FROG-4000 User`s Manual
Contents
1. 9 Section 1 Getting to Know the FROG 4000 oo cececessesecessesescereeeeees 11 1 1 Manual Overview siens 11 1 2 Operations Overview Nb 12 Section 2 Components and Systems 15 2 1 Instrument COMPONEIIS cuss cii Rd RI RDR CU DEN FF 16 2 2 Purge and Trap System scccccssseccesececcescccsescesseeeeesaesecsauees 20 2 2 1 L ad Analyze RYN LUN ORA DYDD OF 22 2 2 2 Sparge Bottle POSITIONS pe 23 2 3 Gas Phase Analysis 9ystemn pp 24 2 4 Gas Sample Analysis Flow Diagrams 27 2 4 1 Sample Loading ah ue y fn 27 2 4 2 Sparge and Collection 28 2 4 3 Release Separation and Analysis 29 2 5 Gas Sampling Analysis Flow Diagrams Air Sampl r 30 2 8 1 Sample 2 5 2 Release Separation and Analysis 31 Section 3 Overview of Ellvin Chromatography Software 32 Section 4 Field and Lab Analysis Procedures pp 33 4 1 Powering On Charging the Battery pt 37 4 2 Connecting to Computer Ellvin ss 41 4 3 Instrument Settings 45 4 4 Instrument Preparation ss 49 4 4 1 Rinsing the Instrument err YAA LY AW YF ei nnneuon 49 4 4 2 Creating a Clean Baseline YY Y H Hi Ynrineuuon 50 4 4 3 Connecting the Air Sample Adaptor pb 53 4 5 Loading a Sample 57 4 6Running AS amp leu SR y GU y ne ere 61 Importing Data to EMI SR dan 67 7 Defiant T rh FROG 4000 User s Manual de TABLE OF CONTENTS CONTINUED2. 43 Defiant pige DD a FROG 4000 User s Manual lt FROG 4000 4 2 Connecting to Computer Ellvin Continued 5 Click Port on the display screen then select a COM 2 Live Data Analyze Calibration Settings MERE PARAMS UPDATED 5 PARAMSUPDATED The connection port should now read CONNECTED indicating that the FROG and Ellvin are connected The user may now manage settings and run analyses from Ellvin 44 FWDWR FROG 4000 User s Manual SEX Section 4 Field and Lab Analysis Procedures Continued The FROG 4000 comes with general default setting for VOCs which are shown in Figure 4 3 2 on the following page The settings determine the duration of different analysis phases as well as the desired temperature of the GC column The settings are defined and applied using Ellvin Table 4 3 1 on the following page describes the various settings The FROG 4000 default settings are best for the analysis of Benzene Toluene Ethylbenzene and Xylenes BTEX but the settings can be altered for analyzing a wide variety of compounds and concentrations See Appendix I for a list of detectable chemicals The current operational settings are stored in the FROG 4000 M memory and do not revert to the default settings when the instrument is disconnected from the software or power They are retrieved and displayed under the Settings Window when the ins
3. Ethlybenzene P M Xylene 3 43 283 760450 4369484 01 0Xiene 4 43077 1400475 343137 120 C Users afruj Figure 6 2 1 List of Analytes 98 FROG 4000 Technologies FROG 4000 User s Manual SEX Create the List of Analytes e Enter the name of the calibration analyte you desire to add in the Analyte Name window Analyte Name Benzene e Create and enter an abbreviated name for the analyte in the Analyte Alias maximum of 5 Characters The Analyte Alias will be displayed on instrument screen Analyte Alias Benz e To make an addition to the List of Analytes click the ADD button e To delete an analyte from the list click on the analyte in the List of Analytes The desired analyte will be highlighted blue when selected Click Delete on keyboard to delete the analytes from the list Analytes Benzene 99 Technologies FROG 4000 User s Manual Ma WR 6 2 Calibration Window Features Continued 6 2 2 CORRELATION CHART AND EOUATIONS This feature in the Calibration Window displays the degree of correlation between analyte standards of varying concentrations and the instrument s response to them See Figure 6 2 2 The correlation is calculated as both a linear eguation and a 2nd order guadratic eguation The user may choose to view the eguations and a chart for either Peak Area correlation or for Peak Height correlation This correlation is important because Ellvin uses the
4. Section 5 Ellvin Chromatography Software pe 73 LE TR FN FF HYN os te 74 5 2 Applying Ellvin Features ss 80 5 2 1 OPEN Button ee 80 5 2 2 Magnifying GlaSS AN NA FA 82 a LEE ANON PRE ER O CEFIN OD GOD 84 91 Call 566 6 1 Calibration 5 92 6 1 1 Standards for Liquid or Soil Samples pe 92 6 1 2 Standards for Air Samples Ynn Y YH Ln nein 95 6 2 Ellvin Calibration Window Features 99 6 2 1 List of Analytes 99 6 2 2 Correlation Chart and Equations pp 100 6 3 Calibration Procedure Rs 102 SC HO UT MAINS ne 111 7 1 Routine Cleaning a ae 111 7 1 Annual CEN INE 112 7 3 Cleaning the Scrubber ss 112 Section 8 Trouble Shooting sisaccsssissacssasaavadsaesavsdsoassasvensevsarsacsaesesenoonrdas 117 8 1 Inverting the FROG with Water in the Sparge Bottle 117 8 2 Degrading Chromatograph Scrubber is NOT secured properly pp 121 8 3 Cannot Achieve a Clean Baseline pe 122 8 4 Black Instrument Screen 1114444444 124 Appendix Accessories Spare Parts 127 Appendix ll Detectable Chemicals 131 Defiant lt gt FROG 4000 User s Manual dl COMMONLY USED ACRONYMS PC Preconcentrator PID Photo lonization Detector GC Gas Chromatography Column VOCs Volatile Organic Compounds BTEX Benze
5. Figure 2 3 3 Gas Phase Analysis System external components 26 Defiant T iD FROG 4000 User s Manual ae Section 2 Systems and Components Continued 2 4 GAS FLOW DIAGRAMS This section describes and illustrates the flow of a sample from loading through the components of the Gas Phase Analysis System Section 2 2 241 SAMPLE LOADING Diagram 2 4 1 The sparge bottle is in the UP position for a liquid or air sample The load analyze valve is in the LOAD position sample is loaded into the sample inlet with a 5mL syringe Activated Charcoal Sparge Valve SR X Molecular Sieves Flow Selection Valve cad Preconcentrator Bypass Valve Sample m Line Sample Sparge Bottle Micro GC Diagram 2 4 1 Sample Loading 27 Defiant ee D FROG 4000 User s Manual ET 2 4 Gas Flow Diagram Continued 242 SPARGE AND COLLECTION Diagram 2 4 2 After the sample has been loaded the load analyze valve is placed in the ANALYZE position The start button is pressed and the pump flow starts The carrier gas moves through 1 the flow selection valve 2 activated charcoal and 3 the sparge valve Air sparges the liguid if a liguid sample to release the VOCs into the headspace of the sparge bottle and onto the preconcentrator PC Activated Charcoal HO SOOO Molecular Sieves Flow Selection Valve nee amp Sparge Valve 0 Load Preconce
6. Follow the location path displayed in the Analyze Window to the folder that contains the data file of interest Location Path Example C Users DE 2014093011716 LOG xxx xml The highlighted numbers correspond to the date the storage folder and data file were created by Ellvin In this example September 30 2014 15 Open the folder with the location path date 16 The folder contains a list of files The file names are derived from the time Ellvin converted the data In the example in Figure 4 7 3 the file named 1716 was converted at 5 16 PM on 9 30 2014 17 Select the file of interest 70 FROG 4000 Pefanl 5 FROG 4000 User s Manual fx Folder name is the Date File name is the Time Look in Ji 20140930 97 By Name n Date modified Type 4 1703 LOG _056xml 9 30 2014 5 03 PM XML Do Places e 1703 LOG 056 Annotationsxml 9 30 2014 5 03 PM XML Do E 11716 LOG 057 xml 9 30 2014 5 25PM XML Do 2 1716_LOG_057_Annotations xml 9 30 2014 5 25PM XML Do sktop 1731 106 _058 xml 9 30 2014 5 31 PM XML Do 1731 106 058_Annotations xml 9 30 2014 5 31 PM XML Do is Ov LOG 059 xml 9 30 2014 5 41 PM a raries 2 1732 106 059 Annotations xml 2 1745 106 060 Size 663 KB L 1745 LOG _060_Annotations xml Date modified 9 30 2014 5 41 PM Do Type XML Document Figure 4 7 3 Data files named and stored by Ellvin 18 A preview chromatogram
7. Function Detects VOCs E Sparge Valve Function Directs pump flow into sparge bottle to purge VOCs from sample F Flow Selection Valve Function Determines where the flow will be directed during Sparge or Analysis Mode G Internal Bypass Valve Function Allows the VOCs to pass over the PC and bypass the GC and PID H Pump Split Function Provides a small leak in pump flow for improved flow control X Internal Injection Split Function Provides a small leak to prevent rebound injection 24 S FROG 4000 Defiant FROG 4000 M User s Manual df H y Activated Charcoal Sparge Valve pr E N Flow Selection Valve A Preconcentrator Bypass Valve Bypass Line Load Sample Sample Sparger 1 se Micro GC C Figure 2 3 1 Gas Phase Analysis System components Bypass Valve GC column Figure 2 3 2 Gas Phase Analysis System internal components 25 Defiant CP D FROG 4000 User s Manual K 2 3 Gas Phase Analysis System Continued Gas Phase Analysis System Components and their Functions Figure 2 3 3 C Display Screen Function Shows the user which stage of analysis is being performed and displays an estimate of analysis results U Start Button Function Initiates the analysis cycle can also be initiated through Ellvin V Pump Inlet Function Carrier gas intake for pump W Exhaust Function System flow exits
