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HAPSITE Smart Operating Manual

Chapter 6

Methods

6.1

Introduction to Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-1

6.1.1

Sensitivity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-1

6.2

Survey Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-1

6.2.1

Building a Survey Method Library File . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-3

6.2.1.1

Creating Survey Methods for Target Compounds . . . . . . . . . . . . . . . . . . . . 6-3

6.2.1.2

Building a Survey Target Compound Library . . . . . . . . . . . . . . . . . . . . . . . . 6-3

6.3

GC/MS Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-6

6.3.1

Building a GC/MS Method and Target Compound Library File . . . . . . . . . . 6-8

Chapter 7

Tune

7.1

Introduction to Autotune and Manual Tune . . . . . . . . . . . . . . . . . . . . . . . . . 7-1

7.2

Autotune . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-2

7.2.1

Starting Autotune from the Manual Tune Screen . . . . . . . . . . . . . . . . . . . . . 7-4

7.3

Viewing a Tune Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-5

7.4

Autotune Failure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-7

7.5

Manual Tune Settings and Controls . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-9

7.5.1

Tool Bar . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-11

7.5.2

Tune Drop Down Menu . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-12

7.5.2.1

Tune Properties Window . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-13

7.5.3

Tune Control Panel. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-14

7.5.3.1

Tune Parameters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-15

7.5.4

Peak Scan Window . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-17

7.5.4.1

Peak Scan Window Controls . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-17

7.5.5

Full Scan Window. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-19

7.5.6

Tune and Mass Calibration Status . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-20

7.5.7

Mass Calibration Status . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-22

7.5.8

Right Mouse Button (RMB) Menus. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-23

7.5.8.1

RMB in Scan Window. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-23

7.5.8.2

RMB in Tune Status Window . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-24

7.5.8.3

RMB on Y Axis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-25

7.6

Performing Manual Tune . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-25

7.6.1

Adjusting Base Peak Gain . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-26

7.6.2

Adjusting Resolution. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-29

7.6.3

Adjusting the Ion Energy . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-31

Summary of Contents for HAPSITE Smart

Page 1: ...O P E R A T I N G M A N U A L HAPSITE Smart Chemical Identification System IPN 074 397 P1G ...

Page 2: ......

Page 3: ...O P E R A T I N G M A N U A L HAPSITE Smart Chemical Identification System IPN 074 397 P1G www inficon com reachus inficon com 2006 INFICON ...

Page 4: ... are trademarks or registered trademarks of their respective companies The HAPSITE Smart runs a Linux Operating System The source code for the Operating System is available from INFICON by request for a nominal operating fee Linux is the registered trademark of Linus Torvalds in the U S and other countries Disclaimer The information contained in this manual is believed to be accurate and reliable ...

Page 5: ...period of ten years after the date on which the equipment was last manufactured In additional to this file technical installation maintenance and application information concerning this equipment can also be found in the Operating Manual s for this product or product family Equipment Description HAPSITE Smart Portable GC MS with or without wireless communications including the HAPSITE Service Modu...

Page 6: ...United Kingdom None Applicable Standards Units without wireless communications Safety EN 61010 1 2001 Emissions EN 61326 1 1997 A1 1998 A2 2001 Radiated Conducted Emissions Class A Emissions per Table 3 EMC Measurement Control Laboratory Equipment EN 61000 3 2 2000 Harmonics EN 61000 3 3 1995 A1 2001 Flicker Immunity EN 61326 1 1997 A1 1998 A2 2001 General EMC Class A Immunity per Table A 1 EMC Me...

Page 7: ...ocumentation File is also available for review by competent authorities and will be maintained for a period of ten years after the date on which the equipment was last manufactured In additional to this file technical installation maintenance and application information concerning this equipment can also be found in the Operating Manual s for this product or product family Equipment Description Si...

Page 8: ...ntative Duane H Wright Operations Quality Manager ISS INFICON Inc ANY QUESTIONS RELATIVE TO THIS DECLARATION OR TO THE SAFETY OF INFICON S PRODUCTS SHOULD BE DIRECTED IN WRITING TO THE VICE PRESIDENT OF OPERATIONS AT THE ABOVE ADDRESS Revised 11 04 08 Rev C ...

Page 9: ...ocumentation File is also available for review by competent authorities and will be maintained for a period of ten years after the date on which the equipment was last manufactured In additional to this file technical installation maintenance and application information concerning this equipment can also be found in the Operating Manual s for this product or product family Equipment Description He...

Page 10: ...tative Duane H Wright Operations Quality Manager ISS INFICON Inc ANY QUESTIONS RELATIVE TO THIS DECLARATION OR TO THE SAFETY OF INFICON S PRODUCTS SHOULD BE DIRECTED IN WRITING TO THE VICE PRESIDENT OF OPERATIONS AT THE ABOVE ADDRESS Revised 11 04 08 Rev B ...

Page 11: ...on Seller shall not be liable for any further damages which could have been avoided if Seller had been provided with immediate written notification THIS WARRANTY IS MADE AND ACCEPTED IN LIEU OF ALL OTHER WARRANTIES EXPRESS OR IMPLIED WHETHER OF MERCHANTABILITY OR OF FITNESS FOR A PARTICULAR PURPOSE OR OTHERWISE AS BUYER S EXCLUSIVE REMEDY FOR ANY DEFECTS IN THE PRODUCTS TO BE SOLD HEREUNDER All ot...

Page 12: ......

Page 13: ...R This is a Danger paragraph Failure to heed these messages has a high likelihood of resulting in serious personal injury or even death WARNING This is a Warning paragraph It warns of actions that may cause physical injury WARNING Risk Of Electric Shock This Warning paragraph warns of the presence of electrical voltages which may cause physical injury CAUTION This is a Caution paragraph It caution...

Page 14: ...drive letter being used for a It is assumed that the hard drive used is drive c If using another drive substitute the hard drive letter being used for c Left click means to press and release the left mouse button LMB and right click means to press and release the right mouse button RMB The HAPSITE software operates in the Windows environment using the Windows Graphical User Interface GUI Actions i...

Page 15: ...4 Electronic Systems 1 9 1 6 4 1 Mass Spectrometer Control 1 9 1 6 4 2 Gas Chromatograph Control 1 9 1 6 4 3 Main Processor 1 9 1 6 4 4 Interfaces 1 9 1 6 5 Software Systems 1 9 Chapter 2 HAPSITE Components and Assemblies 2 1 Introduction 2 1 2 2 Ship Kit Contents 2 1 2 3 Basic Assembly 2 4 2 3 1 Attaching the Probe 2 5 2 3 2 Remove Exhaust Vent Cap 2 6 2 3 3 Installing the Gas Canisters 2 7 2 3 3...

Page 16: ...Probe Sampling Options and Attachments 2 37 2 10 1 Probe Nut Assembly 2 37 2 10 2 Attaching a Bag Sample 2 38 2 10 3 VX G Conversion Tube 2 38 2 10 3 1 VX G Conversion Tube Installation 2 39 2 10 3 2 VX G Conversion Tube Removal 2 40 2 11 Batteries 2 41 2 11 1 How to Remove a Battery 2 41 2 11 2 Battery Charger 2 42 2 11 2 1 Battery Charger Components Received 2 42 2 11 2 2 Battery Charger Connect...

Page 17: ...Tri Bed Concentrator Cleanout 3 32 3 5 2 Quick Reference SOP Tri Bed Concentrator Method 3 32 3 6 GC MS Mode with Tenax Concentrator 3 33 3 6 1 Quick Reference SOP Tenax Cleanout 3 35 3 6 2 Quick Reference SOP Tenax Concentrator Method 3 35 3 7 GC MS Mode with Headspace Sampling System and Sample Loop in Portable Mode 3 36 3 7 1 Quick Reference SOP GC MS Mode with HSS and Sample Loop in Portable M...

Page 18: ... the USB Drive 4 15 4 10 Reviewing the Data Retrieved from the USB 4 17 Chapter 5 Operating HAPSITE in Laptop Mode 5 1 Starting the HAPSITE in Laptop Mode 5 1 5 1 1 Quick Reference SOP Starting the HAPSITE 5 7 5 2 Survey Mode 5 8 5 2 1 Quick Reference SOP Running Survey Mode 5 12 5 3 GC MS Mode with Loop 5 13 5 3 1 Quick Reference SOP Running GCMS Loop Method 5 17 5 4 GC MS Mode with Tri Bed Conce...

Page 19: ...anual Tune Screen 7 4 7 3 Viewing a Tune Report 7 5 7 4 Autotune Failure 7 7 7 5 Manual Tune Settings and Controls 7 9 7 5 1 Tool Bar 7 11 7 5 2 Tune Drop Down Menu 7 12 7 5 2 1 Tune Properties Window 7 13 7 5 3 Tune Control Panel 7 14 7 5 3 1 Tune Parameters 7 15 7 5 4 Peak Scan Window 7 17 7 5 4 1 Peak Scan Window Controls 7 17 7 5 5 Full Scan Window 7 19 7 5 6 Tune and Mass Calibration Status 7...

Page 20: ... 8 6 2 Configuring the HAPSITE for Communications 8 22 8 6 3 Establishing Communication with the Service Module 8 26 8 7 Establishing Communications between the HAPSITE and Laptop Computer Using the Wireless Connection 8 28 8 8 Designating a Startup Method 8 28 8 9 Setting the HAPSITE Time Zone 8 32 8 10 Access Levels 8 34 8 10 1 Changing Access Levels 8 34 8 10 2 Setting or Changing the Access Le...

Page 21: ...unction in the TIC RIC Window 9 16 9 6 2 Using The Zoom Spectrum Function 9 18 9 7 Displaying Reconstructed Ion Chromatograms RIC 9 19 9 7 1 RIC Plot to Locate Specific Compounds 9 20 9 8 NIST Library Searches 9 23 9 8 1 Searching Peaks 9 25 9 8 2 Analyzing Data Using AMDIS 9 29 9 8 3 How To Access AMDIS 9 29 9 8 3 1 Accessing NIST from AMDIS 9 31 9 8 4 Analyzing Data Using NIST 9 32 9 8 5 How to ...

Page 22: ...States 11 12 11 4 2 GC Temperature Profile 11 17 11 4 3 Use Internal Standard 11 18 11 4 4 Scan Events 11 18 11 4 5 Concentrator Selection 11 19 11 4 6 Headspace Flow Parameter 11 19 11 4 7 SituProbe Flow Parameter 11 20 11 5 Tune Page 11 20 11 5 1 Param Page 11 20 11 5 2 Report Page 11 20 11 6 Full Scan Page 11 23 11 7 SIM Page 11 25 11 7 1 SIM for GC MS 11 26 11 7 2 SIM for Survey 11 28 11 8 Sea...

Page 23: ...cted Mass Peaks 12 9 12 3 7 Calibration 12 9 12 4 Display Function 12 10 12 5 The Quantitation 12 12 12 6 Using the Calibrate Function 12 12 12 7 Using the ID Unknown Function 12 20 Chapter 13 Headspace Sampling System 13 1 Introduction 13 1 13 1 1 How the HSS Operates 13 2 13 1 2 Performance Specifications 13 3 13 1 3 HSS Indicators 13 3 13 1 4 Consumables Required 13 4 13 1 5 Connecting the HSS ...

Page 24: ... the Service Module 14 3 14 3 1 Backup Batteries 14 3 14 3 2 MDP Turbo Pump 14 3 14 3 3 Manifold Vent Valve 14 3 14 3 4 Foreline Vent Valve 14 4 14 3 5 Roughing Pump 14 4 14 3 6 Vacuum Interconnect Valve Actuator 14 4 14 3 7 Battery Charger 14 4 14 3 8 Power Supply 14 5 14 3 9 Communications 14 5 14 4 When to Use the Service Module 14 6 14 5 Smart IQ Software for the Service Module 14 7 14 5 1 The...

Page 25: ... Decontaminate 15 9 15 6 NEG Troubleshooting 15 11 15 6 1 Bakeout Procedure 15 13 15 6 2 Reactivating the NEG Pump 15 14 15 7 NEG Pump Removal Installation and Activation 15 15 15 7 1 Required Tools and Equipment 15 16 15 7 2 Part 1 NEG Pump Removal 15 17 15 7 3 Part 2 Service Module Vacuum Interconnect VI Valve Cleaning 15 22 15 7 4 Part 3 Install the New NEG Pump 15 27 15 7 5 Part 4 Leak Check o...

Page 26: ...TE Upgrade for 930 280 GX series HAPSITE 18 4 18 6 HAPSITE Smart Training 18 4 18 6 1 On Site Training Course 18 4 18 6 2 Syracuse Training Course 18 5 18 6 3 Usage Fees 18 5 18 7 Headspace Spare Parts 18 5 18 8 Service Module Spare Parts 18 6 18 9 HAPSITE SituProbe Spare Parts 18 6 Appendix A HAPSITE Target Compounds A 1 Compounds In Order Of Elution A 1 Appendix B Calibrating Gas Mixtures B 1 Ac...

Page 27: ...TOC 13 IPN 074 397 P1G HAPSITE Smart Operating Manual Appendix C Shipping the HAPSITE and Consumables C 1 Introduction C 1 C 2 Shipping the Canisters C 1 C 3 Empty Canisters C 2 Index ...

Page 28: ...TOC 14 IPN 074 397 P1G HAPSITE Smart Operating Manual This page is intentionally blank ...

Page 29: ...rdware modules comprise the HAPSITE System HAPSITE Often referred to as the Analytical Module AM The AM contains the gas chromatograph and mass spectrometer cylinders of carrier gas and internal standard gas high vacuum chemical pump portable operation control electronics battery keypad display and a battery charger Probe Also known as the Hand Control Unit this consists of a hand piece and a heat...

Page 30: ...rogen Column Temperature Range 60 o C to 180 o C Maximum Sample Moisture Content 8 by weight pH Range of Sample 2 11 Boiling Point of Sample 250 o C Chemical Composition of Sample 1 12 Carbon atoms GC Column 100 methyl silicone phase 30 m x 0 32 mm ID x 1 0 film SIM Channels 10 External Communications Ethernet Port Carrier gas use rate 1 canister per 8 hours of operation depending on the details o...

Page 31: ...meter In the mass spectrometer the gas stream of eluting compounds is bombarded with electrons The electrons fracture the molecules into a characteristic combination of smaller molecules or mass fragments The mass spectrometer measures and plots the response of these mass fragments to display a mass spectrum See section 1 6 2 Mass Spectrometer on page 1 6 for more information on how the MS works T...

Page 32: ...TE The Service Module and the HAPSITE module contain a Vacuum Interconnect Valve and electrical connectors through which their vacuum systems join and the modules communicate when the two modules are coupled together Figure 1 1 Major HAPSITE Subsystems 1 6 Description Of Subsystems The HAPSITE is comprised of the following subsystems Gas Chromatograph Mass Spectrometer Vacuum System Electronic Sys...

Page 33: ...n individual compound to travel from injection into the system until the compound elutes from the column is referred to as the retention time RT If the GC conditions remain constant the same compound will elute from the column at nearly the same retention time for each injection An important part of the operation of the HAPSITE is the use of Internal Standards to verify the performance of the gas ...

Page 34: ...es the face of a membrane mounted in the membrane isolation valve This membrane has the special characteristic of transmitting the flow of organic compounds to the mass spectrometer while effectively blocking the flow of inorganic gases such as the nitrogen carrier gas When the membrane isolation valve is opened the appropriate gases are permitted to enter the Mass Spectrometer for analysis while ...

Page 35: ...ds some ions are light enough to oscillate harmonically with the RF field picking up energy and increasing speed until the ions impact one of the rods and are neutralized Much heavier ions moving more slowly cannot respond to the RF field The heavier ions are dragged from the center by the DC field landing on one of the rods Once on the rod the heavier ion is neutralized At a specific combination ...

Page 36: ...ted The Service Module is not needed again until the NEG pump in the HAPSITE must be changed The two vacuum pumps of the HAPSITE continue to provide the pumping necessary for operation These two pumps are the non evaporate getter NEG pump and the smaller sputter ion pump The NEG pump incorporates a special zirconium alloy arranged in sintered disks which when heated adsorb gas molecules very aggre...

Page 37: ... line and the control logic for all the valves and heaters of the GC system 1 6 4 3 Main Processor The main processor is supported by a hard disk drive and is located in the central electronics assembly The main processor accepts data from many points within the system and controls all the other electronic sub assemblies both in routine operation and in managing the data taking methods 1 6 4 4 Int...

Page 38: ...equire the use of the HAPSITE Application software on an external PC The HAPSITE Application software Smart IQ is a Windows XP and Windows 2000 based system for use in the accessory personal computer The Smart IQ software is used to design and modify the methods under which the HAPSITE can operate view the data analyze the results and generate and print reports The PC is linked to the HAPSITE by a...

Page 39: ...chapter contains the assembly instructions for the HAPSITE and the available accessories CAUTION The HAPSITE instrument should be operated a minimum of every 3 weeks Recommended storage is in extended standby mode 2 2 Ship Kit Contents The following items are provided in a typical HAPSITE Smart Ship Kit See Figure 2 1 ...

Page 40: ...21 G1 Gasket Kit 930 022 G1 Tool Kit 930 249 G2 Concentrator Cover 930 251 G1 Concentrator Tube Tenax TA 930 716 G1 Concentrator Tube Tri Bed 930 0221 G1 Concentrator Nut and Ferrule 930 0231 G1 Probe Nut and Ferrule 930 2020 G1 Cap Kit 930 612 P1 USB Flash Drive 512M Special Cords for International Ship Kits Extra Cords for SM and Battery Charger Qty 2 Ship Kit Location Cord 930 0241 G1 USA N A 9...

Page 41: ...Ship Kit Box 4 and 5 Contents Box 2 Contents 930 470 G1 Battery Charger 24 V Power Supply see table Power Supply Ship Kit Usage 930 469 P1 930 0241 G1 110 V USA 930 469 P2 930 0241 G2 230 V European 930 469 G3 930 0241 G3 230 V UK 930 469 G4 930 0241 G4 230 V Australia Box 3 Contents In two separate boxes Battery Pack NiMH 930 4061 G1 Box 4 and 5 Contents ...

Page 42: ...ion a laptop computer and accessories are shipped The ship kits vary depending on the type of laptop ordered The laptop kits will include the Smart IQ Software CD and NIST Library Install CD 2 3 Basic Assembly Figure 2 6 HAPSITE Parts for Basic Assembly The basic assembly of the HAPSITE can be accomplished in six easy steps AC to DC Power Converter Batteries ...

Page 43: ...into the port on the top of the HAPSITE as illustrated in Figure 2 7 Figure 2 7 Attaching the LEMO Connector on the Probe Line to the HAPSITE HINT Save all of the caps to cover ports in the event the instrument needs to be washed or decontaminated Spare caps are provided in the Ship Kit See Figure 2 8 Figure 2 8 Spare Cap Kit ...

Page 44: ...emoved for the HAPSITE to function properly The HAPSITE is shipped with the cap removed See Figure 2 9 Figure 2 9 Exhaust Cap CAUTION Failure to remove the exhaust cap will cause the HAPSITE to not operate properly WARNING Compounds sampled will vent into the room through the exhaust When sampling hazardous materials either attach tubing and vent to a hood or attach an activated charcoal filter ...

Page 45: ...alling A Gas Canister NOTE The openings that hold the gas canisters are color coded to ensure the correct placement of the canisters The upper opening is color coded purple indicating the correct location of the purple banded Nitrogen Carrier Gas canister The lower opening is color coded yellow to indicate the correct location of the yellow banded Internal Standard canister The position of the gas...

Page 46: ...e The internal standard canister will need to be replaced after 3 to 4 days of continuous use These numbers are guidelines and will vary WARNING Do not re fill the canisters after use These canisters are disposable and not designed for re filling Canisters may fail upon refilling causing bodily injury CAUTION Closing the front panel when the canisters are not properly installed may damage the HAPS...

Page 47: ...nnector aligns with the corresponding red line on the receptor of the HAPSITE if the red dot is not visible on the HAPSITE the red dot on the power supply should be facing forward Plug the AC to DC power converter into a 110 V ac outlet See Figure 2 14 Figure 2 14 The AC To DC Power Converter Power Supply and Correct Connection to the HAPSITE 2 3 6 Connect Laptop if desired The HAPSITE Smart has t...

Page 48: ...pposite end plugs into the COM1 port on the laptop computer Once connected the crossover ethernet cable provides the communication connection between the HAPSITE and laptop computer See Figure 2 15 and Figure 2 16 Figure 2 15 Ethernet Connection to HAPSITE Figure 2 16 Ethernet Connection to Laptop 2 3 6 2 Connect laptop with Wireless Connection Refer to Chapter 4 Wireless and USB for information o...

Page 49: ...p and Service Module pumps together Use expired Internal Standard gas Use a LAN or Ethernet cable between laptop and HAPSITE Attach a bag sample without first checking the ferrules in the probe nut DO Leave a battery installed when operating even when AC is connected Run a background blank once per week or more Use Extended Standby instead of cold storage whenever possible Place appropriate caps o...

Page 50: ... on Service Module with SituProbe and Sample Loop or concentrator tube 2 6 Headspace Sampling System The Headspace Sampling System is an accessory used to test water and solid samples Samples are heated to release any VOC s into the sample vial headspace The sampling needle is inserted into the vial and the headspace is sampled through the needle and transfer line into the HAPSITE For additional i...

Page 51: ...duces the energy required to heat and maintain the temperature of the Transfer Line extending battery life INFICON part number 931 405 P1 Replacement Needle Kit Replacement when the original needle for a worn plugged or broken needle assembly INFICON part number 931 402 P1 HSS Carrying Shoulder Strap A strap which connects to the strap mounts on the sides of the HSS to facilitate carrying the inst...

Page 52: ...ocedure 1 Install a fully charged battery into the HAPSITE 2 Unplug the AC to DC power converter power supply from the HAPSITE See Figure 2 17 Figure 2 17 Power Supply to HAPSITE from AC To DC Power Converter 3 Connect the single end of the Y cable see Figure 2 18 to the power supply connector removed in step 2 4 Plug one end of the Y cable into the HAPSITE 24 V dc connector 5 Plug the other end o...

Page 53: ...n labeled in yellow THIS END TO HAPSITE should coincide with the end of the transfer line labeled in yellow THIS END TO HAPSITE See Figure 2 19 Figure 2 19 HAPSITE End of Transfer Line 7 The white label THIS END TO ACCESSORY on the insulation should coincide with the white label THIS END TO ACCESSORY on the transfer line See Figure 2 20 Y Connector and 24 V dc Supply Cable Plug into HAPSITE and HS...

Page 54: ...he marks on the HAPSITE and Headspace Sampling System connectors Figure 2 21 Attaching the Transfer Line to the HAPSITE NOTE If using a concentrator tube with the HSS wait to attach the transfer line until after running the appropriate concentrator cleanout method From the Front Panel see section 3 5 1 Quick Reference SOP Tri Bed Concentrator Cleanout on page 3 32 section 3 6 1 Quick Reference SOP...

Page 55: ...lace a battery in the HSS Open the front door of the HSS and insert a charged battery into the rectangular slot below the round carrier gas slot until it is engaged Make sure when inserting the battery that the lettering is right side up to insure proper orientation of the battery When inserted correctly it will click into place and remain snug See Figure 2 23 CAUTION The HSS is not sealed against...

Page 56: ...ce Module 2 7 1 Setting Up the Service Module Required Components RS 232 communication cable Power cord for Service Module PC with Smart IQ software installed When stored the Service Module should have an aluminum plug placed on the top opening This plug is used to keep the Service Module free of moisture and debris during storage NOTE The aluminum storage plug is supplied with the Service Module ...

