Environmental Solutions with HPLC Solutions GuideApril 2000 General Description Agilent Technologies has developed a large number of key HPLC applications for the environmental market in Agilent Technologies' own laboratories or together with industrial laboratories and public agencies. This guide gives a condensed overview of the application solutions for this market. We have written this guide to make ordering of the entire systems easy, correct and complete. The information includes: • • • • • Detailed chromatographic conditions. Reference chromatograms. Performance of the HPLC method. Accessories from external suppliers, if applicable. References to the configuration example section at the end of the guide. Here a detailed description of the required HPLC equipment is given, including all ordering information necessary to perform the described application. Please note that the described instruments are recommendations only. Introduction Application Overview High performance liquid chromatography (HPLC) has been increasingly applied to the analysis of environmental samples. The method enables complex mixtures to be separated into individual compounds and to be identified and quantified by suitable detectors and data handling systems. Separation and detection occurs at ambient temperature or slightly above and therefore the method is ideally suited for compounds of limited thermal stability. Although HPLC detectors in general are not as sensitive as gas chromatography detectors, HPLC is a sensitive method, mainly due to the possibility of injecting large sample amounts up to 1- 2 ml per injection. Modern sample preparation techniques, like solid phase extraction and supercritical fluid extraction are also responsible for high sensitivity HPLC analysis in the ppt (parts per trillion) range. Below is an overview of environmental samples typically analyzed with HPLC, which are shown in this Solution Guide. Samples Polynuclear Aromatic Hydrocarbons Non-volatile pesticides Phenoxy-acid herbicides Carbamates Glyphosate Paraquat Benzidines and phenols Aldehydes Polynuclear Aromatic Hydrocarbons Explosives Matrix water water water water water water water air soil soil Examples naphthalene, fluorene, pyrene desethylatrazine, metoxuron, atrazine dicamba, bentazone, mecoprop butocarboxim, methomyl, aldicarb glyphosate, AMPA diquat, paraquat benzidine formaldehyde, acetaldehyde naphthalene, fluorene, pyrene octogen, nitrodiglycol, hexogen Page 4 5 6 7 8 9 10 11 12 13 Table 1 Environmental samples typically analyzed with HPLC 2 hardware must be ordered from the external vendor. Most important spare parts and consumables are available as Agilent Technologies part numbers. Documentation This document also includes ordering information for: • columns • guard cartridges (if applicable) • mobile phase modifiers (if applicable) • user guides (if applicable) 3 . Non-Agilent hardware For some applications. In this case we have set up procedures with the vendor to ensure smooth ordering and delivery of the product.Agilent hardware and Agilent ChemStations HPLC hardware and Agilent ChemStations are ordered using standard product and option numbers. This leaves all flexibility to configure the system according to local regulations and company specific requirements. Consumables. for example the Pickering Post Column Derivatization System for Carbamate Analysis. "Handbook for the HPLC analysis of polycyclic aromatic hydrocarbons" Agilent Technologies.1.4 ml/min 22 °C 2 µl of stock solution (20 ng/µl each) sample wavelength: 270/40 nm reference wavelength: 450/80 nm excitation wavelength: 275 nm emission wavelength: 350 nm Time programmed Ex and Em (for above chromatogram) Time(min) 7. A. R. Agilent Technologies primer. 1995.1 mm (Agilent p/n 79918PAH-582) A = water B = acetonitrile at 3 min 50% B to 60% B at 14.5 16. EPA Methods 550 and 550. 1993. Agilent part number 01050-90300 3. Agilent Technologies application note.05 to 1.5 21 Ex(nm) 260 270 260 290 290 250 Em(nm) 420 440 420 430 430 500 Sample Agilent PAH standard 500 µg/ml for each PAH (8500-6035) Sample preparation • liquid/liquid extraction • solid phase extraction HPLC method performance Limit of detection. "Polynuclear aromatic hydrocarbons by HPLC".5 8.8 pg <0. 