CN113917066A - Method for synchronously detecting MMA (methyl methacrylate) in atmosphere by adopting ion chromatography+、DMA+、TMA+And DEA+Method (2) - Google Patents

Method for synchronously detecting MMA (methyl methacrylate) in atmosphere by adopting ion chromatography+、DMA+、TMA+And DEA+Method (2) Download PDF

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CN113917066A
CN113917066A CN202111459214.1A CN202111459214A CN113917066A CN 113917066 A CN113917066 A CN 113917066A CN 202111459214 A CN202111459214 A CN 202111459214A CN 113917066 A CN113917066 A CN 113917066A
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cation
column
suppressor
regen
eluent
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胡清静
曲克明
崔正国
姚小红
郑洪国
刘燃
朱玉姣
陆长坤
宋若晗
白莹
崔鸿武
陈剑磊
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Yellow Sea Fisheries Research Institute Chinese Academy of Fishery Sciences
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    • 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
    • G01N30/96—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 using ion-exchange
    • 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
    • G01N30/96—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 using ion-exchange
    • G01N2030/965—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 using ion-exchange suppressor columns

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Abstract

The invention relates to a method for synchronously detecting MMA in atmosphere by adopting ion chromatography+、DMA+、TMA+And DEA+The method belongs to the field of environmental monitoring, and adopts Saimer fly online ion chromatography (URG-9000D) with the configuration model of DionexTMSC‑CERSTMMethod of combining 500(2mm) salt-switching cation electrolytic regeneration suppressor, cation protection column of Dionex Ionpac CG 20 (2X 50mm) and cation analysis column of Dionex Ionpac CS20 (2X 250mm) to realize organic amine salt (MMA)+、DMA+、TMA+And DEA+) The separation is normally carried out within 27 minutes, so that the accuracy of detection data is improved, and the technology can also be applied to online detection of organic amine in the atmosphere.

Description

Method for synchronously detecting MMA (methyl methacrylate) in atmosphere by adopting ion chromatography+、DMA+、TMA+And DEA+Method (2)
Technical Field
The invention belongs to the field of environmental monitoring, and particularly relates to a method for synchronously detecting MMA (methyl methacrylate) in atmosphere by adopting ion chromatography+、DMA+、TMA+And DEA+The method of (1).
Background
Recent research proves that organic amine gases such as monomethylamine (MMA), Dimethylamine (DMA), Trimethylamine (TMA) and the like in the atmosphere can promote the generation and growth of new particles, and the formed cloud condensation nuclei can change the radiation compelling of the earth, so that the potential important climate effect is achieved. This aspect is also one of the international research hotspots today. Therefore, accurate detection of gaseous and particulate organic amines in the atmosphere is of great significance in understanding the formation mechanism of new particle generation and growth in the atmosphere.
At present, Thermo ScientificTMDionexTMThe Ion Chromatograph (IC) and an organic amine special analytical column (model is Sammerfei CS17) is one of the most common methods for detecting organic amine in the atmosphere, and compared with other methods, the method has the advantages of stable detection, good separation effect and simple operation. Therefore, the detection data is often reported in international well-known journals, and the method can also be used for comparing the concentration of the organic amine in the atmosphere in different regions around the world. Vanderboer et al (Vanderboer T.C., Petroff A., Markovic M.Z., and Murphy J.G.size distribution of alkyl amines in continuous molecular and their on-line distributions in the gas and particulate phase&Physics.2011,11(9): 4319-4332; VandeBoer T.C., Markovic M.Z., Petroff A., Czar M.F., Borduas N., Murphy J.G., Ion chromatographic separation and quantification of alkyl methyl and ethyl amides in an immobilized gas and particulate matter use monitoring and subsequent control detection of journal of Chromatography A,2012.1252(2012):74-83.) study found that when the column of URG-9000D Ion Chromatography plus CS17 was used to analyze the organic amine, DMA was detected+And TMA+Etc., but there are also some problems: (1) when NH is present4 +Or K+At higher concentrations, MMA is hindered+Detecting; (2) TMA when analyzed on CS17 column+With diethylamine ion (DEA)+) Easy to overlap and poor in separation effect (fig. 1).