Page 57: ...g and store it in a safe location Figure 2 25 Yellow Plastic Protective Cover on Service Module To prepare the Service Module for use with the HAPSITE the aluminum plug must be removed If under vacuum then the vacuum must be released by proceeding as follows The Service Module requires a power cable and a RS232 communications cable to allow communication with the laptop computer Figure 2 26 shows ...

Page 58: ...nual Figure 2 26 Power Cable Attached at Back Left of the Service Module The RS232 communication cable is shown in Figure 2 27 Figure 2 27 RS232 Communication Cable Attach the RS232 communications cable to the Service Module as shown in Figure 2 28 ...

Page 59: ...k Right Side of Service Module Now attach the RS232 cable to the laptop computer as shown in Figure 2 29 Figure 2 29 RS232 Communication Cable Attached to PC Turn on the Power switch for the Service Module located at the back right corner of the Service Module refer to Figure 2 26 Open the Smart IQ program ...

Page 60: ...odule Figure 2 31 Vent Service Module Confirm Window Select Yes to vent the Service Module A window will appear counting down a fifteen second delay while the vent procedure completes Once completed remove the aluminum plug Next clean any debris or dust from the Viton o ring using a lint free wipe with methanol Wipe the top of the o ring following the contour to clean the entire top exposed sectio...

Page 61: ...seated in the grove 2 7 2 Placing the HAPSITE on the Service Module CAUTION Never operate the HAPSITE on the Service Module in a moving vehicle Remove the yellow plastic protective cover from the bottom of the HAPSITE The yellow cover is shown in Figure 2 33 NOTE Store the yellow cover in a clean dry place where it will be easily accessible for later use This protective cover keeps dust and debris...

Page 62: ...the Bottom of the HAPSITE Carefully place the HAPSITE on top of the Service Module The opening at the bottom of the HAPSITE should be placed onto the opening on the Service Module Attach the Service Module to the HAPSITE using the black latch at each side of the Service Module Figure 2 35 shows the right side Service Module latch Figure 2 35 Service Module Showing Latch on Right Side Figure 2 36 s...

Page 63: ...d to Service Module using Service Module Latches Left Side View Continue by following the instructions in section 14 6 Starting Up HAPSITE on the Service Module on page 14 11 CAUTION The Service Module is not sealed against moisture debris or contamination with the front door open CAUTION Never attempt to move the Service Module when the Turbo pump is spinning ...

Page 64: ... HAPSITE from the Service Module 2 8 SituProbe For assembly information on the SituProbe refer to the SituProbe Purge and Trap System Operating Manual 2 9 Sample Collection Modes The Sample Loop is used to detect chemicals in the low ppm to high ppb concentration range Concentrator tubes are used to detect chemicals in the low ppb to high ppt concentration range The following procedures are used t...

Page 65: ...the wide end of the cone toward the center of the sample loop as shown in Figure 2 37 WARNING The elbow fittings and nuts may be hot If necessary let the elbow fittings and nuts cool down before continuing 3 While holding the ferrule and nut in place insert one end of the sample loop into the bottom elbow fitting 4 Lift the top elbow fitting slightly so that the top of the sample loop will fit bet...

Page 66: ... on the top elbow and tighten the top nut finger tight See Figure 2 39 Figure 2 39 Tightening the Top Nut 7 Using the 7 16 open end wrench supplied with the HAPSITE tighten both the top and bottom nut approximately a quarter turn See Figure 2 40 Figure 2 40 Wrench tighten ...

Page 67: ...becomes free 3 Remove the Sample Loop being careful not to lose the ferrules on the top and bottom Store the Sample Loop in a safe place for future use 2 9 3 Installing the Tri Bed Concentrator 1 Refer to section 2 9 2 Removing the Sample Loop on page 2 29 to remove the sample loop or to section 2 9 5 Removing the Concentrator Tube on page 2 36 to remove the currently installed concentrator tube 2...

Page 68: ... Bed Concentrator tube into the lower elbow fitting 5 Carefully lift up on the top elbow fitting and insert the end of the tube with the grooved metal sleeve into the fitting 6 Keep the Concentrator tube aligned between the two elbow fittings while gently pressing down on the top elbow fitting with just enough force to seat the tube 7 While maintaining steady pressure on the top elbow fitting firs...

Page 69: ...concentrator tube is properly installed NOTE The Concentrator Cover contains two metal contacts inspect the contacts prior to assembly to be sure the contacts are not bent or crimped 11 Close the front panel 2 9 4 Installing the Tenax or Carbopack Concentrator Figure 2 43 The Carbopack and Tenax Concentrator tubes 1 Refer to section 2 9 2 Removing the Sample Loop on page 2 29 to remove the sample ...

Page 70: ...in place put the bottom of the concentrator tube into the lower elbow fitting See Figure 2 44 Figure 2 44 Placing Concentrator in Bottom Elbow 3 Carefully lift up on the top elbow and insert the top of the concentrator tube See Figure 2 45 Figure 2 45 Inserting the Top of the Concentrator ...

Page 71: ...bow assembly with just enough force to seat the Concentrator Tube See Figure 2 46 Figure 2 46 Pressing Down on Elbow Assembly 5 Maintain the pressure on the top of the elbow and tighten the bottom nut only until it begins to contact the ferrule See Figure 2 47 Tighten Bottom Nut on page 2 33 Figure 2 47 Tighten Bottom Nut ...

Page 72: ...nce the nuts have been finger tightened use a 7 16 inch wrench to finish tightening Turn the nuts 1 8 to 1 4 of a turn more WARNING Using too much force may cause the fragile glass tube to break 8 The concentrator cover has two sets of metal arms that are used to make contact with the concentrator tube If these contacts are too close together the pressure from installing the cover may break the co...

Page 73: ...2 35 IPN 074 397 P1G HAPSITE Smart Operating Manual Figure 2 49 Back of Concentrator Cover 9 Install the concentrator cover See Figure 2 50 Figure 2 50 Concentrator Cover ...

Page 74: ...bow fittings and nuts cool down before continuing 2 Using the 7 16 open end wrench suppled by INFICON loosen the nuts on the top and bottom of the concentrator tube until the tube becomes free 3 Lift the top elbow and gently angle the concentrator tube out of the fixture 4 Remove the concentrator tube from the bottom elbow being careful not to lose the ferrules on the top and bottom 5 Store the co...

Page 75: ...th the beveled side facing up The cone shaped ferrule should be placed over the extension with the narrow end facing up Refer to Figure 2 51 Carefully remove the nut assembly from the narrow end of the guide and gently tap the nut so that the ferrules seat properly into the nut Thread the nut ferrule assembly onto the probe Finger tightening is sufficient WARNING Ferrule orientation is critical to...

Page 76: ...e complete counter clockwise revolution 7 Proceed with the desired method See Chapter 6 Methods 2 10 3 VX G Conversion Tube This procedure describes the steps required to prepare the HAPSITE to sample for VX or R 33 using the VX G conversion tube To detect VX or R 33 you must insert the VX G conversion tube following the guidelines below The process of detecting VX or R 33 on the HAPSITE requires ...

Page 77: ...nt ferrule cone facing forward See Figure 2 52 Figure 2 52 Ferrule Location NOTE If the nut on the HAPSITE probe is in place the nut does not need to be removed The VX G conversion tube can be slid inside the nut opening using the following procedure If the nut is removed to check the ferrules make sure the ferrules are not dropped Ferrule placement is critical to insure a leak free fit around the...

Page 78: ...ee Figure 2 54 Figure 2 54 Inserting the Swagelok Tube 4 Tighten the Swagelok nut finger tight Pull gently on the conversion tube it should be held firmly in place See Figure 2 55 Figure 2 55 Tightening the Swagelok Nut 2 10 3 2 VX G Conversion Tube Removal 1 Loosen the Swagelok nut 2 Gently pull the VX G Conversion Tube out of the probe 3 Make sure the ferrules remain properly seated in the Swage...

Page 79: ...increments See Figure 2 56 Figure 2 56 Battery Test Button and Charger Indicator 2 11 1 How to Remove a Battery The black button to the right of the battery is the battery release button Two clips hold the battery in the battery compartment See Figure 2 57 Firmly push in on the battery and simultaneously press and hold the battery release button located to the right of the battery compartment As t...

Page 80: ...s low as 90 V and as high as 253 V The frequency can be from 50 to 60 Hz The Battery Charger draws 120 W when fully loaded The AC power connects to the Battery Charger through a Type IEC 320 male plug a two wire grounded connector rated for the full range of voltages The connector is recessed at the right hand side of the rear of the Battery Charger and incorporates a pair of fuses The Battery Cha...

Page 81: ...ach battery to be charged in one of the charging receptacles The respective light will illuminate green and charging will commence immediately CAUTION Do not use excessive force when placing the battery in the Battery Charger CAUTION Do not charge batteries in a moving vehicle 2 11 2 4 Understanding the Battery Charger Indicators Each battery receptacle is associated with an indicator light which ...

Page 82: ...dicates that communication with the battery is unsuccessful Off The receptacle is ready to charge a battery If the indicator remains extinguished when a battery is inserted the battery is severely discharged In this case leave the battery in the receptacle and unplug the power cord Reconnect the power cord and the battery will start to charge ...

Page 83: ...ling System Strap Attach the HAPSITE and Headspace Sampling System straps as illustrated below in Figure 2 59 Figure 2 59 Attaching the HAPSITE Strap WARNING Failure to connect strap as shown increases the risk of strap failure possibly resulting in dropping the HAPSITE and or bodily injury HAPSITE Or Sampling Accessory Strap must be attached to HAPSITE or Sampling Accessory as shown Strap Eyelet ...

Page 84: ...per fit HINT Use a mirror to visually check the fit 5 Take the backpack off 6 If a height adjustment is needed use the grommets and pins to move the hip belt up or down 7 If the spacing between the shoulder straps needs adjustment tilt the buckles out of their current slots and insert them in the correct slots 8 Try on the empty pack again Repeat as necessary to achieve a proper fit 9 Release the ...

Page 85: ...lon 2 13 Hot Swap Cable IPN 930 246 G1 The Hot Swap Cable is used to provide an external power source for the HAPSITE When connected between an external battery and the 24 V dc power port on the HAPSITE the Hot Swap Cable permits changing the internal battery without the loss of power to the HAPSITE 2 13 1 Connecting The Hot Swap Cable WARNING Do not use the Hot Swap Cable in the rain 1 Plug the L...

Page 86: ...lug the power connector into the HAPSITE 24 V dc power port 2 Plug the power connector into the 24 V dc power port on the HAPSITE The discharged internal battery can now be replaced After replacing the internal battery disconnect the Hot Swap Cable See Figure 2 61 CAUTION Do not open the HAPSITE front panel in a contaminated environment Figure 2 61 Power Connector HAPSITE 24 V dc Power Port ...

Page 87: ...ontaminated environments by wrapping the battery and cable connection in a protective plastic bag when not in use See Figure 2 62 Figure 2 62 Storing 2 13 3 Use As An Additional Battery Source When using the Hot Swap Cable and battery to provide an additional battery source attach the battery to the HAPSITE via the Hot Swap Cable when the front panel shows the level of charge on the internal batte...

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Page 89: ...ION Never open the front panel outside while raining 2 Press the power button on the inside of the front panel The HAPSITE takes 1 to 2 minutes to power on See Figure 3 1 NOTE The power button is a toggle switch and once pressed and released returns back to the original placement HINT The HAPSITE should be powered on while connected to AC power The power on sequence will consume over 40 of the bat...

Page 90: ... Step 3 on page 3 2 through Step 5 on page 3 5 will be automatically run Currently instruments are shipped with the Survey method selected as the startup method 4 Select a method to run To select a menu option use up and down arrows to highlight the desired method press SEL OR press the number of the selection and then press SEL HINT Refer to Section 3 3 Survey Mode on page 3 18 or Section 3 4 GC ...

Page 91: ...gin to heat up the system When the heating sequence is completed the software will check the tune of the instrument and automatically make any necessary adjustments See Figure 3 4 If autotune fails refer to Section 7 4 Autotune Failure on page 7 7 NOTE The HAPSITE takes about twenty minutes to complete the warm up and short autotune Once completed the HAPSITE is ready to run samples ...

Page 92: ...3 4 IPN 074 397 P1G HAPSITE Smart Operating Manual Figure 3 4 Front Panel Display Checking Pressures Heating and Tuning ...

Page 93: ...Operating Manual Figure 3 5 Autotune Results 5 When the warm up is complete the start Method prompt will appear Press RUN when ready to sample See Figure 3 6 NOTE Press ESC to not perform the method Figure 3 6 Method Ready to Run Screen ...

Page 94: ...red 7 Highlight the desired method Air 15 min Loop or Survey NOTE The HAPSITE will now heat up the all zones and perform a tune check A run method prompt will appear when the HAPSITE is ready to run a sample The process for heat up and tune takes approximately 20 minutes 3 2 HAPSITE Front Panel Main Menu The folder tree on the HAPSITE is a menu of operations that can be performed by pressing butto...

Page 95: ...e The standard configuration is shown in this manual Figure 3 8 Method Menu Recent Methods Selecting entry 1 will display a list of up to 10 most recently used methods GCMS Selecting entry 2 will show a of list folders containing the available GCMS methods Survey Selecting entry 3 will show a list of available Survey methods 3 2 2 Review Data The Review Data menu provides access to the data files ...

Page 96: ...ode Highlight a file and press SEL to review the data 3 2 3 Service Module Service Module is the third option on the Main Menu Refer to Chapter 14 Service Module for more information Highlight Service Module and press SEL to show the screen displayed in Figure 3 9 Figure 3 9 HAPSITE Main Menu with Service Module Highlighted Two options are available from this menu See Figure 3 10 Each option requi...

Page 97: ...e 2 23 Detach SM Service Module menu selection number 2 will Detach the HAPSITE by sequentially closing off the vacuum connection between the HAPSITE and Service Module and shutting down the Service Module pumps Refer to Section 2 7 3 Detaching the HAPSITE from the Service Module on page 2 26 Figure 3 11 shows the message which will appear when Attach Service Module is selected Press 1 and SEL to ...

Page 98: ...ystem to advance to the screen shown in Figure 3 13 Figure 3 13 System Window Selected from Main Menu System menu selection number 1 is Update Software This selection requires the updated HAPSITE Smart software to have been previously copied to the HAPSITE Root Directory NOTE The Update Software function is best accomplished from the Laptop System menu selection number 2 is NEG Options as shown in...

Page 99: ...rent NEG conditions Figure 3 15 NEG Status Screen NEG Options menu selection 2 Use NEG selects when the NEG pump will be used to provide vacuum Figure 3 16 shows the four options available Figure 3 16 Use NEG Options Screen Always Option 1 is selected to always use heat to operating temperature the NEG pump when running the HAPSITE ...

Page 100: ... is selected to never use the NEG pump This is the preferred selection when the HAPSITE does not have a NEG pump installed and will be run using the Service Module Prompt User Option 4 will prompt the user whether or not to use the NEG pump each time a method is selected to run System menu selection number 3 is HAPSITE Probe Options as shown in Figure 3 17 Figure 3 17 HAPSITE Probe Options Screen ...

Page 101: ...his is best accomplished attached to a Service Module but can be done without the Service Module System menu selection number 5 Set Date and Time provides the option to set the date and time on the HAPSITE as shown in Figure 3 19 NOTE The Time Zone can only be set from the Laptop Figure 3 19 HAPSITE Current Date and Time System menu selection number 6 Set Network Info displays network computer con...

Page 102: ...versions 1 10 and higher 3 2 5 Exit HAPSITE Main Menu selection number 5 Exit provides the options shown in Figure 3 21 Detailed procedures for the Exit sub menu can be found in Section 3 10 Exit Options on page 3 46 Figure 3 21 Exit Menu Selected Shutdown System Shuts down and powers off the system Reboot System Reboots the system Completes power down and restart cycle Restart Program Restarts th...

Page 103: ...mp remains on to maintain vacuum in the MS and a higher state of readiness No gasses are required HINT Extended Standby is the preferred storage mode for the HAPSITE Cold Sets the system into a Cold Standby state which shuts down all heaters but leaves the HAPSITE powered on Used when attached to the Service Module Return To Main Menu Returns the system back to the HAPSITE Main Menu ...

Page 104: ...System Host name Serial Number Version Number Date and Time Built Free Disk Space Startup Method Information TUNE Tune File Name Time Instrument Tuned Date Instrument Tuned Press SEL for Tune Report HTR1 Heaters Page 1 Current Column Membrane Valve Oven Sample Probe and NEG Heater Temperatures Their Setpoint Temperatures State of Heaters On Off or In Control HTR2 Heaters Page 2 Current temperature...

Page 105: ...ervice Module Information TIME Date Time Time zone NET Network Information IP Address User Host GPS GPS Information Latitude Longitude Number of Satellites Found CAN Internal Standard Canister Information Fill Date Expire Date Actual PPM concentrations of BPFB and TRIS FIRM Firmware Versions for GC Gas Chromatograph FP Front Panel PR Probe MS Mass Spectrometer SM Service Module and HS Headspace ...

Page 106: ... second minute sample directly over the point of concern to see what additional chemicals are present Procedure 1 From the main menu on the front panel select 1 Run Method by pressing 1 then SEL See Figure 3 23 Figure 3 23 HAPSITE Main Menu 2 The Method menu will display Select the 1 Recent Methods choice on this menu to display up to the last ten methods run 3 Arrow down to highlight Survey and p...

Page 107: ...3 19 IPN 074 397 P1G HAPSITE Smart Operating Manual Figure 3 24 Selecting Survey Method using Recent Methods Menu ...

Page 108: ...es and run a Tune check approximately 2 minutes 5 Press RUN from the Front Panel or from the Probe both buttons are active When the sample pump turns on collect air for one minute away from the sample and then place the probe over the sample until the sample is identified the TIC count is 2 to 3 times the background without exceeding 60 million or one minute has passed A plot will appear on the Fr...

Page 109: ...ethod being run the second line displays the name of the data file the third line displays the MAX TIC for the run and the TIC count at the cursor The bottom line displays the run time 6 Press RUN again to stop the sampling The bottom of the LCD panel will prompt to press SEL for the report Figure 3 27 Figure 3 27 Survey Run Complete ...

Page 110: ... confirmation of the results 3 3 1 Quick Reference SOP Survey Method 1 From the main menu on the front panel highlight 1 Run Method and press SEL 2 Highlight Survey and press SEL 3 Highlight Survey and press SEL 4 Wait for heaters to gain control of set temperatures 5 Press RUN on the front panel or probe wait one minute before sampling 6 Hold the probe over the sample for one minute 7 Press RUN t...

Page 111: ...r the Survey method must be followed by a GC MS method in order to give a positive identification of the unknown This section will describe the process required to run a sample with the sample loop installed Refer to Section 2 3 Basic Assembly on page 2 4 and Section 2 9 1 Installing the Sample Loop on page 2 26 Assumptions made are that the HAPSITE is heated up tuned and ready to go If the HAPSIT...

Page 112: ...ccess the Method Menu See Figure 3 30 Figure 3 30 Selecting the Method using Method Menu 3 In the Method menu arrow down to GCMS To select the item press SEL when the menu item is highlighted or type the number of the selection and then press SEL After selecting the GCMS option the following menu will be shown See Figure 3 31 Arrow down to 3 Loop and press SEL Figure 3 31 Selecting the Physical Co...

Page 113: ... prompt will appear Press the RUN button to start the method See Figure 3 32 Figure 3 32 Selecting the Loop Method NOTE When the RUN button is pressed the sample pump will turn on and the word Loopfill will appear in the bottom left corner of the Front Panel display Hold the probe over the sample for the entire Loopfill event the sample pump will be audible if not in a noisy environment or in PPE ...

Page 114: ...Depending on the temperature profile the column temperature must down before the software will allow another run to begin 6 Once the Run is complete a report can be viewed on the Front Panel of the HAPSITE Press SEL for the report and use the arrow keys to navigate through the pages of the report See Figure 3 34 HINT The results page shows option 1 Summary and option 2 Qual The Summary report give...

Page 115: ...highlight Run Method and press SEL 2 Highlight GCMS and press SEL 3 Highlight Loop and press SEL 4 Highlight the Air 15 min Loop method and press SEL 5 Wait for heaters to gain control of set temperatures 6 When prompted press RUN from the front panel or Probe 7 Hold the Probe over sample for the entire Loopfill event one minute 8 Review data at the end of run ...

Page 116: ... Bed Concentrator on page 2 29 for instructions Once installed the Tri Bed concentrator must be cleaned before sampling begins NOTE These methods can also be used for the Carbopack concentrator which has been discontinued For instructions on installing the Carbopack concentrator refer to Section 2 9 4 Installing the Tenax or Carbopack Concentrator on page 2 31 1 From the main menu on the Front Pan...

Page 117: ...arbon Conc Cleanout and press SEL See Figure 3 38 Figure 3 38 Selecting the 3 min Carbon Conc Cleanout Method The system will raise the column temperature to 150 C which will take a few minutes When all the zones are heated the Run Method prompt will be displayed on the front panel of the HAPSITE See Figure 3 39 and Figure 3 40 Figure 3 39 Heater Warm up for the 3 min Carbon Conc Cleanout ...

Page 118: ...ered clean If the MAX TIC number is greater than 500 000 repeat the 3 min Carbon Conc Cleanout method until the MAX_TIC number becomes less than 500 000 Please note in Figure 3 41 the MAX_TIC is 1 551 539 therefore the concentrator is NOT clean The 3 min Carbon Conc Cleanout would need to be run again in this example Figure 3 41 Front Panel 3 min Carbon Conc Cleanout Run 6 When the 3 min Carbon Co...

Page 119: ...mpt when ready to run a sample See Figure 3 43 Figure 3 43 Air 15 min Carbon Conc Run Prompt 9 Hold the Probe over the sample and press RUN from the Front Panel or the probe HINT The sampling process takes two minutes one minute to flush the system and one minute to collect the sample The probe needs to be held over the sample for the entire two minutes while the Sample Pump is running The bottom ...

Page 120: ...tures 6 When prompted press RUN from the Front Panel or Probe HINT If the TIC_Max count is less than 500 000 at the end of this run proceed to the Air 15 min Carbon Conc method If the TIC_Max count is greater than 500 000 rerun the 3 min Carbon Conc Cleanout method Repeat tis until the TIC_Max is less than 500 000 3 5 2 Quick Reference SOP Tri Bed Concentrator Method 1 The 3 min Carbon Conc Cleano...

Page 121: ...pter 6 Methods for additional information on GC MS methods NOTE Before a GC MS can be run in this Concentrator mode the Tenax concentrator must be installed Refer to Section 2 9 4 Installing the Tenax or Carbopack Concentrator on page 2 31 for instructions Once installed the Tenax concentrator must be cleaned before sampling begins 1 From the main menu on the Front Panel display of the HAPSITE sel...

Page 122: ...an 500 000 repeat the 3 min Tenax Conc Cleanout method until the MAX TIC number is less than 500 000 7 When the 3 min Carbon Conc Cleanout method is completed and the MAX_TIC count is less than 500 000 press ESC to exit the method The system is now clean enough to run the Air 15 min Carbon Conc method 8 Highlight the Air 15 min Tenax Conc menu option by using the up or down arrows in the Concentra...