1993. Agilent Technologies application note.15 % <2 to 4 % & Instrumentation see configuration example 1 on page 16 1.S. Schuster "Improved Data Quality in the Automated HPLC Analysis of PNAs (PAHs)".Hüsgen et al. FLD: Repeatabilty of RT: Repeatability of area: 50 to 500 pg 0. A.G.7 11 14. publication number 5964-3540E 4. DAD: Limit of detection.Hüsgen.G.5 min 50 %B to 90% B at 22. publication number 5968-9346E 4 . publication number 5091-7260E 2. “A New Approach to Lower Limits of Detection and Easy Spectral Analysis”.Polynuclear Aromatic Hydrocarbons ins Water Chrysene mAU 35 30 10 11 15 25 Compounds 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 naphthalene anthraquinon acenaphthylene acenaphthene fluorene phenanthrene anthracene fluoranthene pyrene benzo(a)anthracene chrysene benzo(b)fluoranthene benzo(k)fluoranthene benzo(a)pyrene dibenzo(ah)anthracene benzo(ghi)perylene indeno(123-cd)pyrene 20 6 5 8 14 12 7 1 4 15 10 5 0 9 13 16 17 23 5 10 15 Time [min] 20 25 Column Mobile phase Gradient Flow rate Column temperature Injection volume Detection UV-DAD Fluorescence 250 x 2. U. Environmental Protection Agency 5. 2000.5 min 50 %B to 95%B 0. (Agilent p/n 7992618-362) Mobile phase A = water. publication number 5952-2229 5 . "HPLC determination of 29 controlled herbicides in water supplies”Agilent Technologies application note. R. 500/80 nm HPLC method performance Limit of detection: Repeatabilty of RT: Repeatability of area: 50 ng/l (500 ml-sample) ~ 0. Reupert et al. 3 µm . B = acetonitrile Gradientat start 20 % B at 10 min 30 % B at 26 min 40 % B at 34 min 60 % B at 39 min 90 % B Flow rate 0. 350/50 nm 245/20 nm.Non-volatile Pesticide Analysis System in Water 4-nitrotoluene CH 3 mAU 350 NO2 1 2 3 4 5 6 7 9 8 13 10 11 12 14 16 15 245/20 nm 300 250 17 Compounds 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 desethylatrazine metoxuron hexazinone simazine cyanazine methabenzthiazuron chlortoluron atrazine monolinuron diuron isoproturon metobromuron metazachlor sebutylazine terbutylazine linuron metolachlor 200 150 100 50 0 0 5 10 15 20 Time [min] 25 30 35 230/20 nm 214/10 nm Sample preparation • Solid phase extraction on reversed phase disposable cartridges (see page 29 for external suppliers of disposable cartridges) Column 125 x 2 mm Hypersil ODS. 1990. 400/80 nm reference wavelengths: 214/10 nm.2 % <2% Instrumentation see configuration example 2 on page 17 & 1.2 ml/min Post time 10 min Column temperature 38°C Injection volume 3 µl or 1 µl Detection: UV DAD sample wavelengths: 230/20 nm. 2 % Repeatability of area: 1.2 % Instrumentation see configuration example 3 on page 18 & 1. (Agilent p/n 79926OD-354) A: 0.5-T dichlorprop mecoprop 2. Methods 643 and 555.5-TP 2. Environmental Potection Agency 6 .S.4.005 m KH2PO4 + 0.5 ng absolute 20 ng/l with 1000fold enrichment and 25 µl Repeatabilty of RT: < 0. 5 µm. Hypersil ODS.4-DP MCPB 10 0 5 10 Time [min] 15 Column Mobile phase Sample preparation • Solid phase extraction on reversed phase disposable cartridges (see page 29 for external suppliers of disposable cartridges) Gradient Flow rate Column temperature Detection: UV VWD 100 x 4.001% CH3COOH at 0 min 15 % B at 16 min 50 % B at 21 min 15 % B 0.35 ml/min 45 °C 230 nm as detection wavelength HPLC method performance HPLC method performance Limit of detection: 0. U.4-D MCPA 2.0 mm.4.001% CH3COOH B: ACN/methanol = 1/1 + 0.Phenoxy-acid Herbicides in Water Bentazone O N N H CH CH3 SO 2 CH3 4 mAU 2 20 1 6 9 3 5 10 7 8 11 12 Compounds 1 2 3 4 5 6 7 8 9 10 11 12 dicamba 8-OH-bentazone 6-OH-bentazone bentazone 2. Carbamates in Water Methiocarb CH3 CH3S CH3 O OCNHCH3 LU 900 µl injection volume 19 1 18 2 3 4 5 6 Aldicarb sulfone 6 Aldicarb Aldicarb sulfoxide 7 Propoxur Oxamyl 8 Carbofuran Methomyl 9 1-Naphthol 3-OH-Carbofuran 10 Carbaryl 11 Methiocarb 7 8 9 10 1 2 3 4 5 Compounds 1 2 3 4 5 6 7 8 9 10 11 aldicarb sulfone aldicarb sulfoxide oxamyl methomyl 3–hydroxycarbofuran aldicarb propoxur carbofuran 1–naphthol carbaryl methiocarb 17 11 16 15 14 10 15 20 Time [min] Column Mobile phase Gradient Run time Post time Column temperature Injection volume Detection: UV VWD 150 x 4.5–5 % Instrumentation see configuration example 7 on pages 22–24 & 1. C8 phase (Pickering Laboratories). A: water = 100 % B: methanol = 0 % at 1 min 0 % B at 31 min 75 % B 45 min 5 min 42 °C 900 µl + 800 µl Fluorescence excitation wavelength 330 nm emission wavelength 450 nm photo-multiplier gain 12 4s 0. 5 µm. 108.3 ml/min 100 °C ambient 25 30 35 800 µl injection volume 250 ppt each Matrix • drinking water Sample preparation • water is direct-injected (according to EPA Method 531. 2000. Environmental Protection Agency 3.3 ml/min 0.1) Response time Post-column derivatization Reagent pump flow rate for hydrolization agent (0. 1994 2. U.S.6 mm. Post-column LC analysis of 23 n-methylcarbamates”.1. Agilent Technologies primer. “A New Approach to Lower Limits of Detection and Easy Spectral Analysis”. Method 531. publication number 5968-9346E 7 .1 % 0. Pickering Laboratories application note.05 m NaOH) flow rate for derivatization agent (OPA) hydrolysis temperature derivatization temperature HPLC method performance Limit of detection: Repeatabilty of RT over 10 runs: Repeatability of area over 10 runs: 100 ppt with 900 µl injection volume with S/N = 2 < 0. 