8. allen wrench 2 Lightly pull scrubber off FROG place any O rings back in place if they come out Figure 7 3 2 Four corner screws removed and scrubber removed from FROG 3 Turn the scrubber block upside down e Position 1 has widely spaced ports This chamber holds the molecular sieves e Position 2 has narrowly spaced ports This chamber holds the activated carbon Position 1 g Position Position2 Position 2 2 Figure 7 3 3 Upside down scrubber with ports visible 113 Defiant T a gt FROG 4000 User s Manual dt 7 3 Cleaning the Scrubber Continued 4 Turn the scrubber right side up and remove the two center position 4 40 screws with the 3 32 allen wrench Figure 7 3 4 Two Center Screws 5 Remove the scrubber lid put any O rings back in place if they come out Position 1 Position2 Figure 7 3 5 Open scrubber 114 Technologies FROG 4000 User s Manual 0 6 Dispose of dirty activated carbon and molecular sieves 7 Use a paper funnel to put new activated carbon into Position 1 8 Use a paper funnel to put new molecular sieves into Position 2 9 Replace the lid 10 Tightly replace the two center position 4 40 screws with the 3 32 allen wrench 11 Place the scrubber back onto FROG make sure Position 1 is in correct spot 12 Snuggly replace the four corner 4 40 screws with the 3 32 allen wrench 13 There should be NO space in between the scr
9. 05 Figure 5 2 3 6 Integration complete Width Concentration 263786 Toluene 128 982 314392 4324296 Ethylbenzene 256 304 172353 2121650 p m Xylene 274 647 0 7970630 o Xylene 323 368 112029 2876477 Data Grid 89 FROG 4000 User s Manual C 90 Defiant pee su D FROG 4000 M User s Manual dea NF FROG 4000 SECTION 6 CALIBRATION This section provides detailed instructions for calibrating the instrument The system is calibrated by testing a series of analytes at varying known concentrations As with all GC work these analytes are selected from an established list of chemicals that are of foremost interest in the environment under investigation e Before beginning a calibration it is recommended that the user become familiar with Ellvin Refer to Section 5 e The user should also be familiar with analytical techniques for GC calibration e The preparation and use of standards for calibrating the instrument differs for air liquid and soil samples Section 6 1 introduces the procedure for preparing standards e Section 6 2 provides detailed instruction for using the features found in Calibration Window e Section 6 3 provides detailed instructions for calibrating the instrument 91 TM CT Technologies FROG 4000 User s Manual CE FROG 4000 Section 6 Calibration Continued 6 1 CALIBRATION STANDARDS NOTE The instruction in Sections 6 1 1 and 6 1 2 correspond
10. 4000 User s Manual Ma a 5 2 Applying Ellvin Features Continued 522 MAGNIFYING GLASS The Magnifying Class can be used in Live Data Window during data import or while in Analyze Window Click on the magnifying glass icon to start To Magnify e Left click and hold e Drag mouse over desired magnified area Figure 5 2 2 1 e Release the mouse button e The area being magnified is highlighted light blue e The display screen then readjusts to show the magnified area Figure 5 2 2 2 To De Magnify e Double click left side of mouse on the display area e OR click the circle on the scroll bars e OR double click the magnifying glass icon 82 gt See FROG 4000 User s Manual a NP FR Figure 5 2 2 1 Desired Magnified Area Figure 5 2 2 2 Magnified Area 83 FROG 4000 User s Manual A 5 2 Applying Ellvin Features Continued 5 2 3 INTEGRATOR 2 Integrator 2 can be used only in Analyze Window This tool calculates the area under a peak and the peak height The area or peak height helps determine the concentration of the analyte Click on the Integrator 2 button to start dd Technique to Integrate Refer to Diagrams 5 2 3 1 and 5 2 3 2 e Begin at the lowest point Valley 1 e Drag the mouse to draw an integration line past the peak to the second lowest point Valley 2 e The integration line should NOT cross the data line Avoiding this ensure
11. 4000 M User s Manual There are two possible connections between the FROG and a computer To send information such as settings and analysis commands from Ellvin to the instrument connect a computer to the serial data port O on the FROG with the Serial Data Cable To import data from the instrument s internal SD card to Ellvin connect a computer to Port N on the FROG with the USB Cable NOTE Detailed instructions for exporting data with the USB cable are given in Section 4 7 USB Cable 41 FROG 4000 M User s Manual Serial data cable Connection 1 Connect the serial data cable from the FROG s serial data port O to a USB port on a computer Set the instrument power switch O to the ON position If necessary install Ellvin onto laptop or PC Open Ellvin by double clicking on the Ellvin icon Serial Data Cable 42 ho gt z FROG 4000 User s Manual SC After Ellvin has opened the default screen that appears is the chromatogram display screen in Live Data Window Figure 4 2 1 Figure 4 2 2 shows details of the display screen 2 a e 9 OBEN PORT co 1 CanaryFrog Version 2 0 4 13 D 1 3 BH 8 o 3ZATYNY Figure 4 2 1 Ellvin default screen Chan1 Chan2 PCTemp GCTemp Notes CONNECTED PARAMSHOADED Dao vos ANALYZEOD OD E 68 PORT 8
12. 9 Log File WAIT The screen returns to the original display and shows the Log File for the NEXT analysis WAIT indicates that the GC temperature is above the lower GC set point 64 Defiant ss D FROG 4000 User s Manual dt The FROG is ready for another sample loading and analysis once the GC Temperature indicator appears green and READY is displayed on the FROG screen Samples of the same analyte may be run consecutively from low concentration to high without rinsing the instrument and creating a clean baseline NOTE Before loading another sample the user should complete the following procedures Liquid or Air Sample perform Soil Sample Remove and discard disposable sparge bottle If not using a disposable bottle remove sparge bottle from instrument and fill it with deionized water Rinse it thoroughly to remove all dirt from bottle Then perform Continued on next page gt TM ec Technologies FROG 4000 User s Manual C Final Step If desired use Ellvin for detailed results analysis after completing the analysis run e lf the sample was run while connected to Ellvin open the data file in Analyze Window and use Integrator 2 See Sections 5 2 1 and 5 2 3 e lf the sample was not run while connected to Ellvin import the data to Ellvin Section 4 7 then open the file in Analyze Window and use Integrator 2 66 Defiant T D FROG 4000 User s Manual
13. Epichlorohydrin Ethyl acetate Ethyl tert butyl ether Ethylbenzene WO UT m N oo Co o 00 gt Ethylene oxide 75 21 8 lodomethane 74 88 4 o o wo UT Ke CO 00 Methacrylonitrile 126 98 7 Methyl methacrylate 80 62 6 o UJ Isobutyl alcohol 78 83 1 WO N Methyl tert butyl ether Naphthalene WO N m oF Nitrobenzene n Propylamine o Toluidine Propargyl alcohol t Butyl alcohol Tetrachloroethene Toluene 00 oo T gt Isopropylbenzene 98 82 8 m Win m o WO UJ oO W Co Co 132 FROG 4000 M User s Manual df S FROG 4000 Common Chemicals Detectable by FROG 4000 CA Number IE eV trans 1 2 Dichloroethene 156 60 5 NOTE This list is by no means exhaustive The FROG 4000 uses a 10 6eV lamp so many analytes with activation energies below 10 6eV may be detectable with the instrument 133 FROG 4000 User s Manual C Notes 134 FROG 4000 Technologies FROG 4000 User s Manual SE Notes 135 FROG 4000 User s Manual C Notes 136
14. PURGE AND TRAP SYSTEM Purge and Trap System Components and their Functions Figures 2 2 1 and 2 2 2 A Scrubber Activated Carbon and Molecular Sieves Function Cleans the ambient air to prevent external VOCs from interfering in analyses See NOTE on following pages for replacement supplies B Load Analyze Valve Function Opens and closes the sample inlet for sample loading The valve has two positions LOAD and ANALYZE See Section 2 2 1 for operating instructions E Sparge Valve Function Prevents liguid from entering air scrubber system G Sparge Manifold Function Routes gas to the proper ports for sparging and analysis functions J Sample Inlet Function Attachment for syringe to load a sample K Sparge Bottle with PEEK Tube Needle type sparge bottle 0 5 x 5mL Function Holds sample to purge VOCs Collects VOCs in the headspace gas collection area The Sparge bottle has two positions UP and DOWN See Section 2 2 2 for operating instructions L Sparge Bottle Nut Function Holds Sparge bottle in place and provides gas tight Seal M Syringe 5mL with Luer Lock Function Loads a fixed sample volume to the sparger Attaches to sample inlet J 20 Defiant se D FROG 4000 User s Manual FX gt Figure 2 2 1 Purge and Trap System Figure 2 2 2 Purge and Trap System 21 Defiant T ee FROG 4000 User s Manual lt a 2 2 Purge and Trap System Continued mm LOAD ANALY
15. ae Section 4 Field and Lab Analysis Procedures Continued Ellvin allows the user to view live results change operating parameters re plot stored data and overlay data for comparison It also has tools for integrating peak areas measuring retention times and calibrating the instrument The FROG 4000 stores data from every analysis on an internal SD card The following steps describe the process for extracting data from FROG 4000 for analysis with Ellvin 1 Connect Port N on the FROG 4000 to a computer using the USB Cable To Computer USB 2 Turn the instrument on O Continued next page 67 Defiant T a gt FROG 4000 User s Manual 0 4 7 Importing Data Continued 3 The computer screen will display an option to Open folder and view files Open the folder 4 The computer screen now displays a list of seguential files named LOG XXX The file names are created and assigned by the instrument They appear on the instrument screen at the beginning of each analysis cycle as shown in Figure 4 7 1 Figure 4 7 1 FROG 4000 display screen at the beginning of a sample run NOTE If the instrument is NOT connected to Ellvin when running analyses the user must record the LOG file numbers of sample runs intended for future analysis The LOG file numbers as well as the instrument estimates are only available on the instrument s screen at the time the sample is run 5 Select the LOG