Page 123: ...the Front Panel or Probe NOTE If the TIC_Max count is less than 500 000 at the end of this run proceed to the Air 15 min Tenax Conc method If the TIC_Max count is greater than 500 000 rerun the 3 min Tenax Conc Cleanout method Repeat this until the TIC_Max is less than 500 000 3 6 2 Quick Reference SOP Tenax Concentrator Method 1 The 3 min Tenax Conc Cleanout method must be run prior this method R...

Page 124: ...ore information on the Headspace System Refer to Section 2 6 Headspace Sampling System on page 2 12 for assembly instructions Refer to Chapter 6 Methods for additional information on GC MS methods 1 Select 1 Run Method from the main menu on the front panel of the HAPSITE See Figure 3 47 Figure 3 47 Run Method From Main Menu 2 Select GCMS from the Method menu on the front panel of the HAPSITE See F...

Page 125: ...HAPSITE Smart Operating Manual 3 Select the Headspace folder from the GCMS menu See Figure 3 49 Figure 3 49 Selecting The Headspace Folder 4 Select HSS 15 Min Loop See Figure 3 50 Figure 3 50 Selecting The Headspace Method ...

Page 126: ...mpt window to open See Figure 3 51 Figure 3 51 Front Panel Heat up And Run Prompt 6 Place the headspace needle in the 40 mL vial that contains the sample Gently depress into sample vial See Figure 3 52 See Section 13 2 3 Loading the Wells on page 13 10 WARNING The headspace needle assembly may be hot ...

Page 127: ...al Figure 3 52 Headspace Needle 7 Press the Run button on the front panel of the HAPSITE 8 When prompted chromatogram completed place the headspace needle in the purge vial and press SEL See Figure 3 53 Figure 3 53 Purging the Head Space 9 Review data ...

Page 128: ...for additional information on GC MS methods CAUTION The concentrator feature is designed to enhance HAPSITE sensitivity when analyzing low concentration samples The accumulated sample VOCs are transferred from the concentrator adsorbent bed to the HAPSITE as a concentrated sample Care should be taken to avoid overloading the HAPSITE and causing excessive carryover of VOCs in subsequent runs 1 Refe...

Page 129: ...un Method from the main menu on the front panel of the HAPSITE See Figure 3 54 Figure 3 54 Selecting Run Method from the Front Panel 5 Select GCMS from the Method menu on the front panel of the HAPSITE See Figure 3 55 Figure 3 55 Selecting GC MS from the Method Menu 6 Select the Headspace folder from the GCMS menu See Figure 3 56 ...

Page 130: ...n which concentrator is installed See Figure 3 57 Figure 3 57 Selecting the HSS 15 Min Carbon Conc Method 8 Wait for temperatures to stabilize See Figure 3 58 Figure 3 58 Front Panel HSS Heater Display 9 Place the headspace needle in the 40 mL vial that contains the sample Gently depress into sample vial See Figure 3 59 See Section 13 2 3 Loading the Wells on page 13 10 ...

Page 131: ...g Manual WARNING The headspace needle assembly may be hot Figure 3 59 Loading the Wells 10 Press the Run button on the front panel of the HAPSITE See Figure 3 60 Figure 3 60 Run Prompt 11 Wait for the method to run to completion See Figure 3 61 ...

Page 132: ...SITE Smart Operating Manual Figure 3 61 Sample Run in Process 12 When prompted place the headspace needle in the purge vial and press SEL See Figure 3 62 and Figure 3 63 Figure 3 62 Purge Needle Request Figure 3 63 HSS Purging ...

Page 133: ...3 45 IPN 074 397 P1G HAPSITE Smart Operating Manual 13 Review results at end of run See Figure 3 64 Figure 3 64 Completed Run 14 View report See Figure 3 65 Figure 3 65 Sample Run Results on Front Panel ...

Page 134: ...ce the headspace needle in the 40 mL vial that contains the sample Gently depress into sample vial 7 Press the Run button on the front panel of the HAPSITE 8 When prompted place the headspace needle in the purge vial and press Sel 9 View results 3 9 SituProbe For information on running SituProbe methods refer to SituProbe Purge and Trap System Operating Manual 3 10 Exit Options Option 5 on the Mai...

Page 135: ... Arrow down or press 4 and SEL to select Standby Modes See Figure 3 67 Figure 3 67 Selecting Standby Options 4 Arrow down or press 2 and SEL to select Extended Standby See Figure 3 68 Figure 3 68 Selecting Extended Standby 5 Wait for system to cool and enter Extended Standby See Figure 3 69 ...

Page 136: ...HAPSITE is attached to the Service Module In this state the Ion pump is on and the NEG pump if installed is not powered All heated zones are off Refer to Chapter 14 Service Module for more information on the Service Module and refer to Section 2 7 2 Placing the HAPSITE on the Service Module on page 2 23 for additional information on attaching the HAPSITE to the Service Module 1 Press the ESC butto...

Page 137: ...3 Arrow down or press 4 and SEL to select Standby Modes See Figure 3 72 Figure 3 72 Selecting Standby Modes 4 Arrow down or press 1 and SEL to select Cold Standby See Figure 3 73 Figure 3 73 Selecting Cold Standby HAPSITE will turn off filaments heaters and valves to enter Cold Standby See Figure 3 74 ...

Page 138: ...ss the ESC button on the front panel until reaching the Main Menu 2 Arrow down or press 5 and SEL to select the Exit Menu 3 The first choice is Shutdown System Press 1 then SEL 4 When asked to Halt System press 1 then SEL to shutdown The system will automatically shut itself down Remove the gas canisters and the battery once the shutdown is complete See Figure 3 75 ...

Page 139: ...3 51 IPN 074 397 P1G HAPSITE Smart Operating Manual Figure 3 75 Shutting Down the HAPSITE ...

Page 140: ... the HAPSITE to autotune or if the HAPSITE has frozen similar to a PC 1 Press the ESC button on the front panel until reaching the Main Menu 2 Arrow down or press 5 and SEL to select the Exit Menu See Figure 3 76 Figure 3 76 Exit Option on Main Menu 3 Arrow down or press 2 and SEL to select Reboot System See Figure 3 77 Figure 3 77 Reboot Option on Exit Menu 4 Arrow down or press 1 and SEL to conf...

Page 141: ...e HAPSITE Smart software This option is most commonly used after saving a previous tune file to the current default tun file to 1 Press the ESC button on the front panel until reaching the Main Menu 2 Arrow down or press 5 and SEL to select the Exit Menu See Figure 3 79 Figure 3 79 Selecting Exit Option on Main Menu 3 Arrow down or press 3 and SEL to select the Restart Program See Figure 3 80 ...

Page 142: ...anual Figure 3 80 Selecting Restart Program Option 4 Arrow down or press 1 and SEL to confirm restart See Figure 3 81 Figure 3 81 Confirming Restart Program 5 HAPSITE will shutdown the HAPSITE Smart software then restart the HAPSITE Smart software ...

Page 143: ...area around the device s There is a hardware switch to turn off the wireless radio so that the HAPSITE may still be used in areas where these hazards are a concern Consult applicable regulations and policies when using the HAPSITE with the wireless device active in such environments 4 2 FCC Compliance Information This section of the Operating Manual lists FCC and Industry Canada IC compliance info...

Page 144: ...diate radio frequency energy and if not installed and used in accordance with the instructions may cause harmful interference to radio communications However there is no guarantee that interference will not occur in a particular installation If this equipment does cause harmful interference to radio or television reception which can be determined by turning the equipment off and on the user is enc...

Page 145: ...nce is 50 ohms To reduce potential radio interference to other users the antenna type and gain should be so chosen that the equivalent isotropically radiated power EIRP is not more than required for successful communications 4 3 Wireless Range The HAPSITE Smart is equipped with an 802 11b wireless adapter The typical range for a signal is 300 ft 100 meters line of sight with no obstructions The fo...

Page 146: ...r that emits electromagnetic radiation EMR This radiation in a tactical or operational environment may potentially be used to locate the HAPSITE and its operators This radiation also has the potential to detonate some types of unexploded ordnance UXO or improvised explosive devices IEDs or both if the HAPSITE is transmitting in the safety exclusion area around the device s There is a hardware swit...

Page 147: ...d Mode Table 4 2 gives directions to set up this mode 4 5 1 Setting the User Access Level The HAPSITE Smart leaves the factory in Normal operating mode Setting up communication requires the user to be in Advanced Mode For information on setting the user level see Table 4 2 Table 4 2 Setting User Access Level Step Description 1 Open the Smart IQ software 2 From the System Setup page click on Tools ...

Page 148: ...tting Up Smart IQ for Communication with the HAPSITE The first step to communication between the HAPSITE and laptop is to set up a Sensor Icon in Smart IQ This is the HAPSITE Icon seen on the bottom of the System Setup window of Smart IQ See Table 4 3 for instructions Table 4 3 Adding a Sensor Icon in Smart IQ Step Description 1 Open Smart IQ From the System drop down menu select Properties NOTE T...

Page 149: ... For example H172 Select Add 4 The newly added HAPSITE will appear in the HAPSITE List Select OK 5 Select OK in System Properties to close the window 6 If the HAPSITE Sensor appears as shown in the Smart IQ System Setup window communication has been established 7 If the HAPSITE Sensor appears with a Blue X through it communication has not been fully established Continue with the instructions in Ta...

Page 150: ...e 4 4 Setting the IP Address Step Description 1 If communication between the HAPSITE and the laptop could not be established using Table 4 3 then continue with Step 2 2 Press the STAT key on the Front Panel of the HAPSITE 3 Using arrow keys select NET The IP address of the HAPSITE will be displayed Example 10 210 0 110 255 252 0 0 Each HAPSITE will have a unique IP address 4 From Start Menu on the...

Page 151: ...PSITE Smart Operating Manual 5 From the Wireless Network Connection Status Window select Properties 6 In the General tab highlight Internet Protocol TCP IP select Properties Table 4 4 Setting the IP Address Step Description ...

Page 152: ...bers must have 128 added to it In this example the third set of numbers is 0 This would be entered as 128 NOTE This is necessary in order for the system to configure communication properly Example 10 210 0 172 becomes 10 209 128 172 Select OK 8 Select OK in Wireless Network Connection Properties to close the window 9 Communication between the HAPSITE and the laptop is now established Verify by not...

Page 153: ...or specific instructions on setting up the wireless radio The Dell website has a section on wireless communications called the Wireless Center This section can be accessed at http support dell com by clicking the Technical Support tab then selecting Wireless Center The content applies to many manufacturer s laptop computers not just Dell laptop computers 4 6 Wireless Module Indicator Lights Locate...

Page 154: ...onate some types of unexploded ordnance UXO or improvised explosive devices IEDs or both if the HAPSITE is transmitting in the safety exclusion area around the device s Discussed below is a hardware switch to turn off the wireless radio so that the HAPSITE may still be used in areas where these hazards are a concern Consult applicable regulations and policies when using the HAPSITE with the wirele...

Page 155: ...red for communication via ethernet or wireless connections In this instance data can be placed on the USB drive and later transferred to the laptop for analysis Table 4 6 Saving Files to the USB Drive Step Description 1 Open the front panel of the HAPSITE 2 Insert the USB drive into the USB port located on the top left hand side Close the front door of the HAPSITE NOTE When inserting the USB drive...

Page 156: ...ess SEL 6 If the method was a GC MS file highlight the correct configuration Loop Concentrator or Headspace and press SEL 7 Highlight the data file folder enter and press SEL 8 Highlight the data file to be saved and press SAVE 9 Repeat as needed Table 4 6 Saving Files to the USB Drive continued Step Description ...

Page 157: ...e front panel and remove the USB drive See section 4 9 for details on transferring the files from the USB drive to the laptop computer NOTE Data files are saved to the USB drive with a hpz file extension Table 4 6 Saving Files to the USB Drive continued Step Description Table 4 7 Retrieving Files from the USB Drive Step Description 1 Insert the USB drive into the USB port in the laptop computer 2 ...

Page 158: ... would be Smart IQ H172 Data Loop Air 15 min Loop 7 Now the data files can be accessed using Data Review in Smart IQ Refer to Table 4 7 for more information NOTE Use the Safely Remove Hardware feature of Windows to unplug the USB drive from the PC Failure to do so can corrupt the USB drive This is not necessary when unplugging the USB drive from the HAPSITE Smart Table 4 7 Retrieving Files from th...

Page 159: ... the Laptop Step Description 1 Open Smart IQ software 2 Double click on the Data Review icon 3 Designate PC in the top portion of the window NOTE Any files transferred from the USB drive to the laptop will reside on the PC 4 Double click on the appropriate folder GCMS or Survey 5 Double click on the appropriate configuration Loop Headspace Concentrator folder 6 Double click on the method name Air ...

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Page 161: ...r ethernet cable Laptop computer Mouse optional Power supply AC To DC Power Converter power supply unless powered by a Service Module Procedure 1 Refer to Section 2 3 Basic Assembly on page 2 4 2 Press the power button on the inside of the front panel to turn on the HAPSITE The HAPSITE takes 1 2 minutes to power on See Figure 5 1 NOTE The power button is a toggle switch Once the power button has b...

Page 162: ...following message will appear during the power on sequence see Figure 5 2 Figure 5 2 NEG Full Power 5 If the HAPSITE has a startup method designated then it will run Autotune when powered up If no startup method is designated then the HAPSITE will show the main menu at startup If Autotune runs and completes the Autotune OK message will appear Click OK See Figure 5 3 If Autotune fails refer to Sect...

Page 163: ...rder to heat up the system and run a tune check which takes 20 minutes total a method must be selected Once the method is selected the HAPSITE will automatically heat up and run Autotune Figure 5 4 shows the icons needed to access the software and to run a method Figure 5 4 Software Icons and Setup Page ...

Page 164: ... Run Method icon A dialog is displayed to choose the type of method to run This example is a GC MS run so double click the GCMS folder See Figure 5 5 NOTE Use the buttons at the top of the dialog to choose the methods on the HAPSITE Figure 5 5 Choosing the Mode of Operation ...

Page 165: ...mart Operating Manual 8 Choose a folder that matches the physical configuration of the HAPSITE In this example the Sample Loop is installed double click the Loop folder See Figure 5 6 Figure 5 6 Selecting the Physical Configuration ...

Page 166: ...ee Figure 5 7 Figure 5 7 Selecting the Air 15 Min Loop Method 10 The software will check the pressure in the gas canisters heat up all the zones run an autotune if required and make tune adjustments as necessary The process may take up to 20 minutes When it is done heating a prompt will appear to indicate the HAPSITE is ready to run a sample Click RUN ...

Page 167: ...onnection see Chapter 4 Wireless and USB 5 Plug in the mouse optional 6 Turn on the laptop 7 Double click the Smart IQ software icon 8 Double click the Run Method icon HINT If a startup method is enabled the HAPSITE will perform step 8 through step 10 9 Double click a Method Folder e g GCMS or Survey 10 Double click the desired method e g Air 15 min Loop Survey 11 The HAPSITE will now go through t...

Page 168: ...background to determine what if anything currently exists in the area For the second minute sample directly over the area of concern to see what additional chemicals are present HINT Refer to Chapter 6 Methods for additional information on the survey method 1 Open the Smart IQ software by double clicking on the icon shown in Figure 5 8 Figure 5 8 Smart IQ Icon 2 Double click the Run Method icon Se...

Page 169: ...he dialog is showing HAPSITE methods and double click the Survey folder Alternately select the Survey folder and click OK See Figure 5 10 Figure 5 10 Selecting the Survey Folder 4 Double click the Survey mth method Figure 5 11 Figure 5 11 Selecting Survey Method ...

Page 170: ... the sample probe over the sample until a peak is seen or for one minute HINT Allow the plot to return to baseline while sampling background before stopping the run CAUTION Do not place the sample probe in liquids while sampling 8 Click the Stop button to end the run This is located on the right side of the Run Method window in the Control Panel Figure 5 14 Stop Button 9 To view the data note the ...

Page 171: ...r and then look for the data file that was just run See Figure 5 16 Full instructions for data review are found in Chapter 9 Data Review HINT Remember that this is a tentative identification For a more positive identification run a GC MS method for confirmation of the results Figure 5 16 Survey Run Complete ...

Page 172: ...urvey Folder 4 Double click the Survey method 5 Wait for heaters to reach the set temperatures 6 Click the RUN button in the pop up window sample background for one minute 7 Hold the Probe over the sample for one minute or until observing a response 8 Press RUN again to stop the sampling and save the data HINT This is a tentative identification For more positive identification run a GCMS method ...

Page 173: ...must be followed by a GC MS method in order to give a positive identification of the unknown This section will describe the process required to run a sample with the sample loop installed Refer to Section 2 3 Basic Assembly on page 2 4 and Section 2 9 1 Installing the Sample Loop on page 2 26 Assumptions made are that the HAPSITE is heated up tuned and ready to go If the HAPSITE is not warmed up f...

Page 174: ...5 14 IPN 074 397 P1G HAPSITE Smart Operating Manual 3 Double click the GCMS folder on the HAPSITE See Figure 5 19 Figure 5 19 Choosing the Mode of Operation ...

Page 175: ...E Smart Operating Manual 4 Double click the Loop folder See Figure 5 20 Figure 5 20 Choosing Loop Folder 5 Double click the Air 15 min Loop method Or select the method and click OK See Figure 5 21 Figure 5 21 Selecting the Method ...

Page 176: ... the probe over the sample for the entire loopfill event CAUTION Do not place the sample probe in liquids while sampling HINT An audible sound indicates the sample pump has turned on and the word Loopfill will be displayed on the front panel in the bottom left corner Hold the probe over the sample for this entire 60 second period 8 Wait for the method to run to completion the 3 plots shown in Figu...

Page 177: ...ck the Smart IQ icon to open the software 2 Double click the Run Method icon 3 Double click the GCMS folder 4 Double click the Loop folder 5 Double click the Air 15 min Loop method 6 Wait for heaters to gain control of set temperatures 7 Click the Run button in the pop up window of the software 8 Hold the probe over the sample for the entire Loopfill event 9 Review data when run is complete ...

Page 178: ...ection 2 9 3 Installing the Tri Bed Concentrator on page 2 29 for instructions Once installed the Tri Bed concentrator must be cleaned before sampling begins NOTE The discontinued Carbopack Concentrator tube uses the same methods outlined below To install the Carbopack Concentrator tube refer to Section 2 9 4 Installing the Tenax or Carbopack Concentrator on page 2 31 1 Open Smart IQ Software by d...

Page 179: ...PN 074 397 P1G HAPSITE Smart Operating Manual Figure 5 27 Selecting GC MS Folder using the Methods Menu 4 Double click the Concentrator folder See Figure 5 28 Figure 5 28 Selecting the Physical Configuration ...

Page 180: ...ystem will raise the column temperature to 150 C which will take a few minutes When all the zones are heated the Run Method prompt will be displayed See Figure 5 30 and Figure 5 31 Figure 5 30 Heater Warm up for the 3 min Carbon Conc Cleanout Figure 5 31 Run Prompt 6 Press the RUN button This run will take three minutes to complete The progress of the run can be seen on the laptop ...

Page 181: ...eat the 3 min Carbon Conc Cleanout method until the TIC_Max number is less than 500 000 See Figure 5 33 Figure 5 32 Clean 3 min Carbon Conc Cleanout Run Figure 5 33 3 min Carbon Conc Cleanout Run Further Cleanup Required 7 When the 3 min Carbon Conc Cleanout method is completed close the Data Review Window 8 From the Setup Page on the laptop select the Run Method icon by double clicking on the ico...

Page 182: ...mart Operating Manual 9 Double click the GCMS folder See Figure 5 35 Figure 5 35 Selecting GC MS Folder using the Methods Menu 10 Double click the Concentrator folder See Figure 5 36 Figure 5 36 Selecting the Physical Configuration ...

Page 183: ...mple See Figure 5 38 Figure 5 38 Air 15 min Carbon Conc Run Prompt 13 Hold the Probe over the sample and press RUN CAUTION Do not place the sample probe in liquids while sampling 14 The sampling process takes two minutes one minute to flush the system and one minute to collect the sample The probe needs to be held over the sample for the entire two minutes while the Sample Pump is running The bott...

Page 184: ...each set temperatures 6 When prompted press RUN HINT If the TIC_Max count is less than 500 000 at the end of this run proceed to the Air 15 min Carbon Conc method If the TIC_MAX count is greater than 500 000 rerun the 3 min Carbon Conc Cleanout method 5 4 2 Quick Reference SOP Tri Bed Concentrator Method 1 The 3 min Carbon Conc Cleanout method must be run prior to this method Refer to Section 5 4 ...

Page 185: ...es a Tenax adsorbent in the concentrator Refer to Chapter 6 Methods for additional information on GC MS methods NOTE Before a GC MS can be run in this Concentrator mode the Tenax concentrator must be installed Refer to Section 2 9 4 Installing the Tenax or Carbopack Concentrator on page 2 31 for instructions Once installed the Tenax concentrator must be cleaned before sampling begins 1 Double clic...

Page 186: ...5 26 IPN 074 397 P1G HAPSITE Smart Operating Manual 3 Double click the GCMS folder See Figure 5 41 Figure 5 41 Choosing the Mode of Operation ...

Page 187: ...he 3 min Tenax Conc Cleanout mth method NOTE The system will raise the column temperature to 150 C which will take a few minutes When all the zones are heated the Run Method prompt will be displayed See Figure 5 43 Figure 5 43 3 min Tenax Conc Cleanout Warm up 6 Click the RUN button displayed in the pop up window on the laptop This run will take three minutes to complete ...

Page 188: ...an 500 000 for the concentrator tube to be considered clean If the TIC_Max number is greater than 500 000 repeat the 3 min Tenax Conc Cleanout mth method until the TIC_Max number is less than 500 000 7 Double click the Run Method icon See Figure 5 44 Figure 5 44 Software Icons and Setup Page ...

Page 189: ...5 29 IPN 074 397 P1G HAPSITE Smart Operating Manual 8 Double click the GCMS folder See Figure 5 45 Figure 5 45 Choosing the Mode of Operation 9 Double click the Concentrator folder See Figure 5 46 ...

Page 190: ...d the probe over the sample the entire time the sample pump is running from the Linepurge until the Concfill event is completed This takes two minutes NOTE The software will automatically open up a data review window as the sample is running to show the chromatogram Peaks can be identified as shown during the run See Chapter 9 Data Review for details on viewing the results CAUTION Do not place the...

Page 191: ...n 500 000 repeat the 3 min Tenax Conc Cleanout mth method until the TIC_Max number is less than 500 000 5 5 2 Quick Reference SOP Tenax Concentrator Method NOTE The 3 min Tenax Conc Cleanout method must be run prior this method Refer to Section 5 5 1 Quick Reference SOP Tenax Cleanout on page 5 31 1 Double click the Smart IQ software icon 2 Double click on the Run Method icon 3 Double click the GC...

Page 192: ...to Chapter 13 Headspace Sampling System for more information on the Headspace System Refer to Section 2 6 Headspace Sampling System on page 2 12 for assembly instructions Refer to Chapter 6 Methods for additional information on GC MS methods 1 Double click the Smart IQ icon 2 Double click on the Run Method icon 3 Double click the GCMS folder SeeFigure 5 47 Figure 5 47 Choosing the Mode of Operatio...

Page 193: ...mart Operating Manual 4 Double click the Headspace folder See Figure 5 48 Figure 5 48 Selecting the Physical Configuration 5 Double click the HSS 15 min Loop mth method See Figure 5 49 Figure 5 49 Selecting the Headspace Loop Method ...