5 10 Time [min] 12. 8 µm (Pickering p/n 1954150) Mobile phase A: 5 mM KH2PO4. publication number 5091-3621E 2.0 B: 5 mM KOH A:B = 100:0 Gradient at 15 min 0 % B at 17 min 100 % B Flow rate 0. Method 547.5 5 Matrix • drinking water Sample preparation • water is direct-injected (according to EPA method 547) 2. Rainer Schuster.2 % Instrumentation see configuration example 7 on pages 22–24 & 8 1.5 7 Glyphosate AMPA Compounds • • glyphosate AMPA (aminomethylphosphonic acid) 6.3 ml/min HPLC method performance Limit of detection Repeatability of RT over 10 runs Repeatability of areas over 10 runs 1 ppb with S/N = 2 < 0.and post-column sample treatment for the analysis of glyphosate”. pH 2.5 20 Column 150 x 4 mm.S.4 ml/min Column temperature 55 °C Injection volume 50 µl Detection: Fluorescence excitation wavelength: 230 or 330 nm emission wavelength: 465 nm slit width excitation: 2 mm (25 nm) slit width emission 1: 4 mm (50 nm) slit width emission 2: 4 mm (50 nm) photo-multiplier gain: 12 cut-off filter: 370 nm lamp: 55 Hz always on response time: 4s Post-column derivatization Reagent pumps flow rate for oxidation agent OCl. cation exchange. 1992.8 % 2.5 5 7.3 ml/min flow rate for derivatization agent OPA = 0. “A comparison of pre. K+ form.= 0.5 6 5.Glyphosate in Water Glyphosate O HO CH 2 %F H N OH P CH 2 O OH 7. Agilent Technologies application note. from Pickering Laboratories.5 15 17. U. Environmental Protection Agency . ODS Hypersil.5 4 310 nm 256 nm Sample preparation • solid phase extraction on reversed phase disposable cartridges 4. page 19 Repeatability of RT Repeatability of areas & 1.Paraquat in Water Paraquat mAU CH3 N+ N+ CH3 Diquat Paraquat 175 150 Compounds • • diquat paraquat 125 100 75 50 25 0 0 0.5 Time [min] 3 3.5 ml/l TEA (triethylamine) pH = 2.12% < 1% Instrumentation see configuration example 4. U.5 with phosphoric acid 0.1. Method 549. 5 µm.S.5 1 1.1 mm. 0. (Agilent p/n 79916OD-552) water + 0.5 g hexane-sulfonic acid = 3.5 2 2.4 ml/min 15 °C 10 µl sample wavelengths: 256/10 nm and 310/10 nm reference wavelength: 450/100 nm HPLC method performance Limit of detection 1 ng (injected amount).5 Column Mobile phase Flow rate Column temperature Injection volume Detection: UV-DAD 100 x 2. Environmental Protection Agency 9 .4 µg/l with an enrichment factor of 100 ~ 0. 13 ppb < 0. with AgCl/KCl reference electrode response time: 4 s range: 0.3 % <2% Instrumentation see configuration example 5.001 M Na2EDTA) and acetonitrile.08 ppb 0. 5 µm (Agilent p/n 79924O2-584) water (with 0. 50:50 0.3-Dichlorobenzidine 18.6 pg Sample preparation • liquid/liquid extraction 4 6 Time [min] 8 10 12 Column Mobile phase Flow rate Injection volume Detection: 250 x 4 mm Spherisorb ODS-2. page 20 10 .3-dichlorobenzidine 3.Benidines and Phenols in Water Benzidine H2N NH2 Benzidine 24 pg Compounds • • benzidine 3.7 V HPLC method performance Limit of detection benzidine 33'-dichlorobenzidine Repeatability of RT Repeatability of areas 0.8 ml/min 20 ml Electrochemical glassy carbon working electrode.1 M NaAc and 0.5 mA temperature: 40 °C potential: 0. Aldehydes in Air Formaldehyde O H C H mAU -0.19 % 0.VWD 100 x 2. 5 µm (Agilent p/n 79916OD-552) A= water.80 % Instrumentation see configuration example 3.79 to 2.4-dinitrophenylhydrazine -1. page 18 11 . B= acetonitrile at start 27 % B in 13 min 98 % B 0.5 -3 0 2 4 6 Time [min] 8 10 12 Column Mobile phase Gradient Flow rate Column temperature Injection volume Detection: UV.5 -2 -2.1 mm. Hypersil ODS.5 1 3 6/7 2 4 5 8/9 10 11 13 12 -1 Compounds 1 formaldehyde 2 acetaldehyde 3 aceton 4 acroleine 5 propionaldehyde 6/7 butanon + crotonaldehyde 8/9 n-butyral+methacroleine 10 benzaldehye 11 valeraldehye 12 m-toluoaldehyde 13 hexanaldehyde Sample preparation • 15 µg/ml of each aldehyde was derivatized with 2.40 to 0.45 ml/min 30 °C 1 µl 365 nm HPLC method performance Limit of detection Repeatability of RT Repeatability of areas ~ 10 pg 0. 1995.5 260 8. FLD: Repeatabilty of RT: Repeatability of area: 50 to 500 pg 0. Castelli. R. 1993. D. Schuster "Improved Data Quality in the Automated HPLC Analysis of PNAs (PAHs)".4 ml/min 22 °C 2 µl of stock solution (20 ng/µl each) sample wavelength: 270/40 nm reference wavelength: 450/80 nm excitation wavelength: 275 nm emission wavelength: 350 nm Time programmed Ex and Em (for above chromatogram) Time(min) Ex(nm) Em(nm) 7. C. Agilent Technologies. Agilent Technologies application note.Hüsgen. GC.5 min 50 %B to 90 % B at 22. page 16 1. part number 01050-90300 3.8 pg <0. GC/MSD and HPLC Applied to Several Types of Environmental Samples" Journal of Chromatographic Science.05 to 1. DAD: Limit of detection. J.1 mm (79918PAH-582) A = water B = acetonitrile at 3 min 50 % B to 60 % B at 14. "Handbook for the HPLC analysis sis of polycyclic aromatic hydrocarbons". Gere. 1993. July 1993 4. "Polynuclear aromatic hydrocabons by HPLC". publication number 5091-7260E 2. publication number 5964-3540E 12 . A.5 290 21 250 Sample preparation • soxhlet extraction • ultrasonic-stimulated liquid extraction • supercritical fluid extraction according to EPA Method 8310 420 440 420 430 430 500 HPLC method performance Limit of detection.5 290 16. A. Hedrick. P.15 % <2 to 4 % & Instrumentation see configuration example 1.R. L.5 min 50 %B to 95 %B 0. Randall "Bridging the Automation Gap between Sample Preparation and Analysis: An Overview of SFE.R.G. Knipe.G.Polynuclear Aromatic Hydrocarbons in Soil Anthracene mAU 200 175 150 6 10 11 15 14 12 8 7 DIN/EPA standard 16 5 1 4 Compounds 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 Naphthalene Anthraquinon Acenaphthylene Acenaphthene Fluorene Phenanthrene Anthracene Fluoranthene Pyrene Benzo(a)anthracene Chrysene Benzo(b)fluoranthene Benzo(k)fluoranthene Benzo(a)pyrene Dibenzo(ah)anthracene Benzo9ghi)perylene Indeno(123-cd)pyrene 9 13 17 125 100 50 23 75 25 Extraction via SFE 0 5 10 Time [min] 15 20 25 Column Mobile phase Gradient Flow rate Column temperature Injection volume Detection UV-DAD Fluorescence 250 x 2.Hüsgen et al.G.7 270 11 260 14. Agilent Technologies application note. Reupert.6-Trinitrotoluene 2-Amino 4. page 21 & 1. LWA Düsseldorf 13 .5-Trinitrobenzene 1. 3 µm (Agilent p/n 7992618-362) A= water B= acetonitrile at start 15 % B in 30 min 50 % B in 40 min 90 % B 0. Method 8330. publication number 5091-7626E 2.3. 6-Dinitrotoluene 2-Nitrotoluene 4-Nitrotoluene 3-Nitrotoluene Nitropenta Diphenylamine 60 1 2 3 40 20 0 0 5 10 15 20 Time [min] 25 30 35 40 * Column Mobile phase Gradient Flow rate Post time Column temperature Injection volume Detection: UV-DAD Sample preparation • Sample was extracted with ACN and ultrasonic bath (according to EPA Method 8330) 125 x 2 mm Hypersil ODS.S. 6-Dinitrotoluene 2.31 ml/min 8 min 38°C 5 µl sample wavelength: reference wavelength: sample wavelength: reference wavelength: 235/20 nm 400/80 nm 215/20 nm 350/50 nm HPLC method performance Limit of detection Repeatability of RT Repeatability of area 8-20 mg/kg < 0. 4-Dinitrotoluene 2. Environmental Protection Agency * Method developed by R.4. 6-Dinitrotoluene 4-Amino-2. "HPLC analysis of explosive constituents in soil samples" Agilent Technologies application note. Rainer Schuster et al.Explosives in Soil 4-nitrotoluene CH 3 mAU 215/20 nm 18 5 11 12 6 4 7 9 8 10 13 14 15 16 17 235/20 nm 80 NO2 Compounds 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 Octogen Nitrodiglycol Hexogen Nitroglycol 1.2 % ~ 2 % except tetryl and nitroglycerine due to decomposi- Instrumentation see configuration example 6. U.3-Dinitrobenzene Nitroglycerine Tetryl 2. 1993. high sensitivity diode-array detector for qualitative and quantitative analysis. extensive self. multimedia tools for effective maintenance. temperature-controlled column compartment with a standard Peltier element for heating and cooling. Through its design the most demanding laboratory objectives are achieved: • reduces operating cost: no need for helium through all electric design. online spectral acquisition and spectral libraries. FLD data can be combined with diode-array detector data. • helps to comply with regulations and quality standards through built-in.Instrumentation Agilent 1100 Series modules and systems The Agilent 1100 Series HPLC systems and Agilent ChemStations are ideally suited for analysis of environmental samples. at and below ambient temperature. which removes trace levels of air for higher detector sensitivity and stability of retention times. for example in detector sensitivity for lowest detection limits through new designs.950 nm. Further features for the environmental laboratory include: variable-volume autosampler with integrated injector program for precolumn derivatization. • saves operator training time through intuitive user interface and built-in online tutorials. online vacuum degasser. Agilent Technologies' 24-hour service response. in the wavelength range of 190 . • maximizes instrument uptime through use of field proven parts. • maximizes productivity through fast system set up and intelligent automation. which eliminates analytical errors due to temperature fluctuations above. and • highest system performance. fast. trouble-free and labor-saving autovalidation features. works with 2-mm columns to reduce solvent costs. high sensitivity fluorescence detector (FLD) with multiple signal detection.and remote diagnostics. 