HYDRA AF Automated Mercury AnalyzerManual

150-00214

Leeman Labs, Inc.6 Wentworth Drive

Hudson, New Hampshire 03051U.S.A.

41540065 Rev, 1

HYDRA AFAutomated Mercury Analyzer

Operations Manual

P/N 150-00216Rev. 2 4/4/01LEEMANSLABS, INC6 Wentworth DriveHudson, New Hampshire 03051TEL: 603-886-8400FAX: 603-886-4322

Table of ContentsTable of Contents 1HOW TO USE THIS MANUAL 2Section 1 2SYSTEM OVERVIEW 3Section II 3

2.1 Configuring Software 4HYDRA AF Only (Standalone) 5HYDRA PREP Only (Standalone) 5HYDRA AF / HYDRA PREP Combination (running on one computer) 6

WARRANTY 7Section III 7NOTICE 8Section IV 8SHIPPING DAMAGE 9Section V 9

HOW TO USE THIS MANUALSection I

This manual is written for the HYDRA AF automated mercury analyzer. Themanual is divided into sub manuals separated by tabs identifying the various sub manuals.For instance, to learn how to run the HYDRA AF analyzer the HYDRA AF sub manualshould be read.

The manual is designed to aid in the installation, operation, and maintenance of theHYDRA AF.

The HYDRA AF family of atomic fluorescence instruments is comprised of threeproducts. The HYDRA AF is a mercury analyzer utilizing atomic fluorescence for themeasurement of mercury. The HYDRA AF GOLD is similar to the HYDRA AF with theaddition of a gold amalgamation preconcentrator to yield sub ppt detection limits. TheHYDRA AF GOLD PLUS is a dual optical cell/ detector instrument that offers both modes ofatomic fluorescence measurement. The operators manual is designed for all threeinstruments. Special features available on a particular model will be noted in the manual(i.e. - <AF GOLD PLUS only> or <AF GOLD and AF GOLD PLUS only>.

SYSTEM OVERVIEWSection IIThe HYDRA AF/HYDRA PREP constitutes the most advanced mercury analysis systemavailable. The HYDRA PREP has been designed to fully automate the digestion of varioussample types to make the resulting solution conducive to modern mercury analyzers. TheHYDRA AF is a fully automated CVAFS* mercury analyzer. The WinHg software yieldseasy user interface and the most advanced capability in any mercury analyzer. Originally,mercury analysis was performed by attaching an option to a standard atomic absorptionspectrometer. In 1991 Leeman Labs introduced the PS200, the first automated standalonemercury analyzer. Today Leeman Labs offers a full line of mercury analysis and samplepreparation products to increase a laboratories productivity. Combined, the HYDRA AFor HYDRA AA and the HYDRA PREP system is an extremely efficient mercury analysissystem. Raw sample in and results out.Based on a laboratories needs, various combinations of instrumentation can be run torealize complete mercury analysis. Examples of the various configurations supported byLeeman Labs hardware and software are shown below:

• HYDRA PREP and HYDRA AF run from one computer simultaneously or individualcomputers

• Manual digestion and HYDRA AF automated analysis• HYDRA PREP and HYDRA AF run from one computer simultaneously or individual

computers.

• HYDRA PREP with computer and any mercury analyzer that can handle reducedvolume digested samples

2.1 Configuring SoftwareIf you have purchased the HYDRA PREP/HYDRA AF combination, the HYDRA PREPstandalone, or the HYDRA AF standalone the software has been configured, on thecomputer, at the factory for your particular system. If, however, you want to alter theconfiguration as shipped or have purchased a retrofit system please continue reading.The software can be easily configured to run any combination of Leeman Labs,Inc.mercury systems in either standalone mode or combination from one computer. Theconfiguration is performed utilizing what is called the startup file.The startup file is read by the PS software(HYDRA PREP) or the WinHgsoftware(HYDRA AF). The software then configures its screens and operations based onthe parameters supplied by the startup file. To alter the way in which the software isconfigured the startup file must be edited.To edit the startup file perform the following steps:HYDRA AF with WinHg:• Double click on the WinHg icon• Pull down the Edit menu and select the Startup File• An edit dialog box appears• For help click on the Help button• NOTE - For those who know how to navigate directories, the HYDRA AF/WinHg

startup file is typically found in the HG directory.

HYDRA PREP only:

• Double click on the HYDRA PREP icon• Go to the Utility: Startup file page ( U S )• Edit the startup file using the Hotkeys, cursor keys, etc.• Restart the software ( S )• NOTE - For those who know how to navigate directories, the HYDRA PREP startup

file is typically found in the ICP directory.Not all parameters in the startup file are necessary for proper operation of the instruments.However, several parameters are critical in configuring the software for the instrument(s)attached to the computer. Below is a list of the parameters that are critical along with theappropriate values. The list is categorized by the hardware configuration of your choice.

HYDRA AF Only (Standalone)PS = 220AF = 2CO = 7,6,5,4,3,2,1 Recommended but not necessary; denotes, order of check standardsrunSP = 1 Connect from serial port #1 (C0M1) to HYDRA ART = 44

HYDRA AFGOLD Only (Standalone)PS = 221AF = 2CO = 7,6,5,4,3,2,1 Recommended but not necessary; denotes, order of check standardsrunSP = 1 Connect from serial port #1 (C0M1) to HYDRA AFRT = 44

HYDRA AFGOLD PLUS Only (Standalone)PS = 222AF = 2CO = 7,6,5,4,3,2,1 Recommended but not necessary; denotes, order of check standardsrunSP = 1 Connect from serial port #1 (C0M1) to HYDRA AFRT = 44

HYDRA PREP Only (Standalone)PS = 211Delete parameter AF =Delete parameter CO =Delete parameter HC =HP = C:\PS\HELPDelete parameter PC =PD = C:\PS\PREPHGIISC = C:\PS\SCRNAP.SDCSP = 0,2 Connect from serial port #2 (COM2) to HYDRA PREPRT = 4401 "H2SO4conc.H 1.84002"HNO3 cone." 1.40003 "KMnO4 5%" 1.03104 "K2S2O8 5%" 1.03005 "HydroxylamineSO4 12%" 1.08506 "AquaRegia 50%(t 1.32907 MK2Cr2O7:HNO3 .5%:50%" 1.20308 "K2S2O8 4%" 1.02409 "HydroxylamineCl 10%" 1.01710 "Antifoam : DI H2O" 1.000

11 "Water DI" 1.00012 "Water DI" 1.00013 "Water DI" 1.00014 "Water DI" 1.00015 "Water DI" 1.000

HYDRA AF / HYDRA PREP Combination (running on one computer)The HYDRA AF startup is configured as a HYDRA AF standalone as above.The HYDRA PREP startup is configured as an HYDRA PREP standalone as above.

NOTE - A limitation exists for combination systems running on the same computer. AWinHg/HYDRA PREP DOS combination system has a limitation. If the HYDRA PREP is tobe run, the DOS window must be open and Windows "focused" for the HYDRA PREP tooperate properly. If a user leaves the window to operate another application, such as theWinHg running the HYDRA AF, the HYDRA PREP will stop operation until the operatorreturns focus to the DOS window. This can cause problems if the HYDRA PREP isperforming a critical task, such as, filling the heater bath with water. Therefore, to run bothinstruments at the same time the HYDRA AF should be started first and then the HYDRAPREP started. Do not leave the HYDRA PREP software until the preparation of samplesis complete.

WARRANTYSection IIILeeman Labs warrants the HYDRA AF / HYDRA PREP to be free from defects inmaterial and workmanship for a period of one year from date of shipment. This warrantydoes not apply to damage caused by misuse. Warranty service for the HYDRA AF /HYDRA PREP is by telephone support and express shipment of replacement parts. Ifrequired, warranty repair/replacement of the system will be within five business days fromdate of receipt of the system by Leeman Labs. On-site warranty service by a factorytrained service technician is available at current rates for labor and travel. Non-warrantyfield or factory service is also available.Other terms and conditions may exist under Leeman Labs, Inc. Standard Terms andConditions outlined in the Purchase Terms.

NOTICESection IVMany of the reagents used in conjunction with the HYDRA AF / HYDRA PREP systemsare hazardous. It is necessary to follow good laboratory practices when using thisequipment. Always read MSDS sheets supplied with reagents. Always wear protectivegear while running, or servicing the instrumentation.

