Environmental Solutions with HPLC Solutions Guide

April 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

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.

Non-Agilent hardware

For some applications, for example the Pickering Post Column Derivatization System for Carbamate Analysis, hardware must be ordered from the external vendor. In this case we have set up procedures with the vendor to ensure smooth ordering and delivery of the product. Most important spare parts and consumables are available as Agilent Technologies part numbers.

Consumables, Documentation

This document also includes ordering information for: columns guard cartridges (if applicable) mobile phase modifiers (if applicable) user guides (if applicable)

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

13

16 17

23

10

15
Time [min]

20

25

Column Mobile phase Gradient Flow rate Column temperature Injection volume Detection UV-DAD Fluorescence

250 x 2.1 mm (Agilent p/n 79918PAH-582) A = water B = acetonitrile at 3 min 50% B to 60% B at 14.5 min 50 %B to 90% B at 22.5 min 50 %B to 95%B 0.4 ml/min 22 C 2 l of stock solution (20 ng/l 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) 7.5 8.7 11 14.5 16.5 21 Ex(nm) 260 270 260 290 290 250 Em(nm) 420 440 420 430 430 500

Sample Agilent PAH standard 500 g/ml for each PAH (8500-6035) Sample preparation liquid/liquid extraction solid phase extraction

HPLC method performance Limit of detection, DAD: Limit of detection, FLD: Repeatabilty of RT: Repeatability of area: 50 to 500 pg 0.05 to 1.8 pg <0.15 % <2 to 4 %

&

Instrumentation see configuration example 1 on page 16

1. A.G.Hsgen et al, "Polynuclear aromatic hydrocarbons by HPLC", Agilent Technologies application note, 1993, publication number 5091-7260E 2. "Handbook for the HPLC analysis of polycyclic aromatic hydrocarbons" Agilent Technologies, 1993, Agilent part number 01050-90300 3. A.G.Hsgen, R. Schuster "Improved Data Quality in the Automated HPLC Analysis of PNAs (PAHs)", Agilent Technologies application note, 1995, publication number 5964-3540E 4. EPA Methods 550 and 550.1, U.S. Environmental Protection Agency 5. A New Approach to Lower Limits of Detection and Easy Spectral Analysis, Agilent Technologies primer, 2000, publication number 5968-9346E

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, 3 m , (Agilent p/n 7992618-362) Mobile phase A = water, 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 0.2 ml/min Post time 10 min Column temperature 38C Injection volume 3 l or 1 l Detection: UV DAD sample wavelengths: 230/20 nm, 400/80 nm reference wavelengths: 214/10 nm, 350/50 nm 245/20 nm, 500/80 nm

HPLC method performance Limit of detection: Repeatabilty of RT: Repeatability of area: 50 ng/l (500 ml-sample) ~ 0.2 % <2%

Instrumentation see configuration example 2 on page 17

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1. R. Reupert et al, "HPLC determination of 29 controlled herbicides in water suppliesAgilent Technologies application note, 1990, publication number 5952-2229

Phenoxy-acid Herbicides in Water

Bentazone

O N N H CH

CH3 SO 2 CH3

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 2,4-D MCPA 2,4,5-T dichlorprop mecoprop 2,4,5-TP 2,4-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 4.0 mm, Hypersil ODS, 5 m, (Agilent p/n 79926OD-354) A: 0.005 m KH2PO4 + 0.001% CH3COOH B: ACN/methanol = 1/1 + 0.001% 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: 0.5 ng absolute 20 ng/l with 1000fold enrichment and 25 l Repeatabilty of RT: < 0.2 % Repeatability of area: 1- 2 %

Instrumentation see configuration example 3 on page 18

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1. Methods 643 and 555, U.S. Environmental Potection Agency

Carbamates in Water

Methiocarb

CH3 CH3S CH3

O OCNHCH3
LU 900 l 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 3hydroxycarbofuran aldicarb propoxur carbofuran 1naphthol 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 4.6 mm, C8 phase (Pickering Laboratories), 5 m, A: water = 100 % B: methanol = 0 % at 1 min 0 % B at 31 min 75 % B 45 min 5 min 42 C 900 l + 800 l Fluorescence excitation wavelength 330 nm emission wavelength 450 nm photo-multiplier gain 12 4s 0.3 ml/min 0.3 ml/min 100 C ambient 25 30 35 800 l injection volume 250 ppt each