16. an opened file into Microsoft Excel program for further EXPERT analysis 76 Technologies FROG 4000 User s Manual P Chromatogram Display Screen The software display screen shows sample analysis data e The X axis is time in seconds e The Y axis shows the instrument s PID response and GC temperature C e The peaks correspond to separated analytes Instrument PID Response 2 e4me4oduio 95 Time seconds Key The Key explains colored lines that are shown on display screen Chani Chan2 PCTemp GCTemp Show Temps 77 FROG 4000 User s Manual C 5 1 Features of Ellvin Continued Sample Notes This tool allows the user to records notes about samples while in Live Data or Analyze Window The notes are saved when the sample analysis is completed It is important to record the date and time that data files are created in order to locate and retrieve them for further analysis Sample Notes Magnifying Glass Use this tool to zoom into a chromatogram while data is being collected in Live Data Window or while in Analyze Window to help with integration Detailed instructions for using Magnifying Glass follow in Section 5 2 2 MOVE Use this tool to move the chromatogram up and down the Y axis 78 A FROG 4000 User s Manual KZ FROG 400 Integrator 1 This feature only operates while in Analyze W
17. creates a chromatogram from sample analysis data In this window Ellvin retrieves analysis data that was previously stored on a computer In Analyze Window the user can examine chromatograms closely integrate chromatogram peaks and export data to Excel Calibration Window In this window Ellvin uses analysis data from chemical standards to calibrate the FROG Settings Window In this window Ellvin manages the settings for the FROG The settings define temperature and duration parameters for various phases of the instrument s analysis cycle There are several general features of Ellvin as well as a few features specific to Analyze Window that are described in Section 5 The user should be familiar with all the features before starting a sample analysis 32 FROG 4000 Defant uae us D FROG 4000 User s Manual dest SECTION 4 FIELD AND LAB ANALYSIS PROCEDURES The simplest way to use the FROG is to load samples and run analyses while the instrument is connected to a computer and Ellvin The software analyzes sample data and displays a live chromatogram during analyses The cycle takes about five minutes Data is stored both on the FROG s internal SD card and on the computer The FROG can also analyze samples when not connected to Ellvin An analysis cycle takes the same amount of time five minutes and an estimate of the results are displayed on the instrument s screen Data is stored on the FROG S internal S
18. gas moves through 1 the flow selection valve 2 activated charcoal and 3 the sparge valve The air sampler pulls sample through its own valve onto to place the VOCs onto the preconcentrator PC Arvad Charcoal Diagram 2 5 1 Sample Collection 30 FROG 4000 Defiant T cc D FROG 4000 User s Manual ae 2 5 Gas Flow Diagram Continued 252 INJECTION RELEASE SEPARATION AND ANALYSIS Diagram 2 5 2 Once the VOCs are collected onto the PC the PC is heated to release the VOCs and inject them into the Micro Gas Chromatograph Column GC The VOCs separate through the column and then continue to the Photo lonization Detector PID The PID signal is analyzed and displayed through the software The excess exits through the exhaust eve wd Cher tow Diagram 2 5 2 Injection Separation and Analysis FROG 4000 User s Manual GL SECTION 3 OVERVIEW OF ELLVIN CHROMATOGRAM ELF SOFTWARE The Chromatogram Elf Software Ellvin has four windows that are accessed with tabs when the software is open Live Data Window Tabs in Ellvin e Live Data Window This is the default window for Ellvin In Live Data Window Ellvin creates a chromatogram from sample analysis data The data source may be a From a sample loaded and simultaneously analyzed by Ellvin b From sample data previously recorded on the instrument s SD card then imported to Ellvin e Analyze Window As in Live Data Window Ellvin
19. look for water where the scrubber mounts on the sparge manifold Figure 8 1 2 Positions 1 and 2 Repeat Steps 2 through 5 until water no longer emerges from the sparge manifold 119 Defiant T D FROG 4000 User s Manual E 8 1 Inverting the FROG Continued 6 Replace the activated carbon and molecular sieves in the scrubber then reinstall the scrubber block See Section 8 1 3 Cleaning the Scrubber for procedure details 7 Load a blank sample deionized water and run a third Sparge Cycle Look for bubbles in the sparge bottle e lf bubbles appear the liquid was an successfully removed from the sparge manifold e lf bubbles do not appear then contact Defiant Technologies for consultation Email info defiant tech com Phone 505 999 5880 Figure 8 1 4 Look for Bubbles in the sparge bottle 120 Technologies FROG 4000 User s Manual Ma a Section 8 Troubleshooting Continued 8 2 DEGRADING CHROMATOGRAPHY SCRUBBER IS NOT SECURED PROPERLY If the Chromatography is degrading over time Check the scrubber block The scrubber block may NOT be sealed correctly There should be no space in between the scrubber block and the scrubber holder Figures 8 2 1 and 8 2 2 Refer to Section 8 1 3 Cleaning the Scrubber Figure 8 2 1 Figure 8 2 2 Correct scrubber position Incorrect scrubber position Performance can also be affected by high concentrations of analytes or high back
20. mass of analyte must be converted into an eduivalent volume to determine the concentration on a volume by unit volume basis In a typical calibration process a volume of the liguid standard is injected into an air filled 1 liter Tedlar bag and the analyte in the injection is allowed to come to eduilibrium with the air in the bag If the mass of the analyte in a liquid injection is Mi then the volume of the analyte after reaching equilibrium in the Tedlar bag IS M Re T p MW gt P Where V volume of analyte L M mass of analyte g R gas constant 0 0821 L atm K mol P pressure atm T Temperature K MW molecular weight of analyte g mol Once this volume is known the concentration on a volume unit volume is V ppb v 109 V Where V2 volume of the dilution gas In the case of a 1 Liter Tedlar bag filled with air V gt is 1 L 96 Defiant p mr DD FROG 4000 M User s Manual dw AS FROG 4000 Standard Preparation and Loading Continued 2 Immediately a ter drawing up 5mL Air 6 10 11 Fill Tedlar bag with one liter air Use a metered pump 1 liter gas tight syringe Load Tedlar bag with a volume of liguid standard The concentration in ppb v has been calculated and recorded See previous page Let the Tedlar bag to rest for five minutes to eguilibrate the gases Attach a disposable needle to the empty 5mL syringe Insert the needle into s
21. nut counter clockwise until finger tight to secure the sparge bottle The sparge bottle should not spin in the sparge bottle nut See Section 2 2 2 58 Defiant T ss D FROG 4000 User s Manual ae 3 Attach 5mL syringe to the instruments sample inlet Liquid Sample Load the sample into the instrument Soil Sample First fill the 5mL syringe with deionized water Then attach it to the instrument s sample inlet and load 5mL of deionized water into the sparge bottle 4 Immediately place the load analyze valve in the ANALYZE position closed The syringe may now be removed 2 Sila w ANALYZE Position _ gt gt oo Oe amp 1 ysy ya 59 gt Technologies FROG 4000 User s 4 5 Loading a Sample Continued The instrument display screen shows READY throughout Steps 1 4 of Loading a Sample The Log is automatically generated and assigned to the data file produced by the current analysis cycle 60 Technologies FROG 4000 User s Manual ee Section 4 Field and Lab Analysis Procedures Continued 4 6 Running A Sample This section describes the procedure for running an analysis and the instrument s stages during an analysis cycle Procedure Record notes for future reference e f not connected to Ellvin the user should record the LOG s and other relevant information for future reference The instrument records this number in the file name on th
22. of the selected file appears to the right of the file list Figure 4 7 4 19 Click Select to open the file of interest and proceed to analyze the data with Ellvin Integrator 1 or 2 See Section 5 2 3 Lookin 20140930 7 m Name Date modified ay 21703 LOG 056xml 9 30 2014 5 03 PM Recent Places 1793 LOG 056_Annotationsxml 9 30 2014 5 03 PM e 1716 LOG 057xml 9 30 2014 5 25 PM 2 1716 1006 057_Annotations xml 9 30 2014 5 25 PM Desktop 2 1731_LOG_058xml 9 30 2014 5 31 PM 2 1731 1006 058_Annotations xml 9 30 2014 5 31 PM 1732 LOG 059xml 9 30 2014 5 41 PM XML Doct Libraries 1732_L0G_059_Annotations xml Type XML Document Doct 2 1745_LOG_060 xml Size 663 KB Doct A 2 1745 1006 _060_Annotations xml Date modified 9 30 2014 5 41 PM Doc Computer 0 104 208 312 Notes FROG FROG13 MBTEX Open As Overlay 4 m File name 1732_LOG_059 xml Fies of ype Figure 4 7 4 File Selection Screen 71 FROG 4000 User s Manual C 72 FROG 4000 M User s Manual dea 7 gt FROG 4000 SECTION 5 ELLVIN CHROMATOGRAM ELF SOFTWARE The chromatogram software Ellvin is primarily used to perform detailed analyses of sample data Ellvin uses calibration data to e Assign analytes to chromatogram peaks based on GC retention times e Report the analytes concentrations based on peak heights and integrated peak areas Ellvin also manages the instrument se