SHIPPING DAMAGESection VUnless stated to the contrary on the face hereof all goods furnished hereunder will beshipped FOB point of shipment, and title in and the right of possession to such goods passto the Buyer upon LLI's delivery to carrier at point fo shipment. Subject to LLI's right tostop delivery of goods in transit, such carrier shall thereafter be deemed to be acting forthe Buyer regardless of the carrier used or the freight terms.Shipments will be made "Best Way" freight collect and insured. LLI shall determine "BestWay" for shipment of equipment.If the Buyer requests prepaid shipment, actual charges incurred will be billed and are dueand payable to LLI within (10) days. LLI will not assume any liability in connection withshipment nor constitute any carrier as its agent.

HYDRA AFAutomated Mercury Analyzer

Operations Sub Manual

P/N 150-00215Rev. 4 4/17/01LEEMANSLABS, INC.6 Wentworth DriveHudson, New Hampshire 03051TEL: 603-886-8400FAX: 603-886-4322

Table of ContentsSYSTEM INTRODUCTION HYDRA AF 4SECTION 1 4

1.1 How to use this Sub-Manual 41.2 System Overview 41.3 Theory of Operation 51.4 Features 81.5 System Support 8

SYSTEM INSTALLATION HYDRA AF 10SECTION II 10

2.1 Installation Overview 102.2 Site Requirements 102.4 Unpacking and positioning 102.5 Hardware Setup 102.6 Electrical Setup 112.7 Plumbing and Dryer Setup 11

2.7.1 Liquid Plumbing Setup 112.7.2 Soda Lime Dryer Setup (AFGOLD and AFGOLDPLUS only) 13

2.8 WinHg Installation 162.9 WinHg Overview 16

2.9.1 WinHg Runner Main Screen 172.9.2 WinHg Database Main Screen 19

2.10 Autosampler Calibration 212.11 HgLamp 21

2.11.1 Lighting the Hg Lamp 212.11.2 Adjusting the Hg Lamp 21

2.12 Testing System (Optional) 22SYSTEM OPERATION HYDRA AF 23SECTION III 23

3.1 Operation Overview 233.2 System Preparation 23

3.2.1 Preparation of Reagents 233.3 Starting the Analyzer 24

3.3.1 Lighting the Hg Lamp 243.3.2 Turning on the Peristaltic Pump and Gas Flow 24

3.4 Creating a Protocol 243.4.1 Protocol Setup 24

3.5 Creating a Report Specification 273.6 Autosampler Setup 28

3.6.1 Autosampler Rack Creation 283.6.2 Cup Actions 29

3.7 Using the WinHg Runner to Collect Data 303.7.1 Creating a Data Set 303.7.2 Preparing the Autosampler 30

3.8 Calibration 303.8.1 With Autosampler 313.8.2 Without Autosampler 313.8.3 Reviewing the Calibration Data 32

3.9 Sample Analysis 333.9.1 With Autosampler 333.9.2 Without Autosampler 333.9.3 Guidelines for Running in the sub ppt levels 35

3.10 Report Generation 36SYSTEM ROUTINE MAINTENANCE 39SECTION IV 39

4.1 Maintenance Schedule 394.2 Maintenance Procedures 404.3 Special Maintenance Procedures 40

4.3.1 Replacement of Teflon lined tubing 404.3.2 Servicing the electronics 42

TROUBLESHOOTING 45SECTION V 45

5.1 Autodiagnostics 455.2 Manual Diagnostics 45

5.2.1 Isolating Blank problems (HYDRA AFGOLD or HYDRA AF GOLD PLUS only)... 45REPLACEMENT PARTS / 47REAGENTS / ACCESSORIES 47SECTION VI 47

6.1 Replacement parts 476.2 Reagents 486.3 Accessories 486.4 Options 48

APPENDIX A - EPROM INSTALLATION PROCEDURE 49

Table of Contents (Continued)List of Figures

Figure 2.7A Sample tip assemblyFigure 2.7B Pump tubingFigure 2.7C Rinse cup placementFigure 2.9A WinHg RunnerFigure 2. 9B WinHg DatabaseFigure 2.10A Rinse tank and rack arrangementFigure 3.4A New Protocol Dialog BoxFigure 3.4B Protocol Parameters TabFigure 3.4C Line Info TabFigure 3.5 A Report Specification Dialog BoxFigure 3.6A Autosampler Rack EditorFigure 3.8A Calibration and Standard SelectionFigure 3.8B Reviewing Calibration DataFigure 3.9A Sample AnalysisFigure 3.9B Output TabFigure 3. 9C Report TabFigure 3.10A Report GenerationFigure 3.1 OB Selecting Report DestinationFigure 4.1A Scheduled Maintenance Dialog BoxFigure 4.2A Scheduled Maintenance WizardFigure 4.3.1A Cross section of a good tubing connection.Figure 4.3. IB Cross section of a side impacted tubing on fittingFigure 4.3.1C Cross section of a end-on impacted tubing on fittingFigure 4.3.2A Electronic Card CageFigure A. 1 EPROM location (CPU board)

SYSTEM INTRODUCTION HYDRA AFSECTION I1.1 How to use this Sub-ManualThis sub manual is written for the HYDRA AF automated mercury analyzers. There arethree models of the HYDRA AF series of automated mercury analyzers outlined in thismanual. The three models are HYDRA AF, HYDRA AF GOLD, and HYDRA AF GOLD PLUS-

If a feature is for a particular instrument the feature heading will state which instrument itis exclusive to. The sub manual is divided into sections numbered by a roman numeral.Sub sections within the each section will be numerically referred to by section numberfollowed by a period and sub section number. Example, the third sub section withinSection IV will be marked 4.3. Subsequent sub headings under a sub section will benumbered. Example, the first sub heading under the third sub section within Section IVwill be marked 4.3.1.The sub manual is designed to aid in the installation, operation, and maintenance of theHYDRA AF series.The WinHg is multi-tasking and when combined with the PS software operating theHYDRA PREP the combination is a multi-instrument operating system. References tooperating the HYDRA AF with the HYDRA PREP automated mercury preparationsystem will be made.

1.2 System OverviewThe HYDRA AF system is designed to analyze liquid samples that contain mercury insolution. The system is comprised of a HYDRA AF analyzer, personal computer, andprinter. The analyzer is configured as semi-automated (without autosampler) or fullyautomated. The analyzer contains a high efficiency sample introduction system and a highoptical throughput atomic fluorescent (AF) spectrometer. The HYDRA AF electronicsinclude a slave computer that is driven by the personal computer. The slave computerfrees the personal computer from low level tasks which would otherwise slow multi-tasking operations.The state of the art WinHg software on the personal computer allows for not only multi-tasking but also multi-instrument operation simultaneously. This capability makes itpossible to run both a HYDRA AF and HYDRA PREP on one computer while generatingreports. All at the same time !

1.3 Theory of Operation(See schematic diagrams of all three AF models below.)A sample is prepared such that the final constituents are in solution. The mercury must bein the +2 state for proper analysis. To assure that all mercury within an unknown sample isin the +2 state a digestion is typically performed. (Reference USEPA methods 245.7 and1631) (See the HYDRA PREP submanual for more information on sample digestion.)The liquid sample with mercury present enters the system and is mixed with a reducingagent (usually stannous chloride) to form elemental mercury vapor. The mixture flows intoa liquid-gas mixer where argon or nitrogen is introduced to carry the mercury vapor.The gaseous-liquid mixture enters the liquid-gas separator where the liquid is drainedaway and the mercury bearing gas continues to the drying tube. The counterflow Nafiondrying tube dehumidifies the gaseous mixture. If the CVAFS only method is chosen as inthe HYDRA AF or HYDRA AF GOLD PLUS the gas proceeds directly to the atomicfluorescence detector. If the CVAFS with gold amalgamation is selected as in theHYDRA AF GOLD or HYDRA AF GOLD PLUS, the gas is concentrated onto a goldamalgamation trap. Subsequently, the trap is heated and the mercury is swept toward thedetector.The dry vapor or concentrated dry vapor then enters the fluorescence optical cell whichhas been optimized for fast response time and high sensitivity. A mercury lamp controlledby the error signal of the reference beam delivers a stable source of emission at 254nm.Fluorescence by the mercury cold vapor is measured using a solid state detector with awide dynamic range.The HYDRA AF guards against the problem that occurs when a sample with high mercurycontent is measured. In such cases, adsorption of high mercury levels results in slowelution from internal surfaces, characterized by long baseline return times. Once a systemhas been exposed, it can take hours to clean out, during which time the instrument isunavailable for use. The HYDRA AF detects high mercury levels early—before the vaporhas a chance to saturate the system. When the detector senses an abnormally rapid rate ofsignal increase, the system automatically performs a high speed flush of the liquid andgaseous phases. The detector signal is constantly monitored to determine when the systemis free of mercury. Once the system has returned to baseline the analysis of the next sampleproceeds.In the case of gold amalgamation trapping no such safe guard can be performed becausethe signal is committed to the detector once the trap is heated. To prevent overloading thehighly sensitive gold amalgamation analysis a prescreen can be performed using the lesssensitive fluorescence detector provided on the HYDRA AF GOLD PLUS-

Fig. 1.3 A HYDRA AF SCHEMATIC

Fig. 1.3B HYDRAAFGOLD SCHEMATIC

FAN1

FAN 2

VALVE 1

VALVE 2

VALVE 3

VALVE 4 |

DAQ

GAS

PUMP

1631 METHOD TIMING DIAGRAM

:

RINSETIME

•

[TIP

TO

CU

P

UPTAKETIME

•

5OH0.