14 . AgilentChemStation Agilent ChemStations are recommended for instrument control and data evaluation. • automation of potential optimization. • easy change of electrodes. Other features for the environmental laboratory include: • electrochemical self-cleaning routines. The detector can be controlled from the integrated keyboard and from the Agilent ChemStations. 15 . Electrochemical detector The Agilent 1049A electrochemical detector is recommended for special applications such as phenols and aromatic amines. Features for the environmental laboratory include: • system suitability software for automated and customized method validation and system suitability testing. and • software for automated identification and quantitation based on diode-array detection and spectral libraries (Agilent ChemStation for LC 3D systems). • report generator to print analysis reports according to regulatory and client requirements. Configuration Example 1 Description Order Agilent 1100 Series automated quaternary LC 3D sys. (This handbook was developed for the HP 1050 Series. . software and peripherals.page 12 CAN 5181-1516 G1315A HP-IB 10833D G1321A G1319A Printer Note for all Agilent ChemStation systems: Due to the rapid progress in PC hardware. .0. . 16 . . . . Microsoft ® Windows NT 4. . . . Includes: • Agilent 1100 Series quaternary pump with Agilent 1100 Series vacuum degasser (G1354A) • Agilent 1100 Series autosampler (G1313A) • Agilent 1100 Series diode-array detector (G1315A) • Standard flow cell. . . HP computer. . . . Agilent 1100 Series fluorescence detector. . the components of the Agilent ChemStation systems may be replaced by equivalent or better models. . Guard cartridge holder.1. 500 µg/ml. . . 610. . . it can be used as a guideline for the Agilent 1100 Series. CD-ROM drive. G2180AA spectral processing software. PAH guard cartridges (30 x 2 mm). PAH operating procedures.) Minimum instrument for PNAs according to EPA methods 550. . . . . 2/pk. 550. 8310: • Gradient pump • Manual injector • Column oven • Variable wavelength detector • Fluorescence detector • Data system is recommended. Agilent 1100 Series thermostated column compartment. . 10. .mm path length (G1315A #018) • Hypersil ODS column and check-out sample • Agilent ChemStation for LC 3D systems (G1319A) Includes G2170AA single instrument Agilent ChemStation software. . . PAH standards. . CAN 5181-1516 G1327A CAN 5181-1516 G1354A G1316A G1321A 8500-6035 79918PA-532 79918PA-100 01050-90300 CAN 5181-1516 G1316A Configuration example for: PAHs in water .page 4 PAHs in soil . . . . . . .G1357AA tem. . LaserJet printer. Pesticide standards.) G1316A 5062-2500 01090-90300 CAN 5181-1516 G1354A CAN 5181-1516 G1327A CAN 5181-1516 Configuration example for: Non-volatile pesticides in water . It can be used as a guideline for the Agilent 1100 Series. Microsoft® Windows NT 4. (This handbook was developed for the HP 1090 Series. Pesticide operating procedures. LaserJet printer. . Agilent 1100 Series thermostatted column compartment. HP computer. G2180AA spectral processing software. 10 mm path length • Hypersil ODS column and checkout sample • Agilent ChemStation for LC 3D systems (G1319A) Includes G2170AA single instrument Agilent ChemStation software.0.Configuration Example 2 Description Order Agilent 1100 Series automated quaternary LC3D G1357AA system. Includes: • Agilent 1100 Series quaternary pump with Agilent 1100 Series vacuum degasser (G1354A) • Agilent 1100 Series autosampler (G1313A) • Agilent 1100 Series diode-array detector (G1315A) • Standard flow cell.page 5 G1316A HP-IB 10833D G1315A G1319A Printer 17 . CD-ROM drive. . . . . . Agilent ChemStation for LC 2D systems. . . . Includes 2170AA single instrument LC ChemStation software. . . CD-ROM drive. . .page 11 G1316A HP-IB 10833D G1314A G1319A Printer 18 . . . . . . . LaserJet printer. . . . . . . . Includes: • Agilent 1100 Series quaternary pump with Agilent 1100 Series vacuum degasser (G1354A) • Agilent 1100 Series autosampler (G1313A) • Agilent 1100 Series variable wavelength detector (G1314A) • Standard flow cell.Configuration Example 3 Description Agilent 1100 Series automated quaternary LC 2D system.page 6 Aldehydes in air . .0. . . . . . . HP computer. Minmum requirements for chlorinated acids and bentazone (phenoxy-acid) according to EPA method 555: • Gradient pump • Diode-array detector • Manual injector or cooled autosampler • Data system is necessary CAN 5181-1516 G1354A CAN 5181-1516 G1327A CAN 5181-1516 Configuration example for: Phenoxy-acid herbicides in water . . Agilent 1100 Series thermostatted column compartment. . Order G1356AA G1356AA #880 G1317A G1316A Minmum requirements for bentazone (phenoxy-acid) according to EPA method 8643: • Gradient pump • Variable wavelength detector • Manual injector for 100 µl • Data system is recommended. . . . and Microsoft Windows NT 4. 