废水中硝基芳香化合物检测方案(液相色谱仪)

智能文字提取功能测试中

Using the Agilent 1290 Infinity SeriesLC Method Development System andAgilent MassHunter Walkup Softwarefor Multiple-Method Analysis ofEnvironmental Samples Application Note Environmental Author Abstract A.G.HuesgenAgilent Technologies， Inc. Waldbronn， Germany The Agilent 1290 Infinity Series LC Method Development Solution in combinationwith the Agilent MassHunter Walkup Software provides easy and convenientaccess to an LC system for different users with different applications. For theanalysis of the submitted samples， predefined methods including appropriatecolumn， mobile phases， and chromatographic methods are available. If needed，the information about the results are send remotely by， for example， e-mail aftercompletion of the run. The super-users take care of the LC and/or LC/MS system，providing the chromatographic methods，keeping the LC and LC/MS systemrunning， and， in case of errors， taking appropriate action. Agilent Technologies Introduction Frequently， several different applicationshave to be run on the same system ina laboratory using different columns，different mobile phases， differentcolumn temperatures， and differentchromatographic parameters. Changingthe column or changing mobile phasesis time consuming， and the risk of badcolumn connections increases with thenumber of installations. Change of themobile phase is often required due todifferent pH requirements or the needfor a different organic mobile phase. TheAgilent 1290 Infinity Series LC MethodDevelopment Solution' in combinationwith the Agilent MassHunter Walkup23offers a convenient solution. Column and mobile phases are includedin the chromatographic method by theappropriate valve position and otherparameters such as flow rate， gradientpercentage， and so forth. The super-userdefines the chromatographic methodsfor all needed applications and the userselects the appropriate method for hissamples. After submitting his samples，the analyst starts using the correctcolumn and mobile phases. The resultsare stored and sent to the user by， forexample， email. The super-user establishes the definitionof user profiles， pass words， and othersystem relevant parameters. Thesingle user or a user group can havedifferent access levels， reflecting theirchromatographic expertise. In the following， we show different tasksof an environmental laboratory， analysisof nitro aromatics， analysis of aldehydes，and analysis poly-nuclear aromatics(PNAs). Different users submittedtheir samples selecting differentchromatographic methods. Table 1. Instrumentation used. Module Product number Quaternary pump G4204A Auto sampler G4226A ALS cooler G1330B Column compartment 1 equipped with high pressure column switching valve + G1316C valve drive option #58 Column compartment 2 equipped with low pressure column switching valve + G1316C valve drive option#58 Solvent selection valve for the aqueous phases G1160A Solvent selection valve for the organic phases G1170A Diode array detector， with 10-mm path length cell G4212A Method development valve kit (1，200 bar) G4230B Sample Dr. Ehrenstorfer Nitroaromatic-Explosive Mix no. 3 (p/n 08330300)， 10 ng/pL each， Column Agilent Poroshell 120 C18， 4.6×150mm， 2.7 pm (p/n 683975-902) Mobile phase A=Water， B=Methanol Gradient 0 minutes 20 % B， at 10 minutes 30 % B. at 30 minutes 95 % B， at 31 minutes 95 % B Flow rate 0.8 mL/min Stop time 40 minutes Post time 5 minutes Injection volume 3 pL of undiluted sample was injected Column temperature 35°C DAD 254/214，235/10 nm Ref 400/80 nm Peak width： <0.013 minutes (20 Hz) Chromatographic conditions for aldehydes Mobile Phase A： Water， B： Acetone Flow rate 0.25 mL/min Gradient at 0 minutes 45 %， at 12 minutes 53 % B， at 28 minutes 67% B， at 32 minutes 67 % B，. at 33 minutes 95% B Stop time 34 minutes Post time 20 minutes Injection volume 2.1 pL lemperature 45°C Detection 360 nm/10nm Peak width > 0.025 minutes (0.5 second response time， 10 Hz) Chromatographic conditions for PNAs Column Agilent ZORBAX Eclipse PAH， 4.6×150 mm， 5 pm (p/n 959993-918) Solvents A： Water， B： Acetonitrile Gradient at 0 minutes 40 % B， at 20 minutes 95 %B Flow rate 1.5 mL/min Stop time 30 minutes Post time 5 minutes Injection volume 3pL Nitroaromatics 1Nitroguanidin23456789 Octogen (HNX) Hexogen (RDX) 1，3，5 Trinitrobenzene 2-Amino-6-Nitrotoluene 1，2-Dinitrobenzene 1，3-Dinitrobenzene 2-Amino-4-Nitrotoluene Nitrobenzene 10. Tetyl 11. 2，4，6-dinitrotoluene 12. 4-Amino-2，6-dinitrotoluene 13. 2，6-Dinitrotoluene 14. 2-Nitrotoluene 15. 4-Nitrotoluene 16. 3-Nitrotoluene 17. Nitropenta Formaldehyde-2，4-dinitrophenylhydrazone Acetaldehyde-2，4-dinitrophenylhydrazone Acrolein-2，4-dinitrophenylhydrazone Acerone-2，4-dinitrophenylhydrazone Propionaldehyde-2，4-dinitrophenylhydrazone Crotonaldehyde-2，4-dinitrophenylhydrazone Methacrolein-2，4-dinitrophenylhydrazone 2-Butanone-2，4-dinitrophenylhydrazone Butyraldehyde-2，4-dinitrophenylhydrazone Benzaldehyde-2，4-dinitrophenylhydrazone 11. Valeraldehyde-2，4-dinitrophenylhydrazone 12. m-Tolualdehyde-2，4-dinitrophenylhydrazone 123456789 Napthalene 1456789 Acenaphtylene Acenaphtene Fluorene Phenanntrene Anthracene Fluoranthene Pyrene Benzo(a)anthracene 10. Chrysene 11. Benzo(b)fluoranthene 12. Benzo(k)fuoranthene 13. B[enzo(a)pyrene 14.D[ibenzo(a，h)anthracene 15. Benzo(g，h，i)perylene 16. Indeno(1，2，3-cd)pyrene 