F

|

10 sec.DRYTIME

DESORP1TIME

ION

STABILITIME

Z E ANALYSIS

ri[

L

t.

r

Fig. 1.3C Timing Diagram of the HYDRA AFGOLD or GOLD PLUS in CVAFS with trap mode

Fig. 1.3D HYDRA AFQOLDPLUS SCHEMATIC

1.4 FeaturesLow detection limits <O.5ppt (AF), <O.O5ppt (AF GOLD, AF GOLD PLUS)

High throughput 3 minute/sample in AF only mode4-9 minutes/sample in the AF with gold trap mode

1.5 System SupportReference ManualsUSEPAmehtodl631BUS EPA method 245.7Computer Manual(s)Printer ManualApplication Support

For special applications please call LEEMAN LABS, INC. customer support @ 800-LEEMANS, (800-533-6267) or 1-603-886-8400.ConsumablesLeeman Labs can supply all of your consumable needs. Please contact us for any of yourreagent or component needs on the HYDRA AF.

SYSTEM INSTALLATION HYDRA AFSECTION II

2.1 Installation Overview• Read and follow the Quick Installation Sheets (P.N. 150-00217) supplied with this

manual.• Use the on line help and videos under the Help pull down menu in the WinHg

software.• Check calibration of autosampler (see 2.10 Autosampler Calibration)• Adjust lamp (see 2.11 Adjusting the Lamp)• Optional: Run System Test from the pull down menu Tools to test performance of

HYDRA AF (see 2.12 Testing System)

2.2 Site RequirementsThe system site must meet the following specifications:

• Clean Gas: Argon or Nitrogen (99.995% purity)• Venting: minimum of 25 CFM for vent tubing of mercury vapor exhaust• Waste Bottle (or other provision for waste analysis materials)NOTE - For greater detail see the preinstallation guide originally mailed or faxed to yoursite. If you need another copy please contact Leeman Labs customer support for moredetails.

2.4 Unpacking and positioning• See the Quick Installation sheets supplied with this manual (P.N. 150-00217)

2.5 Hardware SetupThe HYDRA AF requires a gas input of between 75 and 90 psi. Connect the gas input lineto the back of the instrument using the tubing assembly (P.N. 120-00432-1). A gasexhaust line (P.N. 120-00063) is supplied to allow the venting of the mercury cold vaporinto a mercury trap (not supplied) or a chemical vent hood.The computer, video monitor, and HYDRA AF use modular power cords. Plug the powercord into the component and then into an electrical receptacle of the proper voltage(115VAC or 220VAC). The printer is plugged into a power receptacle.The computer communicates with the HYDRA AF through a serial communication cable(P.N. 115-00033). The computer end of the cable has 9 pins and connects to the C0M1port on the computer. The HYDRA AF end of the cable has 25 pins and connects to theserial communication port. The computer communicates with the printer through a parallel

10

cable (P.N. 115-00005). The computer end of the cable has 25 pins and connects to theLPT1 port on the computer. The printer end of the cable has pins and connects to themating connector on the printer.The video monitor connects to the video driver card in the computer (15pin connector).The keyboard plugs into the back of the computer. The connector plugs into a roundconnector with the TOP' mark up.

2.6 Electrical SetupSee the HYDRA AF Quick Installation sheet (P.N. 150-00217) supplied as the first sheetof the manual.

2.7 Plumbing and Dryer Setup2.7.1 Liquid Plumbing SetupAs an aid view the photographs and videos in the pull down help menu in the Runnerapplication. See figures 2.7A, 2.7B, and 2.7C for aids.The sample tip assembly (P.N. 120-00277-1) should be secured in the autosampler head asshown in figure 2.7 A. The barbed end of the sample tip assembly connects to the tabbedend of the sample pump tubing (blue) (P.N. 309-00104-1). The exit end (right) of thesample pump tubing connects to the barbed tubing on the process panel.

SAMPLE TIPASSEMBLY120-00277

Figure 2.7A. Sample tip assembly

The reductant tubing (P.N. 120-00282-1) connects to the top of the reductant bottle (P.N.120-00431-1) and then connects to the tabbed end of the reductant pump tubing (red)(P.N. 309-00088-3). The exit end (right) connects to the reductant tubing on the processpanel.

11

The drain pump tubing (P.N. 120-00412-1) connects from the tabbed end (left) to thebottom drain fitting on the liquid-gas separator. The exit end of the drain pump tubing(right) connects to the waste tubing assembly (P.N. 120-00284-1). Place the end of thewaste tubing into a waste container that is lower than the HYDRA AF. Connect the flowthrough rinse cup small tubing to the exit end (right) of the rinse pump tubing (black)(P.N. 309-00088-6). Connect the rinse tubing from the black topped 4 liter rinse bottle tothe tabbed end (left) of the rinse pump tubing (black). Place the end of the large draintubing of the flow through rinse cup into a waste container. IMPORTANT - the rinsedrain tubing should have a drop of 3 feet or more and the end of the tubing can never besubmerged in liquid. Failure to adhere will cause the rinse cup to overflow.

1L

REDUCTANT120-00431-1

A4L

RINSE 120-00431-2

The Rinse waste linemust drop at least3 feet and never besubmerged in thewaste liquid.

Figure 2.7B. Pump tubing

12

Figure 2.7C. Rinse Cup Placement

2.7.2 Soda Lime Dryer Setup (AFGOLD and AFGOLDPLUS only)The following is a step by step instruction for the packing and installation of the soda limedryer. This dryer acts as a second dryer following the Nafion dryer to aid in "super" dryingthe carrier gas. The other function of this dryer is to remove potentially harmful halo-acidsthat come from the liquid gas separation of the digested samples. This function greatlyextends the life of the gold traps.

1: Parts needed

TUBE DRYING#318-00016

HP

13

' ' * - , ' • ;

QUARTZ WOOL#0240-1118

s&6

I.'

Sod-'i Lime *

2. Install quartz wool in one end of dryer tube.

0a ^

Put Marble sized piece ofquartz wool into end of tube

ock«.k"4 -»-

6 >

14

3. Pack soda lime and contain it with quartz wool on the oppositeend.

Fill with soda lime

Put Marble sized piece ofquartz wool into end of tube

4. Muffle the soda lime dryer in a muffle furnace at 200-300°C for 1 hour. Let cool.5. Reassmble the soda lime trap with fittings and tubing.

Reassemble dryer

6. Install the soda lime dryer in the HYDRA AF instrument by clipping in place. Connectthe short tubing to the right fitting and the long tubing to the left fitting.

15

2.8 WinHg InstallationThe software can be installed using the supplied installation disk. If the computer is set toallow auto-installing the installation will begin when the disk is inserted. Otherwise, usethe Run from the START button and run the SETUP.EXE on the disk.

2.9 WinHg OverviewThe WinHg program is comprised of three separate applications: WinHg Runner, WinHgDatabase and Rack Edit. Each of these applications has specific functions and capabilities.

The Runner is exactly what the name implies. The purpose of this application is to run theanalyzer. Any command that results in the analyzer performing an action (running samplesor performing a lamp adjust, for example) will come form this application.

The Database is where protocols can be created/modified, analytical data examined, andreports generated. In addition, the database is a stand-alone application and does notrequire the presence of the Runner or the analyzer in order to function. This means that acopy of the database can be placed on another computer and all its capabilities retained.

The structure of each of these two applications is as follows:

Title barShows the name of the application and allows minimizing or closing the application.

Menu barOffers pull down menus for less common operations of the software.

Tool barOffers icon short cuts to more common operations that may be used in a random access sense.

Information barShows the present pertinent information on the software or instrument independent of whichtab the user may be on.

Tab pagesThe tabs represent the major function groups that a user may want to access, modify, andcontrol within the application. The tab pages are where a user spends most their dialog timewith the software. Within each tab page some functions may have a border around them with aname, this is known as a group.

Status barShows timely information related to the application activity and/or cursor status.