Matrix drinking water Sample preparation water is direct-injected (according to EPA Method 531.1)

Response time Post-column derivatization Reagent pump flow rate for hydrolization agent (0.05 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 l injection volume with S/N = 2 < 0.1 % 0.55 %

Instrumentation see configuration example 7 on pages 2224

&

1. Post-column LC analysis of 23 n-methylcarbamates, Pickering Laboratories application note, 108, 1994 2. Method 531.1, U.S. Environmental Protection Agency 3. A New Approach to Lower Limits of Detection and Easy Spectral Analysis, Agilent Technologies primer, 2000, publication number 5968-9346E

Glyphosate in Water

Glyphosate
O HO CH
2

%F
H N OH P CH
2

O OH

7.5 7

Glyphosate AMPA

Compounds glyphosate AMPA (aminomethylphosphonic acid)

6.5 6 5.5 5

Matrix drinking water Sample preparation water is direct-injected (according to EPA method 547)

2.5

7.5

10 Time [min]

12.5

15

17.5

20

Column

150 x 4 mm, cation exchange, K+ form, from Pickering Laboratories, 8 m (Pickering p/n 1954150) Mobile phase A: 5 mM KH2PO4, pH 2.0 B: 5 mM KOH A:B = 100:0 Gradient at 15 min 0 % B at 17 min 100 % B Flow rate 0.4 ml/min Column temperature 55 C Injection volume 50 l 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- = 0.3 ml/min flow rate for derivatization agent OPA = 0.3 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 < 0.8 % 2.2 %

Instrumentation see configuration example 7 on pages 2224

&
8

1. Rainer Schuster, A comparison of pre- and post-column sample treatment for the analysis of glyphosate, Agilent Technologies application note, 1992, publication number 5091-3621E 2. Method 547, U.S. Environmental Protection Agency

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 1 1.5 2 2.5 Time [min] 3 3.5 4

310 nm 256 nm

Sample preparation solid phase extraction on reversed phase disposable cartridges

4.5

Column Mobile phase Flow rate Column temperature Injection volume Detection: UV-DAD

100 x 2.1 mm, ODS Hypersil, 5 m, (Agilent p/n 79916OD-552) water + 0.5 g hexane-sulfonic acid = 3.5 ml/l TEA (triethylamine) pH = 2.5 with phosphoric acid 0.4 ml/min 15 C 10 l sample wavelengths: 256/10 nm and 310/10 nm reference wavelength: 450/100 nm

HPLC method performance Limit of detection 1 ng (injected amount), 0.4 g/l with an enrichment factor of 100 ~ 0.12% < 1%

Instrumentation see configuration example 4, page 19

Repeatability of RT Repeatability of areas

&

1. Method 549.1, U.S. Environmental Protection Agency

Benidines and Phenols in Water

Benzidine

H2N

NH2

Benzidine 24 pg

Compounds benzidine 3,3-dichlorobenzidine

3,3-Dichlorobenzidine 18.6 pg

Sample preparation liquid/liquid extraction

Time [min]

10

12

Column Mobile phase Flow rate Injection volume Detection:

250 x 4 mm Spherisorb ODS-2, 5 m (Agilent p/n 79924O2-584) water (with 0.1 M NaAc and 0.001 M Na2EDTA) and acetonitrile, 50:50 0.8 ml/min 20 ml Electrochemical glassy carbon working electrode, with AgCl/KCl reference electrode response time: 4 s range: 0.5 mA temperature: 40 C potential: 0.7 V

HPLC method performance Limit of detection benzidine 33'-dichlorobenzidine Repeatability of RT Repeatability of areas 0.08 ppb 0.13 ppb < 0.3 % <2%

Instrumentation see configuration example 5, page 20

10

Aldehydes in Air

Formaldehyde

O H C H

mAU -0.5
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 g/ml of each aldehyde was derivatized with 2,4-dinitrophenylhydrazine