Page 194: ...Display 7 Refer to Section 13 2 3 Loading the Wells on page 13 10 for detailed instructions and information on loading the sample vials into the wells 8 Place the headspace needle in the 40 mL vial that contains the sample Gently depress into sample vial See Figure 5 51 WARNING The headspace needle is very sharp Figure 5 51 Headspace Needle ...

Page 195: ... the Run button See Figure 5 52 Figure 5 52 Run Button 10 When prompted at the end of the run place the headspace needle in a clean empty purge vial and press Select See Figure 5 53 Figure 5 53 Purge Vial Prompt 11 To analyze the data see Chapter 9 Data Review ...

Page 196: ...on levels in the low part per billion to high part per trillion range This method is used when the Headspace Sampling System with the Sample Loop method fails to detect a chemical Refer to Chapter 6 Methods for additional information on GC MS methods CAUTION The concentrator feature is designed to enhance HAPSITE sensitivity when analyzing low concentration samples The accumulated sample VOCs are ...

Page 197: ...tor Cleanout on page 5 24 or Section 5 5 1 Quick Reference SOP Tenax Cleanout on page 5 31 depending on the type of concentrator installed NOTE Concentrator Cleanout methods require the probe to be attached 4 Double click on the Run Method icon 5 Double click the GCMS folder See Figure 5 47 Figure 5 54 Choosing the Mode of Operation ...

Page 198: ... the Headspace folder See Figure 5 48 Figure 5 55 Selecting the Physical Configuration 7 Select HSS 15 Min Carbon Conc or HSS 15 min Tenax Conc method depending on which concentrator is installed See Figure 5 56 Figure 5 56 Selecting the HSS 15 Min Carbon Conc Method ...

Page 199: ...e heated for 20 minutes prior to sampling 10 Place the headspace needle in the 40 mL vial that contains the sample Gently depress into sample vial See Figure 5 58 Refer to Section 13 2 3 Loading the Wells on page 13 10 WARNING The headspace needle is very sharp Figure 5 58 Loading the Wells 11 Press the Run button 12 Wait for method to run See Figure 5 59 ...

Page 200: ... P1G HAPSITE Smart Operating Manual Figure 5 59 Sample Run in Process 13 When prompted at end of run place the headspace needle in a clean empty purge vial and press Sel See Figure 5 60 Figure 5 60 Purge Needle Request ...

Page 201: ...e Tri Bed Concentrator on page 2 29 or Section 2 9 4 Installing the Tenax or Carbopack Concentrator on page 2 31 to install the concentrator tube 3 Follow the instructions in Section 5 4 1 Quick Reference SOP Tri Bed Concentrator Cleanout on page 5 24 or Section 5 5 1 Quick Reference SOP Tenax Cleanout on page 5 31 depending on the type of concentrator installed 4 Double click the Smart IQ icon un...

Page 202: ...S oven gently depress the headspace needle into the 40 mL sample vial 11 Wait for the method to run 12 When prompted at end of run place the headspace needle in the purge vial and press Sel 13 Review results at the end of the run 5 8 SituProbe Methods Refer to the SituProbe Purge and Trap System Operating Manual for information on running SituProbe methods ...

Page 203: ... 6 2 Survey Method Survey is used to quickly screen a location for volatile compounds The sample is drawn in through the probe and sent directly to the Mass Spectrometer bypassing the GC and providing quick response The survey mode of sample collection is also referred to as MIMS Membrane Interface Mass Spectrometry The quick response of a survey method is due to the direct flow of the sample into...

Page 204: ...ontinue to sample for up to 1 minute If the TIC count increases above 5 000 000 sample for 15 seconds and then allow the TIC graph to return to the baseline level If the TIC count increases above 10 000 000 then move back from the source or discontinue sampling Allow the TIC to return to the background level before stopping the run See Figure 6 1 Running Survey Method from the Front Panel on page ...

Page 205: ... combined spectrum selecting the appropriate mass fragments for each compound Compounds that share mass fragments cannot be run in the same standard 6 2 1 1 Creating Survey Methods for Target Compounds Collection of survey data is controlled by the method Survey methods like GC MS methods are generated or modified using the Method Editor The Method Editor is covered in detail in Chapter 11 Method ...

Page 206: ...as the file type and select OK The File selection dialog box will be displayed Locate and select the Method that was used to collect the calibration runs Use the Browse button in the Data Files section to select and open the data file collected during the calibration run This file will be used to build the target library template See Figure 6 3 Highlighting the data file and pressing the Display b...

Page 207: ...pound library The spectrum is recorded by placing the scan cursor on the response curve e g the TIC at a location that represents the concentration of the calibration standard See Figure 6 4 Figure 6 4 Placing Cursor on Response Curve at Location of Calibration Standard Figure 6 5 Grab Spectrum for Template Window ...

Page 208: ...ked to the method and can be saved using any name Additional calibration points can be added to the curve by using the Browse button to select additional data files and then processing them as described above and saving them to the library See Figure 6 6 Figure 6 6 Additional Calibration Points Additional compounds are added by following the same steps NOTE The Reset Library function is used to de...

Page 209: ...ure for a GC MS method is dependent on the HAPSITE configuration Sample Loop Refer to section 3 4 GC MS Mode with Loop on page 3 23 and section 5 3 GC MS Mode with Loop on page 5 13 for additional information on running methods with the Sample Loop Concentrator Tube Refer to section 3 5 GC MS Mode with Tri Bed Concentrator on page 3 28 through section 3 6 GC MS Mode with Tenax Concentrator on page...

Page 210: ... the SituProbe 6 3 1 Building a GC MS Method and Target Compound Library File Collection of GC MS data is controlled by the method GC MS methods are generated or modified using the Method Editor The Method Editor is covered in detail in Chapter 11 Method Editor The target compound library is built using the Calibrate Function The calibrate function is described in detail in Chapter 12 Target Compo...

Page 211: ...at control the MS and is linked to a data acquisition method Multiple Tune files can be created for specific methods requirements However the default Tune is generally all that is required The default Tune is stored on the HAPSITE as default tun The parameters set in Tune that affect the quality of the spectrum include Base Peak Gain Sets the sensitivity level of the MS Mass Axis Calibration Mass ...

Page 212: ...e will check if all parameters are within specification record the dwell statistics Baseline Threshold create a Tune report and proceed to the Run Method function If corrections are required the program will automatically make the correction measure the dwell statistics create the report and then proceed to the Run Method function Figure 7 1 through Figure 7 4 show sample screens displayed during ...

Page 213: ...rs in the MS including the emission current and focus and extractor voltages of the ionizer The Long Autotune is intended to be run when an ionizer has been replaced or the Short Autotune cannot maintain system performance The Long Autotune must be invoked from the Manual Tune program NOTE INFICON recommends the use of Short Autotune as the primary technique for auto tuning from Manual Tune ...

Page 214: ...an run Manual Tune Figure 7 6 Manual Tune Icon 3 Wait until the EM and Emission buttons in the control panel turn green then click the Short Tune icon See Figure 7 7 Figure 7 7 Short Tune Icon CAUTION Adjusting other parameters without proper training may damage the instrument 4 Allow the Short Autotune to run to completion and click OK and close the Manual Tune after receiving the message Final R...

Page 215: ...ighlighting the HAPSITE icon pressing the right mouse button and selecting Tune Reports Tune Reports are stored by default for the last 30 days The Tune Reports display offers the following functions Remove Deletes the selected report Caution no confirmation is requested Remove Older Than Will delete files older than the number of days specified Confirmation is requested before the files are delet...

Page 216: ...he front panel display select the STAT button and then Tune See Figure 7 10 Pressing the SEL key will then display the last Tune Report To scroll through the Tune Report use the up or down arrows on the keypad See Figure 7 11 Figure 7 10 Status and Tune Data Figure 7 11 Tune Report ...

Page 217: ...check IS canister pressure and expiration date Replace if necessary 2 Check reservoir pressure to ensure the reservoir pressure is at least 400 kPa Replenish if necessary by inserting a full can of Nitrogen 400 kPa 3 Rerun Autotune by restarting the HAPSITE 4 If Autotune fails again select File and click on View Tune Reports See Figure 7 12 Figure 7 12 Selecting View Tune Reports ...

Page 218: ...t Operating Manual 5 Select default tun file and press OK See Figure 7 13 Figure 7 13 Select default tun File 6 Highlight a good tune report Select Export to Tune File See Figure 7 14 Figure 7 14 Export Good Tune to Current Tune File ...

Page 219: ...PSITE 10 If the HAPSITE fails to tune after steps 1 9 have been performed see section 7 6 Performing Manual Tune on page 7 25 for information on performing a manual tune 7 5 Manual Tune Settings and Controls Manual Tune is run from the laptop computer The Manual Tune screen can be accessed by selecting the Tune icon from the System Setup screen or by highlighting the HAPSITE Icon clicking the righ...

Page 220: ...7 10 IPN 074 397 P1G HAPSITE Smart Operating Manual Figure 7 16 Manual Tune Screen CAUTION Adjusting other parameters without proper training may damage the instrument ...

Page 221: ...ct a mass peak and drag the mass peak to a different position on the mass axis Short Autotune Starts the Short Autotune function Long Autotune Starts the Long Autotune function Mass Calibration Checks and corrects the ten calibration masses for correct location within the mass range Noise Check Scans a quiet mass range no peaks to determine the electronic baseline and threshold noise level Perform...

Page 222: ...correct location within the mass range Noise Check Scans a quiet mass range no peaks to determine the electronic baseline and threshold noise level Perform Tune Checkup Runs a mass calibration and noise check Save Tune Parameters Saves the Tune File Load Tune Parameters Loads a new Tune File and restarts tuning Load Factory Defaults Loads the default tune settings from a factory tune file This is ...

Page 223: ...mass peaks on the mass axis by linear extrapolation of the digital to analog control settings Autotune Tolerances Sets the autotune tolerance for mass resolution and mass axis position NOTE The Advanced functions should only be used under the direction of INFICON Support personnel 7 5 2 1 Tune Properties Window Figure 7 19 Tune Properties Window Show Tune Parameters Displays the EM Voltage Ionizer...

Page 224: ...Peak Bounds Displays the peak centroid and the target peak width at 10 peak height Leave emission on at exit Leaves the filament and Electron multiplier on when exiting tune This should not be used except for special service procedures Turn Cal Gas on at Tune start Turns ON the Calibration gas when the tune program is started This is checked for normal operation 7 5 3 Tune Control Panel Figure 7 2...

Page 225: ...ers EM Volt Used to increase or decrease the gain of the system EM voltage should be set to a value that achieves a Base Peak Gain of between 0 8 and 2 0 Emission Current Used to optimize the ionization efficiency of the ionizer Emission Current is set to achieve maximum intensity for mass 117 Range is 100 1000 Extractor Volt Used to optimize the ionization efficiency of the ionizer Extractor Volt...

Page 226: ...n within the mass range Full Scan Switches between Full Scan display mode and Peak Scan display mode Short Auto Tune Starts the Short Autotune function Long Auto Tune Starts the Long Autotune function Noise Check Scans a quiet mass range no peaks to determine the electronic baseline and threshold noise level Tune Checkup Runs a mass calibration and noise check Zoom Enables the cursor to select a s...

Page 227: ...7 21 The Peak Scan Window and Controls 7 5 4 1 Peak Scan Window Controls Mass Adjust Enables the cursor to select a mass peak and drag the mass peak to a different position on the mass axis Zoom Enables the cursor to select a section of the peak scan window and zoom to that section Zoom Out Returns the window to the original X axis and Y axis scale Zoom Out Y axis Returns the Y axis to original sc...

Page 228: ...ing controls The Left Mouse Button LMB is used to increment by 1 shift LMB increments by 10 Ctrl LMB increments by 100 Shifts the mass peak left Increases the peak resolution Decreases the peak resolution Shifts the mass peak right Decreases the Ion energy Increases the Ion energy Zooms to a single peak scan display window ...

Page 229: ...ull Scan Window and Controls Zoom Enables the cursor to select a section of the peak scan window and zoom to that section Zoom Out Returns the window to the original X axis and Y axis scale Zoom Out Y Axis Returns the Y axis to the original scale Placing the mouse cursor on the x axis of the full scan window and pressing the right mouse button will display the Set Scan Range Window see Figure 7 23...

Page 230: ... and end mass 7 5 6 Tune and Mass Calibration Status The Tune Mass Calibration Status screen is shown in Figure 7 24 Figure 7 24 Tune Mass Calibration Status Panel The Tune Status Panel displays information pertinent to tune and can be used to change some parameters of the Tune The Tune and Mass Calibration Status Panel can be displayed with a right mouse click in the Peak Scan window or by using ...

Page 231: ... change in Ion energy value Position DAC Value Current DAC setting for mass position Scan Width Displays the points measured per AMU Min OK Target Percentage Displays the minimum target percentage required for the mass peak to meet the OK LOW criteria Min Target Percentage Displays the minimum target percentage required for the mass peak to meet OK criteria Will turn red if actual percentage is be...

Page 232: ... last Mass Calibration Tune See Figure 7 26 The Mass Calibration Status panel can be displayed by Right Mouse Button RMB click in the Peak Scan window or by using the Tune drop down menu and selecting the Mass Calibration Status Figure 7 26 Mass Calibration Status Columns can be displayed or hidden with a right mouse button click on the column headings See Figure 7 27 Figure 7 27 Mass Calibration ...

Page 233: ...lerance OK HIGH Outside of maximum value but within acceptable tolerance LOW Below minimum value needs adjustment HIGH Above maximum value needs adjustment FAILED Cannot located mas peak within window Autotune or Manual Tune is required 7 5 8 Right Mouse Button RMB Menus In addition to the functions described above the following menu items are available by pressing the right mouse button RMB 7 5 8...

Page 234: ... the EM voltage Ionizer Control Baseline Threshold and Rod Polarity settings on the Control Panel Show Mass Tune Controls Displays the mass tune controls on the mass peak scan windows Show Tune Status Panel Displays the tune status panel Show Mass Calibration Status Displays the mass calibration status control panel Control Panel Displays the control panel Properties Displays the properties window...

Page 235: ...isplays the Properties window 7 5 8 3 RMB on Y Axis Positioning the mouse cursor on the Y axis scale near the top and selecting the right mouse button will bring up a Y axis scale scroll window 7 6 Performing Manual Tune CAUTION Manual tune is a procedure that should only be attempted by experienced HAPSITE users who preferably have taken the Advanced Training course provided by INFICON Read secti...

Page 236: ...uble click on the Tune Icon See Figure 7 31 HINT Manual Tune can only be opened in Advanced User Mode Figure 7 31 Manual Tune Icon 3 Select default tun file and press OK See Figure 7 32 Figure 7 32 Select default tun File 4 Wait for the automated process of opening the tune to complete 5 Check the Base Peak Gain BPG Is the value between 0 8 and 2 0 See Figure 7 33 ...

Page 237: ... 074 397 P1G HAPSITE Smart Operating Manual Figure 7 33 Checking BPG and EM Voltage 5a If yes then the BPG does not need adjustment Proceed to Step 8 5b If no the BPG will need to be adjusted Proceed to Step 6 ...

Page 238: ...lts See Figure 7 34 7 Check the BPG value to see if the BPG is now in the range 0 8 to 2 0 7a If the Base Peak Gain is still out of range repeat Step 6 until the value comes into range 7b If the Base Peak Gain is in range continue with Step 8 8 Check the Tune and Mass Calibration Status panel to see if any of the masses are highlighted in red A red box indicates the mass is High or Low See Figure ...

Page 239: ...usting Base Peak Gain on page 7 26 2 Resolution needs to be adjusted for masses that read High or Low in the Tune and Mass Calibration Status panel Ideally the tune report should have an OK reading for all masses no red boxes HINT Resolution can also be adjusted for masses that read OK High and OK Low in the Mass Calibration Report press F5 to update the report 3 On the Tune and Mass Calibration S...

Page 240: ...ed to Step 4 and follow with Step 4c if needed See Figure 7 37 Figure 7 37 Target Percentage Low 3b If the red box is in the Max Target Percentage the Target Resolution needs to be decreased Use increments of 0 05 to make changes to the Resolution If the Target Resolution reaches 0 85 proceed to Step 4 and follow with Step 4c if needed 4 Check to see if the Resolution is in range red box has disap...

Page 241: ...y on page 7 31 See Figure 7 38 7 6 3 Adjusting the Ion Energy 1 Prior to performing this procedure follow the steps outlined in section 7 6 1 Adjusting Base Peak Gain on page 7 26 and section 7 6 2 Adjusting Resolution on page 7 29 2 Check the Actual Percentage column 2a If the Actual Percentage is above the acceptable range Red box appears to the right of the column indicating the mass response i...

Page 242: ... manual adjustments stay within the following limits 3 After making Ion Energy adjustments 3a If the red boxes no longer appear indicating the Actual Resolution is within range proceed to Step 4 See Figure 7 39 Table 7 1 Manual Adjustments Guidelines MASS IE low IE high 50 90 170 55 90 170 69 90 170 93 90 170 117 140 170 167 140 220 213 175 230 246 180 230 263 185 250 282 190 255 ...

Page 243: ...e Manual Tune procedure Proceed to section 7 6 1 Adjusting Base Peak Gain on page 7 26 If this procedure is repeated more than 2 times contact INFICON Figure 7 39 Good Manual Tune 4 Save the Tune file Click Save Tune button on the upper Toolbar See Figure 7 40 and Figure 7 41 Figure 7 40 Save Tune Button ...

Page 244: ...7 34 IPN 074 397 P1G HAPSITE Smart Operating Manual Figure 7 41 Tune Saved 5 Exit Manual Tune by closing the Tune window The HAPSITE is ready for sampling ...

Page 245: ...accessories The software controls instrument operation and runs analyses Smart IQ can also view and interpret data collected by HAPSITE Smart managing files and creating reports The Smart IQ software operates on a Personal Computer PC The main window of the Smart IQ software is called System Setup This appears as the first screen when the Smart IQ software is run See Figure 8 1 Figure 8 1 System S...

Page 246: ... Smart IQ software are the same CAUTION The most important point to remember is to always update the HAPSITE Smart software prior to updating the Smart IQ software on the computer 8 3 1 Updating the HAPSITE Smart Software The HAPSITE Smart is delivered with factory installed software These instructions explain how to upgrade that software The HAPSITE will need to be connected to the laptop compute...

Page 247: ... HAPSITE Software See Figure 8 2 Figure 8 2 Update HAPSITE Software 3 Click on My Computer to open the folder Click on the D drive or the CD drive for the laptop if different to highlight Press Open See Figure 8 3 Figure 8 3 Open the CD Drive 4 Select the HAPSITE Smart Software folder Press Open See Figure 8 4 ...

Page 248: ...der 5 Select the HAPSITE upd file Press Open See Figure 8 5 Figure 8 5 Selecting the HAPSITE upd File 6 Click OK when the prompt Update Complete is displayed See Figure 8 6 Figure 8 6 Update Complete Prompt 7 Continue with Section 8 3 2 Installing and Updating the Smart IQ Software on page 8 5 if needed ...

Page 249: ...ore performing this procedure perform Section 8 3 1 Updating the HAPSITE Smart Software on page 8 2 1 Click on My Computer Click on the D drive or the CD drive for the laptop if different to highlight Press Open See Figure 8 3 Figure 8 7 Open the CD Drive 2 Select the Setup Icon Double click to Open See Figure 8 8 ...

Page 250: ...Operating Manual Figure 8 8 Selecting the Setup Icon 3 The InstallShield Wizard will load See Figure 8 9 Figure 8 9 InstallShield Wizard 4 An installation wizard will automatically open to the Welcome Screen Select Next See Figure 8 10 ...

Page 251: ...tination folder of the Smart IQ program Select the components desired and press Next See Figure 8 11 CAUTION Do not change the destination folder for the Smart IQ program Figure 8 11 Select Components Screen 6 A prompt will appear to start copying data files press Next Copying data files will take a few minutes See Figure 8 12 ...

Page 252: ...ear asking to unzip the NIOSH Database Select Unzip See Figure 8 13 Figure 8 13 Unzip Prompt 8 A window will appear indicating the unzip was successful press OK See Figure 8 14 Figure 8 14 Unzip Success 9 Select Close on the WinZip window 10 The installation complete message will appear Press Finish See Figure 8 15 ...

Page 253: ...before proceeding to Step 11 Figure 8 15 Installation Complete 11 The Smart IQ Application window will appear containing the Smart IQ Application icon Left click on the Smart IQ Application icon and drag to the desktop to create a shortcut See Figure 8 16 Figure 8 16 The Smart IQ Application Folder 12 Close the Smart IQ Application folder 13 Close the CD Drive window 14 Installation Update is comp...

Page 254: ...or identifying VOCs contained in samples 1 Insert the NIST Installation CD into the CD Drive of the laptop 2 Select Start Run See Figure 8 17 Figure 8 17 Selecting the Run Function 3 Type D setup exe Press OK See Figure 8 18 Figure 8 18 Running the Setup exe Program 4 The welcome window for the NIST and AMDIS setup will appear press Next See Figure 8 19 ...

Page 255: ...ome Window 5 On the Setup window select Typical See Figure 8 20 Figure 8 20 NIST and AMDIS Installation Setup Window 6 Press Next See Figure 8 20 7 When prompted to choose the software destination location ensure the Install check boxes are checked for NIST and AMDIS and press Next See Figure 8 21 ...

Page 256: ...indow 8 When prompted to find and connect to user libraries make the selections shown in Figure 8 22 and press Next Figure 8 22 NIST and ADMIS Libraries 9 When prompted to select a program folder use the default shown in Figure 8 23 and press Next Figure 8 23 Choosing the NIST and AMDIS Program Folder ...

Page 257: ... existing files press Yes See Figure 8 25 Figure 8 25 Overwrite Files Prompt 12 The installation will proceed automatically lasting a few minutes See Figure 8 26 Figure 8 26 NIST and ADMIS Installation Progress Window 13 A series of setup windows will appear followed by a create program files window When the Setup Complete window appears press Finish to close the installation program See Figure 8 ...

Page 258: ...ed or used as they are 8 5 1 Locating Default Methods Right click on the HAPSITE icon to access the menu Highlight the Edit Method option and a second menu will appear On this menu the bottom choice is HAPSITE Default Method which provides access to the default methods See Figure 8 28 Figure 8 28 Finding Default Methods Clicking on the HAPSITE Default Method option will bring up a window with the ...

Page 259: ...r 15 Min Carbon Conc Basic Carbon Concentrator method 15 minute analysis time Air 15 Min Loop VOC and Chemical Warfare Agent analysis using Sample Loop 15 minute analysis time Air 15 Min Tenax Conc VOC and Chemical Warfare Agent Air Analysis using Tenax Concentrator 15 minute analysis sample time 1 minute inlet purge plus one minute sample collection HSS 15 Min Carbon Conc VOC and Chemical Warfare...

Page 260: ...nd SituProbe 15 minute analysis SP 15 Min Tenax Conc General purpose analysis for VOCs in a water matrix using Tenax concentrator and SituProbe 15 minute analysis Survey Quick analysis to determine if there are VOCs in an area by passes GC analysis time is determined by the user 2 minutes is suggested NOTE In addition to the standard 15 minute methods there are 25 minute methods for the Sample Loo...

Page 261: ...ge 8 14 to find the default methods 2 Press the Load button See Figure 8 29 3 Press the Save button at the bottom of the Method Editor Description window See Figure 8 30 NOTE The method file name is built based on the default method name with a two digit number appended e g 01 If the two digits are not desired then remove them from the file name before pressing the Save button Figure 8 30 Default ...