The Rack Edit application is designed to create and edit autosampler rack files. Like the

16

Database, this application is also designed to be standalone and can be copied to anothercomputer.

2.9.1 WinHg Runner Main ScreenWhenever the Runner application is launched, its Main screen will appear. The "WinHgRunner" (Figure. 2.9A) is the application specifically designed to run the instrument. Anythingthat directly deals with the operation of the instrument can be found here.

l#d*&&$ j Hgppb £j

f#aTpha 3 •&«?

Mant ] Control j Sfemrtattf j Sample \ Otrfpal \ Report]

Figure 2.9A WinHg Runner

The Status Box, located in the top portion of the screen, provides information about whatis happening with the system, the current operating parameters, the names of the protocoland dataset in use, etc. In addition, any interlocks or errors will appear here when theyhave been activated.

17

A brief description of each tab in the Runner is given in the figure below

Runner RACK EDITOR Create, modify autosampler racks

DATABASE Create, modify protocols and reporting functions

CONTROL Sample introduction parameters, Hg Lamp control

STANDARD

SAMPLE

OUTPUT

REPORT

UTILITY

Calibrate instrument, define positions for standardsand check standards

Run samples, Select analysis type

Display sample signals and chart recorder while sample is analyzed

"<5lass" printer

Instrument diagnostics

18

2.9.2 WinHg Database Main ScreenThe WinHg Database can be launched from either the Database command button on theRunner's Main tab or the button labeled "DB" in the toolbar. Once the Database application inlaunched (Figure 2.9B), protocols can be created or updated and data reports generated. Anydatabase function can be performed while the analyzer is running samples.

tftest

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sjosr4n?

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Figure 2.9B WinHg Database

19

A brief description of each tab in the Database is given in the figure below

Database

PROTOCOL

CALCURVE

REPORT

Edit parameters in loaded protocol

LINE INFO Edit element parameters, cone, of standards, etc.

Calibration curve display and selection

Select data from dataset for reporting, generate reports,edit reoort soecif ications

CTRL CHART

VIEWER

Plot data over time, quality controlchart

"Glass" printer

20

2.10 Autosampler CalibrationTo calibrate the autosampler first install the rinse tray, standards rack, and sample racks(see figure 2.10A). Then go to the Utility Tab. Select Calibrate Autosampler selection.Using the dialog box as a guide, go to and adjust the autosampler to the three alignmentcups. When satisfied, with the accuracy of going to the cups, click Accept.

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Figure 2.10A. Rinse tank and rack arrangement

2.11 Hg LampThe Hg lamp is the source of photons used to detect Hg in the optical cell. For optimalperformance there is an automatic adjustment of the Hg lamp that should be performedperiodically. The recommended period between adjustment is typically 3 months. Thelamp adjustment should be performed any time any of the optics have been cleaned orremoved including the optical cell. If any problems are found with the optical system amessage will appear.

2.11.1 Lighting the Hg Lamp

1. From the Runner, select the "Control" tab2. Click the "On" button in the Hg lamp group. The Hg lamp will light.

2.11.2 Adjusting the Hg Lamp

1. If necessary, the lam]} can be adjusted by clicking the "Adjust" button. (Thiswill turn on both t fe« |p flow and peristaltic pump during the adjustmentprocedure. At the end oFjjje procedure, they will be turned off.) Adjustingthe lamp will take approximately 2-2/4 minutes.

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2.12 Testing System (Optional)Go to CONTROL tab in the RUNNERAdjust Optics. This will take only 2 minutes while the system automatically adjusts theoptics for optimal performance .Run the system test selection in the Tools pull down menu. Once started the wizard willstep you through the setup of the system. In preparation, make solutions of the following:

• 2L 1% HC1 blank• 500mL O.5ppt Hg in 1% HC1• 500mL 1 .Oppt Hg in 1% HC1• 500mL lOppt Hg in 1% HC1• 500mL lOOppt Hg in 1% HC1• 500mL lOOOppt Hg in 1% HC1Interpreting the resultsThe first page printed is a hard copy of what revisions of software are being used on theinstrument. This is extremely useful when talking to customer support over the phone.The second page printed is a copy of the data acquisition test results. The most importantitems to check are:

Sample This is the transmittance value of the sample beam. It should be below5000.Lamp Voltage This is how hard the circuitry is driving the Hg lamp. The valueshould be between 4.0 and 11.0. If the value is incorrect try Adjusting the Optics (see2.11.2), cleaning the optical cell (go to scheduled maintenance in the pull down menufor more details), or replacing the Hg Lamp (P.N. 317-00048).

The third page printed is a copy of the gas control test results. The most important itemsto check are:

Input Pressure This is the gas pressure supplied to the instrument. The valueshould be between 75 and 90 psi. If the value is not correct check the pressure at thetank and adjust.5V, 12V, -12V These are the system power supply voltages. The values andacceptable ranges are as follows, 5V +/- 0.25, +12V +/- 0.5, -12V +/-0.5.

The next two sheets printed are the results of an extended range of calibration. The resultsof running are the calibration of the higher concentration protocol followed by limits ofdetection and method detection limit results. The second tier of the run calibrates thelower concentration range followed by a limit of detection and method detection limit. Thebest results when preparing standards are using weight dilution and NOT volume dilution.Also, the acid matrix and purity is critical. The best performance is based on low Hg HC1acid. Do not use any acid matrix other than pure diluted HCl.Each facility will have its own acceptance of this test, because running in the low and sub-ppt levels is facility and reagent related.NOTE - Because this test is extremely exhaustive, and only takes approximately 1.5hours, it is a typical test requested by Leeman Labs customer support when a difficultproblem is encountered. The individual sheets can be faxed to Leeman Labs for reviewwhen such a problem occurs.

22

SYSTEM OPERATION HYDRA AFSECTION III

3.1 Operation OverviewThe typical operation of the HYDRA AF follows a sequence as below:

• Load or create a protocol which defines the operating parameters of the system• Load or create a dataset where the data will be stored.• Turn on Gas, Pump, and Hg lamp• Sample rack editing (Add sample names, Dilution factors, Weight factors, etc.)• Standard concentration and unit entry.• Check standard concentration and limits entry.• Run standards for calibration of HYDRA AF• Accept calibration curve• Run samples using calibration stored in protocol.• Post run reporting of data.

3.2 System PreparationTo assure proper results the standards, sample cups, rinse tray, and reagents must be ofhigh purity. The standards and reagents can be purchased from Leeman Labs, Inc. Thiswill assure proper operation of the HYDRA AF. If reagents other than Leeman Labs areused make sure they are of ultra pure grade. It is extremely important that reagents arelow in mercury and molecular chlorine. The rinse tray and sample cups should be leachedwith 1:1 HC1 for 1 hour prior to use. After leaching rinse with at least 5 volumes of DIwater. A more exhaustive leaching should be considered for limits of detection below0.2ppt. Read EPA method 163 IB for bottle leaching procedure.

3.2.1 Preparation of ReagentsWhen running low concentration (ppt) samples use 2% HC1 as the rinse. When runningpart per billion level samples consider using 10%HCl as the rinse. The reductant is madefrom SnC12 in HC1.NOTE - Because of the detection limit requirements in today's mercury analysis only thehighest purity of reagents should be used on the HYDRA AF. Leeman Labs can supply allof your reagent requirements for this and other products. Please call for more information.

23

3.3 Starting the AnalyzerThe section will describe how to bring the system up in preparation for analysis.

3.3.1 Lighting the Hg Lamp1. From the Runner, select the "Control" tab2. Click the "On" button in the Hg lamp group. The Hg lamp will light.

3.3.2 Turning on the Peristaltic Pump and Gas Flow

1. From the Runner, select the "Control" tab2. Click the "On" button in the Pump group. When this is done, the gas flow is

automatically turned on.3. To turn on the gas flow without turning on the pump, click the "on" button in the

"Gas" group.

3.4 Creating a ProtocolThis section will illustrate the steps necessary to create and use a protocol. In order toobtain more information on the steps and options available, see the appropriate section inthe Operations manual.

To make calibration standards for this protocol, make aO, 0.5, 1.0, 10.0 and 100 ppt Hgstandards in 1% hydrochloric acid. If an autosampler is to be used, place a 2%hydrochloric acid in the rinse bottle.

3.4.1 Protocol Setup

3.4.1.1 Naming the Protocol1. From the Runner, click the toolbar button labeled "DB" or the "Database"

command button on the "Main" tab.

24

fetfoeoiHams J 1 6 3 1

~

r o

r

r

EPA 1631 ultra low level

Figure 3 4A New Protocol Dialog Box2. From the "Database", select "File" from the pull down menu. Then select "New

Protocol1.