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for detecting MMA in atmosphere by adopting ion chromatography+、DMA+、TMA+And DEA+Method for the preparation of four organic amines by means of Saimer fly on-line ion chromatography (URG-9000D) using DionexTMSC-CERSTMMethod of combining 500(2mm) salt-switching cation electrolytic regeneration suppressor, cation protection column of Dionex Ionpac CG 20(2 x 50mm) and cation analysis column of Dionex Ionpac CS20(2 x 250mm) to realize organic amine salt (MMA)+、DMA+、TMA+And DEA+) Separating normally within 27 min to improve the accuracy of the detected data, and the technologyThe method can also be applied to online detection of organic amine in the atmosphere.
The invention is realized by the following technical scheme:
method for synchronously detecting MMA (methyl methacrylate) in atmosphere by adopting ion chromatography+、DMA+、TMA+And DEA+Using an apparatus comprising a URG-9000D online ion chromatograph system, model DionexTMSC-CERSTMA 500(2mm) salt-switching cation electrolytic regeneration suppressor, a cation guard column model Dionex IonPac CG 20(2 x 50mm) and a cation analytical column model Dionex IonPac CS20(2 x 250 mm); the ion chromatograph with the model of URG-9000D is provided with a model of DionexTMSC-CERSTM500(2mm) salt-switching cation electrolytic regeneration suppressor, a cation guard column of Dionex Ionpac CG 20 (2X 50mm) and a cation analytical column of Dionex Ionpac CS20 (2X 250mm) model, DionexTMSC-CERSTMThe 500(2mm) salt conversion cation electrolysis regeneration Suppressor comprises two modules, namely an Eluent supressor module and an alkaline Converter module, wherein the Eluent supressor module is called ES for short, and the alkaline Converter module is called AC for short, and the connection mode is as follows:
flow path of detection sample: URG-9000D is provided with a sample inlet (Injection Valve) and a conductivity Cell (Cell) on an online ion chromatograph system, the sample inlet is connected with one end of a cation protective column of Dionex Ionpac CG 20(2 x 50mm), the other end of the cation protective column is connected with a cation analysis column of Dionex Ionpac CS20(2 x 250mm), and the cation analysis column of Dionex Ionpac CS20(2 x 250mm) is connected with ES-ELUENT IN; the ES-ELENT OUT is connected with the AC-ELENT IN; the AC-ELENT OUT is connected with CELL IN of the conductance CELL;
suppressor regeneration liquid flow path: the conductance CELL CELL OUT is connected with the ES-REGEN IN; the ES-REGEN OUT is connected with the AC-REGEN IN; the AC-REGEN OUT is connected with the waste liquid collecting pipe;
the method for detecting by using the device comprises the following steps: the ES and AC modules are activated prior to use of the device: the specific activation method comprises the following steps:
activation step of ES: removing the tube from the interface of the ES cation suppressor, positioning a first tubular member from the ES-ELUENT IN to a first waste fluid collector, and injecting at least 3 ml of deionized water into the ES-ELUENT OUT; connecting a second tubular body from ES-REGEN OUT to a second waste liquid collector, injecting at least 5ml of deionized water into ES-REGEN IN, standing for at least 20 min to fully wet and activate the ion exchange membrane and the ion exchange screen IN the ES suppressor;
activating AC: removing the hose from the interface of the AC cation suppressor, connecting a third tubular body from the AC-fluent IN to a third waste collector, and injecting at least 3 ml of deionized water into the AC-fluent OUT; connecting a fourth tubular body from AC-REGEN OUT to a fourth waste liquid collector, injecting at least 5ml of deionized water into AC-REGEN, standing for at least 20 minutes to fully wet and activate an ion exchange membrane and an ion exchange screen IN the AC suppressor;
cation analytical columns of ion-protected columns Dionex Ionpac CG 20 (2X 50mm) and Dionex Ionpac CS20 (2X 250mm) were installed on URG-9000D ion chromatography; before the ion protection column and the cation analysis column are installed, in order to prevent storage liquid and residual substances of the ion protection column and the cation analysis column from entering a cation suppressor, after the ion protection column and the cation analysis column are connected, outlets of the ion protection column and the cation analysis column are connected to a waste liquid collector, flushing is carried out for at least 30 minutes at a standard flow rate, and then the ion protection column and the cation analysis column are connected to the cation suppressor after flushing is finished; the machine was started and the apparatus allowed to equilibrate for at least 48 hours to bring the background signal value of the cation suppressor to within 2.