Page 262: ...rt Operating Manual 4 Double click the GCMS folder or Survey folder for a Survey method See Figure 8 31 HINT Make sure HAPSITE is selected at the top of the Save Method File dialog See Figure 8 31 Figure 8 31 Choosing the GCMS Folder ...

Page 263: ...ropriate folder for the method to be saved SeeFigure 8 32 HINT If using a Survey Method skip Step 5 Figure 8 32 Choosing the Concentrator Folder 6 The default name is automatically modified by Smart IQ or it can be manually renamed Press OK The method is now saved to the HAPSITE ...

Page 264: ...cations 1 Open Smart IQ From the System drop down menu select Properties See Figure 8 33 Figure 8 33 Selecting Properties from the System Drop down Menu NOTE You must be in Advanced User Mode to set up communications See Section 8 10 Access Levels on page 8 34 2 Press the HAPSITE List button See Figure 8 34 Figure 8 34 HAPSITE List Button 3 Enter the letter H followed by the last 3 or 4 significan...

Page 265: ... Port Settings List 5 Press OK on the System Properties Window See Figure 8 34 6 The newly added HAPSITE icon will now appear at the bottom of the System Setup Window If the HAPSITE appears as in Figure 8 37 then communications have been established Figure 8 37 Newly Added HAPSITE 6a If the HAPSITE icon appears with a Blue X through the icon then communication has not been fully established See Fi...

Page 266: ...nications on page 8 20 continue with Step 2 2 Press the STAT key on the Front Panel of the HAPSITE 3 Use the arrow keys to select NET The IP address of the HAPSITE will be displayed Example 10 210 4 62 255 254 0 0 Each HAPSITE will have a unique IP address See Figure 8 39 Figure 8 39 HAPSITE IP Address 4 On the laptop press Start Depending on the laptop s setup follow either Step 4a or Step 4b 4a ...

Page 267: ... Classic View 4b Click on Connect to drag the cursor over Show All Connections and click left mouse button Click on Local Area Connection See Figure 8 41 Figure 8 41 Network Connections Standard View 5 The Local Area Connection Status Window will open press Properties See Figure 8 42 ...

Page 268: ...ITE Smart Operating Manual Figure 8 42 Local Area Connection Status Window 6 In the General tab scroll down and highlight Internet Protocol TCP IP press Properties See Figure 8 43 Figure 8 43 Selecting Internet Protocol TCP IP ...

Page 269: ...n order for the system to configure communications properly Example 10 210 4 62 becomes 10 210 132 62 See Figure 8 44 Press OK Figure 8 44 Entering IP Address 8 Press OK in the Local Area Connection Properties Window to close the window See Figure 8 43 9 Communication between the HAPSITE and the laptop is now established as indicated by the HAPSITE Sensor in the Smart IQ System Setup Window See Fi...

Page 270: ... so Smart IQ will automatically recognize and communicate when a Service Module is connected using a RS 232 cable In case the COM port communication has been removed select the Add Port button shown in Figure 8 46 Figure 8 46 Port Settings in System Properties Window When Add Port is selected the window shown in Figure 8 47 will appear Select the appropriate COM port to add Select COM1 or the appr...

Page 271: ... Properties window as shown in Figure 8 48 Figure 8 48 Port List in Port Settings Tab of System Properties Press the OK button and the system will automatically establish communications with a Service Module if powered on and connected using a RS 232 cable Please refer to Section 2 7 1 Setting Up the Service Module on page 2 18 for more details ...

Page 272: ... laptop computer 8 8 Designating a Startup Method Designating a Startup Method allows the HAPSITE to autotune and automatically run a blank when started 1 Run the Smart IQ software See Figure 8 49 HINT Advanced access level required Refer to Section 8 10 Access Levels on page 8 34 for additional information Figure 8 49 Smart IQ Icon 2 Double click on the HAPSITE Sensor Icon See Figure 8 50 Figure ...

Page 273: ... Operating Manual 4 Check the box for Use Startup Method See Figure 8 51 5 Click on Browse to select a method See Figure 8 51 6 Double click on the desired method folder Example GCMS See Figure 8 52 Figure 8 52 Selecting Startup Method ...

Page 274: ...8 30 IPN 074 397 P1G HAPSITE Smart Operating Manual 7 Double click on the desired configuration EXAMPLE Loop See Figure 8 53 Figure 8 53 Method Folders ...

Page 275: ...8 31 IPN 074 397 P1G HAPSITE Smart Operating Manual 8 Double click on the desired method EXAMPLE Air 15 min Loop See Figure 8 54 Figure 8 54 Choose Method ...

Page 276: ...cted 11 Press OK to finish Refer to Figure 8 55 This method will automatically run whenever the HAPSITE is turned on 8 9 Setting the HAPSITE Time Zone Setting the HAPSITE to the correct time zone is important and is accomplished with a few easy steps 1 Open the Smart IQ software See Figure 8 56 Figure 8 56 Smart IQ Icon 2 On the System Set up Page double click on the HAPSITE Sensor Icon See Figure...

Page 277: ...ab 4 Select the correct Time Zone from the drop down list above the map 5 Press OK and restart the HAPSITE A restart is required to set the Time Zone 6 Return to the dialog shown in Figure 8 58 to synchronize the PC and HAPSITE data and time 7 Click on Set HAPSITE Date Time to PC Date Time Press OK Refer to Figure 8 58 8 The HAPSITE will be synchronized with the Date and Time of the computer ...

Page 278: ...ced user password should be set Once the password is set the password must be entered each time the Smart IQ program is restarted or whenever the access level is changed from Normal to Advanced 8 10 1 Changing Access Levels NOTE When Normal access level is selected a message will appear stating that some areas of Smart IQ will be restricted from access 1 To change the access level click on Tools o...

Page 279: ...on page 8 34 Step 3 for additional information return to the Change Access Level Window See Figure 8 60 3 Press the Change Password button See Figure 8 62 Figure 8 62 Change Password Button 4 The window shown in Figure 8 63 will appear Figure 8 63 Change Password Window 5 In order to change the password the correct existing password must be entered in the Old Password box and the new password must...

Page 280: ...ars as shown in Figure 8 64 upon initial installation Figure 8 64 Smart IQ System Setup View The screen includes various user interfaces including A menu located at the top of the window Toolbars to perform various actions A main screen which displays component connections such as HAPSITE and Service Modules connected This screen also shows the status of the selected HAPSITE or Service Module When...

Page 281: ...ted and the user Access Level selected See Figure 8 65 Figure 8 65 System Setup Main Menu 8 11 1 1 File The File drop down menu is shown in Figure 8 66 Figure 8 66 File menu selection 8 11 1 2 Functions Functions are only available when a component is selected System HAPSITE Service Module etc 8 11 1 3 System The System menu accesses Properties See Figure 8 67 Figure 8 67 System Menu ...

Page 282: ...so a choice to use large Toolbar buttons 8 11 1 6 Window Menu The window menu is a standard menu for maximizing and minimizing windows in the program 8 11 1 7 Help Menu The Help menu provides version information about Smart IQ At this time no online help is provided with the program 8 12 Software Versions for the HAPSITE and Laptop Table 8 1 Smart IQ and HAPSITE Smart Compatibility Guide Smart IQ ...

Page 283: ...n Refer to Section 3 2 6 STAT on page 3 16 to determine how to check the version of the HAPSITE Smart software installed on the HAPSITE CAUTION If possible both the laptop and HAPSITE should always have installed the most current version of the software available The chart above shows the compatibility of the Smart IQ and HAPSITE Smart software Do not try to run incompatible versions of software t...

Page 284: ...sses the NIOSH Database Accesses the AMDIS software and library Allows transfer of files between HAPSITE and Laptop Allows editing and creating methods Accesses the Service Module when attached Accesses HAPSITE Properties Accesses the HAPSITE tune program Opens the HAPSITE Front Panel display on the Laptop screen Icon Description ...

Page 285: ...e current screen to the System Setup screen Accesses Smart IQ software information Accesses the Calibrate function Accesses the ID Unknowns function Navigates through files in Data Review Navigates through peaks in search for peaks Returns to the complete full chromatogram TIC display in search for peaks Icon Description ...

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Page 287: ...w in a Reconstructed Ion Chromatogram RIC Select Scan ranges to be viewed in the TIC Zoom in out of TIC RIC Subtract backgrounds from TIC Subtract specific scans from acquired spectra Grab spectra for analysis utilizing the full NIST database program Go to AMDIS Automated Mass Spectral Deconvolution and Identification System with TIC for qualitative identification Review data file information Labe...

Page 288: ...e Data Review Feature The Data Review feature can be accessed as follows Double click the Data Review icon see Figure 9 1 or Figure 9 1 Data Review Icon Right click the HAPSITE icon The menu shown in Figure 9 2 will appear Click Data Review Figure 9 2 Data Review Menu ...

Page 289: ... 3 Data Recall Window There are three data file extensions that are available hps HAPSITE Smart data file extension hpz Compressed HAPSITE Smart data file extension acq HAPSITE 5 2 and below data file extension Once selected the Data Review screen with the requested data file will be displayed The Data Review screen divides into three sections as shown in Figure 9 4 ...

Page 290: ... selecting peaks is conducted Control Panel Window This window allows the input of masses to plot RICs for the specified mass Check Search NIST User to search the NIST library for the current spectrum Scan Spectrum Window This window displays the spectrum generated from the TIC RIC window This window will also display NIST matches if Search NIST User is checked in the Control Panel TIC RIC Window ...

Page 291: ...toolbar is shown in Figure 9 5 Figure 9 5 Data Review Toolbar Aborts a running method Start Stop a method Pause a Run in Progress Access Data File Information Page see Figure 9 6 Figure 9 6 Data File Information Page View search reports for this data file Open NIST Program Open NIOSH Database ...

Page 292: ...peak when Search for Peaks function has been run Move to next peak when Search for Peaks function has been run Returns to the full chromatogram display 9 4 RMB Menus within Data Review All functions within Data Review can be obtained by right clicking the mouse button on the appropriate window be it the TIC window the Spectrum window the RIC window or the Control Panel window 9 4 1 RMB in the TIC ...

Page 293: ...w the GC temperature profile from the method Change Plot Color Changes the color of the TIC plot Label Chromatogram Brings up a text box to label the chromatogram The label can be moved with the cursor and can be saved with the data file Scan Subtract Subtracts the current scan from the displayed RIC plots Peaks gives you the following submenu Switch to AMDIS Switches to the AMDIS program Also acc...

Page 294: ...splays current Spectrum Scan window Control Panel When checked displays the Control Panel Properties Allows access to the properties of the display 9 4 2 RMB in the Spectrum Display Window The Spectrum display is shown in the Scan Window Every time the LMB is double clicked in the TIC window a spectrum for that scan is displayed Clicking the RMB in the Scan Spectrum window will access the menu sho...

Page 295: ...Cursors Unlocks the mass cursors to change any RICs assigned to the display Spectrum Mass List Displays a report of all the masses in the spectrum Delete Masses Deletes masses from the display and for the purpose of searching the NIST library Does not delete data Grab Spectrum for Template Used for target compound methods See Chapter 12 Target Compound Methods Grab Spectrum for Calibration Used fo...

Page 296: ...ick and hold the LMB then drag the cursor to the peak area of interest or Double click the left mouse button over the peak area of interest 9 5 2 How to Use Background Subtraction Background subtraction is a key component in cleaning up spectra before attempting to search against a database such as NIST In order to obtain background spectra there are two triangles cursors one with one blue line de...

Page 297: ... Background Subtraction Figure 9 10 Original Chromatograph 1 Using the Scan Cursor select a peak of interest in the chromatograph Refer to Figure 9 10 2 Perform a manual NIST search by pressing F7 key or by checking the box in the Control Panel The search shows multiple results Refer to Figure 9 10 ...

Page 298: ...le from the lower left side of the chromatogram and drag to an area on either side of the selected peak Refer to Figure 9 11 4 The identification is now chlorobenzene with three duplications The first ID has an SI of 706 Refer to Figure 9 11 NOTE Both background subtract tools can be used if two background subtract ranges are desired ...

Page 299: ...rea Refer to Figure 9 12 1 Place the cursor on the triangle with ONE blue line B1 Click and hold the LMB then drag B1 to the location where the background should be subtracted 2 Move the cursor to the tip of the B1 marker The cursor should change to a vertical double headed arrow Holding the Left Mouse Button while moving the double headed arrow up widens or selects a range for the background Movi...

Page 300: ...e on the x axis 9 5 3 Utilizing the Range Tool The Range Tool provides the analyst the ability to average spectra over a range of scans in a given peak This is helpful when analytes are in low concentrations or to select a section of a peak when there is co elution The ability to establish a range and average the spectra within that range will allow better matches with the NIST database The range ...

Page 301: ...hold the LMB then drag R1 to the location where the scans should be averaged Refer to Figure 9 14 2 Move the cursor to the tip of the R1 marker The cursor should change to a vertical double headed arrow Holding the LMB moving the double headed arrow up widens a range Moving the arrow down narrows the range of the peak averaging The red range lines should intersect the peak sides at 50 of their hei...

Page 302: ...ct Current Spectrum Subtract the current spectrum Green Triangle from the range 9 6 Using the Zoom Function The Zoom function allows targeting a particular section of the chromatogram for a detailed view Co elution of peaks can be detected by zooming in on odd shaped peaks 9 6 1 Using the Zoom Function in the TIC RIC Window There are two ways to Zoom into a TIC RIC 1 Move the mouse cursor to the M...

Page 303: ...m in on the area selected Figure 9 16 Selecting Area to Zoom 2 Click and hold the LMB at the point in the TIC where Zoom should begin A vertical line will appear Drag the cursor to the position that Zoom should end and release LMB Place the mouse cursor within the two vertical lines the cursor will turn into a magnifying glass Click the LMB and the display will zoom in on the area selected Refer t...

Page 304: ... Function Zooming into a spectrum requires selection of the zoom buttons on the right side of the spectrum window 1 Click the zoom button and a rectangle is displayed in the spectrum window 2 Place the cursor in the middle of the rectangle until the cursor turns into a four headed arrow See Figure 9 18 Figure 9 18 Selecting Area to Zoom 3 Press and hold the LMB then drag the box to the zoom locati...

Page 305: ...when locating specific compounds in a chromatogram A RIC plot of the top 2 or 3 mass fragments can help locate the peak of interest There are two ways to display RICs Using the Control Panel window click on the Mass box type in the desired RIC mass then press the Enter key Multiple masses can be entered and displayed in the RIC plot Each RIC will have a unique color plot displayed in the RIC windo...

Page 306: ... RIC selected 9 7 1 RIC Plot to Locate Specific Compounds NOTE Before running NIST position the scan cursor over the peak of interest in the TIC plot 1 Either from the System Setup View or the Data Review screen double click on the NIST icon See Figure 9 21 Figure 9 21 NIST Icon 2 Click on the NAMES tab at the bottom of the NIST screen See Figure 9 22 Figure 9 22 NIST Names Tab ...

Page 307: ...masses 78 77 and 51 See Figure 9 24 Figure 9 24 Top 10 Masses 6 Minimize the NIST window and return to the Smart IQ Data screen displaying the TIC chromatogram 7 Enter the 3 largest peaks from the compound in step 5 in the control panel box Enter each mass number in the boxes under the Ma Mass column See Figure 9 20 8 Check the box to the left of the mass or press ENTER This will plot the mass in ...

Page 308: ...masses peaks align in the RIC plot Use F7 NIST program to confirm identification of the suspected compound See Figure 9 27 NOTE There may or may not be a peak visible in the TIC plot Figure 9 27 RIC Plot to locate Benzene Three Masses Selected 11 The compound was not detected in the unknown sample if all three masses peaks are not present or do not align together in the RIC plot ...

Page 309: ...he TIC Window the Spectrum Window and the Control Panel Window Steps required to invoke a qualitative search are 1 Click the cursor on the TIC of interest in the TIC window 2 The spectrum will be displayed in the Spectrum window 3 Press the F7 key or use the RMB to display the pop up windows as shown or check the Search NIST User box in the Control Panel window to initiate a NIST search 4 The sear...

Page 310: ...9 29 Search Results Display Additional information may be obtained by checking the boxes in the Control Panel These boxes when checked will provide information so that the NIST Match and the spectrum generated by HAPSITE Smart IQ can be compared See Figure 9 30 ...

Page 311: ...d relative intensities are displayed for the unknown spectrum 9 8 1 Searching Peaks The Search for Peaks function allows the analyst the capability to search the entire TIC for qualitative identification of each peak detected by the search function The Search for Peaks function will also integrate each peak area that meets the search criteria then give the analyst a report showing the area percent...

Page 312: ...will determine what peaks are found The Peak Search Parameters window is divided into sections of Peak Search AMDIS Libraries and Elimination Rules These can be modified to make the search as selective or as general as required Figure 9 32 Peak Search Parameters Window After the Peak Search parameters have been optimized select Peaks Search for Peaks After analysis the following will be displayed ...

Page 313: ...retention time of each peak is displayed in the TIC RIC window At the top of the TIC RIC window the black triangles mark each peak that met the search parameters To display the results select Peaks Show current search results The results screen will be displayed The results screen displays the information pertaining to each peak that met the search criteria See Figure 9 34 Figure 9 34 Results Disp...

Page 314: ...h peak in the Hits Found section to display all of the hits as per the Search Parameters NOTE When the Hits Found are displayed the hits found in the AMDIS library will have the words AMDIS displayed NIST hits do not display the word NIST From the Peaks Found screen other functions can be accessed NIST Search Setup where the libraries that NIST will use are defined Peak Search Parameters where par...

Page 315: ...ng Data Using AMDIS AMDIS is an additional program provided by NIST and can be used to analyze data generated by the HAPSITE Smart IQ AMDIS is the acronym for Automated Mass Spectrum Deconvolution and Identification System AMDIS utilizes its own databases The HAPSITE Smart IQ utilizes the HAPSITE msl AMDIS library 9 8 3 How To Access AMDIS AMDIS can be accessed by the following methods Selecting t...

Page 316: ... The results screen includes Retention Time Window Identifications Window Component Window Match Quality Window Library Tab Figure 9 37 AMDIS Results Screen This provides the results of the AMDIS data analysis and provides all the data that most analysts need If a particular analysis needs additional confirmation press the Confirm button to access the Confirm Window see Figure 9 38 ...

Page 317: ...hem 9 8 3 1 Accessing NIST from AMDIS To use the NIST database to identify a peak not identified by AMDIS 1 Highlight the peak not identified by clicking on the triangle above the peak 2 Select Analyze Add component scan to search list 3 Select Analyze Go to NIST MS Program This will place the selected component scan from the search list into the NIST program and will utilize the NIST database for...

Page 318: ...earch 9 8 4 Analyzing Data Using NIST By right clicking on the Spectrum window the NIST menu appears See Figure 9 40 Figure 9 40 NIST Menu Grab Spectrum for NIST F9 This function will grab the spectrum selected and put the spectrum in the grab file for use within the NIST program ...

Page 319: ...play delete or plot entries in a Search NIST User database 9 8 5 How to Grab Spectra Utilize the Full NIST Program The sequence of events required to utilize the full NIST program are 1 Double click on the peak in the TIC RIC window for the NIST Full Program analysis 2 Place the cursor in the Spectrum window and RMB click Select NIST Clear NIST Grabfile 3 Place the cursor in the Spectrum window an...

Page 320: ...tabase folder on the laptop and the HELP selection of either program from the Menu selection 9 9 Reporting and Printing Data Reports are generated in Data Review utilizing the HAPSITE Smart IQ software by the method that acquired the data utilizing the Search for Peaks function print a report 9 9 1 Method Generated Reports To access reports generated by the method that acquired the data being revi...

Page 321: ...ds not included in the Target Library will be identified by the AMDIS Library Qualitative Generates a report based upon searching the ADMIS library and displaying a predetermined number of matches based upon the search criteria Quantitative Generates a report based upon a calibrated Target Compound Library Results are reported in the specified units This report can be exported to Excel NOTE This w...

Page 322: ...erate a qualitative search report utilizing either the NIST database the AMDIS database or both The report is displayed as shown in Figure 9 45 Some options are Check the box that says Report as shown in the grid This will display the best match of the search in the report Export to Excel will create an Excel text file then open and display the file in Excel Print sends the report to a printer ...

Page 323: ...ST is showing Alt P Previous NIST Hit when NIST is showing F8 Switch to NIST Program F9 Grab spectrum for NIST Shift F8 Switch to AMDIS F11 Full Plot resumes chromatogram to live data or restores a zoomed area Ctrl P Print Page up Expands the Y Axis view to show twice the current max scale if it was 100 it will show 200 after it is pressed up to 800 Page down Zooms the Y Axis view to show half the...

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Page 325: ...e samples Once created and saved a Method file can be selected to run samples Method files are created and saved using the Method Editor either to a directory on the PC or to the HAPSITE hard drive To save a newly created method from the Method Editor press the Save button at the bottom of the Method Editor window The dialog window shown in Figure 10 1 is displayed Notice that the default location...

Page 326: ...ng the Create Folder button as shown in Figure 10 2 Figure 10 2 Create Folder Button To create a new folder name the new folder then open the new folder before saving the Method file Once the location and name have been chosen press OK to save the file See Figure 10 3 Figure 10 3 Entering a New Method File Name HINT The HAPSITE Smart software is case sensitive Folder names on the HAPSITE and lapto...

Page 327: ...omatically saved to the HAPSITE hard drive in a data directory under a folder named the same as the Method used to run the analysis For example in the case where a Method named Method01 was used to run the analysis the folder where files are saved for that method would be data Method01 The default naming convention for these files is to use the method name and add an underscore and 3 digits to the...

Page 328: ...ormal users do not have access to Manual Tune Refer to section 8 10 Access Levels on page 8 34 for additional information on Access Levels If Manual Tune is performed the file must be saved to the Tune folder on the HAPSITE Figure 10 5 shows a typical Manual Tune screen which is opened by selecting the Tune icon in System Setup or by right clicking on a sensor icon and selecting Tune To save chang...

Page 329: ...ut saving the tune file If saving the tune file the Save Tune File window will appear as shown in Figure 10 7 Select a Tune file name and press OK HINT It is highly recommended to always save the tune as default tun Figure 10 6 Save Changes Prompt Figure 10 7 Save Tune File Screen Once the Tune file is saved the Save Tune File and Manual Tune windows will be closed If the Tune file already exists ...

Page 330: ...or right click on a sensor and select Data Review or select a file from the Recent Files list in System Setup view The Data Review window is shown in Figure 10 9 Refer to Chapter 9 Data Review for additional information on Data Review Figure 10 9 Data Review Recall Window The window opens showing the data folder for the currently selected HAPSITE Data Files organized the same as method files Data ...

Page 331: ... click on the desired data file to open then click the OK button See Figure 10 10 which shows a data file being selected HINT Smart IQ data files are saved with a hps extension at the end of the filename Figure 10 10 Data Review Recall Window The data file is opened in the Recall window as shown in Figure 10 11 ...

Page 332: ...ecall Data window then select the appropriate file from the PC hard drive NOTE Alternately select Manage Files to copy files manage folders or delete files on either the HAPSITE or PC hard drive 10 2 Saving Files to the PC File types are created two ways either by the analyst or by the HAPSITE software when analyses are performed The list of files possible includes Method files Event Log files Dat...

Page 333: ...he dialog window below is displayed Notice that the default location to save a method file is to the HAPSITE Method files are created using the Method Editor Method files may be saved to the PC hard drive similar to the way they are saved to the HAPSITE To save Method files to the PC select the PC option as shown below in Figure 10 12 Figure 10 12 Save Method File Dialog Window PC Option Selected ...

