again, can overcome the conditions of streaking at DCAN peak, guarantees that DCAN normally goes out the peak;
Use above-mentioned heating schedule, the column cap that changes in the instrument parameter is pressed, and finally obtains column cap and presses the Shi Jieke in 60～75kPa scope to guarantee that DCAN normally goes out the peak.
3, method according to claim 1 is characterized in that:
Get the water sample of 20mL after ascorbic acid or ammonium chloride dechlorination and place glass test tube, the pH of regulator solution adds the 4.0g anhydrous sodium sulfate in 4.0～6.0 scopes, and the 1.0min that manually vibrates makes anhydrous sodium sulfate fully dissolve, and the water sample liquid level rises to some extent; Afterwards, add the 2.0mL methyl tert-butyl ether, and manual thermal agitation 5.0min, leave standstill 10.0min, get upper strata extractant methyl tertbutyl ethereal solution, carry out GC/MS and measure;
When GC/MS measured, the concrete parameter of instrument was:
Carrier gas: high-purity helium; Carrier gas flux control mode: pressure control; Column cap is pressed: 60～75kPa; Sample size: 3.0 μ L; Input mode: no split sampling; Data acquisition, analysis: GCMS solution software workstation; Injector temperature: 100～120 ℃; Mass Spectrometer Method actuator temperature: 250 ℃; Ion gun: electron impact ion source; Electron energy: 70eV; Detecting pattern: select ion detection; Molten heating schedule: initial temperature is 30 ℃, keeps 2.0min, and the speed with 7.00/min is warming up to 72.00 ℃ again; DCAN appearance time: 5.57min.This method recovery is between 83.5%～117.2%; Detection limit is below 0.5 μ g/L; Relative standard deviation is less than 10.0%.
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| CN101561372B (en) * | 2009-05-12 | 2011-07-27 | 同济大学 | Rapid analysis method of disinfection side product dibromo-acetonitrile in drinking water |
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| CN113049707A (en) * | 2021-03-22 | 2021-06-29 | 山东省城市供排水水质监测中心 | On-line liquid-liquid extraction gas chromatography-mass spectrometry method for determining monobromo-dichloroacetonitrile in water |
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| CN101561372B (en) * | 2009-05-12 | 2011-07-27 | 同济大学 | Rapid analysis method of disinfection side product dibromo-acetonitrile in drinking water |
| CN105948215A (en) * | 2016-06-29 | 2016-09-21 | 同济大学 | Water sample preservation method of iodo nitrogen-containing disinfection by-product |
| CN108709944A (en) * | 2018-04-27 | 2018-10-26 | 同济大学 | The method for detecting nitrogenous -6 kinds of chlorobenzene acetonitriles of armaticity disinfection by-products in drinking water simultaneously |
| CN108709944B (en) * | 2018-04-27 | 2021-02-12 | 同济大学 | Method for simultaneously detecting 6 chlorobenzene acetonitrile serving as nitrogenous aromatic disinfection by-product in drinking water |
| CN111272891A (en) * | 2020-02-20 | 2020-06-12 | 河海大学 | Method for detecting novel nitrogenous disinfection by-product N-chloro-2,2-dichloroacetamide in drinking water |
| CN111272891B (en) * | 2020-02-20 | 2021-02-12 | 河海大学 | Method for detecting novel nitrogenous disinfection by-product N-chloro-2,2-dichloroacetamide in drinking water |
| CN113049707A (en) * | 2021-03-22 | 2021-06-29 | 山东省城市供排水水质监测中心 | On-line liquid-liquid extraction gas chromatography-mass spectrometry method for determining monobromo-dichloroacetonitrile in water |
| CN114636771A (en) * | 2022-05-07 | 2022-06-17 | 北京和合医学诊断技术股份有限公司 | Method for detecting procaterol content in blood and application |
| CN114636771B (en) * | 2022-05-07 | 2022-08-12 | 北京和合医学诊断技术股份有限公司 | Method for detecting procaterol content in blood and application |
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Application publication date: 20100113 |