Further, the flow rate of the apparatus was set to 0.25ml min-1The column temperature is 60 ℃, the suppressor current is 44mA, methanesulfonic acid is used as eluent, gradient elution is carried out, and the specific eluent gradient is set as follows: the concentration of the methanesulfonic acid was maintained at 5mmol L for 0 to 11 minutes-1(ii) a 11-21 min, the concentration of the methanesulfonic acid is from 5mmol L-1Increasing the pressure to 60mmol L-1(ii) a 21-22.1 min, the concentration of the methanesulfonic acid is adjusted from 60mmol L-1Reduced to 5mmol L-1(ii) a For 22.1 to 27 minutes, the concentration of methanesulfonic acid was kept at 5mmol L-1。
Compared with the prior art, the invention has the beneficial effects that:
the method of the invention installs Dionex on the on-line ion chromatography (URG-9000D) of Saimer flyTM SC-CERSTM500(2mm) salt-switched cation electrolytic regeneration suppressor, a cation-protected column of Dionex Ionpac CG 20 (2X 50mm) combined with a cation analytical column of Dionex Ionpac CS20 (2X 250mm), organic amine (MMA) in atmosphere+、DMA+、TMA+And DEA+) The separation effect is good, so that the accuracy of data is improved, the detection method can be completed within 27 minutes, and the method can be applied to online of organic amine in the atmosphere.
Drawings
FIG. 1 is a graph showing the results of analyzing organic amines by URG-9000D ion chromatography and CS17 chromatography: 1-Na+,2-NH4 +,3-K+,4-DMA+,5-TMA+And DEA+,6-TEA+(trimethylamine)7-Mg2+,8-Ca2+。
FIG. 2 is a schematic structural diagram of the apparatus of the present invention: 1. a sample inlet, a cation protection column of 2 and Dionex IonPac CG 20(2 x 50mm), a cation analysis column of 3 and Dionex Ionpac CS20(2 x 250mm), a cation analysis column of 4, ES-ELLENT IN, 5, ES-ELLENT OUT, 6, AC-ELLENT IN, 7, AC-ELLENT OUT, 8, CELL IN, 9, CELL OUT, 10, ES-REGEN IN, 11, ES-REGEN OUT, 12, AC-REGEN IN, 13, AC-REGEN OUT, 14, a waste liquid collecting pipe, 15, ES, 16, AC, 17, a conductance CELL, 18 and a power line.
FIG. 3 shows the use of URG-9000D in combination with DionexTMSC-CERSTM500(2mm) salt-switching cation electrolytic regeneration suppressor, Dionex Ionpac CG 20 (2X 50mm) cation guard column and Dionex Ionpac CS20 (2X 250mm) cation analytical column to separate conventional ions such as ammonium ion from MMA+、DMA+、TMA+、DEA+Effect diagrams of four organic amine ions;
FIG. 4 shows the use of URG-9000D in combination with DionexTMSC-CERSTMMMA separation by 500(2mm) salt-switching cation electrolytic regeneration suppressor, Dionex Ionpac CG 20 (2X 50mm) cation guard column and Dionex Ionpac CS20 (2X 250mm) cation analytical column+、DMA+、TMA+And DEA+The effect diagram of (1);
FIG. 5 shows MMA+、DMA+、TMA+、DEA+The criteria and correlation coefficients of (c).