Page 334: ...nsor icon and selecting Properties or by double clicking on a sensor or by selecting the menu item Tools Sensor Properties Select the Data Settings tab The window shown in Figure 10 14 below will appear Figure 10 14 Sensor Properties Data Settings On the Maintain Logs line of Data Settings the number of days which the log file will be saved may be changed or to save all log files created indefinit...

Page 335: ... the HAPSITE hard drive To save these files to the PC use the Manage Files dialog to transfer the files from the HAPSITE to the PC For more information on transferring files see section 10 3 Transferring Files Between the HAPSITE and PC on page 10 11 NOTE Report files are embedded in the data files so copying them to the PC is not critical 10 3 Transferring Files Between the HAPSITE and PC Transfe...

Page 336: ...ized by clicking and holding the left mouse button on the line at the right edge of the field then dragging it to resize Double clicking on the right edge of any field will size the field to fit the data Single clicking on a column heading will sort the list based on that column Folders or files may be renamed by selecting the appropriate file or folder then pressing the Rename button The rename d...

Page 337: ...ve files from the PC to the HAPSITE use the right pointed arrow see Figure 10 19 To move files from the HAPSITE to the PC use the left pointed arrow NOTE Only method files may be moved to the HAPSITE Figure 10 19 Right Pointed Arrow For Moving Files From The PC To The HAPSITE HINT New folders may be created using the Create Folder button NOTE Information about a selected file is listed in the bott...

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Page 339: ...ent can be calibrated but may also include unexpected compounds The unexpected compounds are tentatively identified by a NIST library search for which quantitation can only be approximate Before being able to quantify a compound one must develop a HAPSITE Method File to specifically target suspected compounds The information needed for each component of the HAPSITE Method File is programmed on the...

Page 340: ...ge at a time and moves through the pages in a logical sequence while allowing movement forward or back through the pages to make or review changes see Figure 11 1 Figure 11 1 Method Editor Navigation Buttons In non Wizard mode which is recommended only for experienced users all pages are available through a tab interface The Wizard mode setting is available to change through the System Properties ...

Page 341: ...e the Method Editor interface and parameters used to create a HAPSITE Method File A HAPSITE Method File can be deployed in numerous configurations however development of the complete method is done only on the PC and is then downloaded to the HAPSITE 11 2 Description Page The first page displayed in the Method Editor is the Description Page Figure 11 4 which provides selections for the Mode of Ana...

Page 342: ...aph GC and Mass Spectrometer MS to separate and analyze the sample of known and unknown compounds Compounds are tentatively identified by a library search Survey This mode uses only the Mass Spectrometer and provides an immediate response and approximate quantitation Samples flow directly to the Mass Spectrometer with no separation of gases performed by the GC ...

Page 343: ...instrument will be calibrated but may also include unexpected compounds which must be tentatively identified by a library search and for which the quantitation can only be approximate Method elements are If the HAPSITE is to operate separate from the Service Module the HAPSITE must have a NEG pump installed and activated Refer to section 2 7 Service Module on page 2 18 and Chapter 14 Service Modul...

Page 344: ...figuration certain method elements must be defined and set up procedures must be carried out The method elements are If the HAPSITE is to operate separate from the Service Module the HAPSITE must have a NEG pump installed and activated Refer to section 2 7 Service Module on page 2 18 for additional information on the Service Module The quantitation sequence method must be defined This includes the...

Page 345: ...nstrument must be calibrated to the target compounds as defined in the analyte library file See Chapter 12 Target Compound Methods 11 3 Startup Page The Startup Page shown in Figure 11 5 allows for setting the initial parameters for the HAPSITE system heaters and selection of the sample input device Figure 11 5 Method Editor Startup Page for GC MS Methods ...

Page 346: ...p Page for survey methods See Figure 11 6 HAPSITE Temperatures C Column The target temperature the system will achieve on the Column before starting data acquisition Not used for survey methods Membrane The target temperature the system will achieve on the Membrane before starting data acquisition Valve Oven The target temperature the system will achieve in the Valve Oven before starting data acqu...

Page 347: ...wn box for the Sample Input Device Options See Figure 11 7 Figure 11 7 Sample Input Device Options 11 3 1 Headspace To create a Headspace method choose the Headspace Sample Input Device This will bring up another temperature setting window for setting the headspace oven and transfer line temperature See Figure 11 8 Figure 11 8 Headspace Parameters Headspace Temperatures C Oven The target temperatu...

Page 348: ...ItuProbe or Headspace is disabled Probe The target temperature the system will achieve in the SituProbe before starting data acquisition 11 4 Inlet Page NOTE The Inlet page is not used or displayed when creating survey methods Figure 11 10 shows the default settings for the Inlet page for a GC MS Full Scan Method From this page the Inlet States GC Temperature Profiles and Run Time are integrated a...

Page 349: ...GC Temperature Profiles NOTE In the rare case that the settings cannot be automatically synchronized the incorrect cells are colored yellow as a guide to what needs correction Figure 11 10 Method Editor Inlet Page for GC MS Full Scan The only difference on the Inlet page between a GC MS Full Scan method and a GC MS SIM method is that the Run Time parameter entry is replaced with a table showing th...

Page 350: ...t Page Inlet States The basic steps when editing the Inlet States grid is that first the desired Inlet State is chosen in the Inlet State column and then the duration for that Inlet State is entered in the Duration column After the duration is entered the editor will automatically calculate and enter the Start time for the next Inlet State There is always a default Inlet component of Method this c...

Page 351: ... pull down menu in the Inlet State column Selection of an Inlet State will show the Valve States used for that Inlet State see Figure 11 13 An Inlet State of Other can be selected which allows for a custom set of Valve States to be set for that particular Inlet State See Figure 11 14 The selection of some Inlet States is dependent on hardware or desired location in time within the Method Some Valv...

Page 352: ... an Inlet State Any Inlet State can be selected from the pull down within the Inlet State column as shown in Figure 11 15 Some Inlet States are not available as the first state and some are only available after specific states have been selected Some Inlet States can be programmed to occur before Start time 00 00 which is considered the Inject event ...

Page 353: ...le compounds of interest will pass through the precolumn and onto the analytical column prior to Backflush Backflush This Inlet State sets the valves on the GC so that carrier gas is directed to the input of the analytical column and into the output of the precolumn The Backflush state provides the ability to customize the GC method so volatile compounds that pass quickly through the precolumn and...

Page 354: ...is being used ConcFill Equivalent to loopfill when a concentrator is used ConcCooldown This Inlet State provides a duration of time that lets the concentrator cool down to a desired operating temperature Line Purge This Inlet State pulls the sample through the probe and out through the exhaust vent The sample does not go through the concentrator PreDesorb PreDesorb begins the process of removing t...

Page 355: ...t 60 seconds to allow for clearing the sample line of the previous sample as well as good mixing with the Internal Standard if used SPConcFill This sets the GC valves so that the sample pump pulls the sample through the concentrator SPLoopFill This sets the GC valves so that the sample pump pulls the sample through the sample loop The recommended duration is at least 60 seconds to allow for cleari...

Page 356: ...anges to the profiles must be made by editing the Temp Ramp Rate or Hold Time and adding heater profiles 11 4 3 Use Internal Standard The selection to use an Internal Standard is available for Loopfill and LinePurge events Figure 11 17 Selection to Use Internal Standard If Use Internal Standard is checkmarked the Internal Standard will automatically be mixed at a ratio of 1 10 with the sample to b...

Page 357: ... by a solvent peak may shut down the Mass Spectrometer and stop the analysis The Run Time is calculated based on the Inlet Events and GC Temperature Profiles and is the cumulative time of the Method 11 4 5 Concentrator Selection There are three selections available for the Concentrator None Select this when no concentrator will be used with this Method Carbon Select this when a Tri Bed or Carbopac...

Page 358: ... HAPSITE which provides the MS tune parameters used with the method These parameters are updated after every successful tune The default filename is default tun If a different Tune file exists on the HAPSITE then the Browse button can be used to locate and specify the desired tune for the Method The default tun file always contains the most recent Tune parameters This page also has a Show Details ...

Page 359: ...11 21 IPN 074 397 P1G HAPSITE Smart Operating Manual Figure 11 19 Method Editor Tune Parameter Page ...

Page 360: ...11 22 IPN 074 397 P1G HAPSITE Smart Operating Manual Figure 11 20 Method Editor Tune Parameter Page Show Details ...

Page 361: ...r parameters of the Mass Spectrometer operation see Figure 11 22 The full parameter set can be assigned a Scan Set Name for easy identification if desired The Filament Delay from the Inlet Page see section 11 4 4 Scan Events on page 11 18 is also shown on the Full Scan page Changing the Filament Delay on this page may require a review of and changes to the Inlet Page ...

Page 362: ... will start to scan The starting mass can be set from 1 300 AMU NOTE Start as high as possible to decrease the scan time and collect as many scans as possible NOTE If possible avoid starting below 45 AMU There is a significant response to components of air at mass 44 and below This would add to the instrument background and make it more difficult to detect low concentrations of other compounds in ...

Page 363: ... 28 36 or in the form of a range e g 18 36 or a mixture of single masses and ranges The masses entered do need to be within the Start Mass and End Mass to be included in the Method Entry of a mass outside of the Start End Mass range will cause an error that must be fixed before the Method can be saved and run Dwell Time The Dwell Time is the length of time the Mass Spectrometer will sample data at...

Page 364: ...t for the Set can be entered Default settings for each Mass are automatically entered based on the previous Mass As the Mass list is entered the Round Trip Time is automatically calculated and entered in the Scan Sets grid The Scan Sets fields are as follows in the order recommended for editing Begin Time In minutes seconds the time at which collection of the listed masses should start End Time In...

Page 365: ... scanning for ppb level compounds Do not set this for Internal Standards because this will lower the intensity from the other masses causing loss of possible target masses Dwell This is the amount of time the mass spectrometer will sample data at each sampling point The dwell can be set from 128 µs 4000 µs 400 µs is recommended Increasing the Dwell decreases the detection limit Lead In This determ...

Page 366: ... Survey mode provides the ability to create only one Scan Set of multiple masses Refer to Figure 11 24 Scan set name A name should be created here to reference the specific set of ions being detected Timed Mode When selected allows the time of the survey method to be set to a determined length This method will run for a programmed amount of time ...

Page 367: ...sed on the Run button When the RUN button is pressed the sample pump will turn on signaling the beginning of the run Pressing RUN again will turn off the sample pump and end the sample run Scans to average This determines how many scans will be collected and averaged before the results are updated on the chromatogram ...

Page 368: ...and quantify data Calibrated libraries will need to be created in order to quantify results The setting of parameters on this page mostly govern the actions that take place during front panel operation of the HAPSITE See Figure 11 25 HINT SIM Method only allows No Search as the search option Figure 11 25 Method Editor Search Page ...

Page 369: ...antitative report to be generated at the end of a run referencing the library designated by the Library Search Parameters Qualitative Quantitative This option allows for both the AMDIS library to be searched during analysis and for the quantitation library to be searched giving results at the end of a run 11 8 1 Setting Up a Qualitative Search To set up a qualitative search the drop down menu for ...

Page 370: ...ed from the external calibration file as in Use RI Calibration Data type of analysis The internal standards are used only to insure that the instrument functioning correctly or that the sample preparation has been performed correctly The internal standards are not used to calculate retention indices RI Calibration Performance Unlike all of the previous analysis modes this is presumed to be run on ...

Page 371: ...on ranges 30 15 10 3 1 As the value for this parameter increases increasingly noisy and broad peaks are sought at the expense of analysis time and increased risk of false positives An increase in the sensitivity will extract broader peaks resulting in an increase in the extraction of smaller and noisier peaks Resolution High Medium Low Default Medium As the level of resolution goes up the program ...

Page 372: ...gure 11 30 There are several small and specific libraries in addition to the HAPSITE MSL See Figure 11 31 Many of the compounds found in these small libraries that can be detected by the HAPSITE are incorporated in the HAPSITE MSL file NOTE INFICON recommends using HAPSITE MSL HAPSITE MSL NISTEPA MSL NISTCW MSL NISTFDA MSL NISTFF MSL NISTDRUG MSL ...

Page 373: ... 11 32 Advanced Settings NOTE INFICON recommends leaving the Advance Settings at their default settings Noise Thresholding Level Refers to the minimum signal recorded Will filter out noise along the baseline Chromatogram Peak Width Forces deconvoluted peaks to have the same shape by specifying width in AMUs ...

Page 374: ... determines the interval at which AMDIS will run a search The default value for this is 100 scans Every ____ min sec The value typed into the box determines the time interval in which AMDIS will run a search End of Run If this is selected an AMDIS search will only be conducted at the end of a run 11 8 2 Setting Up a Quantitative Search When setting up a quantitative method a quantitative library n...

Page 375: ...arch Parameters Window The Peak Search section is comprised of all the elements that define a peak in the chromatogram Search Window This value indicates the time window allowed for a peak to appear 30 seconds indicates that the acceptable window for a peak is 15 seconds on either side of the expected retention time Window Expand Factor This value has a default of 0 05 This value is multiplied by ...

Page 376: ...e a peak This allows discrimination against a very broad peak Precedence Level When compared to the compound specific precedence level determines which search parameters to use the global parameters specified in Figure 11 35 or the compound specific parameters As a general rule leaving this set to 0 allows one to use specific search parameters for individual compounds as discussed in Chapter 12 Mi...

Page 377: ...op ten peaks will be displayed Keep peaks above This check box defines the percent intensity of a mass peak to be displayed on the mass spectrum 15 is generally used as the low end for intensity Maximum NIST Hits This value is the number of matches reported by NIST NOTE This section also has a Reset button which will set any changed values back to the default setting The Library Action box has fou...

Page 378: ...n be entered which will trigger an alarm The alarm can be set to be either visual or audible by using the Settings button See Figure 11 39 Figure 11 39 Setting the Alarm Report When enabled a concentration can be entered which will create a report when the critical concentration level is reached See Figure 11 40 Figure 11 40 Setting the Report There are two choices for reports the Full TIC Peak Re...

Page 379: ...ge of data in a filename format that increments with each data file stored Figure 11 41 Method Editor Data Page The following parameters can be set on the Data Page Use default filename This check box which is selected as a default allows the Method to use a default format for the data filename The default filename is a combination of the Method filename and an index which is automatically increme...

Page 380: ...a prefix which uses an underscore after the ss information The format of the date and time is yyyy is the year the data was collected mm is the month the data was collected dd is the day the data was collected hh is the hour data collection was started mm is the minute data collection was started ss is the second data collection was started Figure 11 42 Example of Date and Time Appended to the Fil...

Page 381: ...e default directory box is checked Save Data This selection is always enabled and can not be changed Data is saved to the hard drive in the folder directory shown immediately above this check box Save Data to Floppy This parameter when checked automatically saves the data file to the floppy disk drive of the HAPSITE Data is also saved to the hard drive regardless of this selection Use of this sele...

Page 382: ...gure 11 43 provides selections to show any component or all components of the Method in a text summary These selections effect both the displayed and printed information This page allows for a review of the Method settings before saving the Method to a file Figure 11 43 Method Editor Summary Page ...

Page 383: ...hod from scratch is best left to experts however custom methods can be written by modifying a default method 11 11 1 Creating a New Custom Method from an Existing Method 1 On the System Setup View double click on the Method Editor icon See Figure 11 44 Figure 11 44 Method Editor Icon 2 Choose the HAPSITE the method will be applied to and click Open See Figure 11 45 Figure 11 45 Method Editor Open ...

Page 384: ...m the Method Editor press the Save button at the bottom of the Method Editor Summary Page see Figure 11 43 The dialog window shown in Figure 11 47 is displayed Notice that the default location to save a method file is to the HAPSITE NOTE Method files can be saved to the HAPSITE only if the HAPSITE is attached to the PC Refer to section 2 3 6 Connect Laptop if desired on page 2 9 for additional inf...

Page 385: ...Selected 6 On the File Name line type a NEW file name Refer to Figure 11 48 Figure 11 48 Entering a New Method File Name 7 The file location may be changed to save in the GCMS or Survey directory or a new one may be created using the Create Folder button as shown in Figure 11 49 Figure 11 49 Create Folder Button ...

Page 386: ...template 8 Once the location and name have been chosen press OK to save the file Refer to Figure 11 48 or Figure 11 47 11 12 How to Sequence Methods Sequencing methods is very useful when a group of methods needs to be run unattended repeatedly or at timed intervals 1 From the Smart IQ system setup screen double click the Method Editor Icon See Figure 11 50 Figure 11 50 Method Editor Icon 2 Select...

Page 387: ...1G HAPSITE Smart Operating Manual 3 Type a new name for the sequenced method See Figure 11 52 NOTE Method runs i e sequence of methods use the xmth file extension 4 Click Add See Figure 11 52 Figure 11 52 Method Run List ...

Page 388: ...11 50 IPN 074 397 P1G HAPSITE Smart Operating Manual 5 Chose a method file to add to the sequence Click OK See Figure 11 53 Figure 11 53 Chose Method ...

Page 389: ...r each method This selection determines how each method in the run is started Refer to Figure 11 54 8 In the Sleep column chose for or until for each method Refer to Figure 11 54 9 In the Time column enter the desired time for the next method to start or the length of time to sleep before the next method starts Refer to Figure 11 54 10 Click Save Refer to Figure 11 54 11 Save the sequenced method ...

Page 390: ...11 52 IPN 074 397 P1G HAPSITE Smart Operating Manual Figure 11 55 Saving Sequenced Method ...

Page 391: ... used to set up or define the quantitative method The ID Unknowns function is used to process and review results from a quantitative method Quantitative results are automatically displayed on the HAPSITE front panel display after data collection The process of quantitative analysis by developing a HAPSITE method to collect the standard data This method must meet the chromatography performance requ...

Page 392: ...the dialog box to save the library Search Settings Displays the search parameter settings Conc Unit Used to input or select the concentration units 12 2 2 Data Files Browse Used to select the data files for building and calibrating the library when a data file is selected the data is listed as follows D Shows the data file reference number Data File Name Displays the data file name and path Conc R...

Page 393: ...Search Search Performs two functions depending on whether Build Edit Template or Calibrate Library is selected When Build Edit is selected the Search performs a peak detection and integration on the selected files and loads the results into the library template When Calibrate is selected search performs the calibration of the library and calculates response factors Recalculate Recalculates the pea...

Page 394: ...If using Build Edit Template the original template is lost 12 2 4 Analytes Analytes in Library Displays the analytes in the library Analytes in File Displays the analytes in the currently displayed or selected file Search Results in File If a search has been performed with Search for Analytes selected a review of the analytes detected in the file is enabled Individual analytes can then be added to...

Page 395: ...ompound name found in AMDIS NIST library or assigned by the user for the analyte CAS Shows the Chemical Abstracts Service Number for the analyte from the AMDIS or NIST library Q ION Shows the Quantitation Ion for the analyte Ret Time Show the Retention Time for the analyte Area Displays the analyte integrated quantion area Standard Designates the compound as an Analyte or an Internal Standard Conc...

Page 396: ...ss Peaks 12 2 7 Calibration Displays the calibration curve and curve statistics for the selected analyte 12 3 Definition of Terms in the ID Unknowns Control Panel Figure 12 4 ID Unknowns Control Panel 12 3 1 Method Browse Brings up the Method selection window View Edit Opens the Method editor with the current method Save Save the current Method Libraries Displays the currently saved libraries ...

Page 397: ...selected the data is listed as follows File Entry Lists the reference number for the file Data File Name List the file name and path of the selected files 12 3 3 Peak Search Search Performs a peak detection and integration on the selected files producing the quantitation report Recalculate Integrates analyte peak areas and recalculates the concentrations without performing a peak search Typically ...

Page 398: ...Data Reference list the reference to the data file that the analyte was found in Compound Shows the compound name found in AMDIS NIST library or assigned by the user for the analyte CAS Shows the Chemical Abstracts Services Number for the analyte from the AMDIS or NIST library Q ION Shows the quantitation Ion for the analyte Ret Time Shows the Retention time for the analyte Area Displays the analy...

Page 399: ...ual 12 3 6 Extracted Mass Peaks Displays the mass peaks and relative percentages for the selected analyte See Figure 12 6 Figure 12 6 Extracted Mass Peaks 12 3 7 Calibration Displays the calibration curve and curve statistics for the selected analyte ...

Page 400: ...working with RICs Reconstructed Ion Chromatograms and Mass Spectra Data Review is described in Chapter 9 Data Review Additional features are described below Figure 12 7 Calibration Display See Figure 12 8 With the Build Edit Template option selected in the Calibrate screen the Display button will show the peaks detected and selected for the library template when a peak search is performed Peaks se...

Page 401: ...late After selecting the Spectrum for the compound to be added place the cursor in the mass spectrum window and click the right mouse button to open up the spectrum pop up menu Select the Grab Spectrum for Template menu option Figure 12 8 Calibration Display ...

Page 402: ...tes to be quantified If practical prepare all standards in a single sample If not the template library can be built from multiple files If possible prepare standards for multi level calibration by serial dilution Analytes can be prepared at the same concentration for all compounds or at different concentrations When using individual concentrations an initial concentration of each analyte must be e...

Page 403: ... Data File Information page See Figure 12 10 Figure 12 10 Data File Information Page NOTE In this example a series of standards at four concentration levels were prepared by serial dilution The method QuantExample was used to collect the data Start with one method for collection and continue with that method These are arbitrary concentrations for example only and NOT actual concentrations QuantExa...

Page 404: ...ed GC MS or Survey See Figure 12 12 NOTE Methods can be built for Full Scan data or SIM Selected Ion Monitoring data Best practice is for the Select Method First box to be checked as the library is linked to the method Figure 12 12 Selecting the Type of Quantitative Method 3c Click OK 3d The Method File window will be displayed Select the method which will contain the library This will open the Ca...

Page 405: ...e concentration units 6 Select the Concentration field and enter the concentration of the standard The Concentration reference should be set to Global 7 Check the selection box 8 Make sure the Build Edit Template button is selected and then select Start The data file will be processed and the detected compounds displayed Peaks are detected according to the Search Settings The library template will...

Page 406: ...igure 12 16 HINT Only keep one entry for each compound In this example the Internal Standards and the compound of interest are repeated multiple times Delete the duplicate entries Figure 12 15 Right Mouse Button in Calibration Control Panel Select the right mouse button The options available are Duplicate Row Creates a duplicate entry for the highlighted row Fill down Replaces the contents of all ...

Page 407: ...the compound to be quantitated The software always selects the largest mass fragment in the spectrum as the quant Ion To change the quant ion highlight the field and type in the new number Change the quant Ion for TRIS from 213 to 75 The software will warn that a re calibration is required This is true if a quant ion is changed after calibration To signify which quant mass is being used change the...

Page 408: ...c multiplication factor entered in the Conc Factor field in the Data Files control panel Figure 12 17 Extracted Mass Peaks 9e The Extracted Mass Peaks can also be edited to delete mass fragments with intensities below 15 The exception would be a molecular ion if the fragmentation pattern is not very distinct To delete unwanted mass fragments highlight the field and press the delete key Refer to Fi...

Page 409: ...ss the Start button under Peak Search 11c Review the curves for each analyte To review each analyte select the Calibration tab and use the mouse to select each compound See Figure 12 20 Figure 12 20 Calibration Curve 11d Additional calibration points can be added to the curve at any time by using the Browse button under Data Files First add the data file Select the data file added and make sure th...