3. Enter a name in the "Protocol Name" dialog box that appears (Figure 3.4A).

4. Then select one of the check boxes in the "Protocol type" group. This ensures thecorrect analytical conditions for the concentration range desired will be enteredinto the protocol. The EPA 1631 group will generate protocols using the goldamalgamation traps (AFGOLD and AFGOLD PLUS only). If prescreening the samples iswanted simply check the prescreen box (AFGOLD PLUS only). The EPA 245.7 groupwill generate protocols without the gold amalgamation traps (AF and AFGOLD PLUS

only). A new title can be entered into the "Title" dialog box, or the default can beaccepted. Click "OK" to close the "New Protocol" window.

3.4.1.2 Changing Protocol Parameters1. Depending on the check box selected in step 4 above, WinHg will enter the

appropriate instrument operating parameters ("Sample Introduction", "PumpTimes", and "Data Collection") into the protocol. These can be seen on the"Protocol" tab in the "Database" (Figure 3.4B).

2. These parameters can be changed by using the spin buttons to raise or lower thevalue OR by highlighting the field and typing in the desired values and pressing the"Enter" key. (The "tab" key can be used to navigate between each field.) Theseparameters were chosen to provide optimum results and should not be modifiedwithout careful consideration. The contents of the "Method Macro" field shouldnot be changed unless directed by Leeman labs, Inc.

25

3. The remaining parameters can be modified as required by the analyticalrequirements of the protocol.

# test

**~jj 10**~jPsta-ap-f

tfptek-e- - T ] | 240

I J * | r3' HgPrescreen

o • \ Continue

- M j 1 F\MScste ^ j j 1

H j@RUNHG

^ | °-7CI

r

• t*

MR21

Figure 3.4B Protocol Parameters Tab

4. If your instrument is the HYDRA AF GOLD PLUS the method of analysis can bechosen. CVAFS is designed around EPA method 245.7. CVAFS with trap isdesigned around EPA method 163IB. A third method is the Prescreen, whichperforms a CVAFS with trap run on a sample after being prescreened with a fastCVAFS only analysis.

5. To use weight and volume correction, click the check boxes located in the"Calculations" group. The values to be used for the calculation are entered into anautosampler table for each sample.

6. The remaining parameters can be changed by using their drop down boxes. If anychanged are made to the "Frequencies" group, it is necessary that the appropriateconcentrations be entered in the "Line Info" tab (see below). Changing the"Analysis Type" to "Method of Standard Additions" requires spike concentrationsbe entered onto the "Line Info" tab as well. Before one can be selected, a "ReportSpec" must be created in the "Report" tab. See Section 3.5 to create a ReportSpecification.

26

7. If any changes are made, be sure to click the "Apply" before leaving the "Protocol"tab in order to save the changes.

3.4.1.3 Changing Concentration InformationConcentration information for calibration and check standards as well as spikes iscontained on the "Line Info" tab (Figure 3.4C).

1. To change any of the concentrations, simply select the current contents of the fieldand enter the new value. (The values can be selected by "dragging" with themouse pointer.) If the field is empty, click on it and enter the desired value. The"tab" key can be used to move between the fields.

f^fcwat fHgppb

Uftfr Into

IfoooooI 20000

Ifi I oooooUS J5t000

•$4 J1 0000

Sg (5 0000

SS ji bbbtf'

•as

33

fit , j—

n

j t

Kite

Figure 3.4C Line Info Tab

2. Be sure to click on the "Apply" button before leaving the "Line Info" tab.

3. Note: If entries are made in the "Standard additions" group, then the "AnalysisType" on the "Protocol" tab MUST be changed to "Method of StandardsAdditions", otherwise the values entered will not be used.

3.5 Creating a Report SpecificationThe Report Spec controls what information is contained in a printed report. There aretwo types of reports in the WinlCP: real time and post-run. A real time report isgenerated while samples or standards are being analyzed. A Post-run report is generatedwith data that has been previously stored in a data set. In this tutorial, both types ofreports will be generated.

27

1. Click on the "Report" tab in the Database. The "New Report Spec" windowappears.

2. In the edit box labeled "Report Spec Name", enter the name of the reportspecification to be created as "water". Then, click the "OK" button... The "EditReport Spec" window appears (Figure 3.5A).

3. Labels that have filled check boxes will be included in the report. The check boxesact as "toggles". Clicking on a check box (or its label) will change the status of theitem.

I water

rf*"

Figure 3.5A Changing the Contents of a Report Specification

4. Remove all the checks in the "Include in Report" group except the one labeled"Sample. This will result in only sample data being printed.

5. In the "Post Run Reports" group, remove the check from the "Summary Report"

6. Click the "Ok" button to close the window.

3.6 Autosampler SetupBefore the autosampler can be used to analyze samples, an autosampler rack must becreated. The Rack Edit application is launched from the WinHg Runner.

3.6.1 Autosampler Rack Creation1. Click on the "RN" button on the Database toolbar. This will bring the focus back

to the WinHg Runner.2. To launch the Rack Edit application (Figure 3.6A), either click the "Rack Editor"

button on the Runner "Main" tab or click the Autosampler rack icon on thetoolbar.

28

it2

:3:*;5IS;?:8iSiio= 13 f:13•tt

;!U; t5-=18;1?;1S

;1$iaGE

^9"?P+ft Jv 3 05^wij Sequence [

sampledsampleO2sampleO3

satnpieO4

sampleO5

sampleOfi

sarrtpleO7

sampleOS

sampleOS

samplelO

1 OOOO 1 0000

1 OOOC 1 0000

1 0000 1 0000

10000 10000

1 0000 1 0000

1 0000 1 0000

10000 10ODO

1 0000 1 0000

10000 10000

1 OOOO 1 0000

1 00OQ 1 0000

1 0000 1 0000

1 0000 1 0000

1 0000 1 0000

10000 10000 I |1 0000 1 0000

1 0000 1 OOOO

10000 10000

10000 10000

10000 10000

1 0000 1 0000

1 OOOO 1 0000

1 OOOO 1 0000

• * \

d

Figure 3.6 A Auto sampler Rack EditorClick on the ID cell for Cup 1. Type the name "sampled" and press "Enter"Place the mouse pointer on the ID field for Cup 1, hold down the left mousebutton and drag down to the ED field for Cup 10On the toolbar, press the button for "sequence". (The tool tip will identify thebuttons when the mouse pointer is over them.)A pop up window appears, indicating the sample IDs will be sequenced by 1.Click "OK". The sample IDs will then be sequenced from 01 to 10.Save the rack file by clicking on the floppy disk icon on the toolbar. Give the rackfile the name "First" and then click "Save".Click on the "x" to close the Rack Editor.

3.6.2 Cup ActionsThe cup actions are a method of applying various functions to each sample cup after it isrun. An example, apply percent recovery on a spiked sample during the reporting. Whenusing cup actions, leave a space between each cup macro entry, e.g. S P for calculating apercent recovery on a spiked sample. To use this advanced feature read the on line helpfor this feature.

6.

8.

29

3.7 Using the WinHg Runner to Collect DataIn this section, the WinHg Runner will be used to:

• Calibrate the instrument• Analyze samples

3.7.1 Creating a Data SetNow that data is about to be collected, it is necessary to open a file to store the data.

1. Click on "FILE" on the Runner's pull down menu. Select "New Data Set".2. Enter the name "#ALPHA" into the "Create New Data Set" pop up window, then

click "OK". The "#" sign before the name will allow data from any protocol to bestored to this Data Set.

3. Enter a batch name in the "Start New Batch" pop up window. A batch acts as amarker in a data set and can help in selecting data for report generation.

3.7.2 Preparing the AutosamplerEach of the actions listed above can be performed manually or with the autosampler.In this section, both ways will be illustrated. If an autosampler is not going to be used,proceed to section 3.8.2.

1. Click on the "Standard" tab.2. The information displayed on this tab is taken from the protocol (see Figure 3.8

A).3. The active standards are indicated by the buttons. Notice the buttons for standards

S5 through S10 are grayed out as are all the check standards.4. The spin box next to the standard button indicates the position in the autosampler

rack that the standard belongs. The "Active Cups" map illustrates the positionsthat are occupied.

5. Place the standards in the appropriate location in the standards rack on theautosampler.

6. Also, place ten "samples" in positions 1-10 in the first 44-postion sample rack(station 1) for use in later sections. These can simply be some of the standardspoured into some of the 15-ml sample cups.

3.8 Calibration1. Return to the WinHg Runner.2. Select the "Standard" tab (Figure 3.8A).3. In the lower right hand corner, click on the "real time print" check box. This will

generate the real time report.