-1.5

-2

-2.5

-3 0 2 4 6 Time [min] 8 10 12

Column Mobile phase Gradient Flow rate Column temperature Injection volume Detection: UV- VWD

100 x 2.1 mm, Hypersil ODS, 5 m (Agilent p/n 79916OD-552) A= water, B= acetonitrile at start 27 % B in 13 min 98 % B 0.45 ml/min 30 C 1 l 365 nm

HPLC method performance Limit of detection Repeatability of RT Repeatability of areas ~ 10 pg 0.40 to 0.19 % 0.79 to 2.80 %

Instrumentation see configuration example 3, page 18

11

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

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 2.1 mm (79918PAH-582) A = water B = acetonitrile at 3 min 50 % B to 60 % B at 14.5 min 50 %B to 90 % B at 22.5 min 50 %B to 95 %B 0.4 ml/min 22 C 2 l of stock solution (20 ng/l 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) 7.5 260 8.7 270 11 260 14.5 290 16.5 290 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, DAD: Limit of detection, FLD: Repeatabilty of RT: Repeatability of area: 50 to 500 pg 0.05 to 1.8 pg <0.15 % <2 to 4 %

&

Instrumentation see configuration example 1, page 16

1. A.G.Hsgen et al, "Polynuclear aromatic hydrocabons by HPLC", Agilent Technologies application note, 1993, publication number 5091-7260E 2. "Handbook for the HPLC analysis sis of polycyclic aromatic hydrocarbons", Agilent Technologies, 1993, part number 01050-90300 3. D.R. Gere, C.R. Knipe, P. Castelli, J. Hedrick, L.G. Randall "Bridging the Automation Gap between Sample Preparation and Analysis: An Overview of SFE, GC, GC/MSD and HPLC Applied to Several Types of Environmental Samples" Journal of Chromatographic Science, July 1993 4. A.G.Hsgen, R. Schuster "Improved Data Quality in the Automated HPLC Analysis of PNAs (PAHs)", Agilent Technologies application note, 1995, publication number 5964-3540E

12

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 1,3,5-Trinitrobenzene 1,3-Dinitrobenzene Nitroglycerine Tetryl 2,4,6-Trinitrotoluene 2-Amino 4, 6-Dinitrotoluene 4-Amino-2, 6-Dinitrotoluene 2, 4-Dinitrotoluene 2, 6-Dinitrotoluene 2-Nitrotoluene 4-Nitrotoluene 3-Nitrotoluene Nitropenta Diphenylamine

60
1 2

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, 3 m (Agilent p/n 7992618-362) A= water B= acetonitrile at start 15 % B in 30 min 50 % B in 40 min 90 % B 0.31 ml/min 8 min 38C 5 l 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 < 0.2 % ~ 2 % except tetryl and nitroglycerine due to decomposi-

Instrumentation see configuration example 6, page 21

&

1. Rainer Schuster et al, "HPLC analysis of explosive constituents in soil samples" Agilent Technologies application note, 1993, publication number 5091-7626E 2. Method 8330, U.S. Environmental Protection Agency

* Method developed by R. Reupert, LWA Dsseldorf

13

Instrumentation

Agilent 1100 Series modules and systems

The Agilent 1100 Series HPLC systems and Agilent ChemStations are ideally suited for analysis of environmental samples. Through its design the most demanding laboratory objectives are achieved: reduces operating cost: no need for helium through all electric design, works with 2-mm columns to reduce solvent costs, helps to comply with regulations and quality standards through built-in, fast, trouble-free and labor-saving autovalidation features, saves operator training time through intuitive user interface and built-in online tutorials, maximizes productivity through fast system set up and intelligent automation, maximizes instrument uptime through use of field proven parts, multimedia tools for effective maintenance, extensive self- and remote diagnostics, Agilent Technologies' 24-hour service response, and highest system performance, for example in detector sensitivity for lowest detection limits through new designs. Further features for the environmental laboratory include: variable-volume autosampler with integrated injector program for precolumn derivatization, high sensitivity diode-array detector for qualitative and quantitative analysis, in the wavelength range of 190 - 950 nm, high sensitivity fluorescence detector (FLD) with multiple signal detection, online spectral acquisition and spectral libraries. FLD data can be combined with diode-array detector data. online vacuum degasser, which removes trace levels of air for higher detector sensitivity and stability of retention times, temperature-controlled column compartment with a standard Peltier element for heating and cooling, which eliminates analytical errors due to temperature fluctuations above, at and below ambient temperature.