10-mm path length (G1314A #018) • Agilent 1100 Series control module Delete control module. 0. . 10. . Agilent 1100 Series vacuum degasser.mm path length. . Agilent 1100 Series autosampler. Needs to be specified. Minimum for paraquat according to EPA method 549. Agilent 1100 Series diode-array detector.page 9 G1316A HP-IB 10833D G1315A G1319A Printer 19 . . LaserJet printer. G1322A CAN 5181-1516 G1310A CAN 5181-1516 G1313A CAN 5181-1516 Configuration example for: Paraquat in water . .1 • • • • • Isocratic pump Manual injector to deliver 200 µl Column oven Diode-array detector Data system is recommended. and Microsoft Windows NT 4. Agilent 1100 Series thermostated column compartment. . Agilent ChemStation for LC 3D systems. . HP computer. Standard flow cell. . . Includes G2170AA single instrument LC ChemStation software. . CD-ROM drive. G1315A G1315A #018 G1322A G1319A Order G1310A G1316A G1313A Strongly recommended. G2180AA spectral processing software. . .Configuration Example 4 Description Agilent 1100 Series isocratic pump. . electrochemical or fluorescence detector) CAN 5181-1516 G1313A HP-IB 10833D G1316A G1317A Remote 5061-3378 1049A Printer HP-IB 10833D Configuration example for: Benzidines and phenols in water . CD-ROM drive.page 10 20 . solid state reference electrode. Agilent 1100 Series autosampler. outlet tubing.0. Agilent 1049A programmable electrochemical detector. Agilent ChemStation for LC 2D systems. Order G1354A G1316A G1313A 1049A G1317A Minimum requirements for benzidines according to EPA methods 605: • • • Isocratic pump Manual injector Electrochemical detector CAN 5181-1516 G1354A Minimum requirements for phenols according to EPA method T08: • Isocratic pump • Manual injector • Detector (variable wavelength. HP computer. Agilent 1100 Series thermostated column compartment. GPIB interface and remote cable. LaserJet printer. glassy carbon working electrode. . Includes Agilent 1100 Series vacuum degasser. Includes inlet capillary.Configuration Example 5 Description Agilent 1100 Series quaternary pump. Includes G2170AA single instrument LC ChemStation software. and Microsoft Windows NT 4. . and Microsoft Windows NT 4.0. . . . . . . Agilent 1100 Series thermosttated column compartment. G2180AA spectral processing software. 10 mm path length (G1315 #018) • Agilent ChemStation for LC 3D system (G1319A) Includes G2170AA single instrument LC ChemStation software. . . .Configuration Example 6 Description Agilent 1100 Series automated quaternary LC3D system. . HP Vectra color computer. . Includes: • Agilent 1100 Series quaternary pump with Agilent 1100 Series vacuum degasser (G1354A) • Agilent 1100 Series autosampler (G1313A) • Agilent 1100 Series diode-array detector (G1315A) • Standard flow cell. CD-ROM drive. Order G1357AA G1316A Minimum requirements for explosives according to EPA method 8330 • Minmum requirements for explosives according to EPA method 8330 • Isocratic pump • Variable wavelength detector • Manual injector for 100 µl CAN 5181-1516 G1354A CAN 5181-1516 G1313A HP-IB 10833D G1316A G1319A Printer HP-IB 10833D Configuration example for: Explosives in soil . .page 13 G1315A 21 . . LaserJet printer. 400 µl Post column reactor Data system is recommended. . . . Includes 0. HP computer. Post-column reaction kit. Agilent 1100 Series fluorescence detector. Extended injection range option with 900-µl syringe. . . . To be installed in Agilent 1100 Series system when used with Pickering post column reaction system.0. .Configuration Example 7 Description Agilent 1100 Series quaternary pump. Includes PCX5200 post-column reaction instrument plus columns and reagents to convert a conventional HPLC system into a system specific for carbamate analysis (EPA Method 531. G1317A Order G1354A G1354A # 030 G1313A G1313A #021 G1313A #020 G1321A G1313-68712 For glyphosate application only. connection tubing) Minmum requirements for carbamates according to EPA method 8318: same as above. . . Includes Agilent 1100 Series vacuum degasser.1: • • • • • Gradient pump Fluorescence detector Manual injector for 200 .page 7 Glyphosates in water .25-mm id capillary. . Agilent 1100 Series autosampler. . Pickering System for post-column hydrolization and derivatization. Tefzel seal. Seal wash option. Alternatively Minimum requirements for carbamates according to EPA method 531. . .page 8 HP-IB 10833D G1317A Printer 22 . . seat assy (PEEK) and needle assy (PEEK). length 70 cm. . CAN 5181-1516 G1354A PCX 5100 (incl. . Includes G2170AA single instrument LC ChemStation software. except: • Manual injector for 20 µl CAN 5181-1516 G1313A G1321A Configuration example for: Carbamates in water . . . . Agilent ChemStation for LC 2D systems. and Microsoft Windows NT 4. CD-ROM drive. . Multi-draw kit. .1) or glyphosate analysis. See the following two pages for detailed ordering information of Pickering Systems. LaserJet printer. . 