23. s Manual ae Section 4 Field and Lab Analysis Procedures Continued Powering On e Connect power cable to power port R 9V POWER or use battery power Figure 4 1 1 e Turn power switch O to ON fully up position The instrument display screen will be visible To R 9V POWER i on 7 th R 9V Power To Outlet Figure 4 1 1 Power port power cable and power switch e When the FROG 4000 display screen shows READY the instrument is ready to load a sample VOC ANALYZER GC TEMP 37C O oie BTEX V 934 2012 37 FROG 4000 User s Manual A 4 1 Powering On Charging Battery Continued Charging the Battery NOTE The instrument can NOT be used while the battery is charging 1 Remove the sparge bottle from the instrument before charging the battery 2 The Instrument should be powered off and disconnected from the power cable 3 Plug battery charger into Battery charge port S and outlet source 4 Place battery charger switch to 1 8A 5 While the battery is charging the light on the charger switch will appear red 6 When the battery is completely charged the light on the charger switch will appear green 7 Itis highly recommended that the battery be fully charged before the instrument is used in an outdoor setting 38 FROG 4000 M User s Manual df FFROG 4000 39 Defiant ep FROG 4000 User s Manual K 40 FROG
24. D card and can be imported to Ellvin and analyzed at a later time if desired Section 4 7 gives instructions for importing data from the FROG MH Continued next page Defiant et a FROG 4000 User s Manual K Section 4 Field and Lab Analysis Procedures Continued This section provides detailed instruction for various procedures that are essential to operating the FROG 4000 Procedures include Description of components and connections Instructions description for components and connections Set parameters to optimize instrument function Remove interfering contaminants ensure a clean instrument Air liguid and soil sample preparation and loading instructions 4 6 Running A Sample Instructions description for an analysis cycle Import stored data from FROG to Ellvin for analysis Technologies FROG 4000 User s Manual SX gt Complete the following procedures to run an analysis NOTE The user should be familiar with Ellvin before loading and running a sample 4 6 Running A Sample m If not connected to Ellvin D 6 Clean the instrument when all samples have been completed by repeating Step 2 Exception Samples of the same known analyte may be run consecutively from low concentration to high without rinsing the instrument and creating a clean baseline 35 FROG 4000 User s Manual C 36 Defiant T cs D FROG 4000 User
25. FROG 4000 Chemical Analysis System User s Manual Defiant Technologies Inc 2014 Vol 4 This page is intentionally left blank FROG 4000 Chemical Analysis System User s Manual Defant Technologies Defiant Technologies Inc 2014 Vol 4 www defiant tech com FROG 4000 a Defiant rh FROG 4000 User s Manual ET Sparge Bottle Defiant T us D FROG 4000 M User s Manual dt HANDLING INSTRUCTIONS FROG 4000 is a robust portable instrument which can be operated in a lab setting or out in the field The internal components of this instrument can be damaged if the unit is abused The following precautions are given to ensure correct handling of the instrument PRECAUTIONS e DO NOT invert with sparge bottle attached System can NOT analyze a sample when it is inverted Permanent damage to instrument is possible If this does occur the system may require maintenance Refer to Section 8 Trouble Shooting e DO NOT handle or carry system when sample is being analyzed For the best results limit movement to before or after sample analysis e DO NOT transport or store the instrument with liquid in the sparge bottle Do NOT invert 90 Angle Do NOT invert 180 Angle FROG 4000 User s Manual C Defiant pee ss D FROG 4000 User s Manual deat 7 FROG 4000 TABLE OF CONTENTS Handling Instructions issus 5 Commonly Used Acronyms
26. Figure 5 2 1 1 the data file was cre ated at 5 16 PM on September 30 2014 e To locate the data file of interest browse to the folder labeled with the date the sample was run or the date the data file was imported from the FROG to Ellvin Double click to open the folder e Click ona data file of interest A preview of the data chromatogram appears to the right of the list e Click Select to open the file for analysis with Integrator 2 80 FROG 4000 User s Manual cs Folder name is the Date File name is the Time ok 763 Name Date modified y e 1703 106 056xml 9 30 2014 5 03 PM Places fe 1703 LOG 056 Annota i fisxml 9 30 2014 5 03 PM 2 9 30 2014 5 25 PM 1716 LOG 057_Annotations xml 9 30 2014 5 25 PM e 1731_LOG 058xml 9 30 2014 5 31 PM 1731_LOG_058_Annotations xml MAU 5 31 PM 1732 LOG 059 Annotationsaml Type XML Document 5 1745 LOG _060 xml Size 663 KB 5 1745_LOG_060_Annotations xml ookin J 20140930 Name 1703_LOG_056 xml 21716 LOG 057xml 9 30 2014 5 25 PM 2 1716 LOG 057_Annotationsxml 9 30 2014 5 25 PM Desktop 121731 LOG 058xml 9 30 2014 5 31 PM a 1731 106 058 Annotationsxml daa 5 31 PM dde he 3_059 x J 1 Libraries 2 1732 LOG 059_Annotations xml Type XML Document 2 1745_LOG_060 xml Size 663 KB Doct A 1745 _ LOG _060_Annotations xml Date modified 9 30 2014 5 41 PM Doct Computer FROG FROG13 MBTEX Open As Overlay 81 Technologies FROG
27. It is good practice to keep the total volume in the sparger at a constant 5 mL For instance if the user wishes to dilute a water sample 10 to 1 a sample volume of 0 5 mL would be diluted with 4 5 mL of clean water resulting in total volume of 5 mL If analyzing soil samples the user must add water to the sparger to ensure that the sample is appropriately agitated The basic steps for operating the system are Adjust apply the settings as needed Ensure that the instrument displays a clean baseline Load a 5 mL sample Run an analysis either connected or not connected to Ellvin a If not connected to Ellvin during the analysis cycle read analysis data using Ellvin at a later time NOTE A working knowledge of Ellvin is necessary to correctly operate the instrument Users should be familiar with the software before attempting analyses 12 FROG 4000 User s Manual The FROG 4000 is designed for use in the laboratory Connect to Chromatogram Elf Software for more detailed analysis results 13 FROG 4000 User s Manual C 14 Defiant 3 FROG 4000 M User s Manual del SECTION 2 COMPENENTS AND SYSTEMS The FROG 4000 instrument has two main operational systems The Purge and Trap System This system manages the loading of a sample sparging the sample if liguid to release VOCs and the introduction of gas phase compounds to the Gas Phase Analysis System All compone
28. NDIX I AVAILABLE ACCESSORIES SPARE PARTS Rechargeable NiMH DT BT NIMH9V5K 1 Battery 9V 5000 mAhr Serial Data Cable Ellvin software FRS DT DC 1 communication a cable Cable USB A MINI B DEG ASSY stored data import cable Battery Charger Holster for holding DT FG4KHL 1 sparge bottles and syringes 129 Defiant ep FROG 4000 User s Manual K 130 FROG 4000 M User s Manual df Se FROG 4000 Common Chemicals Detectable by FROG 4000 1 1 Dichloroethene CAS Number IE eV 75 35 4 120 82 1 106 93 4 95 50 1 541 73 1 106 46 7 123 91 1 71 23 8 78 93 3 107 07 3 591 78 6 107 87 9 109 06 8 67 63 0 108 10 1 67 64 1 107 02 8 107 18 6 107 05 1 71 43 2 100 44 7 598 31 2 75 27 4 75 25 2 74 83 9 75 15 0 108 90 7 124 48 1 75 00 3 126 99 8 1 2 4 Trichlorobenzene 1 2 Dibromoethane 1 2 Dichlorobenzene 1 3 Dichlorobenzene 1 4 Dichlorobenzene 1 4 Dioxane 1 Propanol 2 Butanone MEK 2 Chloroethanol 2 Hexanone 2 Pentanone 2 Picoline 2 Propanol 4 Methyl 2 pentanone Acetone Acrolein Allyl alcohol Allyl chloride Benzene Benzyl chloride Bromoacetone Bromodichloromethane Bromoform Bromomethane Carbon disulfide Chlorobenzene Chlorodibromomethane Chloroethane Chloroprene 131 FROG 4000 User s Manual C Common Chemicals Detectable by FROG 4000 SAS CASE IE eV Crotonaldehyde Dibromomethane Diethyl ether Diisopropyl ether DIPE
29. TEX 400ppm m 5000 uL Water 5000pL Water 1000mL 0 080ppm m I 80pph m 93 Defiant T D FROG 4000 User s Manual a 6 1 1 Standards for Liquid and Soil Samples Continued Preparation Continued 2 Fill a syringe with 5mL deionized water 3 Load a known volume as calculated on the previous pages of a liguid standard into the syringe 4 Connect to Ellvin and follow the sample loading instructions in Section 4 5 94 Defiant 3 ss D FROG 4000 User s Manual dl 612 STANDARDS FOR AIR SAMPLES Run at least four calibration standards from low to high concentrations Tools Needed e Tedlar bag e Metered pump or 1 Liter gas tight syringe e 5mL Syringe e Disposable needle e Deionized water Tedlar bag filled with 1 Liter of compressed nitrogen and syringe with disposable needle attached Instrument Preparation e Place an empty sparge bottle on the instrument in the UP position e Place the load analyze valve in the LOAD position open e Connect to Ellvin Continued next page 95 gt Technologies FROG 4000 User s Manual Ma a 6 1 2 Standards for Air Samples Continued Standard Preparation and Loading 1 Use the ideal gas law to calculate the concentration in ppb of the calibration samples Calibrating the instrument for air sampling reguires converting concentrations in ppb by volume using the ideal gas law Most standards come in liguid form and the
30. ZE VALVE e Turn the load analyze valve to the LOAD position to load a sample e After loading a sample turn the handle counter clockwise to the ANALYZE position before starting an analysis cycle l 9 0 E A ANALYZE J Se Position 9 N 1 22 gt 6 Technologies FROG 4000 User s Manual a lis SPARGE BOTTLE POSITIONS The sparge bottle moves UP and DOWN and is secured with a sparge bottle nut e The bottle must be in the DOWN position to rinse the instrument or to remove the sparge bottle e The bottle must be in the UP position to load and analyze a sample Sparge bottle Sparge bottle in the DOWN position in the UP position NOTE The Activated Carbon and Molecular Sieves may be purchased premeasured and cleaned through Defiant Technologies Inc Activated Carbon Part Number DT FG4K AC 1 Molecular Sieves Part Number DT FG4K MS 1 23 TM CT Technologies FROG 4000 User s Manual AL Section 2 Components and Systems Continued 2 3 GAS PHASE ANALYSIS SYSTEM Gas Phase Analysis System Components and their Functions Figures 2 3 1 and 2 3 2 A Internal Pump Diaphragm pump Function Circulates carrier gas through system B Internal Preconcentrator PC Function Collects and injects VOCs into GC column C Internal Micro Gas Chromatography Column GC Function Separates VOCs D Internal Photo lonization Detector PID 10 6eV lamp