14

AgilentChemStation

Agilent ChemStations are recommended for instrument control and data evaluation. Features for the environmental laboratory include: system suitability software for automated and customized method validation and system suitability testing, report generator to print analysis reports according to regulatory and client requirements, and software for automated identification and quantitation based on diode-array detection and spectral libraries (Agilent ChemStation for LC 3D systems).

Electrochemical detector

The Agilent 1049A electrochemical detector is recommended for special applications such as phenols and aromatic amines. The detector can be controlled from the integrated keyboard and from the Agilent ChemStations. Other features for the environmental laboratory include: electrochemical self-cleaning routines, easy change of electrodes, automation of potential optimization.

15

Configuration Example 1 Description Order

Agilent 1100 Series automated quaternary LC 3D sys- G1357AA tem. 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, 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, G2180AA spectral processing software, HP computer, CD-ROM drive, LaserJet printer, Microsoft Windows NT 4.0. Agilent 1100 Series thermostated column compartment. Agilent 1100 Series fluorescence detector. PAH standards, 500 g/ml. PAH guard cartridges (30 x 2 mm), 2/pk. Guard cartridge holder. PAH operating procedures. (This handbook was developed for the HP 1050 Series, it can be used as a guideline for the Agilent 1100 Series.)
Minimum instrument for PNAs according to EPA methods 550, 550.1, 610, 8310: Gradient pump Manual injector Column oven Variable wavelength detector Fluorescence detector Data system is recommended.
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 . . . . . . . . . . . . . . . . . . . .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, software and peripherals, the components of the Agilent ChemStation systems may be replaced by equivalent or better models. 16

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, 10 mm path length Hypersil ODS column and checkout sample Agilent ChemStation for LC 3D systems (G1319A) Includes G2170AA single instrument Agilent ChemStation software, G2180AA spectral processing software, HP computer, CD-ROM drive, LaserJet printer, Microsoft Windows NT 4.0. Agilent 1100 Series thermostatted column compartment. Pesticide standards. Pesticide operating procedures. (This handbook was developed for the HP 1090 Series. It can be used as a guideline for the Agilent 1100 Series.) G1316A

5062-2500 01090-90300

CAN 5181-1516

G1354A

CAN 5181-1516

G1327A

CAN 5181-1516 Configuration example for: Non-volatile pesticides in water . .page 5

G1316A HP-IB 10833D G1315A G1319A Printer

17

Configuration Example 3 Description

Agilent 1100 Series automated quaternary LC 2D system. 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, 10-mm path length (G1314A #018) Agilent 1100 Series control module Delete control module. Agilent ChemStation for LC 2D systems. Includes 2170AA single instrument LC ChemStation software, HP computer, CD-ROM drive, LaserJet printer, and Microsoft Windows NT 4.0. 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 l Data system is recommended. 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 . . . . . . . . . . . . . . . . . . . . . . .page 6 Aldehydes in air . . . . . . . . . . . . . . . .page 11

G1316A HP-IB 10833D G1314A G1319A Printer

18

Configuration Example 4 Description

Agilent 1100 Series isocratic pump. Agilent 1100 Series thermostated column compartment. Agilent 1100 Series autosampler. Needs to be specified. Agilent 1100 Series diode-array detector. Standard flow cell, 10- mm path length. Agilent 1100 Series vacuum degasser. Agilent ChemStation for LC 3D systems. Includes G2170AA single instrument LC ChemStation software, G2180AA spectral processing software, HP computer, CD-ROM drive, LaserJet printer, and Microsoft Windows NT 4.0. G1315A G1315A #018 G1322A G1319A

Order
G1310A G1316A G1313A

Strongly recommended.