10 g (2) (3700-2000) Hydrolysis reagent for carbamate analysis. 12 components. 4 x 950 mL (CB910 ) Thiofluor™ crystals.6 x 150 mm (1846150) Carbamate column.6 x 250 mm (1846250) Guard cartridge holder with 3 guard cartridges (18ECG001) o-Phthalaldehyde (OPA) crystals. Application and Post-column Kit Includes: Carbamate column. 5 g (O120) OPA diluent for carbamate pesticide analysis.5 mL (1700-0063) 1152-2211 1152-2212 0352-0001 0352-0002 23 . 4. 12 components. reservoir assemblies for hydrolysis and OPA reagents. 10 g (two) (3700-2000) Carbamate analysis hydrolysis reagent. gas manifold. 1. expanded resolution (0840250) Guard cartridge holder with 3 carbamate guard cartridges (18ECG001) o-Phthalaldehyde (OPA) crystals.5 mL (2) (1700-0063) Application and Post-column Kit Includes: Carbamate column (4. C18. 250 mL (1700-1032) Carbamate test mixture. 1.Description Order (Pickering) Carbamate Analysis System A complete system consists of a PCX5200 post-column instrument. Same as 1152-2211 for 240 Volt operation. 250 mL (1700-0132 ) Carbamate test mixture. 4 x 950 mL (CB130) ChlorAC™ buffer for aqueous samples. Application Kits All kits include the Carbamate Analysis Applications Manual. 4 x 950 mL (CB910) Thiofluor™ crystals. 4. PCX5200 dual reagent post-column derivatizer system. 120 Volt operation.0 x 250 mm) C8. 4 x 950 mL (CB130 ) ChlorAC™ buffer for aqueous carbamate samples. 5 g (O120 ) OPA diluent for carbamate analysis. C18. and one or more application kits containing the columns and reagents for converting a liquid chromatograph into an analyzer specific for carbamate analysis. PCX5200 dual reagent post-column derivatizer system. 120 Volt operation. 2. 5 mM KH2PO4. Application and Post-column Kit Includes: Glyphosate analysis applications manual Glyphosate column.5 µg/mL (1700-0080) 1152-2211 1152-2212 0352-0010 24 .5 mL. 3 x 20 mm (1953020) o-Phthalaldehyde (OPA) crystals. 5 g (O120 ) OPA diluent for glyphosate analysis. 4 x 950 mL (GA104) Hypochlorite diluent for glyphosate analysis. and one or more application kits containing the columns and reagents for converting a liquid chromatograph into an analyzer for glyphosate analysis.Description Order (Pickering) Glyphosate Analysis System A complete system consists of a PCX5200 post-column instrument. 1. 4 x 950 mL (K200) Column regenerant for glyphosate analysis. two components. 4 x 950 mL (GA116) Glyphosate eluent. cation-exchange. 4 x 150 mm (1954150) Glyphosate guard column. reservoir assemblies for hydrolysis and OPA reagents. K+ form. 5 mM KOH. 10 g (2) (3700-2000) RESTORE™ for metal ion decontamination of column or guard (1700-0140) Glyphosate test mixture. pH 2. K+ form. 950 mL (RG019) Thiofluor™ crystals.0. gas manifold. Same as 1152-2211 for 240 Volt operation. V Rysterborgherweg 20 P. 222 Red School Lane Phillipsburg. CA 94043 Tel: +1-650-694-6700 Fax: +1-650-968-0749 e-mail:
[email protected]. 1951 Colony Street. Niles.External Suppliers Materials supplied by the following vendors were used in the referenced applications: External supplier for disposable cartridges (applications pages 5.netcom.647-7600 Fax: + 1-708 647-9600 External supplier for post column derivatization system (applications pages 22–24) Europe LC Tech Bahnweg 41 D-84405 Dorfen. Illinois 60714 Tel: +1-708.Box 1 NL-7400 AA Deventer Tel: +31-5700-87500 Fax: +31-5700-11342 USA J. Baker B. 6.77694 Kehl/Rhein Tel: +49-7851/7069 Fax: +49-7851/75362 USA Cole-Pormer™ International 7425 North Oak Park Ave. Germany Tel: +49-8081-93680 Fax: +49-8081-936810 USA Pickering Laboratories Inc. 9) Europe J. Baker Inc. Suite S Mountain View.com 25 .T.T. NJ 08865 Tel: +1-908-8592151 Fax: +1-908-8599318 External supplier for ultrasonic bath (application page 13) Europe Novodirect GmbH Am Storchennest 24 D. 1 % Hexansulf. 79916OD-552 or 125x4.0/ 285 nm MeOH or 125x4.#) 531. 50% B Electrochemical 0. isocratic VWD or DAD 212 nm 1100 iso /VWD or DAD 26 .6 mm id 79919QA-754 RP-C18.3% TEA.1% H3PO4 0. 79916OD-552 or 125x4. 79926OD-564 RP-C18. 79918PAH-584 H20/ACN VWD or grad. 79926Od-564 H20/ACN 35% B. 100x2.1. 25 to 75% B Post column deriv. 65% B VWD or DAD 220 nm 1100 iso/VWD or DAD 638 (draft) Nitroanilides Oryzalin. 79916OD-552 or 125x4.05% H3PO4/MeOH VWD or DAD 225 nm or DAD 1100 iso/VWD 605 Amines Benzidines Other aromatic amines PNAs 2 ring (naphthalene) to 7 ring (coronene) Surface water drinking water Soil/Sludge Water ODS-2.1 M NaAc/ACN isocratic . 100x2. 100x2.1. 79916OD-552 or 125x4.01 M KxHxPO4. 2.5 Post column deriv.0. 2.0. 