30

3.8.1 With Autosampler1. Select the standards to be used by clicking on the buttons for SI, S2 S3, S4, S5

and S6.2. To set the number of replicates, click on the buttons for Repl, Rep2 and Rep 3.3. Click on the "Stnd Auto" button.

fctatn

F3

£taipui{ £tepartj

cup

!T3

F3

J32iiL

Rep 3 Aulo

iprg-.-in.i.i.v.-.-.-L-f ^ A U A 4

raStraf

8 ^

9 •

10 -J 1W

1 ••"*

1

i

i

: -2

r :

13

f~

.HUM .

Figure 3.8A Calibration and Standard Selection

4. After this entry, the autosampler will begin the calibration sequence. The sequencewill consist of the analysis of standards 1 through 4, with three replicates of each.The calibration curve will use the mean of each of the three replicates.

3.8.2 Without AutosamplerCalibration without the autosampler is just slightly different. It is not necessary to tell theinstrument how many standards are to be analyzed; just which one is to be analyzed

5. To set the number of replicates, click on the buttons for Repl, Rep2 and Rep 3.6. Click on the button for the standard to be run.7. Be sure to place the sample tip in the standard BEFORE the next step.8. Click on the "Stnd Manual" button.9. Repeat for the remaining Standards.10. While the calibration data is being collected, click on the "Output" tab to see the

data real-time.11. When a standard is complete, click on the "Report" tab to see the data.

31

3.8.3 Reviewing the Calibration Data1. Return to the Database application by clicking the "DB" button on the toolbar.2. Click on the "Cal curve" tab (Figure 3.8B).3. Select the Type of curve to fit. In the case of EPA methods 245.7 and 163 IB the

C. Factor type is most commonly used. Other analysis protocols may dictate theuse of a simple linear. The Calibration Factor (C. Factor) type will not allowacceptance unless the proper criteria of %RSD of CF and %Recovery of the lowstandard are met.

4. Calibration data can be accepted by clicking the "Accept" button.

&\m-t?i t I

Cone, 2E5

01 .0000002 .5000003 1.000004 2.000005 5.000006 10,000i

.000

.4691.011.945.15102

.000-.031.013-.057.154,209

2155278790

145107258417649990

.1.266397.

22030%0%OX0ZOX

1999478790

145107258416649989

1266396

23110

Figure 3.8B Reviewing Calibration Data

32

3.9 Sample AnalysisAfter the instrument has been calibrated, the analysis of samples can be performed. Aswith Calibration, sample analysis can be performed with or without an autosampler.

1. Click on the "RN" button to return to the WinHg Runner.2. Click on the "Sample" tab (Figure 3.9A).

ffli * WinH g Runner 1 219

> , ., j . i a 5

3 I01 r l 01 ll 44 *3 \|

I [standards > j j 01 * |

T-a Ic Ta

ITCafewfefe sj Rscjwe^

Figure 3.9A Sample Analysis

3.9.1 With Autosampler1. In the "Autosampler run" group, click on the combo box for station 1.2. Select the autosampler rack file created and name above in Sec. 1.4.1.3. Using the spin boxes set the starting and ending cups to 1 and 10, respectively.

Make sure the "cups per rack" setting is correct.4. Click the "Run auto" button. The "Output" tab automatically pops up.5. The "Output" tab automatically pops up.6. When a sample is complete, click on the "Report" tab to see the data.

3.9.2 Without AutosamplerSample analysis without the autosampler is controlled from the "Manual run" section ofthe "Sample" tab.

33

1. Click on the "sample ID" edit box.2. Enter the name of the sample.3. Click the appropriate sample type for further calculations.4. Click on the "Run Manual" button.5. While the samples are being analyzed, click on the "Output" tab to see the data

real-time (see Figure 3 9B and 3.9C).H. WinHq Runnel 0.013

ftattctfJGE Zl SfiM IDLE

&*8*# JGE2

Cup. id

m&\

Figure 3.9B Output Tab for non-gold trap analysis.

gfe

Sfafisti ftacfe.

r rCup

209259

T\201760 Cl

0 556

| pM i " s

Figure 3.9C Output Tab for gold trap analysis.

6. When a sample is complete, click on the "Report" tab to see the data (see Figure

34

3.9D).

N WinHg Runner 0.013

) IDLE"

JGE2

*s ;j-f Off IBM

*** Sample ID: sampleHg 18.7 ppb .000

Seq: 156 11:14:57 11 Aug 0 0 H & | §18.7

+** Sample ID: sample Seq: 157 11:17:05 11 Aug 00 HGHg 18.6 ppb .000 h 18.6*** Sample ID: sample Seq: 158 11:18:56 11 Aug 00 H&

WMl

Figure 3.9D Report Tab.

3.9.3 Guidelines for Running in the sub ppt levelsRunning mercury samples at the part per trillion level requires some extra care. Pleasefollow the guidelines listed below for the best performance.

• Use only fresh Leeman Labs, Inc. reagents for the digestion and analysis.• For the preparation using the HYDRA PREP use only fresh cups. If preparing the

samples manually or running undigested mercury standards, use cups that have beenleached in 1:1 HC1:H2O for 30 minutes then rinsed thoroughly with deionized water.

• Use fresh Leeman Labs, Inc. pump tubing that has been run with rinse for 45 minutesto break in the tubing. The lever in the pump cassette should be pressed backcompletely.

• Clean the optical cell and windows carefully before analyzing low level samples. Forinstructions on how to clean the cell refer to the Scheduled Maintenance wizard underClean optical cell.

• Clean the mercury lamp with isopropyl alcohol - be careful not to get any fingerprintson the surface. Allow the lamp to warm up for approximately 5minutes then adjust thelamp on the Control Tab.

• When running in a mode without gold amalgamation lower the gas flow and increasethe pump rate in the protocol to increase sensitivity. The default protocols should be agood starting point.

• When running in a mode with gold amalgamation lower the gas flow and increase theuptake time. The lowering of the gas flow will yield less dilution of the Hg gas from

35

the traps. The increase in uptake time will deposit more Hg on the trap. Bothtechniques increase the sensitivity of the analysis. The default protocols should be agood starting point.

• Use only high purity Argon or Nitrogen (99.999%) gas as the carrier gas• Make sure that the environment is free from mercury vapor or volatile organic material

that may interfere with the analysis. Consult the article in American EnvironmentalLaboratory (5/95) for recommendations about laboratory environments. Consult U.S.EPA method 163 IB for sampling and laboratory conditions required to analyze in thesingle ppt range.

• Prior to preparing the bromine chloride oxidation reagent muffle the KBr at 200°C for1 hour.

• After packing the soda lime scrubber muffle the tube, quartz wool, and soda limeassembly at 200°C for 1 hour.

• Sparge the stannous chloride solution with Hg free helium or argon for at least 12hours prior to use.

• Use the purest HC1 acid that can be afforded.

3.10 Report GenerationThe data that printed out during the calibration and sample analyses performed abovewere controlled by the report spec "ALPHA"(see Section 3.5 above). Using the samereport spec, a Post Run report will now be generated

1. Click on the "DB" button.2. Click on the "Report" tab (see Figure 3.10A).3. In the "Report Spec" group, the name "water" should be shown in the combo box.

If not, make it so.4. Click on the "In Box" for the batch created in Section 3.7.1.5. In the "Record List box, all of the standards and sample that were run above are

listed.6. The single batch that was created will appear in the "Batch List" box.

36

Hgppb "3 #alpha

Protocol\ t tee \aia \ £af £t*tve BBJK>H |e*rf ChartJ Vtewer]

-a8 j && J fiSCORC UST,

Hlyi1*1

043347547b

V&t Go. 3! 17 ^

first run

recoveries

05Jun00

~p19 SMP

2d SMP

21 SMP

22 SMP

23 SMP

24 SMP

25 SMP

26 SMP

27 SMP

28 SMP

29 SMP

3d SMP

31 SMP

32 SMP

sampleOlsampleO2sampleO3sampleO4sampled5sampleO6sampled?sampled8sampled3samplelOsamplellsamplel2samplel3samplel4

fiscords

;NUM

Figure 3.10A Report Generation

9.

Click the check box for the batch. The sample and standards in the "Record List"will disappear.Click on the batch check box to get them back. This illustrates the usefulness ofbatches. They make it easier to select data for reports, particularly when a "DataSet" contains large amounts of data.In the lower right corner, click on the "Generate Report" button. The "ReportGeneration" pop up window appears. This window contains the parameters togenerate the report (Figure 3.1 OB).