Minimum for paraquat according to EPA method 549.1 Isocratic pump Manual injector to deliver 200 l Column oven Diode-array detector Data system is recommended.

G1322A CAN 5181-1516

G1310A

CAN 5181-1516

G1313A

CAN 5181-1516 Configuration example for: Paraquat in water . . . . . . . . . . . . . .page 9

G1316A HP-IB 10833D G1315A G1319A Printer

19

Configuration Example 5 Description

Agilent 1100 Series quaternary pump. Includes Agilent 1100 Series vacuum degasser. Agilent 1100 Series thermostated column compartment. Agilent 1100 Series autosampler. Agilent 1049A programmable electrochemical detector. Includes inlet capillary, outlet tubing, glassy carbon working electrode, solid state reference electrode, GPIB interface and remote cable. Agilent ChemStation for LC 2D systems. Includes G2170AA single instrument LC ChemStation software, HP computer, CD-ROM drive, LaserJet printer, and Microsoft Windows NT 4.0.

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, 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 . .page 10

20

Configuration Example 6 Description

Agilent 1100 Series automated quaternary LC3D 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, 10 mm path length (G1315 #018) Agilent ChemStation for LC 3D system (G1319A) Includes G2170AA single instrument LC ChemStation software, G2180AA spectral processing software, HP Vectra color computer, CD-ROM drive, LaserJet printer, and Microsoft Windows NT 4.0. Agilent 1100 Series thermosttated column compartment.

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 l

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

Configuration Example 7 Description

Agilent 1100 Series quaternary pump. Includes Agilent 1100 Series vacuum degasser. Seal wash option. Agilent 1100 Series autosampler. Multi-draw kit. Extended injection range option with 900-l syringe. Agilent 1100 Series fluorescence detector. Post-column reaction kit. To be installed in Agilent 1100 Series system when used with Pickering post column reaction system. Includes 0.25-mm id capillary, length 70 cm, Tefzel seal, seat assy (PEEK) and needle assy (PEEK). See the following two pages for detailed ordering information of Pickering Systems. Pickering System for post-column hydrolization and derivatization. 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 531.1) or glyphosate analysis. Agilent ChemStation for LC 2D systems. Includes G2170AA single instrument LC ChemStation software, HP computer, CD-ROM drive, LaserJet printer, and Microsoft Windows NT 4.0. G1317A

Order
G1354A G1354A # 030 G1313A G1313A #021 G1313A #020 G1321A G1313-68712

For glyphosate application only.

Alternatively

Minimum requirements for carbamates according to EPA method 531.1: Gradient pump Fluorescence detector Manual injector for 200 - 400 l Post column reactor Data system is recommended. CAN 5181-1516 G1354A

PCX 5100 (incl. connection tubing)

Minmum requirements for carbamates according to EPA method 8318: same as above, except: Manual injector for 20 l

CAN 5181-1516

G1313A

G1321A Configuration example for: Carbamates in water . . . . . . . . . . . .page 7 Glyphosates in water . . . . . . . . . . . .page 8

HP-IB 10833D

G1317A

Printer

22

Description

Order (Pickering)

Carbamate Analysis System A complete system consists of a PCX5200 post-column instrument, 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, reservoir assemblies for hydrolysis and OPA reagents, gas manifold. Same as 1152-2211 for 240 Volt operation. Application Kits All kits include the Carbamate Analysis Applications Manual. Application and Post-column Kit Includes: Carbamate column, C18, 4.6 x 150 mm (1846150) Carbamate column, C18, 4.6 x 250 mm (1846250) Guard cartridge holder with 3 guard cartridges (18ECG001) o-Phthalaldehyde (OPA) crystals, 5 g (O120 ) OPA diluent for carbamate analysis, 4 x 950 mL (CB910 ) Thiofluor crystals, 10 g (2) (3700-2000) Hydrolysis reagent for carbamate analysis, 4 x 950 mL (CB130) ChlorAC buffer for aqueous samples, 250 mL (1700-1032) Carbamate test mixture, 12 components, 1.5 mL (2) (1700-0063) Application and Post-column Kit Includes: Carbamate column (4.0 x 250 mm) C8, expanded resolution (0840250) Guard cartridge holder with 3 carbamate guard cartridges (18ECG001) o-Phthalaldehyde (OPA) crystals, 5 g (O120) OPA diluent for carbamate pesticide analysis, 4 x 950 mL (CB910) Thiofluor crystals, 10 g (two) (3700-2000) Carbamate analysis hydrolysis reagent, 4 x 950 mL (CB130 ) ChlorAC buffer for aqueous carbamate samples, 250 mL (1700-0132 ) Carbamate test mixture, 12 components, 1.5 mL (1700-0063) 1152-2211