1100 DAD or VWD 635 (draft) Rotenone Waste water Drinking water Liquid/liquid extraction H220/ACN isocratic.6 mm. Butralin.1 mm id grad .05% TBAS/pH7. Fluorescence 1100 grad/FLD + Pickering system 549. 550.1 610 8310 Liquid/liquid extraction or solid phase extraction Quartz filter/XAD2 Vydac PNA 250 x 2. 2. 2.1 or 4 mm id 100x2. 79916OD-552 or 125x4.7 Volt 1100 iso 1049 550. Pendimethalin.0. 2. 79916OD-552 isocratic 30%B RP-C18.34 g/l KH2PO4 0. 55 to 95% B 0.1 or 4 mm id. VWD or DAD 0.1. 79926OD-564 Filtration and direct injection 0.LC Environmental Quick Reference Guide (EPA Methods) Method Sample Matrix Sample Preparation Direct injection of 400 ml water Liquid extraction Direct injection of 400 ml water Solid phase extraction Cartridge/disk 100 x 4.0.1 (draft) Hexa-/ Dichlorophene Waste water extraction Liquid/liquid 4 mm id. 79926OD-564 RP-C18. 50% B VWD or DAD 294 nm 1100 iso/ VWD or DAD 636 Bensulide (draft) Waste water Liquid/liquid extraction H20/ACN isocratic .1. Fluorescence MWD or DAD 310 and 256 nm 1100 iso/1046 + Pickering system 1100 iso DAD 5091-3621E Column Mobile Phase Detection Instrumentation Reference (pub.1.0. 79926OD-564 RP-C18. 79918PAH-582 250 x 4. 100x2..1 Carbamates 11 N-Methylcarbamates 8318 547 Glyphosate Drinking water Soil/sludge Drinking water Drinking water RP-C18 Pickering H20/MeOH grad.1 mm.1 Quats Paraquat/ Diquat 604. Benfluralin Bendiocarb Waste water extraction Liquid/liquid 79916OD-552 H20/ACN 230 or 285 nm VWD or DAD 1100 grad/ DAD 639 (draft) Waste water Liquid/liquid extraction RP-C18.1 or isocratic 68% 0. 2.1.1 or 4 mm id.0. 250x4 mm id 79924O2-584 0. pH 2.1 or 4 mm id 100x2.1 or 4 mm id 100x2. acid 0. 60 to 100% B DAD or Fluorescence 1100 grad/ VWD/FLD or 5091-7260E TO 13 Air 1100 grad/ DAD/FLD 631 Benomyl/ Carbendazim (as Benomyl) Waste water Liquid/liquid extraction 79926OD-564 RP-C18. 245 nm Ger DIN38407F12 Surface water extraction Water Filtration and solid phase RP-C18. 20 to 50% B VWD or DAD 365 nm 1100 grad DAD or VWD TO8 Phenol Methylphenols Phenol. Br. N03. 79916OD-552 or 125x4. 100x2. Cl. 100x2. 60% B VWD or DAD 274 nm Electrochemical 1. 125 x 2mm. 20 to 50% B DAD 1100 grad DAD 214. 230.0. 100x2.1 mm id 79916OD-552 H20/ACN grad. 20 to 50% B DAD 220 nm 1100 grad DAD Anions F. 100x2. liquid/ solid Adsorption and derivatization (DNPH) Impigner 0. 79916OD-552 ODS-2. N02. 2. 0.1.1 mm id 79916OD-552 H20/ACN grad. 2. 30%B H20-KNO3/MeOH isocratic. #) 1100 iso /VWD or DAD 1100 iso/FLD 640 (draft) 641 (draft) Mercaptobenzothiazole Thiabendazole Waste water RP-C18. Kresol Chlorophenols Air Surface water RP-C18.1 Volt 1100 iso VWD or DAD 1100 iso/1049 LC Environmental Quick Reference Guide Non-EPA Methods Sample Matrix Sample Preparation Solid phase extraction Column Mobile Phase Detection Instrumentation Reference (pub. H20/ACN isocratic .1 mm id 79916OD-552 solid phase H20/ACN grad. 15 to 55% B ODS.05% TBAS/pH 7. 35% B 0. P04. S04 Filtration/direct injection Agilent-IC 79923IC-564 H20/ACN and modifier negative UV 266 nm 1100 iso/VWD degasser 27 .005M KH2PO4/ ACN/MeOH=1/1 grad.01 M KxHxPO4 0.0.0 79926OD-564 H20/ACN grad. #) N-Herbicides Urea Herbicides Surfactants Triazines Water Anilides Alkylsulfonates Soil/sludge RP-C18.1.1 mm id 79916OD-552 RP-C18.1N NaCH Filtration and direct injection RP-C18.1. 79916OD-552 or 125x4. 2.1 or 4 mm id 100x2. 50 to 100% B 0. 2.001%CH3COOH Soil/Water (ultrasonic) 554 8315 TO5. 79926OD-564 RP-C18.1 or 4 mm id 100x2.1. 3 µm H20/MeOH DAD 214/235 nm 1100 grad DAD 5091-7626E VWD or DAD 256 nm 1100 grad DAD 643 555 Waste water Drinking + acids DAD 1100 grad DAD 214 nm ea.LC Environmental Quick Reference Guide (EPA Methods) Method Sample Matrix Sample Preparation Liquid/liquid extraction Direct injection Column Mobile Phase Detection Instrumentation Reference (pub.1 or 4 mm id 100x2.0 79926OD-564 Acetate/ACN isocratic. TO11 Drinking water Soil/sludge Air Derivat.0/ MeOH VWD or DAD 317 nm FLD Ex/Em 300/360 nm Waste water 79926OD-564 642 O-Phenylphenol Biphenyl Phenoxy-acids 9 Phenoxy Bentazone 8330 (draft) Nitroaromatics Explosive constituents Aldehydes isocratic 35% Waste water Liquid/liquid extraction Liquid/liquid extraction or water extraction Liquid extraction 7992618-362 RP-C18.1 or 4mm id 100x2. 250x4 mm id 7992402-584 or 125x4. 79916OD-552 or 125x4. Reproduction. All Rights Reserved. except as allowed under the copyright laws. Published in Germany 04/2000 Publication Number 5968-6726E . For more information on our products and services.agilent. visit our worldwide website at http://www. adaptation or translation without prior written permission is prohibited.com/chem © Copyright 1997-2000 Agilent Technologies Co.S.Microsoft and Windows NT are U. registered trademarks of Microsoft Corp.