Page 410: ...mpounds by selecting the Quantitative tab of the report 12 7 Using the ID Unknown Function Files can be reprocessed on the laptop using the ID UNKNOWNS function 1 The ID Unknowns function can be accessed from the Function drop down menu by clicking the right mouse button on the HAPSITE icon by the toolbar or via the Status icon and Function tab See Figure 12 21 HINT The ID Unknowns function is ver...

Page 411: ...method to be used to process or re process the data After a method is selected the ID Unknowns control panel will be displayed 3 Use browse to select the data file s 4 Select Start to reprocess the data 5 View results See Figure 12 23 Figure 12 23 Quantitation Report ...

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Page 413: ...pounds in air so samples must be introduced in a gas phase HSS technology involves heating samples of soil or water in a closed sample container to a known temperature Heat forces the volatile components to partition between the sample and the headspace above the sample After allowing sufficient time for equilibration to occur a portion of the headspace now containing volatile compounds from the s...

Page 414: ...ow Diagram Two three way valves direct the flow to either bypass the vial in the position shown or purge through the vial While a sample is being transferred to the HAPSITE the flow is directed through the long needle below the surface of the sample The nitrogen flow into the vial is approximately balanced by the HAPSITE s sample pump flow out of the vial The headspace sample is transferred to the...

Page 415: ...Limit toluene 5 µg liter Mounting Requirement Upright 15o 13 1 3 HSS Indicators The HSS has three indicators in the left side of the front panel and under the label Headspace Sampling System When illuminated these indicate POWER RMT PWR and LO BAT The left and center indicators are green when illuminated while the right is red when illuminated POWER When the left indicator is illuminated the HSS p...

Page 416: ...m length to ensure a proper fit in the HSS sample heating block A proper fit allows the sample heating block to most effectively heat the samples Supelco Inc 800 247 6628 offers clear glass vials of this size with PTFE silicone septa and open top phenolic closures The vials are Supelco part number 2 7180 box of 100 Water Water is used for syringe cleaning blank analysis calibration standard prepar...

Page 417: ...APSITE s AC to DC power converter Connect one connector of the Y cable to the HAPSITE s power connection and connect the other connector to the back of the HSS Then connect the two cable connector to the output line of the AC to DC power converter Finally plug the AC to DC power converter into the AC power outlet NOTE Do not use the Y cable to power two HAPSITE instruments HINT If the HAPSITE is n...

Page 418: ...h Headspace Sampling System and Sample Loop in Portable Mode on page 3 36 and section 3 8 GC MS Mode with Headspace Sampling System and Concentrator in Portable Mode on page 3 40 for the standard operating procedures to run samples with the Headspace Sampling System 13 2 2 Loading the Vials Loading of vials is accomplished in a manner which best preserves the integrity of the sample The HSS works ...

Page 419: ... a gloved finger See Figure 13 4 Carefully transfer the sample into the sample syringe Figure 13 4 Transferring the Sample into a Sample Syringe NOTE The 40 mL sample vials are intended for one time use only and should be discarded properly when finished 5 Adjust the amount of sample in the sample syringe to 20 mL while removing the air bubble See Figure 13 5 WARNING Do not insert a vial which is ...

Page 420: ...thin the analysis as compared to Internal Standards These compounds are also injected into the sample at a consistent known concentration similar to the Internal Standard Surrogates are also chosen to avoid interference with compounds in the sample Surrogates are reported as recovery values in percent compared to expected response value 6a Rinse the 10 L syringe with cemented needle pictured in Fi...

Page 421: ... discard the methanol from each rinse rinse once with the calibration mixture discard this as well Inject the desired amount of the calibration mixture through the small end of the sample syringe to complete the calibration standard The following is a set of examples for amounts of standard mix at 200 and 2000 g mL to be injected into 20 mL of water to achieve the stated concentrations See Table 1...

Page 422: ...Uncap a new sample vial tilt the vial and transfer the sample from the sample syringe taking care to avoid aerating bubbling in the sample Cap the sample vial tightly See Figure 13 7 Figure 13 7 Transferring the Sample to a 40 mL Vial 7 Label the vial with the appropriate information 13 2 3 Loading the Wells This section describes the procedure for loading a sample into the well of the HSS 1 Open ...

Page 423: ...o allow for sample expansion during heating Failure to leave an airspace in the vial may result in failure of the vial and or personal injury Do not fill the vial with more then 20mL of liquid 2 Pull up on the needle assembly while grasping each side between the thumb and forefingers Swivel the needle assembly left or right as needed to expose a free path to the sample well 3 Insert the vial plast...

Page 424: ...ple wells allow rotation of samples during analysis for equilibrium times which are longer than a single sample run time Cycling the vials to achieve the desired equilibrium time Insert the first sample after the HSS sample heating block has reached the setpoint temperature Allow the sample to equilibrate for the desired time as determined when the calibration analyses were performed and continue ...

Page 425: ...Clean Out after a High Concentration Sample When high concentration samples are analyzed using the HSS the system can retain analytes which will be detected if the next sample has low levels of those compounds This is typically referred to as a carry over contamination Carry over contamination can be reduced to approximately 0 1 by using Purge In the case of severe carryover use the Flush function...

Page 426: ...ne from the HAPSITE but leaving the line connected to the HSS Once the Transfer Line to the HAPSITE is disconnected press the FLUSH switch inside the front panel of the HSS see Figure 13 9 This will pass nitrogen through the system while heating the sample well to 80 C The length of time the flush will need to operate will depend on the level of contamination NOTE The Flush function will continue ...

Page 427: ...avoid injury HINT When cleaning the wells position the needle assembly inside a well not currently being cleaned Use this as a precaution against possible injury from the sharp needle point of the assembly To remove liquids roll a paper towel or cloth into a tube shape which will fit easily into the well insert twist and remove Loose debris may be removed by turning the HSS upside down with the to...

Page 428: ...urce before continuing WARNING Be careful to avoid burns if the surfaces are still hot WARNING The needle tip is sharp be careful to avoid injury 1 Disconnect the HSS from the external power supply 2 Remove the battery 3 Remove all vials from the HSS heater wells be careful of the sharp needle 4 Disconnect the transfer line at the back of the HSS 5 Close access doors 6 Install the plugs 7 Wash the...

Page 429: ...ting that communication is lost Replacement should be performed between sample runs and in a dry and non hazardous environment since the front door must be opened 1 Open the front door and turn off the HSS by pressing the POWER switch located behind the front door HINT The HAPSITE and laptop if connected will display a message that communication has been lost 2 Hold the HSS instrument in place and...

Page 430: ...Remove the plastic protective cap from a new Nitrogen Canister and insert into the canister slot 5 Press and hold the black release tab while pushing the Canister until the canister stops then release the tab The canister should be snug and locked in place WARNING Do not re fill the canisters after use These canisters are disposable and not designed for re filling Canisters may fail upon refilling...

Page 431: ... inside the front door Insert the battery to be charged into the battery compartment with the lettering right side up until the battery is engaged Leave the HSS power on until the battery is fully charged The battery should take approximately 12 hours to fully charge The approximate level of the battery s charge can be monitored by pressing the TEST button on the battery The battery level is indic...

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Page 433: ...Roughing pump and Turbo pump The Roughing pump has a two or four stage design depending on the version The newer version of the Rouging pump has four stages Each stage of the Roughing pump has a rubber diaphragm which is pushed against a smooth plate several times a second in order to remove air through small holes in the plate The Roughing pump is sometimes referred to as a Diaphragm pump The Rou...

Page 434: ...r models With the exception of input power both models are identical 14 2 1 Service Module 110 220 V ac Input The 110 220 V ac model operates from 110 220 V ac line voltage See Figure 14 1 Figure 14 1 Service Module 110 200 V ac Version 14 2 2 Service Module 24 V dc Input The 24 V dc model operates from an external 24 V dc power supply See Figure 14 2 Figure 14 2 Service Module 24 volts ...

Page 435: ... the same controlled shutdown procedure Backup batteries are kept charged whenever the Service Module is powered 14 3 2 MDP Turbo Pump The Molecular Dispersion Pump MDP also known as MDP Turbo Pump provides high vacuum to the HAPSITE Manifold The top speed is 1500 hertz 90 000 RPM This is controlled by the MDP Turbo Pump controller which is controlled by the Service Module Processor The pump is lu...

Page 436: ... minutes for a dry system to several hours in extreme cases The TMP indicator on the Service Module display will light up ACCL accelerate when the MDP Turbo Pump is accelerating and NORM normal when the MDP Turbo Pump has reached 1480 hertz 14 3 5 Roughing Pump The Roughing Pump is a diaphragm pump During normal operation this pump will evacuate the foreline to about 3 Torr This pump is not design...

Page 437: ...t supplied to the electrical connector at the top of the Service Module unless the Analytical Module is connected The 24 V dc Service Module IPN 930 202 G3 utilizes the external 24 V dc power supply to power the Service Module and Analytical Module 14 3 9 Communications Communications to the Service Module are made through the electrical connector on the top of the instrument This is a RS485 commu...

Page 438: ... is shown in Figure 14 3 Figure 14 3 Service Module Front And Top View The Service Module is used to change NEG pumps quickly without sending the HAPSITE back to the INFICON Service Department WARNING To avoid personal injury maintenance personnel should obtain proper maintenance training before attempting to install and activate a NEG pump an alternative or backup method to using a NEG pump to pr...

Page 439: ... on the Service Module icon See Figure 14 4 Figure 14 4 Service Module Icon Double click on the Status icon Click on the Service Module Tab See Figure 14 5 Figure 14 5 Status Icon Click on the Sensor icon with the right mouse button Click on Properties with the left mouse button Click on the Service Module Tab See Figure 14 6 Figure 14 6 Accessing Service Module in Smart IQ from the HAPSITE Sensor...

Page 440: ...etach Used to release the vacuum between the Service Module and the HAPSITE before the physical removal Vacuum is maintained in the Mass Spectrometer Attach Used to create the vacuum between the HAPSITE and Service Module and within the Mass Spectrometer after physically connecting Pump Down SM Used to place the Service Module in storage Vent SM Used to take the Service Module out of storage ...

Page 441: ...splays control information See Figure 14 8 Figure 14 8 Configure Window Manual Displays additional control information See Figure 14 9 Figure 14 9 Manual Control Window Ion PumpStatus Displays the Ion Pump Status See Figure 14 10 Figure 14 10 Ion Pump Status Window ...

Page 442: ...atus items are reported Supply Volts V The voltage being supplied to the HAPSITE normally about 24 UPS Battery V The Uninterrupted Power Supply UPS voltage nominally 24 V Battery Level Displays the charge percentage of the HAPSITE battery inserted in the battery compartment of the Service Module as a percentage of the nominal design capacity Displays No Battery if a battery is not present Board Te...

Page 443: ...f the Service Module must be moved and the HAPSITE is Attached Turbo Pump is running first Detach the HAPSITE See section 14 8 Detaching the HAPSITE on page 14 17 Before turning on power to the Service Module refer to section 2 7 Service Module on page 2 18 for the physical setup instructions Power for the HAPSITE is provided through the Service Module as long as the Service Module is connected to...

Page 444: ...lves placing or docking the HAPSITE on the Service Module CAUTION Before attaching the HAPSITE to the Service Module the NEG pump must be cooled overnight to allow the NEG Pump to reach room temperature If the Service Module has been in storage refer to section 2 7 Service Module on page 2 18 before proceeding The HAPSITE must be turned on before proceeding refer to section 14 6 Starting Up HAPSIT...

Page 445: ...n the desired HAPSITE sensor then double click the Service Module icon shown in Figure 14 14 Figure 14 14 Service Module Icon in System Setup View after Selecting HAPSITE Sensor Double clicking on the Service Module icon will open the Service Module tab in the HAPSITE Properties window as shown in Figure 14 15 Figure 14 15 Service Module Tab Selected in HAPSITE Properties Window In the Service Mod...

Page 446: ...gin to speed up as shown on the Turbo Speed Hz line in Figure 14 15 above initially listed as 0 NOTE The attach procedure typically takes about 5 minutes to complete After selecting the Attach button the HAPSITE Properties window can be closed at any time Figure 14 17 Attach In Process Figure 14 18 Attach Successful ...

Page 447: ...ready at the main menu repeatedly press the ESC key until the HAPSITE Main Menu is displayed Figure 14 19 HAPSITE Front Panel Main Menu Listing Menu Item 3 Service Module The resulting screen shown in Figure 14 20 has two options 1 Attach SM and 2 Detach SM Figure 14 20 Service Module Screen on HAPSITE Front Panel Display Select 1 Attach SM The screen shown in Figure 14 21 will appear asking to co...

Page 448: ...rm Screen The current status of the system will be displayed and updated as shown in Figure 14 22 Figure 14 22 Attach HAPSITE Status Once the Attach SM operation has completed the system will show the Attach HAPSITE successful screen shown in Figure 14 23 Figure 14 23 Attach HAPSITE Successful ...

Page 449: ...o connect the HAPSITE to the laptop using an ethernet cable before continuing Refer to section 2 3 6 Connect Laptop if desired on page 2 9 if a connection needs to be made In the Smart IQ software left click on the HAPSITE sensor to detach then double click the Service Module icon shown below in Figure 14 24 Figure 14 24 Service Module Icon Double clicking on the Service Module icon will open the ...

Page 450: ...ing the Detach button and selecting Yes on the confirm window the HAPSITE Properties window can be closed Figure 14 28 Detach Successful NOTE To place the Service Module in storage see section 14 10 Storing the Service Module on page 14 22 14 8 2 Using the Front Panel Display to Detach On the HAPSITE Front Panel main menu select 3 Service Module as shown in Figure 14 29 HINT If not already at the ...

Page 451: ... options 1 Attach SM and 2 Detach SM Figure 14 30 Service Module Screen on HAPSITE Front Panel Display Select number 2 Detach SM The screen shown in Figure 14 31 will appear asking to continue the Detach Select 1 Yes to continue with the detach Figure 14 31 Service Module Detach Confirm Screen The current status of the system will be displayed and updated as shown in Figure 14 32 ...

Page 452: ... Detached screen shown in Figure 14 33 Figure 14 33 Service Module Detached To place the Service Module in storage see section 14 10 Storing the Service Module on page 14 22 14 9 Physically Removing the HAPSITE from the Service Module The HAPSITE cannot be physically removed from the SM until a Detach SM has been performed Refer to section 14 8 Detaching the HAPSITE on page 14 17 before physically...

Page 453: ...ce Module release the latches on each side of the Service Module HINT To continue using the HAPSITE place a charged battery in the HAPSITE or connect exterior power before removing the HAPSITE from the docked position on the Service Module Remove the HAPSITE from the Service Module by lifting the HAPSITE straight upward off of the Service Module Once the HAPSITE is undocked replace the yellow plas...

Page 454: ...proceeding HINT The HAPSITE is considered Attached if the HAPSITE is docked on the Service Module and the Turbo pump is running at a speed greater than 0 Hz Clean any debris or dust from the black rubber o ring using a lint free wipe This will help ensure that a good seal to the aluminum storage plug is achieved allowing the system to maintain vacuum more effectively See Figure 14 35 shows the o r...

Page 455: ...232 communication cable is connected to the Service Module and Laptop If the RS 232 communication cable is not attached refer to section 2 7 1 Setting Up the Service Module on page 2 18 before proceeding The Service Module must be pumped down Open the Smart IQ program Double clicking on the Pump Down icon will start the pump down process as shown in Figure 14 37 Figure 14 37 Service Module Pump Do...

Page 456: ...dure turns on the Roughing pump for sixty seconds to create a partial vacuum sealing the aluminum storage plug in place Figure 14 39 Pump Down Service Module Delay Screen After the pump down is complete place the yellow protective cover on top of the Service Module aluminum storage plug as shown in Figure 14 40 Figure 14 40 Yellow Protective Cover Placed Over Aluminum Storage Plug on Service Modul...

Page 457: ...own the pumps properly in case of a sudden loss of supplied power This happens automatically in order to preserve the vacuum in the HAPSITE Mass Spectrometer manifold and to protect the Service Module pumps from being damaged When power is restored the HAPSITE and Service Module will need to be attached again before the Service Module will provide proper vacuum for the HAPSITE Refer to section 14 ...

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Page 459: ...nsumables Additionally the HAPSITE checks the system components each time start up is performed and will notify the user if the following items need to have maintenance performed Turbo Pump usage hours Service Module Roughing Pump usage hours Service Module Ion Pump usage hours HAPSITE NEG Pump usage hours HAPSITE For Turbo Pump Roughing Pump and Ion Pump maintenance service must be performed by a...

Page 460: ...hould occur drop the pump into a bucket of sand and cover with more sand If this is not practical set the pump on its black plastic base on a non flammable surface The NEG pump will burn out in a few minutes WARNING Risk Of Electric Shock Whenever accessing the internal components of the Service Module always disconnect the power cord and remove the battery to reduce the danger of electrical shock...

Page 461: ...tively large 10 to 20 of peak 28 2b Locate the leak source and repair 2c Turbo molecular drag pump or diaphragm backing pump may need servicing 2c Check turbo speed in the Service Module program Service pumps if speed is less then 1480 rps and there are no air leaks 2d NEG is depleted 2d Replace NEG pump Using INFICON part 930 425 P1 See section 15 7 on page 15 15 3 Electron Multiplier fault messa...

Page 462: ...rnal power supplies 6c Contact Customer Support see Chapter 17 7 Mass spectrum drift with time Both in resolution and position 7a Thermal problem on the high voltage Rf board 7a Contact Customer Support see Chapter 17 8 Instrument turns on but fails to boot properly 8a CPU or hard drive failure 8b Contact Customer Support see Chapter 17 9 Pressure to high to read error message at user interfaces 9...

Page 463: ... canister if low 13 Temperature zones read 99 8 oC or higher 13a Component in the zone is hot 13a GCC card has problem and temperature zone has run away Contact Customer Support see Chapter 17 13b If zone is relatively cold to touch 13b Sensor could be bad Contact Customer Support see Chapter 17 14 Unable to read memory chips on gas canister 14a Poor connections or damaged contact 14a Try re seati...

Page 464: ...mber 930 432 P6 20 Leaking carrier or internal standard canisters while installed in the HAPSITE AM 20a Contact Customer Support see Chapter 17 21 Elevated chromatogram baseline 21a HAPSITE is contaminated 21a See section 15 5 Contamination on page 15 7 21b Improper baseline and threshold settings 21b Set baseline and threshold in tune 22 Higher than normal base pressure 22a System could be contam...

Page 465: ...nsure dust moisture oils or other contaminants are not permitted to enter the Mass Spectrometer manifold CAUTION Be especially careful not to touch the inside surfaces of the manifold with bare hands The natural oils on even clean hands will produce an interfering background signal on the HAPSITE s sensitive detection system The use of cotton gloves is required when handling any part of the manifo...

Page 466: ...ontamination will not go away after a full day of pumping the suspect component must be removed and replaced Remember care must be taken when handling internal components of the vacuum system Always use new gloves or a clean lint free cloth to avoid contact with skin oils 15 5 2 Contamination of the Gas Chromatograph Contamination of the Gas Chromatograph GC can occur if hot heavy organic gases ar...

Page 467: ...y Mode or a persistent peak in GC MS Mode possibly a carryover from a previous sample 15 5 3 2 Decontaminate 1 Remove the probe from the HAPSITE 2 Hold the probe and probe line in a U shape 3 Holding the probe pour methanol from a squeeze bottle in the probe nut until methanol is visually seen coming out of the probe line through the lemo connector WARNING For safety precautions wear nitrile glove...

Page 468: ...ethanol remaining in the probe line by tipping one end of the probe line downward until all of the methanol drains from the probe line See Figure 15 3 Figure 15 3 Empty Methanol from Probe and Probe Line 6 Blow out the probe line with Nitrogen to remove any residual methanol that may be left in the probe line See Figure 15 4 ...

Page 469: ...6 NEG Troubleshooting If an MS Pressure Warning message is received on the Front Panel of the HAPSITE or on the laptop see Figure 15 5 go to the PRES option under the STAT menu or to the Service Module Tab in the Properties menu on the laptop in Smart IQ to check the MS Pressure See Figure 15 6 and Figure 15 7 Figure 15 5 MS Pressure Error ...

Page 470: ... 3 order a new NEG Pump If the MS Vacuum Pressure is 6E 3 replace the NEG Pump NEG pumps have an expected life of approximately 150 hours If the NEG Pump has 70 hours or less consider trying a bakeout formerly called Reactivation to extend the NEG Pump s life To check the NEG Pump hours used go to the NEG Status tab on the Properties menu HINT If the NEG Pump has less than 150 hours a bakeout or r...

Page 471: ...mp to 700 degrees Centigrade for a specified length of time usually 2 hours 1 Click on the Service Module tab of the Properties menu 2 Click on the Service button See Figure 15 8 Figure 15 8 Service Button on the Service Module Tab 3 Set the Bakeout Power to 30 The Bakeout Time is usually set to 2 hours Refer to Figure 15 9 Figure 15 9 Service Window 4 Click the Bakeout button ...

Page 472: ...ally the same as activating a new NEG pump Refer to section 2 7 Service Module on page 2 18 for more information on setting up the Service Module 1 Click on the Service Module tab of the Properties menu 2 Click on the Service button See Figure 15 10 Figure 15 10 Service Button on the Service Module Tab 3 Use the Activate NEG settings below as a guideline except change HAPSITE Pumpdown Time to 180 ...

Page 473: ...y of the HAPSITE after completing the boot up routine Replacement of the NEG should be considered at that time NEG Pump removal installation and activation should be performed in the following order Part 1 NEG Pump Removal section 15 7 2 on page 15 17 Part 2 Service Module Vacuum Interconnect VI Valve Cleaning section 15 7 3 on page 15 22 Part 3 Install the New NEG Pump section 15 7 4 on page 15 2...

Page 474: ...op computer New NEG Pump 1 4 Allen wrench Torque wrench set for 70 inch pounds gloves cotton or latex lint free wipes methanol MicroDuster III containing 1 1 1 2 tetrafluoroethane CAUTION Wearing safety glasses and gloves wipe all tools with methanol before starting this procedure Figure 15 12 Required Tools and Equipment ...

Page 475: ...he Service Module 2 If the NEG Pump is hot from recent use let the system cool overnight before performing this procedure The NEG Pump should cool to below 60o C before proceeding WARNING Do not bypass this cool down step 3 Vent the HAPSITE by choosing Vent HAPSITE on the Service window of the Service Module tab in the Properties window see Figure 15 13 or from the Front Panel by selecting System ...

Page 476: ...15 18 IPN 074 397 P1G HAPSITE Smart Operating Manual Figure 15 13 Vent HAPSITE from Smart IQ Software ...

Page 477: ...G HAPSITE Smart Operating Manual Figure 15 14 Vent HAPSITE from the Front Panel NOTE If the HAPSITE is not attached to the Service Module an error message will be displayed and the process will not proceed See Figure 15 15 ...

Page 478: ... pressure while hot If this should occur drop the pump into a bucket of sand and cover the hot NEG Pump with more sand If this is not practical set the pump on its black plastic base on a non flammable surface The NEG Pump will burn out in a few minutes 4 When the screen shows Vent Manifold Has Been Completed unplug the NEG Pump s black cable from the inside of the front panel by loosening the loc...