31. a from chemical standards to calibrate the FROG Settings Window In this window Ellvin manages the settings for the FROG The settings define temperature and duration parameters for various phases of the instrument s analysis cycle Refer to 74 Technologies FROG 4000 User s Manual eg PORT Use this feature to select the correct data port connection from the FROG 4000 The user selects a COM to connect to the FROG PORT COM3 Connection Port Based on the selection of COM the Connection Port will notify the user if the FROG is CONNECTED or DISCONNECTED and if the parameters have been updated Bottom left corner of the software display screen PARAMSUPDATED PARAMS UPDATED GC Column Temperature Indicator This feature monitors and displays the GC temperature The icon is GREEN when instrument is ready for Loading It turns RED during sample analysis oO 75 Prion FROG 4000 User s Manual C 5 1 Features of Ellvin Continued Start Stop Button Clicking on this button causes the FROG 4000 to start an analysis cycle Once the analysis has begun clicking the button will stop the analysis but will NOT save the chromatogram OPEN Button Click on this button to open saved files The files can be from data stored on a computer or on the instrument s internal SD card EXPORT Export only works when Ellvin is in Analyze Window The user can export
32. alysis Procedures Continued NOTE The instrument should have a clean baseline to begin sample loading and analysis Refer to To ensure optimal sample analysis adhere to the following sampling procedures and sample parameters Liquid Sample Pull 5mL of the desired liquid into a 5mL syringe Soil Sample a Remove the sparge bottle from the instrument b Add 1 g of soil to the sparge bottle with then add 5 mL of clean water c Rinse the sparge bottle thoroughly between samples or use Defiant s disposable sparge bottles Air Sample Connect the air sampler adaptor and wand to the FROG Section 4 4 3 When running an analysis Section 4 6 hold the wand in the area desired for sample collection Detailed instruction begin on the following page 57 Defiant T lt lt gt FROG 4000 User s Manual ET 4 5 Loading a Sample Continued e f concentrations are known during calibration for example a series of samples of the same analyte may be run consecutively without rinsing the instrument They must be run in order from low to high concentrations to prevent cross contamination Procedure 1 Place load analyze valve in the LOAD position open See Section 2 2 1 2 Attach the sparge bottle and place it in the UP position Liquid or Air Samples The sparge bottle is clean and rinsed Soil Samples The sparge bottle is loaded with the soil sample Turn the sparge bottle
33. alyze the Data In this section Ellvin analyzes the stored instrument response data to create the information needed for calibration Open the Analysis Window C 1 Click on the OPEN button to access a list of previously run sample files Figure 6 3 1 See Section 5 2 1 for details C 2 Select the calibration sample file desired for data analysis The files are labeled by the time they were created Select Data File Lookin jy 11282011 em ES Mame Date modified Type lt 0853 11 28 2011 853 AM XMLD Pisces 0853 Annotations 11 28 2011 8 53 AM XMLD x 0903 11 28 2011 9 03 AM XML D 0903 Annotations 11 28 2011 9 03 AM XML D Desktop 8 11 28 01 18 AM XML D Fr 918 Annotations 11 28 2011 18 AM XML D 0928 11 28 2011 9 28 AM XMLD Libraries 0928 Annotstions 11 28 2011 9 28 AM XMLD 10938 11 28 2011 9 38 AM XML D L 0938 Annotations 11 28 2011 9 38 AM XML D EE a n Computer 0950 11 28 2011 9 50 AM XMLD 950 Annotations 11 28 2011 9 50 AM XML D a 1001 11 28 2011 10 01 XMLD Blue Mpeh Network Fles of type Chart ami Open As Overlay Figure 6 3 1 Open Sample Files 105 Defiant T D FROG 4000 User s Manual CE 6 3 Calibration Procedure Continued C 3 In the Analyze Window click on the Integrator 2 button to integrate the sample peaks in the chromatogram Refer to Section 5 2 3 for detailed instructions on using t
34. are sparged and collected on the PC 62 gt FROG 4000 User s Manual K 4 Release and Analyze Settle The sample flow is switched to the analysis channel The pressure is allowed to stabilize before the PC fires 5 PC Fire The PC is heated and analytes are injected released into the GC column and continue through to the PID 6 Analyzing The PID measures analytes as they emerge seguentially from the GC 7 Chromatogram The analysis concludes with a chromatogram of the analytes detected NOTE the chromatogram does not appear on the display if the FROG is connected to Ellvin 63 Defiant T gt FROG 4000 User s Manual E 4 6 Running a Sample Continued Analysis Sequence Continued 8 Instrument Estimation When the instrument is not connected to Ellvin it makes an estimate of the analytes concentrations based on Estimate 1 calibration data Click the Start Button to see the next analyte scroll through analytes The estimate Click the yellow start button to two estimates shown in this example are 33ppb Benzene and 63ppb Toluene The GC retention time for Benzene is displayed as 48 33 seconds Estimate 2 NOTE The instrument estimates are only available immediately after the corresponding analysis They are NOT stored on the instrument s SD card Complete analysis data is stored on the SD card and can be imported to Ellvin for further analysis
35. e internal SD card e If connected to Ellvin the user can record relevant information for sample identification in Ellvin s Sample Notes window Ellvin automatically stores the analysis data file in a folder labeled with the date The file itself is labeled with the time it was created Sample Notes After the sample loading is complete Section 4 5 the user may begin sample analysis by pressing the start button If connected to Ellvin click the start button in the software If not connected to Ellvin press the yellow start button on the instrument Start Button on the Frog x 2 EN alyze Calibration Settings Start Button in Ellvin Continued next page 61 gt wats tts LE Technologies FROG 4000 User s Manual CL 4 6 Running a Sample Continued During an analysis cycle the FROG screen displays the analysis steps in sequence as illustrated below and on the following pages This information is only visible on the instrument screen not Ellvin screen Each sequence has a clock counting down the duration of the current analysis step The duration of the analysis step is determined by the instrument settings See Section 4 3 The GC TEMP may vary slightly from the set point Analysis Sequence 1 Cleaning Prior to Sparging The PC is heated to drive off contaminants analytes from previous runs 2 Settle The PC cools before sparge begins 3 Sparge and Collect VOCs
36. ed by the Ellvin A graph of the data points and the curve fit will be displayed in the calibration window for the user to inspect the fit equation Downloading the Calibration to the Instrument Connect the instrument to Ellvin with the USB cable Refer to 1 All analytes listed in the calibration should show a R correlation close to 1 0 The closer the R value is to 1 0 then the better the software can calculate the concentration of an unknown sample 2 Open the Settings Window Live Data Analyze Continued next page 109 D FROG 4000 User s Manual ET 6 3 Calibration Procedure Continued 3 Click on Download Calibration to Device DOWNLOAD CALIBRATION TO DEVICE 4 This will allow the instrument to estimate the concentration of analytes uploaded into the calibration using the peak height linear function NOTE The Ellvin software can compute concentrations using either peak height or area under the peak However when the instrument is running independently its processing power is more limited so peak height is used in the calibration 110 Defiant T FROG 4000 M User s Manual del SECTION 7 MAINTENANCE 7 1 ROUTINE CLEANING It is important to clean the FROG 4000 after analyzing samples in order to prevent cross sample contamination The FROG 4000 M does need to be cleaned if e More than one type of analyte is being tested The user must clean the instrume
37. epta of Tedlar bag and draw up 5mL air Remove the needle and syringe from the septa on Tedlar bag Remove the disposable needle Insert syringe with needle from the syringe and attach the into septa of Tedlar bag syringe to the sample inlet of the WM instrument Load the air sample into the instrument Immediately after the loading place the load analyze valve in the ANALYZE position closed Press the start button and run sample Refer to Repeat for other sample concentrations 97 Technologies FROG 4000 User s Manual Ma WN Section 6 Calibration Continued 6 2 ELLVIN CALIBRATION WINDOW FEATURES e To start using Calibration Window open Ellvin and click on the Calibration Tab 2 gt OPEN EXPERT PORT COME Live Data Calbraion Tyettngs 621 LIST OF ANALYTES This feature allows the user to create a List of Analytes that may be used to calibrate the instrument The analyte names in the List of Analytes will later be associated with analyte peaks from calibration standard runs See Figure 6 2 1 The Retention Time Peak Height and Peak Area in Figure 6 2 1 are generated from previous analyses of standard solutions with known concentrations Analyte Name Benzene Analyte Alias Benz Analyte Window 500 SET Analytes Data seconds MTBE Peak Time Height Area Concentration FileName ee 153 209746 4 CNUsesaiui Touene 2 42 994 175801 1065216 7