Detailed Description
The technical solution of the present invention is further explained by the following examples, but the scope of the present invention is not limited by the examples in any way.
Example 1
Method for synchronously detecting MMA (methyl methacrylate) in atmosphere by adopting ion chromatography+、DMA+、TMA+And DEA+The method adopts a device as shown in figure 2, and comprises a URG-9000D online ion chromatograph system and a Dionex systemTMSC-CERSTM500(2mm) salt-switching cation electrolytic regeneration suppressor, a cation guard column of Dionex IonPac CG 20(2 x 50mm) and a cation analytical column of Dionex ionnppac CS20(2 x 250 mm); the ion chromatograph with the model of URG-9000D is provided with a model of DionexTM SC-CERSTM500(2mm) salt-switching cation electrolytic regeneration suppressors (15 and 16), cation guard column 2 of Dionex IonPac CG 20(2 x 50mm), and cation analysis column 3 of CS20 Dionex lonpac CS20(2 x 250mm), model noTMSC-CERSTMThe 500(2mm) salt conversion cation electrolysis regeneration Suppressor comprises two modules, namely an Eluent supressor 15 module and an Analyte Coverter 16 module, wherein the Eluent supressor module is called ES for short, and the Analyte Coverter module is called AC for short, and the link mode is as follows:
flow path of detection sample (solid line): URG-9000D is equipped with sample inlet 1(Injection Valve) and conductance Cell (Cell)17 on the online ion chromatograph system, wherein the sample inlet 1 is connected with one end of cation protective column 2 of Dionex IonPac CG 20(2 x 50mm), the other end of the cation protective column is connected with cation analytical column 3 of Dionex Ionpac CS20(2 x 250mm), and the cation analytical column of Dionex Ionpac CS20(2 x 250mm) is connected with ES-ELUENT IN 4; ES-ELENT OUT5 is connected to AC-ELENT IN 6; the AC-ELUENT OUT7 is connected with CELL IN8 of the conductivity CELL;
suppressor regeneration liquid flow path (broken line): the conductance CELL CELL OUT9 is connected with ES-REGEN IN 10; ES-REGEN OUT11 is connected to AC-REGEN IN 12; the AC-REGEN OUT13 is connected with the waste liquid collecting pipe 14; the ES has a power line connected to the URG-9000D online ion chromatograph system.
MMA was achieved in 30 minutes using a combination of Dionex SC-CERS-5002 mm Salt model cation suppressor from Sammerfet and a Dionex IonpPac CS20(2 x 250mm) cation analytical column+、DMA+、TMA+、DEA+Thereby improving the accuracy of the detection data.
The using method of the device comprises the following specific steps:
1) activation and installation of suppressors
(1) Dionex is treated firstTMSC-CERSTMTwo modules, namely an Eluent Suppressor (ES) module and an Alkali Coverer (AC) module in a 500(2mm) salt conversion cation electrolysis regeneration Suppressor are respectively activated, and the specific steps of the activation are as follows:
activation step of ES: removing the flexible tube from the interface of the ES cation suppressor, connecting a first tubular body from the ES-ELUENT IN port to a waste liquid first collector, and injecting at least 3 ml of deionized water into the ES-ELUENT out port; additionally, a second tubular body is connected to a second waste liquid collector from an ES-REGEN OUT port, at least 5ml of deionized water is injected into the ES-REGEN IN, and then the ES-REGEN IN is kept stand for at least 20 minutes, so that an ion exchange membrane and an ion exchange screen IN the ES suppressor are fully wetted and activated; activating AC: removing the flexible tube from the interface of the AC cation suppressor, connecting a third tubular body from the AC-ELUENT IN port to a waste liquid third collector, and injecting at least 3 ml of deionized water into the AC-ELUENT OUT port; connecting a fourth tubular body from an AC-REGEN OUT port to a waste liquid fourth collector, injecting at least 5ml of deionized water into the AC-REGEN, standing for at least 20 minutes to fully wet and activate an ion exchange membrane and an ion exchange screen IN the AC suppressor;
(2) mounting Dionex on a line ion chromatograph (URG-9000D)TMSC-CERSTM500(2mm) salt-transfer cation electrolytic regeneration suppressor: linking a cation analytical column of Dionex IonpPac CS20 (2X 250mm) to ES-ELUENT IN; the ES-REGEN IN is linked with the conductance CELL CELL OUT; ES-REGEN OUT is connected with AC-REGEN IN; ES-ELENT OUT is linked to AS-ELENT IN; the AS-ELENT OUT is linked with CELL IN of the conductance CELL; the AC-REGEN OUT is connected to the waste liquid line.