1152-2212 0352-0001

0352-0002

23

Description

Order (Pickering)

Glyphosate Analysis System A complete system consists of a PCX5200 post-column instrument, and one or more application kits containing the columns and reagents for converting a liquid chromatograph into an analyzer for glyphosate analysis. PCX5200 dual reagent post-column derivatizer system, 120 Volt operation, reservoir assemblies for hydrolysis and OPA reagents, gas manifold. Same as 1152-2211 for 240 Volt operation. Application and Post-column Kit Includes: Glyphosate analysis applications manual Glyphosate column, cation-exchange, K+ form, 4 x 150 mm (1954150) Glyphosate guard column, K+ form, 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, 4 x 950 mL (GA116) Glyphosate eluent, 5 mM KH2PO4, pH 2.0, 4 x 950 mL (K200) Column regenerant for glyphosate analysis, 5 mM KOH, 950 mL (RG019) Thiofluor crystals, 10 g (2) (3700-2000) RESTORE for metal ion decontamination of column or guard (1700-0140) Glyphosate test mixture, two components, 1.5 mL, 2.5 g/mL (1700-0080) 1152-2211

1152-2212 0352-0010

24

External Suppliers

Materials supplied by the following vendors were used in the referenced applications:

External supplier for disposable cartridges (applications pages 5, 6, 9)

Europe J.T. Baker B.V Rysterborgherweg 20 P.O.Box 1 NL-7400 AA Deventer Tel: +31-5700-87500 Fax: +31-5700-11342

USA J.T. Baker Inc. 222 Red School Lane Phillipsburg, 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- 77694 Kehl/Rhein Tel: +49-7851/7069 Fax: +49-7851/75362

USA Cole-Pormer International 7425 North Oak Park Ave. Niles, Illinois 60714 Tel: +1-708- 647-7600 Fax: + 1-708 647-9600

External supplier for post column derivatization system (applications pages 2224)

Europe LC Tech Bahnweg 41 D-84405 Dorfen, Germany Tel: +49-8081-93680 Fax: +49-8081-936810

USA Pickering Laboratories Inc. 1951 Colony Street. Suite S Mountain View, CA 94043 Tel: +1-650-694-6700 Fax: +1-650-968-0749 e-mail: picklab@ix.netcom.com

25

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 4.6 mm id 79919QA-754 RP-C18, 2.1 or 4 mm id, 100x2.1, 79916OD-552 or 125x4.0, 79926OD-564 RP-C18, 2.1 or isocratic 68% 0.34 g/l KH2PO4 0.1% H3PO4 0.1 % Hexansulf.. acid 0.3% TEA, pH 2.5 Post column deriv. 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.#)

531.1 Carbamates 11 N-Methylcarbamates 8318 547 Glyphosate

Drinking water Soil/sludge Drinking water Drinking water

RP-C18 Pickering

H20/MeOH grad, 25 to 75% B

Post column deriv. Fluorescence

1100 grad/FLD + Pickering system

549.1

Quats Paraquat/ Diquat

604.1 (draft)

Hexa-/ Dichlorophene

Waste water extraction

Liquid/liquid 4 mm id, 100x2.1, 79916OD-552 or 125x4.0, 79926OD-564 Filtration and direct injection

0.05% 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, 250x4 mm id 79924O2-584