13. Hexaldehyde-2，4-dinitrophenylhydrazone Acquisition and EvaluationSoftware OpenLAB CDS ChemStation versionC.01.05 and MassHunter Walkup softwareC.01.00 Results and Discussion The 1290 Infinity LC Series MethodDevelopment Solution can be used withup to eight columns of different lengthand internal diameter. Having installedtwo solvent selection valves and a 1290Infinity Quaternary Pump， 28 differentsolvents are available. In our example，we used three different columns and fourdifferent mobile phases for the analysis ofnitro-aromatics，aldehydes，and PNAs.The super-user had set up three differentmethods for the three applications，see Figure 1. This is done in theadministration screen， which is typicallyaccessible only by the super-user. Having defined the appropriate methodin the administration tool， the methodsare accessible for submitting samples.Typically， three steps are needed tosubmit samples， see Figures 2， 3， and 4.Figure 2 shows the first step. The userhas to fill in name， password， vial type，and number of samples. Figure 1. Method definition by the super user in the walk up administration screen. User Login Page 1 of 3 Figure 3 shows what additional sampleand method information has to be filledin. Page 2 of 3 In the third step， the sample vial has tobe put into the indicated auto samplerposition， see Figure 4. When step 3 is completed， the samplesubmission is finished and the analysisstarts. Typically， the super-user has setup a pre-run method and equilibrationmethods.An individual equilibration andpost cleaning method has to be set up foreach method with different column andmobile phase combinations. A blank runbefore the analysis of standards and reallife samples is required， otherwise， thecolumn is not sufficiently conditioned. Figure 3. Submitting samples for the analysis of nitroaromatics using the appropriate method. In our example， three samples wereprovided by one user， see Figure 5. Figure 4. Final step during sample submission. Figure 5. One user provides samples for analysis. The data were stored in different foldersaccording to the user group， see Figure 6.Typically， the users get informed aboutthe results remotely through emailor other tools， and can then evaluatethe data in detail. Figure 6 shows thechromatograms of the nitroaromaticsanalysis. The software sends an area percentreport to the user if not otherwisedefined. Figure 7 gives an example.lf calibrated reports are needed， acalibration run has to be performedby the super-user and stored with theappropriate walk-up method. Figure 6. Data storage of nitroaromatics analysis accordingly to the user group. Peak RetTime Type Width Area Area Name # [min] [min] [mAU*s] % 1 3.445 VB 0.4236 22.90172 1.1204 ? 2 3 7.349 VB 0.0868 68.71390 3.3616 ? 8.200 BB 0.0961 255.53972 12.5013 ? 9.543 VV 0.1028 291.95688 14.2829 ? Figure 8 shows an overlay of all createdchromatograms. These applicationsare high-resolution methods using UVdetection. It is also possible to add amass spectrometer for highly selectiveanalysis or to set up fast screeningmethods for high sample throughput. Theanalysis of the nitroaromatics requiredtwo wavelengths to be able to detectCompound 17. Conclusions The combination of the Agilent 1290Infinity Series LC Method DevelopmentSolution and the Agilent MassHunterWalkup Software enables users or usergroups to access an UHPLC system formultimethod applications. All methodparameters such as columns， mobilephases， gradients， and all furtherchromatographic conditions are combinedin one method and are available withoutthe need to change hardware， forexample， columns. Up to eight columnsand up to 28 mobile phases are possiblewith the system setup described inthis Application Note. The super-usercreates all needed methods， which arethen accessible by the users. Submittingsamples is done in three steps andincludes selecting the appropriate methodand putting the sample(s) into theindicated vial position. The reports can beobtained remotely for example，throughemail. References 1. A.G. Huesgen， "Agilent 1290InfinityMulti-method solution"， Agilentapplication note， Publication number5990-5600EN， May 2010. 2. "Agilent MassHunter WalkupSystem， Quick Start Guide"， Agilentpublication， Publication numberG2725-90016， July 2013. 3. "Agilent MassHunter WalkupSystem， Setup Guide"， Agilentpublication， Publication numberG2725-90017， July 2013. 4. A.G. Huesgen，"Seamless instrument-to-instrument methodtransfer of the EPA method 8330A/Bfor nitro aromatics from an Agilent1200 Series LC to the Agilent 1290 Infinity Binary LC using ISET"， Agilent Application note， Publication number 5991-1194EN. 5. S. Schneider，"Analysis of DNPH-derivatized Aldehydes andKetones using the Agilent 1220Infinity LC System with Diode ArrayDetector， Agilent Application note，Publication number 5991-1545EN. January 2013. 6. S. Volk， A. Gratzfeld-Huesgen，"Analysis of PAHs in soil accordingto EPA 8310 method with UV andfluorescence detection"， AgilentApplication note， Publication number5990-8414EN， September 2011. www.agilent.com/chem This information is subject to change without notice. CAgilent Technologies， Inc.， 2013 Published in the USA， September 1， 2013 5991-2581EN Agilent Technologies 结合使用Agilent 1290 Infinity系列液相色谱方法开发解决方案借助安捷伦MassHunter Walkup软件，可轻松便捷具有不同应用程序的不同用户可以访问LC系统。 为了提交样品的分析，预定方法包括适当的方法有色谱柱，流动相和色谱方法可供选择。 如果需要的话，有关结果的信息通过电子邮件发送到远程，例如运行完成。