2) Activation and installation of a protective column and a chromatographic column: a cation guard column of Dionex Ionpac CG 20 (2X 50mm) and a cation analytical column of Dionex Ionpac CS20 (2X 250mm) were installed on the ion chromatography (URG-9000D). Before the installation of the two, in order to prevent the storage liquid and residual substances of the guard column and the analytical column from entering the suppressor, after the guard column and the analytical column are connected, their outlets are not firstly connected to the suppressor, but connected to a waste liquid cylinder, and the waste liquid cylinder is flushed at a standard flow rate for at least 30 minutes and then connected to the suppressor after the flushing is finished. The machine was started and the instrument was allowed to equilibrate for at least 48 hours to bring the background signal value of the suppressor to within 2.
The flow rate of the apparatus was set to 0.25ml min-1The column temperature is 60 ℃, the suppressor current is 44mA, methanesulfonic acid is used as eluent, gradient elution is carried out, and the specific eluent gradient is set as follows: the concentration of the methanesulfonic acid was maintained at 5mmol L for 0 to 11 minutes-1(ii) a 11-21 min, the concentration of the methanesulfonic acid is from 5mmol L-1Increasing the pressure to 60mmol L-1(ii) a 21-22.1 min, the concentration of the methanesulfonic acid is adjusted from 60mmol L-1Reduced to 5mmol L-1(ii) a For 22.1 to 27 minutes, the concentration of methanesulfonic acid was kept at 5mmol L-1。
By using URG-9000D in combination with DionexTMSC-CERSTMRegeneration suppressor for electrolysis of 500(2mm) salt-switched cation, separation of ammonium ion from MMA by CS-20 (2X 250mm), and other conventional ions+、DMA+、TMA+、DEA+The effect graph of the four organic amine ions is shown in figure 3; MMA+、DMA+、TMA+And DEA+The separation effect of four organic amine ions (figure 4) is better. The correlation coefficient of the four organic amines can reach more than 0.999 (figure 5). MMA+、DMA+、TMA+、DEA+The detection limit of these five ions is 0.1ug L-1The reproducibility was. + -. 10%.