37

) & tepOtft

I r v&s m

*i 1

' <" "*"'

J

: fmes-per psge i 55 -;

Neb j

" — "--•'"'—

Figure 3.1 OB Selecting Report Destination

10. In the "Destination" group, click on the "viewer only" radio button. This selectionwill send the report to the "glass printer" under the "Viewer" tab and will allow thereport to be examined before it is sent to the printer. This is helpful especiallywhen a large report is to be created.

11. Under the "Format" group, the type of report can be selected. The "PRN" formatis ASCII while the "WKS" is a spreadsheet. For this report, click the "report"radio button.

12. Click on the "Generate" button. The report progress is shown in the "Status"group. When complete, click on the "x" to close the window.

13. Click on the "Viewer" tab to see the generated report.14. If a hardcopy of the report is desired, return to step 8. When the "Report

generation" pop up appears, select the option for printer in the "Destination"group.

15. Click the "Generate" button. The report will be sent to the printer.

38

SYSTEM ROUTINE MAINTENANCESECTION IV4.1 Maintenance ScheduleThe software offers a simple to use online Scheduled Maintenance page. To view thedialog box go to Perform Maintenance in the Utility pull down menu of the Runnerapplication. A page displaying all items necessary to keep the instrument well maintainedis shown (see figure 4.1 A).

j,Pump Tubing

) Waste Drain Tubing

5 Liquid/Gas Separator

JPump Head

)Hgl_amp

)Reductant Bottle

) Process Tubing

) Clean Optical Cell

) Clean External Optics

) Replace Dryer

200

2500

5000

10000

N/A

400

5000

300

N/A

5000

10-Aug-2000

4-Jul-2000

N/A

Wul-2000

N/AN/A

2GJul-2001

8-Aug-2001

N/A

1-Dec-2000

31-Dec-2000

N/A

N/A

31-Dec-2000

iiMimniiMMiiiniiiimiT

Figure 4.1 A. Scheduled maintenance dialog

Each scheduled maintenance item has a usage counter, timed usage, or both (N/Aindicates that the usage counter or the timed usage is not applicable for that item). If eithercondition expires for a given item a maintenance message will alert the user in theinformation bar of the Runner application.

39

4.2 Maintenance ProceduresAn X will appear next to the item requiring maintenance on the Scheduled Maintenancedialog window. To clear the message click the clear button in the information bar orreplace, clean, or replenish the item using the maintenance wizard. To perform themaintenance on a given item simply double click on the item in the scheduled maintenancedialog window and follow the wizard (see Figure 4.2A) or highlight the appropriate itemand click the Maintenance button. Once the directions are followed to completion (clickFinish button), the usage counter and timed usage gets updated. If you want to reset all ofthe items at the same time the Reset button can be clicked.

MAINTENANCE WIZARD PAGE 1

< S-amste Reefeictart

Figure 4.2A. Scheduled maintenance wizard

4.3 Special Maintenance ProceduresThere are potentially long term maintenance issues that are not easily tracked by software.This section addresses these potential issues with specific instructions.

4.3.1 Replacement of Teflon lined tubingThe HYDRA AF series instruments are plumbed for the gaseous phase of the analyticaltrain using special tubing. The tubing is designed using a durable flexible outer layer withan inert Teflon lining. This combination gives the following important features; flexibilitywithout kinking, gases contact only inert surfaces, the flexible outer jacket forces a tightseal of the Teflon lining and the barbed fittings. In rare occasions the tubing may need tobe replaced in areas of the instrument. If this occurs, special considerations have to bemade when making the connections. Follow the procedure below for proper replacementof tubing.

40

1. Order a length of the 1/8" OD x 1/16" ID Teflon lined tubing (PN 309-00118).Order in units of feet.

2. Using a very sharp razor or X-Acto blade cut the tubing square to the properlength.

3. Remove the piece to be changed by slowly pulling it off of the barbed fitting..4. Carefully, place the end of the tubing over the fitting with a back and forth rotary

action. The rotary action is to assist the tubing in forming to the barb. Continue topush the tubing until it is completely seated on the barbed fitting.

5. Inspect each connection that is made for a good connection (See figure 4.3.1 A).6. There are two possible failed connections using this tubing. One is when the

barbed fitting slips between the Teflon lining and the flexible tubing (See figure4.3. IB). The second failure is when the barbed fitting pushes and bunches the

tllon lining ahead of it (See figure 4.3.1C).

Figure 4.3.1A Cross section of a good tubing connection.

41

Figure 4.3. IB Cross section of a side impacted tubing on fitting

Figure 4.3.1C Cross section of a end-on impacted tubing on fitting

4.3.2 Servicing the electronicsThe HYDRA AF series instruments are as easy to service as a Personal Computer (PC).The electronic printed circuit boards are plugged into a motherboard much like a PC.While most users, will leave this aspect of servicing to a trained Leeman Labs ServiceEngineer, others may want to perform simple service to expedite operation. This section isto aid in recognizing the various circuit boards and their function. See figure 4.3.2A for

42

the position of the circuit boards in the card cage. To gain access to the card cage removethe four mounting screws surrounding the black process panel flange. Turn off power tothe instrument. Remove the tubing connecting the liquid gas separator to the pump tubing.Carefully and slowly slide the drawer forward. When finished servicing carefully push thedrawer back into the chassis. If any resistance is met when sliding the drawer back intoposition stop and inspect the cables that should retract into the autosampler section of theinstrument. The inspection of these cables and manual guidance can be made through thelower largeopejiingir^^ cord enters.

UTOSAMPLER

GAS CONTROL

M f 9 r * JMGOLD TRAP FURNACE

LAMP CONTROLw i

DATA ACQUISITION

Figure 4.3.2A Electronic Card Cage

4.3.2.1 CPU cardThe CPU card (PN 113-3010-XXX) is the smart portion of the instrument. This card hasa computer onboard that communicates with the external PC through the serial port. TheCPU performs all logical functions and basic operation of the instrument. PN 113-3010-XXX where XXX is the revision level of the EPROM.4.3.2.2 PUMP cardThe PUMP card (PN 113-00010-1) performs the control functions of the peristaltic pumpincluding the power electronics to drive the motor. The control of the pump rotationalspeed is governed by this card using the encoder from the pump motor and "locking" themotor to a set frequency as set by the CPU.4.3.2.3 AUTOSAMPLER cardThe AUTOSAMPLER card (PN 113-00085-1) is actual a general purpose stepper motor

43

control card. When the address switch is set to 3 the CPU uses this card to drive themotors in the autosampler. Also, all home sensors in the autosampler are monitoredthrough this card.4.3.2.4 GAS CONTROL cardThe GAS CONTROL card (PN 113-00061-1) performs the solid state control of gasthrough the analyzer. This particular card controls the gas flow by monitoring the pressureacross a precise orifice.4.3.2.5 GOLD TRAP FURNACE cardThe GOLD TRAP FURNACE card (PN 113-00120-1) takes a set point from the CPUand sets its output as a voltage, up to the +24V power supply, to the selected gold trapfurnace. The feedback control of this voltage is governed by the feedback of the currentsupplied to the furnace. This current is compared to the set point and regulated to match.4.3.2.6 Hg LAMP CONTROL cardThe Hg LAMP CONTROL card (PN 113-00123-1) receives a set point from the CPU forthe Hg lamp and utilizes optical feedback to control the lamp intensity. The referenceoptical detector signal is fed-back and compared to the CPU set point. The currentsupplied to the lamp is set to minimize the error between the set point and the opticaloutput measured by the reference optical detector.4.3.2.7 DATA ACQUISITION cardThe DATA ACQUISITION card (PN 113-00125-1) is utilized to measure variousvoltages in the instrument. The most important voltages are those generated by the opticaldetectors in the optical cells which measure the fluorescence of mercury. The referenceoptical cell is included in the list of voltages measured.

44

TROUBLESHOOTINGSECTION V5.1 AutodiagnosticsThe software offers several autodiagnostic functions. Many of these diagnostic systemswill alert the user via the message box in the information bar. Simply, read the messageand take appropriate action. Some messages are simple errors that can be cleared easily.To clear the message click the clear button when a particular message is displayed. If morethan one message is necessary the software will flash them repeatedly in the same area ofthe screen.

5.2 Manual DiagnosticsThe software offers manual diagnostic functions. It is usually not necessary to use thesefunctions. To utilize these functions go to Utility Tab on the Runner application. An arrayof actions are available on this page. The common actions are available by selecting aspecific action and then clicking the Do Action button. The software returns a reading orperforms the output requested.The manual diagnostics are typically used when a problem is unusual and a customersupport representative is guiding the user.