0.1 M NaAc/ACN isocratic , 50% B

Electrochemical 0.7 Volt

1100 iso 1049

550, 550.1 610 8310

Liquid/liquid extraction or solid phase extraction Quartz filter/XAD2

Vydac PNA 250 x 2.1 mm, 79918PAH-582 250 x 4.6 mm, 79918PAH-584

H20/ACN VWD or grad, 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, 2.1 or 4 mm id, 100x2.1, 79916OD-552 isocratic 30%B RP-C18, 2.1 or 4 mm id 100x2.1, 79916OD-552 or 125x4.0, 79926OD-564 RP-C18, 2.1 or 4 mm id 100x2.1, 79916OD-552 or 125x4.0, 79926OD-564 RP-C18, 100x2.1 mm id grad , 55 to 95% B

0.01 M KxHxPO4, VWD or DAD 0.05% TBAS/pH7.0/ 285 nm MeOH or 125x4.0,

1100 DAD or VWD

635 (draft)

Rotenone

Waste water Drinking water

Liquid/liquid extraction

H220/ACN isocratic, 50% B

VWD or DAD 294 nm

1100 iso/ VWD or DAD

636

Bensulide (draft)

Waste water

Liquid/liquid extraction

H20/ACN isocratic , 65% B

VWD or DAD 220 nm

1100 iso/VWD or DAD

638 (draft)

Nitroanilides Oryzalin, Pendimethalin, Butralin, 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, 2.1 or 4 mm id 100x2.1, 79916OD-552 or 125x4.0, 79926Od-564

H20/ACN 35% B, isocratic

VWD or DAD 212 nm

1100 iso /VWD or DAD

26

LC Environmental Quick Reference Guide (EPA Methods)

Method Sample Matrix Sample Preparation
Liquid/liquid extraction Direct injection

Column

Mobile Phase

Detection

Instrumentation Reference (pub. #)

1100 iso /VWD or DAD 1100 iso/FLD

640 (draft) 641 (draft)

Mercaptobenzothiazole Thiabendazole

Waste water

RP-C18, 2.1 or 4 mm id 100x2.1, 79916OD-552 or 125x4.0, 79926OD-564 RP-C18, 2.1 or 4 mm id 100x2.1, 79916OD-552 or 125x4.0,

H20/ACN isocratic , 35% B 0.01 M KxHxPO4 0.05% TBAS/pH 7.0/ 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, 100x2.1 mm id 79916OD-552 RP-C18, 100x2.1 mm id 79916OD-552 solid phase H20/ACN grad, 50 to 100% B 0.005M KH2PO4/ ACN/MeOH=1/1 grad, 15 to 55% B ODS, 125 x 2mm, 3 m 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. 0.001%CH3COOH

Soil/Water (ultrasonic)

554 8315 TO5, TO11

Drinking water Soil/sludge Air

Derivat. liquid/ solid Adsorption and derivatization (DNPH) Impigner 0.1N NaCH Filtration and direct injection

RP-C18, 2.1 or 4 mm id 100x2.1, 79916OD-552 or 125x4.0 79926OD-564

H20/ACN grad, 20 to 50% B

VWD or DAD 365 nm

1100 grad DAD or VWD

TO8

Phenol Methylphenols Phenol, Kresol Chlorophenols

Air Surface water

RP-C18, 2.1 or 4mm id 100x2.1, 79916OD-552 ODS-2, 250x4 mm id 7992402-584 or 125x4.0 79926OD-564

Acetate/ACN isocratic, 30%B H20-KNO3/MeOH isocratic, 60% B

VWD or DAD 274 nm Electrochemical 1.1 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. #)

N-Herbicides Urea Herbicides Surfactants

Triazines Water Anilides Alkylsulfonates

Soil/sludge

RP-C18, 100x2.1 mm id 79916OD-552

H20/ACN grad, 20 to 50% B

DAD 1100 grad DAD 214, 230, 245 nm Ger DIN38407F12

Surface water extraction Water

Filtration and solid phase

RP-C18, 100x2.1 mm id 79916OD-552

H20/ACN grad, 20 to 50% B

DAD 220 nm

1100 grad DAD

Anions

F, Cl, Br, N03, P04, N02, S04

Filtration/direct injection

Agilent-IC 79923IC-564

H20/ACN and modifier

negative UV 266 nm

1100 iso/VWD degasser

27

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