Claims (2)

1. Synchronous atmospheric detection by ion chromatographyMMA+、DMA+、TMA+And DEA+The method of (a), characterized in that the method is carried out using an apparatus comprising an on-line ion chromatograph, a salt conversion cation electrolysis regeneration suppressor, a cation protection column, and a cation analysis column;
the model of the online ion chromatograph is URG-9000D;
the type of the salt conversion cation electrolytic regeneration suppressor is DionexTMSC-CERSTM500, the specification is 2 mm;
the model of the cation protective column is Dionex IonPac CG 20, and the specification is 2 x 50 mm;
the model of the cation analysis column is Dionex IonpPac CS20, and the specification is 2 x 250 mm;
the on-line ion chromatograph is provided with a salt conversion cation electrolysis regeneration Suppressor, a cation protection column and a cation analysis column, wherein the salt conversion cation electrolysis regeneration Suppressor comprises an Eluent Suppressor module and an Analyte Coverter module, the Eluent Suppressor module is called ES for short, and the Analyte Coverter module is called AC for short, and the connection mode is as follows:
flow path connection of detection sample: the online ion chromatograph is provided with a sample inlet and a conductance cell, the sample inlet is connected with one end of a cation protection column, the other end of the cation protection column is connected with a cation analysis column, and the cation analysis column is connected with ES-ELUENT IN; the ES-ELENT OUT is connected with the AC-ELENT IN; the AC-ELENT OUT is connected with CELL IN of the conductance CELL;
the regeneration liquid flow path of the salt conversion cation electrolysis regeneration suppressor is connected with: the conductance CELL CELL OUT is connected with the ES-REGEN IN; the ES-REGEN OUT is connected with the AC-REGEN IN; the AC-REGEN OUT is connected with the waste liquid collecting pipe;
the method for detecting by using the device comprises the following steps: the ES and AC modules are activated prior to use of the device: the specific activation method comprises the following steps:
activation step of ES: removing the hose from the interface of the ES module, connecting a first tubular body from the ES-ELUENT IN to a first waste liquid collector, and injecting at least 3 ml of deionized water into the ES-ELUENT OUT; additionally, a second tubular body is connected to a second waste liquid collector from the ES-REGEN OUT, at least 5ml of deionized water is injected into the ES-REGEN IN, and then the ES-REGEN IN is kept stand for at least 20 minutes, so that the ion exchange membrane and the ion exchange screen IN the ES module are fully wetted and activated;
activating AC: removing the hose from the AC module port, connecting a third tubular body from the AC-ELUENT IN to a third waste collector, and injecting at least 3 ml of deionized water into the AC-ELUENT OUT; connecting a fourth tubular body from the AC-REGEN OUT to a fourth waste liquid collector, injecting at least 5ml of deionized water into the AC-REGEN, standing for at least 20 minutes to fully wet and activate the ion exchange membrane and the ion exchange screen IN the AC module;
installing the cation protection column and the cation analysis column on URG-9000D ion chromatography; before the cation protective column and the cation analysis column are installed, in order to prevent storage liquid and residual substances of the cation protective column and the cation analysis column from entering a salt conversion cation electrolysis regeneration suppressor, after the cation protective column and the cation analysis column are connected, outlets of the cation protective column and the cation analysis column are connected to a waste liquid collector, flushing is carried out for at least 30 minutes at a standard flow rate, and after flushing is finished, the cation protective column and the cation analysis column are connected to the salt conversion cation electrolysis regeneration suppressor; the machine was started and the instrument was allowed to equilibrate for at least 48 hours to reduce the background signal value of the salt conversion cation electroregeneration suppressor to within 2.
2. The method according to claim 1, wherein the flow rate of the apparatus is set to 0.25ml min-1The column temperature is 60 ℃, the suppressor current is 44mA, methanesulfonic acid is used as eluent, gradient elution is carried out, and the specific eluent gradient is set as follows: the concentration of the methanesulfonic acid was maintained at 5mmol L for 0 to 11 minutes-1(ii) a 11-21 min, the concentration of the methanesulfonic acid is from 5mmol L-1Increasing the pressure to 60mmol L-1(ii) a 21-22.1 min, the concentration of the methanesulfonic acid is adjusted from 60mmol L-1Reduced to 5mmol L-1(ii) a For 22.1 to 27 minutes, the concentration of methanesulfonic acid was kept at 5mmol L-1。
CN202111459214.1A 2020-12-29 2021-12-01 Method for synchronously detecting MMA (methyl methacrylate) in atmosphere by adopting ion chromatography+、DMA+、TMA+And DEA+Method (2) Pending CN113917066A (en)

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CN202111459214.1A Pending CN113917066A (en) 2020-12-29 2021-12-01 Method for synchronously detecting MMA (methyl methacrylate) in atmosphere by adopting ion chromatography+、DMA+、TMA+And DEA+Method (2)

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