38. file of interest and drag copy it to the computer desktop or other location of user s choice 6 Open Ellvin 7 Open Live Data Window ive Da ane Cabraton Setngo 8 Click on the OPEN button OPEN 68 Technologies gt 6 FROG 4000 User s 10 11 12 ROG 4 Browse to the location where the LOG file of interest was dragged copied At the bottom of the Select Data File window change Files of Type to LOG Files File name Select Data File ynau Fies xml Select the LOG file of interest and open it The computer screen now displays a chromatogram of the file data as it is imported into Ellvin At this time Ellvin also converts the data to an XML format and stores it The location path of the stored data is displayed at the top of the chromatogram in the Live Data Window Figure 4 7 2 The data can now be opened in the Analyze Window E w oPEN 3 HIERT PORT Eln version 20401 lt Data Location Path 0 120 150 TT CONNECTED PARAMSUPDATED 8756 V 29753900 ANALYZE 4744 45806 Figure 4 7 2 Live Data Window with chromatogram and data location path 69 fochanagles FROG 4000 User s Manual C 4 7 Exporting Data Continued 12 Open the Analyze Window Live Calibration Settings The location path for the stored data is also displayed in Analyze Window 13 Click on the OPEN icon 14
39. gram Peaks 51 709 52205 288173 MTE 0106 41757 400032 7 Geene D 222 025 27246 297169 4 239 372 49086 683288 Ethylbenzene 283 611 15982 232827 P M Xylene Figure 6 3 4 Benzene is Selected for Peak 1 107 Defiant a gt FROG 4000 User s Manual ded 6 3 Calibration Procedure Continued D 3 To view the imported data open the Calibration Window click on List of Analytes and select the desired analyte The imported data for this analyte will be displayed In the example in Figure 6 3 5 Benzene has been selected Analytes MTBE Toluene Ethylbenzene P M Xylene O Xylene Benzene Figure 6 3 5 Select the Desired Analyte from the List of Analytes D 4 In the Calibration Window enter in the corresponding concentration for the calibration standard in the column titled Concentration Standard concentrations were recorded in the Sample Notes window in Section B of the Calibration Procedures See B 4 29 88 48 389 23342 7129 TH Technologies FROG 4000 User s Manual TX Repeat Steps C 1 through D 4 of the Calibration Procedures to import and enter all the standard data to the Calibration Window The Correlation Chart and Equations Section 6 2 2 will NOT appear until three different concentrations per analyte are imported into the Calibration Window Once three or more calibration data points are complete correlation equations are generat
40. grator 2 button to start e Right click and hold the mouse at Valley 1 e Drag to Valley 6 and release e The integrator uses Ellvin to select the baseline on which the integration line is drawn e The highlighted area shows which area is being integrated Figure 5 2 3 5 e The integration is complete when a solid black line appears The result shows the integration line and the splits placed between joined peaks Figure 5 2 3 6 e The Data Grid shows the data that corresponds to the related peak The user can continue integrating peaks OBEN WE EXERRT PORT CanaryFrog Version 2 0 8 5 Detiant C Documents and Settings Administrator Application Data Defianti1101 xml plm Xylene 274 65 Peak Time Height Widh Concentration D Defaut 050 O Chant E Chan i PCTemp DE pue CONNECTED PARAMSLOADED X 367 05 Y 460398 50 ANALYZE 325 05 Figure 5 2 3 5 Integrated area is highlighted 88 FROG 4000 M User s Manual dea FROG 4000 gt EXERRT PORT coms CanaryFrog Version 2 0 8 5 Live Data Analyze Calibration Settings 888 165 C Documents and Settinas Administrator Application Data Defiant 1101 xml Notes Chart Data Do O Default O Chant 128 982 314392 tek vis 25620 172353 PCTem p ALES sp Be zaer am 323368 112029 CONNECTED PARAMSLOADED 5 X 367 05 Y 460398 50 ANALYZE 325
41. ground concentrations in the surrounding environment See next section 121 gt CT Technologies FROG 4000 Users Manual AC Section 8 Troubleshooting Continued 8 3 CANNOT ACHIEVE A CLEAN BASELINE If a clean baseline cannot be achieved after repeatedly following the procedures in Sections 4 4 1 and 4 4 2 Rinsing the Instrument and Creating a Clean Baseline contamination problems may stem from having loaded a sample with a high concentration of analyte or from the presence airborne contaminants NOTE A small peak at the beginning of the chromatogram is normal for a clean baseline Complete the following procedures to eliminate contamination interfering with a clean baseline Perform procedure 4 4 while connected to Ellvin and using warm deionized water Refer to Repeat this procedure up to three times if necessary to achieve a clean baseline Airborne Contaminants If it is still NOT possible to achieve a clean baseline there may be airborne contaminants present in the ambient air An airborne contaminant can enter the sparge bottle when it is lowered This volume of air cannot be scrubbed and will be collected by the PC Airborne contaminants can also enter through the pump with the sparge and carrier gas 122 FWYN FROG 4000 User s Manual SEX Solutions 1 Either circulate air in the testing environment or move to a new location then perform If a clean baseline is stil
42. he Integrator 2 The results of the data analysis are displayed on the chromatogram and in the Data Grid Figure 6 3 2 The example shown in Figure 6 3 2 is for a sample of BTEX Analytes may be run one at a time to determine or confirm retention times O Xyleee CAlUJsers ajtrujillo AppDats Rogie Defiant 1 128201 10950 xml Analyte Peak Time Height Area Width Concentration Ca 3 48 389 0 4 105 327 13843 144611 0 0 00 6 225 76 21078 241724 0 0 00 Figure 6 3 2 Analysis Chromatogram and Data Grid 106 Defiant ee uc D FROG 4000 User s Manual SEX gt D Calibrate the Instrument In this section the data analyzed in Section C is transferred to the Calibration Window Ellvin uses the data to calibrate the instrument for each analyte D 1 To transfer data to the Calibration Window Right click the Data Grid The List of Analytes previously recorded in the Section A of the Calibration Procedures appears D 2 Use the Analyte drop down list to select the analyte that corresponds to each peak based on retention time Match all the peaks with an analyte In the example shown in Figures 6 3 3 and 6 3 4 benzene is selected for Peak 1 because in previous single analyte tests benzene had a retention time of 52 seconds NOTE Retention times are dependent on instrument and temperature profile and will vary from instrument to instrument Benzene Figure 6 3 3 Assigning Analytes to Chromato
43. indow The user creates a baseline and integrates peaks then calculates the peak height and area The baseline integration limits are sets by clicking the left mouse button Integrator 2 This feature only operates while in Analyze Window Ellvin creates a baseline and integrates peaks then calculates the peak height and area Integrator 2 is recommended for the most consistent analysis results Detailed instructions for using Integrator 2 follow in Section 5 2 3 Data Grid Use with Integrator 1 and 2 The Data Grid shows e Analyte Toluene Based on calibration retention times e Peak Reference Number 1 e Retention Time 106 157 e Peak Height 40291 e Peak Area 430363 e Calculated concentration 87 31 Based on calibration concentrations Analyte Peak Time Height Area Width Concentration gt Toluene a 106 157 40291 430363 79 Technologies FROG 4000 User s Manual Ma Section 5 Ellvin Chromatogram Elf Software Continued 5 2 APPLYING ELLVIN FEATURES 5 2 1 OPEN BUTTON To open stored files in Analyze Window e Click on the Analyze Tab Live Dai Pah aaa Settings e Click the OPEN button e A file selection screen appears Figures 5 2 1 1 and 5 2 1 2 NOTE Ellvin automatically labels folders and files as they are created Folders of data files are labeled by the DATE they were created Data files are labeled by the TIME they were created In the example shown in
44. ity conditions is recommended for optimum performance 125 Defiant ep FROG 4000 User s Manual K 126 Tacheologies FROG 4000 User s Manual EX APPENDIX I AVAILABLE ACCESSORIES SPARE PARTS Activated Carbon eS Replacement Activated het Carbon for FROG 4000 i ie DT FG4K AC 1 air scrubber a Pre measured and pre cleaned Molecular Sieves a Replacement Molecular DT FGAK MS 1 Sieves for FROG 4000 air scrubber Pre measured Um and pre cleaned DT FGAK SBGN 1 Sparge a globe Sparge Bottle Nut o DT FG4K SBN 1 Nut to connect Sparge 0 a Bottle to instrument Disposable Sparge Bottles Disposable Sparge Bottle hese i DT FG4K SB6P 1 reguire the disposable sparge bottle adapter Disposable Sparge Bottle Adaptor Disposable Sparge Bottle N FGAK SBA 1 Adapter For use with ere the disposable sparge bottles 127 Defiant CP cc FROG 4000 User s Manual APPENDIX I AVAILABLE ACCESSORIES SPARE PARTS 5mL Glass Syringe DT FGAK SYGG 1 5mL glass syringe with Luer Lock tip 5mL Plastic Syringe a with Luer Lock tip 60mL Rinsing Syringe 60mL syringe with Luer DT FG4K SYGN 1 Lock tip for rinsing _A Sparge Needle DT FGAK LL 1 Attachment for syringe DT FG4K WTB 1 Water Trap Bottle with Insert Tool Kit Assorted tools for DT FG4K TK 1 maintenance of FROG 4000 128 Defiant T uc D FROG 4000 User s Manual del APPE