5.2.1 Isolating Blank problems (HYDRA AFGOLD or HYDRA AF GOLD

PLUS only)Elevated blanks can be difficult to isolate on a "trap and release" method such as EPAmethod 1631. To aid in isolating where the elevated signal is coming from the HYDRAAFGOLD and HYDRA AFGOLDPLUS come with gas flow bypass jumpers (PN 120-00434-1).Simply follow the procedure below to isolate where the signal is coming from. Keep inmind that a peak on the detector may be caused from mercury, water vapor, or organiccontamination.1. Run a blank and record the peak area signal2. Run a blank with the pump off. If the signal drops to below 5000 counts the problem isin your blank or the stannous chloride reductant, if the same acid blank is utilized in thestandards then they are contaminated also. Try sparging the stannous chloride overnightwith ultra pure nitrogen or argon. If the signal is well above 5000 counts then proceed tostep 3.3. Disconnect the liquid/gas separator from the red and black fittings on the panel andplace a gas flow bypass jumper from the red panel fitting to the black panel fitting.4. Run a blank with the pump off. If the signal drops to below 5000 counts the problem isprobably caused by too high a signal from water vapor. The soda lime trap* should bereplaced and the test retried. If the signal is still high then verify the counterflow gas isrunning through the Nafion dryer. Lastly, replace the Nafion dryer**. If the signal doesnot drop below 5000 counts proceed to step 5.5. Disconnect the soda lime dryer from the yellow fittings on the panel and place a gasflow bypass jumper from one yellow panel fitting to the other.6. Run a blank with the pump off. If the signal drops below 5000 counts the problem is

45

probably a spent soda lime trap. Replace the soda lime trap* and run this test again. Runseveral blank runs to make sure the soda lime dryer is conditioned.

* NOTE - The soda lime dryer should be muffled to eliminate water. See soda lime dryerpacking and conditioning else where in manual.** NOTE - It is recommended that you proceed to the next test before replacing theNafion dryer. This may save in the expense of replacing the Nafion dryer needlessly.

46

REPLACEMENT PARTS /REAGENTS / ACCESSORIESSECTION VI6.1 Replacement

P.N. 309-00088-4P.N. 309-00104-1P.N. 309-00088-6P.N. 120-00412-1P.N. 116-2102P.N. 116-2107-1P.N. 116-2110P.N. 120-00063P.N. 120-00432-1P.N. 120-00277-1tubingP.N. 120-00282-1P.N. 120-00413-1P.N. 120-00284-1containerP.N. 120-00433-1P.N. 120-00428-1P.N. 120-00431-1P.N. 120-00431-2P.N. 120-00416-1P.N. 120-00423-1P.N. 120-00426-1P.N. 318-00016P.N. 317-00048P.N. 125-00036-1P.N. 307-00093P.N. 306-00038P.N. 902-00018versionsP.N. 116-3105sample tip.P.N. 304-1015sample tip.

partsReductant pump tubing 12-packSample pump tubing eachRinse pump tubing eachDrain pump tubing eachStandard cups 50mL 10/boxSample cups 15mL 250/boxCaps for sample cups 100/pkg.Gas exhaust tubing assembly with fittingGas connection tubing assembly with fittingSample tip and tubing assembly from autosampler to pump

Reductant bottle tubing from bottle to pump tubingRinse bottle tubing from bottle to pump tubingWaste tubing assembly from drain pump tubing to waste

Waste line from L/G separator to pump tubingReactor mix tubing from pump to L/G separatorReductant bottle (1L) lined with fluoropolymerRinse bottle (4L) lined with fluoropolymerG-3 Liquid/Gas SeparatorNaflon counterflow drying tubeGold amalgamation trap assembly (3 per instrument)Soda Lime scrubber empty tubeHg LampPump Head Replacement KitCassette for pump head eachLubrication oil for autosampler

Fuse set includes 6 each fuse for both 120V and 230V

Thumb screw for autosampler. Used to lock down the

Sample tip guide (lower). Lower teflon piece that guides the

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6.2 ReagentsP.N. 116-00094-1P.N. 606-00015P.N. 604-00004P.N. 604-00002P.N. 602-00159P.N. 602-00163P.N. 604-00164P.N. 602-00161P.N. 602-00160

6.3 AccessoriesP.N. 120-00420-1P.N. 120-00421-1P.N. 120-00414-2P.N. 120-00431-1P.N. 120-00431-2P.N. 121-00041-1P.N. 120-00427-1

Installation kit of acids, SnCb, Hg standard, and Soda LimeSoda Lime - 200gr.HC1 blanking solution 1%HC1 rinse solution 2%Mercury stock solution lug/mL(ppm)2% SnCl2 in 10% HC1 reductant 1L2% SnCl2 in 10% HC1 reductant 2LBromine monochloride digestant solutionHydroxylamine hydrochloride reductant solution

Sample racksStandard racksFlow Through RinseReductant bottle (1L) fiuoropolymer lined w/cap and fittingRinse bottle (4L) fiuoropolymer lined w/cap and fittingComplete Optical Cell with housingSoda Lime Dryer assembly w/tubing and fittings

6.4 OptionsP.N. 125-00085-1 Conversion Kit for HYDRA AF-M manual system toconvert to fully automated system

Please contact sales for more information of options available for the instrument.

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APPENDIX A - EPROMINSTALLATION PROCEDURE(FOR HYDRA AF INSTRUMENTS)The following recommended procedure describes the removal and replacement oferasable, programmable, read-only memory chips (EPROMs) on the CPU board ofHYDRA AF instruments:1. Exit WinHg software.2. Turn off the HYDRA AF and remove the power cord from the back of the instrument.3. Remove the four front panel screws around the edge of the black plastic process panel.4. Slide the drawer forward.5. Locate the CPU board (in card cage in rear of the main chassis, cable from back ofinstrument goes to CPU card), then disconnect the serial communications cable.6. Remove the CPU board by pulling up the board ejector tab, then carefully lifting theboard out of the card cage slot.7. Locate the existing EPROM on the CPU board (refer to Figure A.I). Use a smallscrewdriver to carefully pry the existing EPROM out of its socket. Replace it with theEPROM included with the software upgrade documentation.NOTE: Some software upgrades do not require installation of a new EPROM.

CPU BOARD

EPROM LOCATION

Figure A. 1. EPROM Location (CPU Board)NOTE; When installing the EPROM ensure that:• You are grounded to avoid electrostatic discharge that may damage the

EPROM.• No EPROM pins get bent under the EPROM body.

49

• EPROM is oriented with its notch facing towards the serial communicationscable socket.

• EPROM is fully inserted.8. Replace the CPU board its card cage slot. Ensure that the board is seated correctly,then press the ejector tab down.9. Reconnect the serial communications cable to the CPU board.10. Slide the drawer back into place.NOTE: Be careful not to pinch cables or tubing during this step.11. Replace the cover mounting screws.12. Reconnect the power cord, then power up the HYDRA AF instrument.13. Reboot the computer and start software. If a new software disk is enclosed in thepackage it must be install on the computer. Follow the instructions supplied with the disk.NOTE: EPROMs and software on disk are typically matched. If one is installed, withoutthe other, operational problems may arise.

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HYDRA AF Quick Installation150-00217 Rev. 2

Mar. 20,2001

Open all packages and inspect for damages.Select an area to install the instrument. An area of 65" x 30" is the minimal required.Place the computer on the bench.Place the video monitor on top of the computer.Place the keyboard in front of the computer.Place the HYDRA AF next to the computer (left or right).Place printer next to the computer.

• For correct placement of systems to avoid corrosion due to acid vapors make surethe right side of the instrument is at least 60in. (1.5m) away from any acid source.• Connect computer cables as follows -

- Power to computer, monitor, printer.- Video monitor cable to computer (15 pin)- Printer cable from 'LPT 1' (25 pin) to printer- Keyboard cable to round connector in rear of computer

• Connect HYDRA AF cables and gas lines --Power to HYDRA AF- Serial communication cable from computer 'COM 1' (9 pin) to HYDRA AF 'RS232' (25 pin)- Gas in from pure argon, nitrogen, or air. (75 - 90psig)- Exhaust out to hood, mercury trap, or both

• Installation aid on computer -- Power up HYDRA AF. Switch is in rear where power cord connects.- Power up printer. Follow printer instruction manual for loading paper.- Power up computer and monitor.- When the Windows Desktop appears double click the WinHg icon- The HYDRA AF Runner Application should be displayed.- Pull down the Help menu

Select the Video/Photo guideSelect the Installation photos. Review the photographs to guide you through the setup of theinstrument.

• Help on the software -- Help is only a click away. There is either a help button available or the question mark button will yield

help on a given tab that is currently displayed.

Teledyne Leeman Labs Germany GmbH, Kreuztal, Germany, Mercury Analyser, Sample ... Page 1 of 1

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