45. l not achievable 2 Clean the scrubber See Section 7 3 If a clean baseline is still not achievable 3 Provide and activated charcoal trap at the pump inlet V 123 Technologies FROG 4000 User s Manual Ma Section 8 Troubleshooting Continued 8 4 BLACK INSTRUMENT SCREEN Periodically the instrument display screen will appear black However it should reset to appear normal at the end of an analysis run If the display screen on the FROG remains black it can be a sign that the instrument is overheating Take the following steps to cool the FROG 1 Place instrument in the shade or indoors to help cool the GC Temp to READY status 2 Increase the initial cold GC temperature Ct to a maximum of 50 C a Go to Settings Window Refer to b Change GC initial cold temperature C to the following range minimum of 40 C maximum of 50 C Figure 8 3 1 c Click SET to save changes 124 TS FROG 4000 User s Manual 0 Live Data Anne Carat Sense JUN yo Ta 320 Tb 60 Tc 60 Ht 110 COLLECT 30 CLEAN 14 PRESET TLE 14 SETTLE 2 FIRE 6 SET Figure 8 3 1 Change the GC Settings NOTE Increasing GC Temp will affect retention times The instrument will operate within temperature and relative humidity conditions of 0 557C and O to 90 respectively however an environment comfortable for human habitation reasonable constant temperature and humid
46. nalytes A 1 Open the Calibration Window Live Data Anahe A 2 Begin by adding each of the analytes chosen for calibration one at a time to the Analyte List See Section 6 2 1 e No data will be displayed and the chart display area will be blank Disregard any equations displayed Continued on Next Page 103 Defiant T D FROG 4000 M User s Manual dt 6 3 Calibration Procedure Continued B Run the Calibration Standards In this section the calibration samples are loaded and instrument response data is stored Open the Live Data Window Live Date y alyze Calibration Settings B 1 Create a clean baseline before running any calibration samples Refer to B 2 To begin the calibration load and run a sample containing only deionized water Refer to B 3 Load and run a minimum of four calibration standards of the selected analytes The samples should be of varying concentrations and should be run in order from low to high concentrations See Section 6 1 for sample preparation B 4 For each of the calibration standards record the concentrations in the Sample Notes window This will help identify the files during analysis and calibration Sample Notes 104 Technologies FROG 4000 User s Manual K5 FROG 4000 After the instrument has completed running the four or more calibration standards go to the Analyze Window in Ellvin to analyze the instrument response data C An
47. ne Toluene Ethylbenzene Xylenes Ellvin Chromatography Software FROG 4000 Defiant ep FROG 4000 User s Manual K 10 FROG 4000 M User s Manual deat FFROG 4000 SECTION 1 GETTING TO KNOW THE FROG 4000 1 1 MANUAL OVERVIEW The FROG 4000 uses a practical approach to instrument set up and operations This manual includes the following An overview of the FROG 4000 Moperational systems components and features Diagrams illustrating the flow of a sample during loading sparge collection and analysis Instructions for using the chromatography software Ellvin Detailed procedures for using the FROG 4000 V Instructions for calibrating the instrument Routine maintenance information Troubleshooting information 11 gt TM CT Technologies FROG 4000 User s Manual AL 1 2 OPERATIONS OVERVIEW The FROG 4000 instrument analyzes air water or soil to identify volatile organic chemicals VOCs present in a sample and determine their concentrations The instrument is designed to operate either in the field or in a laboratory and either connected or not connected to a computer running the Ellvin Software Data is stored on the user s hard drive when the FROG is attached to a computer Alternatively data can be stored on the FROG s internal memory card and imported to a computer later The FROG 4000 has a 5 mL sample sparger that can be used for water or solid samples
48. ne on Ellvin Screen A small peak at the beginning of the chromatogram is normal 0 00 50 00 100 00 150 00 200 00 200059000 55000 ao o If Peaks do appear repeat the instrument preparation procedures 4 4 1 Rinsing the Instrument and 4 4 2 Creating a Clean Base line until a clean baseline is achieved 52 gt FROG 4000 User s Manual KL 4 4 Instrument Preparation Continued 3 CONNECTING THE AIR SAMPLE ADAPTOR If analyzing air sample the user must first connect the air sample adaptor to the FROG Valve Control The air sample kit includes a sample wand and an air sample bag adapter The air sample bag adapter enables direct connection to an air sample bag 53 Defiant T rh gt FROG 4000 User s Manual lt a 4 4 3 Connecting the Air Sample Adaptor Continued 1 Attach the air sampler to the FROG sparge needle Be sure the valve is pointed to the right 2 Connect the air sampler s valve connector to the FROG valve connection This VERS z ed 9 12 VDC connection supplies power to POWER CAPER SAMPLER the air sampler 2 Q d 3 Attach the exhaust connector to the FROG exhaust with a twisting motion 54 FROG 4000 User s 6 Connect the air sample wand to the air sampler 55 FROG 4000 User s Manual C 56 Defiant T ss D FROG 4000 User s Manual ae Section 4 Field and Lab An
49. nt between sets of the different analytes The FROG 4000 does NOT need to be cleaned immediately if e Same analyte is being tested The user can run a set of samples of the same analyte from a LOW concentration to a HIGH concentration consecutively The user cleans the instrument at the end of the set e Rinsing the sparge bottle and syringe between uses is always recommended To clean the instrument perform the following procedures The instrument is clean when a clean baseline has been achieved 111 Defiant T D FROG 4000 User s Manual cu Section 7 Maintenance Continued 7 2 ANNUAL CLEANING It is recommended to have the FROG 4000 M cleaned yearly by an authorized representative Please contact Defiant Technologies for support Email info defiant tech com Phone 505 999 5880 7 3 CLEANING THE SCRUBBER It is recommended to clean the carrier gas scrubber every three months or as needed to create a clean baseline Tools needed to clean the scrubber include 1 Clean Activated Carbon 2 Clean Molecular Sieves 3 3 32 allen wrench Figure 7 3 1 Tools needed NOTE Replacement activated carbon and molecular sieves may be purchased premeasured and cleaned through Defiant Technologies Inc Activated Carbon Part DT FG4K AC 1 Molecular Sieves Part DT FG4K MS 1 112 gt z Technologies FROG 4000 User s Manual EX 1 Remove the four corner 4 40 screws with the 3 32
50. ntrator Bypass Valve Sample a ff Exhaust 7 Bypass Line E Sparge Bottle Eee x Carrier Gas F2 Bat 7 gt lt c SEA Micro GC VOCs Diagram 2 3 2 Sparge and Collection 28 243 INJECTION RELEASE SEPARATION AND ANALYSIS Diagram 2 4 3 Once the VOCs are collected onto the PC the PC is heated to release the VOCs and inject them into the Micro Gas FROG 4000 User s Manual Chromatograph Column GC The VOCs separate through the column and then continue to the Photo lonization Detector PID The PID signal is analyzed and displayed through the software The excess exits through the exhaust Activated Charcoal Sparge Valve Molecular Sieves 0 0 0 0 00 0 0 Flow Selection Valve Load Preconcentrator Bypass Valve ms Sample m d aust Sparge Bottle Carrier Gas 1 VOCs Diagram 2 4 3 Injection Separation and Analysis 29 Defiant FROG 4000 User s Manual SX 0 P Section 2 Systems and Components Continued 2 5 GAS FLOW DIAGRAMS THROUGH AIR SAMPLER This section describes and illustrates the flow of a sample from loading through the components of the Gas Phase Analysis System through the air sampler Section 2 2 254 SAMPLE COLLECTION Diagram 2 5 1 The air sampler is connected to the Frog 4000 The start button is pressed and the pump flow starts The carrier
51. nts of the Purge and Trap System are visible on the instrument exterior The Gas Phase Analysis System The Gas Phase Analysis System receives the VOCs from the Purge and Trap System and carries them through all stages of sample analysis Collection Injection gt Separation Detection The instrument s components are briefly described on the following pages 15 Technologies FROG 4000 User s Manual Section 2 Components and Systems Continued 2 1 INSTRUMENT COMPONENTS Components Reference for FROG 4000 M Scrubber Load Analyze Valve Display Screen Sparge Valve Line Sparge Valve Flow Selection Valve Sparge Manifold 2 3 D Pump Split Pump Split Cover not shown Sample Inlet Sparge Bottle with PEEK Tube Sparge Bottle Nut ZE NN 5 mL Syringe to load sample 16 A 0 e gt a r FROG 4000 D FROG 4000 M User s Manual 17 Technologies FROG 4000 User s Manual Ma a 2 1 Instrument Components Continued USB Port for stored data Power Switch Port for Serial Data Plug Port for 9V Power Plug Port for Battery Charge Plug Port for Air Sampler Plug Battery Start Button Pump Inlet for Carrier Sparge Gas 5 gt proz Exhaust from Gas Analysis Module 18 FROG 4000 User s Manual del 19 gt TM CT Technologies FROG 4000 User s Manual AL Section 2 Systems and Components Continued 2 2
52. s the correct calculation for the peak area Figure 5 2 3 2 84 FROG 4000 User s Manual K5 Integration Line Valley 1 Valley 2 Diagram 5 2 3 1 Valleys and Peaks Valley 1 Diagram 5 2 3 2 Crossing Data Line 85 gt Defiant pe D FROG 4000 User s Manual K 5 2 3 Integrator 2 Continued Integrating a Single Peak Using the correct techniaue illustrated on the previous page select the desired peak for integration e Select Integrator 2 2 e Right click the mouse and hold at Valley 1 e Drag to Valley 2 and release e The Integrator 2 tool uses the software to select the baseline on which the integration line is drawn e The highlighted area will show which area is being integrated Figure 5 2 3 3 e The integration is complete when a solid black line ap pears e The Data Grid shows the data that corresponds to the related peak The user can continue integrating peaks 86 FROG 4000 M User s Manual dw AS FROG 4000 LL dlr glo po oam Dan DL dep aei Figure 5 2 3 3 Desired Peak Integrated Area Cheers ar ah gwl ete Bg bwt yy TO 43008 one Figure 5 2 3 4 Integration Line gt Toere EN Data Grid 87 Defiant T n FROG 4000 User s Manual a 5 2 3 Integrator 2 Continued Integrating Multiple Peaks To integrate multiple peaks follow the same procedures for integrating a single peak using Integrator 2 Click on the Inte
53. se parameters to calculate concentrations for future samples 100 1 Sy Cc gt 0 o 0 D F o o o Wi o O cc LL wey pue suonenbg uoue 941109 7 7 9 94n814 69 LOL 00166 0 000 26116 X900 3Z 9 E A 97666 0 000 32612 L 0900 238666 0710 29069 C A gdd uopeguso2u07 69 8 69 19 69 LF 69 Le UDIH 9 ealy ad Lo T a gt ae 101 Defiant T D FROG 4000 User s Manual cu Section 6 Calibration Continued 6 3 CALIBRATION PROCEDURE The Calibration Procedure consists of running a series of analysis cycles with standards of varying concentrations for a given analyte Ellvin then uses the analysis data for the standard solutions to calibrate the instrument Before beginning a calibration the user should be familiar with And Using Ellvin See Section 5 102 Technologies FROG 4000 User s Manual 4 It is recommended to run a minimum of four standards from low to high concentration to create data points for calibrating the instrument The concentration range for calibration standards depends on the analyte and its unique retention time Example standards concentrations for a calibration 2 10 50 100ppb Calibration Procedure Steps A Add the Calibration Analytes to the List of Analytes See Section 6 2 1 The steps in this section prepare the software to calibrate using selected a
54. the start button and display screen are in the software If the instrument is not connected to Ellvin the start button and display screen are on the instrument Rinse the instrument as described in Section 4 4 1 before attempting to achieve a clean baseline Procedure 1 Place load analyze valve in the LOAD position See Section 2 2 1 2 Place rinsed sparge bottle in the UP position and turn the sparge bottle nut counter clockwise only finger tight to secure it See Section 2 2 2 3 Attach syringe with 5 mL deionized water to FROG 4000 4 Load deionized water into FROG 4000 5 Remove the empty syringe 6 Place the load analyze valve in the ANALYZE position Continued following pages 50 gt FROG 4000 User s Manual CK e gt LOAD 5 Fa WN Le D P tis H 9 2 9 Defiant T D FROG 4000 User s Manual ET 4 4 2 Creating a Clean Baseline Continued 7 Begin an analysis cycle using deionized water If connected to Ellvin click the start button in the software If not connected to Ellvin press the yellow start button on the instrument Start Button Start Button in Ellvin When the analysis is finished a clean baseline should appear A clean baseline is basically smooth with no significant peaks A small peak at the beginning of the chromatogram and small waves in the clean baseline are acceptable 20000 Clean Baseli
55. to Step B 3 in Section 6 3 on STANDARDS FOR LIQUID OR SOIL SAMPLES Run at least four calibration samples from low to high concentrations Preparation 1 Calculate the dilutions for the intended calibration samples Traditionally a ppb concentrations of analytes in water are expressed in micrograms of analyte per liter of water 1 Kg water Standards typically come pre diluted in methanol which cannot be ionized and therefore not detected by the instrument s PID The following page provides examples for calculating dilutions ug mL ppm mass ug L ppb mass BTEX Benzene Toluene Ethylbenzene p m Xylene o Xylene 92 FROG 4000 Technologies FROG 4000 User s Manual SEX Diluting from a Standard Using the 2000 ug mL BTEX in MEOH standard you want to make a 200 ug mL BTEX in MEOH standard in 5mL MEOH How much 2000ug mL BTEX in MEOH is needed to make this dilution 200 E BTEX in MEOH 5mL MEOH 2000 55 BTEXin MEOH mL 0 5mL x 1000 _ 500 ul BTEX in MEOH Inject 500uL of the 2000 ug mL BTEX in MEOH into 5mL MEOH to create a 200ug mL BTEX in MEOH Diluting 5mL Water with Standard Convert mLto uL 5mL water filled syringe into 5000uL 1000 nL imL 1 5000 uL Spiking the 1 5000 water filled syringe You have a 200ppm BTEX standard What is the resulting concentration from injecting 2uL of the 200ppm BTEX standard into the SOOOuL water filled syringe 2uL 200ppm m B
56. trument is connected to a computer through Ellvin Instructions for adjusting the settings begin on the following pages Connect to Ellvin to manage the settings 45 gt CT Technologies FROG 4000 User s Manual C 4 3 Instrument Settings Continued Table 4 3 1 Description of Settings Hold time at lower GC temperature seconds Ramp time from GC cold to GC hot temperature C Hold time at hot GC temperature C Initial cold GC temperature C NOTE If used outdoors the user must consider ambient conditions Final hot GC temperature C COLLECT Collection time of VOCs onto PC seconds This corresponds to the sparge time CLEAN Time cleaning PC by heating seconds PRESETTLE Time PC cools between cleaning seconds SETTLE Time allowed for pressure to stabilize before PC FIRE seconds FIRE Time PC is Heated to Release VOCs seconds Temperature C Time sec Figure 4 3 1 Description of GC Temperature Settings 46 gt 1 FROG 4000 User s Manual SX Defining and applying the settings 1 Connect to Ellvin Refer to 2 Click on the Ellvin Settings Tab Live Data Analyze Calibrati 3 Type in a non zero integer then click SET to apply the settings to the instrument Changes to the settings are stored on the instrument and DO NOT revert to the default settings when power is removed or computer is disconnected The minimum and maxim
57. ttings and calibrates the instrument Several general features of Ellvin as well as a few features specific to Analyze Window are described in the following pages The user should be familiar with all the features before starting a sample analysis Software Features gt OPEN EXERT PORT Coms Figure 5 1 Ellvin default screen details To start using Ellvin refer to Continued next page 73 FROG 4000 User s Manual A Section 5 Ellvin Chromatogram Elf Software Continued 5 1 FEATURES OF ELLVIN WINDOWS The Chromatogram Elf Software Ellvin has four windows that are accessed with tabs when the software is open Live Data Analyze Calibration Settings Window Tabs in Ellvin Live Data Window This is the default window for Ellvin In Live Data Window Ellvin creates a chromatogram from sample analysis data The data source may be a From a sample run on the FROG while connected to Ellvin and simultaneously imported to Ellvin b From sample data previously recorded on the instruments SD card then imported to Ellvin Analyze Window As in Live Data Window Ellvin creates a chromatogram from sample analysis data In this window Ellvin retrieves analysis data that was previously stored on a computer In Analyze Window the user can examine chromatograms closely integrate chromatogram peaks and export data to Excel Calibration Window In this window Ellvin uses analysis dat
58. ubber holder on the instrument body and the scrubber block Figures 7 3 6 and 7 3 7 14 To fix space in between remove the block and make sure O rings are in the proper position Figure 7 3 6 Figure 7 3 7 Correct scrubber position Incorrect scrubber position 115 Defiant ep FROG 4000 User s Manual K 116 Defiant 3 ss D FROG 4000 M User s Manual dl SECTION 8 TROUBLE SHOOTING 8 1 INVERTING THE FROG WITH WATER IN THE SPARGE BOTTLE If the FROG has been inverted with water in the sparge bottle it is likely that water will enter the sparge manifold Scrubber CE 4 Sparge Manifold The steps on the following pages can be used to remove the water 117 Defiant T D 606 4000 7 User s Manual det 8 1 Inverting the FROG Continued 1 Remove the scrubber Look for liquid in Position 1 or Position 2 on the sparge manifold Position lae Position 2 Figure 8 1 2 Look for liguid 2 Turn the load analyze valve to the ANALYZE position 3 With the scrubber removed install an empty sparge bottle Figure 8 1 3 Close the valve to the ANALYZE position 118 Pefanl 4 FROG 4000 User s Manual oe 4 Press the start button on the FROG and allow the system to run through the sparge stage of the analysis cycle a sparge cycle Turn the FROG off when the screen displays SPARGE OFF Refer to 5 After the sparge cycle power the unit down and
59. um values are listed next to the Figure 4 3 2 Ta 360 Tb 60 Tc 30 Ct 40 Ht 100 COLLECT 2 CLEAN 4 PRESETTLE 4 SETTLE 2 FIRE 6 SET Figure 4 3 2 Setting Window 47 FROG 4000 M User s Manual Figure 4 4 1 Rinsing the Instrument Steps 1 3 48 facing FROG 4000 M User s Manual eg Before running analyses the instrument should be rinsed and display a clean baseline aad RINSING THE INSTRUMENT 1 Place the load analyze valve in the LOAD position See Section 2 2 1 2 Place sparge bottle in the DOWN Position See Section 2 2 2 3 Attach syringe with 5 mL deionized water to FROG 4000 Figure 4 4 2 Load Analyze Valve Figure 4 4 1 opposite page 4 Load deionized water into FROG 4000 M 5 Remove sparge bottle and empty deionized water into waste container 6 Repeat steps 3 5 twice for a total of three rinses 7 Remove and rinse sparge bottle with deionized water 8 Replace the sparge bottle in the DOWN position Proceed to demonstrate a clean baseline following pages 49 gt FROG 4000 TM CT Technologies FROG 4000 User s Manual KE 4 4 Instrument Preparation Continued 442 CREATING A CLEAN BASELINE A Clean Baseline should be achieved before analyzing a sample This procedure ensures that there are no contaminants in the instrument that could effect the analysis results If the instrument is connected to a computer and Ellvin
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