Page 479: ...HINT The aluminum gasket can not be reused Bend the old gasket to avoid possible reuse Place the USED sticker which came with the new NEG Pump on the old NEG Pump Follow the instructions provided with the new NEG Pump to return the used NEG Pump CAUTION Gloves must be worn while performing all of the following steps 8 Continue with section 15 7 3 Part 2 Service Module Vacuum Interconnect VI Valve ...

Page 480: ...nnect VI Valve Cleaning 1 Remove the HAPSITE from the Service Module see section 14 9 Physically Removing the HAPSITE from the Service Module on page 14 20 2 On the underside of the Analytical Module remove the VI valve using the 1 4 Allen wrench See Figure 15 17 Figure 15 17 Removing the VI Valve ...

Page 481: ...15 23 IPN 074 397 P1G HAPSITE Smart Operating Manual 3 Wearing safety glasses and gloves clean the o ring on the VI valve with methanol See Figure 15 18 Figure 15 18 Cleaning VI Valve O ring ...

Page 482: ...15 24 IPN 074 397 P1G HAPSITE Smart Operating Manual 4 Clean the bottom of manifold where the VI valve was removed with methanol See Figure 15 19 Figure 15 19 Cleaning Bottom of Manifold ...

Page 483: ...15 25 IPN 074 397 P1G HAPSITE Smart Operating Manual 5 Replace the VI valve into the bottom of manifold Hand tighten See Figure 15 20 Figure 15 20 Replacing the VI Valve ...

Page 484: ...Figure 15 21 Cleaning O ring on the Service Module 7 Place the HAPSITE on the Service Module and lock down with the black side latches Refer to section 2 7 2 Placing the HAPSITE on the Service Module on page 2 23 for additional instructions if needed 8 Continue with section 15 7 4 Part 3 Install the New NEG Pump on page 15 27 ...

Page 485: ...mp 1 Wearing safety glasses and gloves clean the manifold flange with methanol on a lint free wipe See Figure 15 22 Figure 15 22 Cleaning Manifold Flange 2 Remove the new NEG Pump and aluminum gasket from the shipping container See Figure 15 23 Figure 15 23 New NEG Pump and Aluminum Gasket ...

Page 486: ... edges on the inner ring get nicked See Figure 15 24 Figure 15 24 Cleaning Aluminum Gasket 4 Remove the new NEG Pump from the protective container See Figure 15 25 CAUTION The NEG Pump is stored under a vacuum in Nitrogen environment The shelf life is 5 years If the vacuum is compromised the shelf life is reduced to 1 year HINT Remove the o ring and seating ring assembly from the new NEG Pump ...

Page 487: ... 15 26 Cleaning Flange with Methanol 6 Save the rubber O ring assembly and container to dispose of the old NEG Pump 7 Place the new aluminum gasket on the new NEG Pump See Figure 15 27 HINT Inspect the manifold face ionizer and manifold inside for nicks residue and scratches HINT Write down the Serial Number of the New NEG Pump O ring and seat ing ring assembly ...

Page 488: ... IPN 074 397 P1G HAPSITE Smart Operating Manual Figure 15 27 Aluminum Gasket on NEG Pump 8 Insert the new NEG Pump and aluminum gasket into the manifold See Figure 15 28 Figure 15 28 Installing New NEG Pump ...

Page 489: ... the torque wrench and tighten to 70 inch pounds or 8 Nm See Figure 15 29 Figure 15 29 Torquing Chain Clamp CAUTION DO NOT connect the black plug from the new NEG Pump to the black socket at this time This will avoid any accidental heating of the NEG Pump until the system has been leak checked and the NEG has been activated ...

Page 490: ...15 7 5 Part 4 Leak Check of the Vacuum System on page 15 32 15 7 5 Part 4 Leak Check of the Vacuum System CAUTION Checking for leaks is very important Air leaks will shorten NEG Pump life NOTE In this instruction a MicroDuster will be used to locate the leaks Any aerosol type canned air or dust cleaner will work as long as the canned air has the following component 1 1 1 2 tetrafluorefloroethane P...

Page 491: ... Icon See Figure 15 32 NOTE Only the Advanced user access can open manual tune Figure 15 32 Manual Tune Icon 3 Select default tun file See Figure 15 33 Figure 15 33 Select default tun File 4 Wait for the automated process of opening tune to complete 5 Click on View Sensor Status Grid See Figure 15 34 ...

Page 492: ...nsor Status Grid 6 Turn off the IS Supply and Tune Feed valves See Figure 15 35 Figure 15 35 Sensor Status Grid 7 Close the Tune Status Panel and the Mass Calibration Status by deselecting each See Figure 15 36 Figure 15 36 Closing Tune Status Panel and Mass Calibration Status ...

Page 493: ... the RMB on the X axis to access the Full Scan Range See Figure 15 38 Figure 15 38 Setting Full Scan Range 10 Select Custom Type in a range of 60 to 90 This will enable the analyst to scan for both the 69 and 83 masses these are the predominant masses in the MicroDuster 1 1 1 2 tetrafluorefloroethane that is being used to check for leaks See Figure 15 39 ...

Page 494: ...the laptop in the tune program If there is a leak the response for the 69 and 83 masses will increase See Figure 15 40 The critical areas to be checked are The seam between the NEG and the manifold The seam between the Service Module and Analytical Module on the manifold side The seam between the membrane and the nut that screws into the manifold The seam between the Ion Pump and where it screws i...

Page 495: ... Pump can be plugged into the black socket above the NEG Pump 13 In the Tune window turn the IS Supply and Tune Feed on See Figure 15 35 14 At this point a tune check should be performed on the system Click on the Short Tune icon See Figure 15 41 Refer to section 7 2 Autotune on page 7 2 Figure 15 41 Short Tune Icon 15 Follow with section 15 7 6 Part 5 Activation of the NEG Pump on page 15 38 ...

Page 496: ...e tab of the Properties menu 2 Click on the Service button See Figure 15 42 Figure 15 42 Service Button on the Service Module Tab 3 Use the Activate NEG settings below as a guideline HAPSITE Pump Down Time min 60 NEG Activation Power Watts 30 Activation Time min 480 NEG Run Temp C 400 Cooldown Time min 720 See Figure 15 43 ...

Page 497: ...ervice Module NOTE When completed the Activate NEG process will automatically detach the HAPSITE from the Service Module 8 Repeat the leak check portion of this process Instead of checking for a leak between the Analytical Module and Service Module check the VI valve on the bottom of the HAPSITE where the Service Module physically attaches Refer to section 15 7 5 Part 4 Leak Check of the Vacuum Sy...

Page 498: ...d Flat head screw driver Ionizer removal tool 13 mm open end wrench 13 mm torque wrench methanol lint free cloth powder free gloves replacement aluminum seal ring if NEG is to be installed CAUTION If the NEG is to be reinstalled the NEG Pump must be removed when it is at room temperature If the NEG Pump has been used within 8 hours let it cool overnight prior to removal 1 This procedure requires t...

Page 499: ...PSITE on the Service window of the Service Module tab in the Properties window or from the Front Panel by selecting System Service HAPSITE Vent HAPSITE This starts a process which includes monitoring the cooling of the NEG Pump See Figure 15 44 Figure 15 44 Vent HAPSITE from Smart IQ Software ...

Page 500: ...ure while hot If this should occur drop the pump into a bucket of sand and cover the hot NEG Pump with more sand If this is not practical set the pump on the black plastic base on a non flammable surface The NEG Pump will burn out in a few minutes 4 When the screen shows Vent Manifold Has Been Completed unplug the NEG Pump s black cable from the front panel by loosening the locking ring then pull ...

Page 501: ... the old aluminum seal ring NOTE Be careful not to touch any part of the pump with hands 9 Look inside the manifold to see the ionizer and a 3 16 inch diameter stainless steel tube entering the manifold from the left and connecting to the small cylindrical ion volume at the center of the ionizer See Figure 15 46 This tube transfers the sample from the membrane isolation valve into the ion volume a...

Page 502: ...n on the ionizer removal tool is facing toward the left manifold wall Figure 15 47 Ion Source Removal Tool 12 Apply pressure using the stainless steel pin as a leverage point slide the extension tube from the membrane isolation valve into the ion volume The extension tube should disengage completely from the membrane isolation valve NOTE If the extension tube does not slide easily into the ion col...

Page 503: ... 15 49 Ionizer Removal Tool 15 Use a slight rocking motion pulling straight back and remove the ionizer from the manifold 16 Remove the extension tube from the old ionizer and carefully insert into the ion volume of the new ionizer 17 Thread the ionizer removal tool onto the stud in the center of the new ionizer and insert the ionizer into the manifold Position the ionizer so the ceramic filament ...

Page 504: ...e forked end of the ionizer removal tool grab the extension tube and slide the extension tube into the membrane isolation valve so the extension tube is not protruding into the ion volume 20 Install a new NEG Pump or reinstall the old NEG Pump with a new aluminum sealing ring and go through the activation process Or put the blank off flange with o ring on the manifold NOTE See section 15 7 4 Part ...

Page 505: ...open end wrench needle nose pliers flat head screw driver 2 Phillips head screwdriver Procedure for Replacing the GC Column 1 To replace a column first remove the top yellow cover Remove the captive screws and the LEMO connector nut See Figure 15 50 Figure 15 50 Removing Yellow Cover 2 Remove the top GC cover as shown in Figure 15 51 This cover serves two purposes 1 it keeps the heat in the oven a...

Page 506: ...r Removal WARNING If not cooled sufficiently the gas chromatograph and the isolation valve may be hot enough to cause burns 3 The lines to the column module must to be removed Using a 1 4 wrench unscrew both Swagelok nuts as shown Figure 15 52 Figure 15 52 Column Line Detach ...

Page 507: ...ent module as shown in Figure 15 53 Figure 15 53 Column Module Replacement 6 Insert the replacement column in the exact same manner as the old column was removed Ensure that the module sits correctly on the connector on the bottom of the column See Figure 15 54 7 Reconnect the two stainless steel lines Figure 15 54 Replacement Column Module ...

Page 508: ...ION The Gas Chromatograph will not operate properly without this cover in place 9 The temperature of the new column should read room temperature on initial start up If the temperature of Column Module is not reading accurately then the Column module is not seated to the Column Control board properly Reset the column to the column control board and verify the column temperature To test the replacem...

Page 509: ...NG The needle tips are sharp be careful to avoid injury WARNING Be careful to avoid burns if the surfaces are still hot Procedure 1 Open the top yellow cover of the HSS to expose the needle assembly 2 Using the Phillips screwdriver loosen and remove the two screws on top of the assembly 3 Remove the top cover of the needle assembly to expose the needle and the 1 4 connection fittings 4 Using the 1...

Page 510: ...he needle 6 Place the nut and ferrules on both parts of the needle where they will be re inserted into the assembly See Figure 15 57 Figure 15 57 Needle Assembly with Nuts and Ferrules 7 Place the replacement needle back through the opening from which the used needle has just been removed 8 Guide the two connections to the appropriate openings and while firmly holding down the needle to properly s...

Page 511: ...lding Down the Needle while Tightening the Nuts So Ferrules Seat Properly 9 Now that the needle is securely in place replace the cover and two screws Tighten both screws using the Phillips screwdriver 10 The HSS is now equipped with a new needle and is ready to operate ...

Page 512: ...o reduce the danger of electrical shock WARNING Risk Of Electric Shock The cover of the HAPSITE should never be removed while the Service Module is connected while the battery is installed or when the external power supply is connected as high voltages may be present The Service Module has air filters on the inlet air and also on the exhaust air Both should be checked for cleanliness periodically ...

Page 513: ...h the HAPSITE disconnected turn off the Service Module and unplug the power supply 3 Place the soft yellow plastic cover over the Vacuum Interconnect Valve to protect the VI valve 4 Turn the instrument over Do not rest on the plastic latches 5 In the middle of each of the four rubber feet are Phillips head screws Unscrew and remove all four The screws will stay with the rubber feet 6 Lift the plas...

Page 514: ...ace NOTE Check the cable connection to the printed circuit board to be sure the connection has not loosened NOTE The brackets holding the electrical and pneumatic connections may impede the placement of the plastic cover The cover has small ledges which go inside the brackets As the cover drops down however the brackets may need to be pressed against the ledges 2 When the cover is fully in place t...

Page 515: ... 15 12 2 Troubleshooting The Battery Charger 15 12 2 1 If No Indicators are Illuminated This indicates that AC power is not reaching the power supply within the Battery Charger Check the AC outlet to be sure it is live by connecting some other device such as a lamp Unplug the power cord from the outlet and examine the power cord for wear or breakage Disconnect the power cord from the back panel co...

Page 516: ...xamining the center pin for any insulating material or for signs of looseness If nothing seems wrong contact INFICON Customer Support See Chapter 17 Customer Support 15 12 2 3 If a Battery does not Accept a Charge If a battery s charge status does not change during the charging cycle although the respective indicator has been green the battery may be at the end of life To be certain that the probl...

Page 517: ...MDIS Automated Mass Spectral Deconvolution and Identification System Software AMU Atomic Mass Unit The dimension in which a number of protons and neutrons are stated Analyte That portion of a sample which comprises compounds to be analyzed that is separated identified and measured Atomic Weight The AMU representation of the number of protons and neutrons in a specified atom Baseline A measure of t...

Page 518: ...Concentration A measure of the amount of a compound in a given volume or weight This is represented as a ratio either in mass mass mass volume or volume volume terms For example 10 ppm v refers to a mix in which the specified compound is present as 1 X 10 5 parts of the whole in volume terms DAC Digital to Analog Converter An element of the electronic circuitry which converts the microprocessor s ...

Page 519: ...ent preserving measure which allows components of the air peak or solvents to pass through the mass spectrometer before the filament is turned on Fit A description of how well a reference spectrum matches an acquired spectrum in location and intensity of peaks Flow Pressure This setting controls the flow rate of Nitrogen through the HSS during the Sample and Purge states Flush A Headspace Sampling...

Page 520: ...vial from which a gaseous sample is taken for analysis Heated Line The inlet line to the HAPSITE comprising a PEEK tube with a heating jacket temperature sensors and protective sheath HSS Headspace Sampling System This includes components which when used in conjunction with the HAPSITE allows the user to quantify and qualify volatile compounds in liquid and solid matrices Initialization The act of...

Page 521: ...izer The assembly of parts in the mass spectrometer into which the sample flows and which projects a beam of mixed ions into the mass filter I S Reference This section of the Compound Library identifies the target ion of the internal standard which will be used for quantification of the chosen compound kPa Kilo Pascal Unit of pressure measurement which is equivalent to approximately 0 145 PSI LCD ...

Page 522: ...ane Isolation Valve The valve which supports the Mass Spectrometer s inlet membrane and when closed interrupts the flow of analyte from the membrane into the Mass Spectrometer Method A set of instructions for a function of the HAPSITE Molecular Weight The AMU representation of the total number of protons and neutrons in a specified molecule MS Mass Spectrometer ms milliseconds MSDS Material Safety...

Page 523: ...PT Parts per trillion concentration level Purge A Headspace Sampling System state which is used to remove moisture and sample from the system by pushing clean nitrogen through the HSS and HAPSITE This function is specified in the Inlet Method in the Acquire program Purity A description of how well an acquired spectrum matches a reference spectrum in location and intensity of peaks Recalculate An o...

Page 524: ...hic record which extracts from the TIC and displays the intensity of the ion or ions specified Round Trip Time The amount of time required to complete a scan of all the masses specified in a SIM method This includes the number of masses integration time number of extra measurements lead in time and peak width RL Right Limit RMA Return material authorization document Returning material can not be s...

Page 525: ...l ion peaks without scanning the entire spectrum SIM Method Selected Ion Mode method This allows the user to set up specific masses to be detected during an analysis This is used for better response to specific masses for known compounds SituProbe The SituProbe Purge and Trap System is a sampling accessory for the HAPSITE Smart portable GC MS for in situ testing of volatile organic compounds VOCs ...

Page 526: ... using the Noise Check feature in the Tune program TIC Total Ion Chromatogram A presentation of the flow from the GC as measured by the mass spectrometer adding up the signals from all the masses programmed and presented as a function of time TMP Turbo Molecular Pump Torr Unit of sub atmospheric pressure Equivalent to 133 3 pa Tune A term noun or verb which generally refers to mass spectrometer se...

Page 527: ...11 IPN 074 397 P1G HAPSITE Smart Operating Manual Y Cable A cable which connects to the power supply and enables powering of both the HAPSITE and Headspace Sampling System simultaneously from one converter ...

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Page 529: ...messages that you may have received To contact Customer Support see Support at www inficon com 17 2 Returning Your Instrument to INFICON Do not return any component of your instrument to INFICON without first speaking with a Customer Support Representative You must obtain a Return Material Authorization RMA number from the Customer Support Representative If you deliver a package to INFICON without...

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Page 531: ...1 No NEG Pump 1 930 281 G2 NEG Pump Installed 2 Ship Kit 1 930 0241 G1 Standard 120V 1 Inlet System N A None 0 930 206 G1 Hand Control Unit 1 Laptop with NIST and Hapsite Smart IQ Software CDs 930 261 G3 Standard Laptop w Windows XP C 930 261 G4 Ruggedized Laptop w Windows XP w V erizon D 930 261 G5 Ruggedized Laptop w Windows XP E Service Module N A None 0 930 202 G1 100 120 230 VAC 1 Software In...

Page 532: ...t 10 each 930 022 G1 Tool Kit with Torque Wrench Kit 930 0231 G1 Probe Nut and Ferrule Kit 5 each 930 2020 G1 Decon Cap Plug Kit 930 705 G1 Sample Loop Tube Kit 930 206 G1 Hand Control Unit Probe 930 249 G1 Concentrator Cover 930 250 G1 Sample Loop Cover Concentrator Tubes 930 251 G1 w Heater Tenax 930 252 G1 w Heater Carbopack X Modified 930 716 G1 w Heater Tri Bed Concentrator Tube Kit 930 4051 ...

Page 533: ...489 G3 30 m SUPELCOWAX 10 1 UFdF 930 489 G4 30 m J W DB 1701 1 0 um 930 489 G5 30 m SPB 624 0 32 mm 1 8 um 930 489 G6 30 m SPB 1 4 0 um 930 489 G7 30 m SPB 5 0 32 mm 930 489 G8 30 m SPB 5 1 0 um 930 489 G9 30 m Restek RTX 200 1 0 um 930 489 G10 30 m EQUITY 1 1 0 um 930 489 G11 30 m 1 5 um RTX 200 930 489 G12 30 m RTX 624 0 32 mm 18 4 HAPSITE Smart Consumables NEG Pumps 930 070 G1 CERTIFICATE for F...

Page 534: ... Standard 071 747 Performance Standard Concentrator Air 5 analytes in Methanol 1 2 mL 071 760 HAPSITE Chemical Standards Kit 12 part for training practice 930 703 G1 Ion Pump Kit 930 205 G1 Ionizer With Magnet 18 5 HAPSITE Upgrade for 930 280 GX series HAPSITE 930 718 G1 1 HAPSITE Smart IQ Factory Upgrade Non DOD 930 719 G1 1 HAPSITE Smart IQ Upgrade U S DOD only 18 6 HAPSITE Smart Training 18 6 1...

Page 535: ...truments will be incurred Contact INFICON for details 930 831 P1 HAPSITE Shipping within the continental U S 930 832 P1 HAPSITE Shipping outside the U S not Asia 930 833 P1 HAPSITE Shipping to Asia 930 834 P1 Headspace Shipping within the continental U S 930 835 P1 Headspace Shipping outside the U S not Asia 930 836 P1 Headspace Shipping to Asia 18 7 Headspace Spare Parts 070 1204 Sample Vials Cas...

Page 536: ...n 931 405 P1 Thin 931 408 P1 Heavy 600 1131 P30 Y Power Cable 18 8 Service Module Spare Parts 068 002 Battery Charger Service Module Power Cord U S 930 0211 G1 Torque Wrench Kit 930 465 P1 Shipping Case Service Module 600 1001 P15 RS232 Cable 15 ft 18 9 HAPSITE SituProbe Spare Parts 940 700 G1 SituProbe Vessel and Plugs 933 700 G1 Collection Tube Replacement Kit 931 401 P2 Transfer Line Line Insul...

Page 537: ...3CH3 1 07 97 99 71 55 6 Benzene C6H6 1 22 78 69 71 43 2 Carbon Tetrachloride CCl4 1 26 117 125 56 23 5 1 2 Dichloropropane CH2ClCHClCH3 1 51 63 69 78 87 5 Bromodichloromethane BrCl2CH f 1 59 83 69 75 27 4 Trichloroethene ClCH CCl2 f 1 61 130 99 79 01 6 cis 1 3 Dichloropropene CClH CCClH2 H g 2 08 75 69 542 75 6 4 Methyl 2 Pentanone CH3COCH2CH CH3 CH3 g 2 11 43 58 69 108 10 1 trans 1 3 Dichloroprop...

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Page 539: ...ITE See section B 1 2 on page B 3 3 Gas cylinder safety and contamination checks corrective steps in the equipment See section B 1 3 on page B 5 B 1 1 How to Establish the Desired Concentrations There are two basic ways to obtain several concentrations of a given mix of compounds The most obvious is to buy the compounds premixed to specification in cylinders containing the several concentrations d...

Page 540: ...iaphragms To minimize stagnant volumes where VOCs can accumulate the regulator body should be designed with minimum internal dead volume Use 1 diameter gauges or eliminate the gauges altogether The regulators and the tubing following should be rated for high purity mildly corrosive or corrosive service if any halogenated VOC s are to be delivered NOTE A regulator transfer line system must be well ...

Page 541: ...ith the sample in a ratio which is dependent on the flow rate of the sample gas and the suction of the pump CAUTION Connecting the inlet of the Hand Control Unit to a sample at a pressure above or below atmospheric will cause the mixing ratio of the internal standards to be incorrect so the resultant calibration will be invalid There are two basic approaches to assuring that the calibration mix is...

Page 542: ...out 60 HAPSITE samplings of the contents between refills The use of properly filled Tedlar bags inherently assures that the gaseous contents are at atmospheric pressure for sampling A properly filled Tedlar bag will have plenty of flex left in the bag walls so that the bag can be easily kneaded to mix the contents The bag should not be filled to the point where the bag appears like a firm air pill...

Page 543: ...ety A safety certified gas cylinder cart should be available in the vicinity of where the cylinders are normally used for moving them and replacing empty cylinders Gas cylinders should never be transported with the regulator attached Tedlar bags may be cleaned for reuse or replaced with new bags To clean a Tedlar bag for use with different VOC s or concentrations partially fill with VOC free N2 or...

Page 544: ...alternative to gaseous cylinder mixes in such uses as new applications development or verification of unknown VOCs by component spiking This should be qualified by saying that accurate gas standard preparation by direct liquid injection is only recommended at levels greater than 5 ppmv because the minimum liquid volume deliverable by syringe at an acceptable accuracy and precision is about 0 5 L T...

Page 545: ... shipped in the box in which they are received A NEG pump installed in the HAPSITE will not be damaged by shipment C 2 Shipping the Canisters The canisters of Carrier Gas and Internal Standards Gas are pressurized to 700 kPa 100 psig or more The canisters are approved by the Department of Transportation DOT but they are considered hazardous cargo because of the pressure They are permitted to be tr...

Page 546: ... Overpack Used The Kg number refers to the total mass of the gas not the gross weight In the Packing Inst column write 200 The Authorization column is left blank The signature section is very important fill it out completely The Shipper s Declaration for Dangerous Goods is a Style F83R from Label master in Chicago their phone number is 800 621 5808 They are carbon less four part forms and may be a...

Page 547: ... people and stand upwind of the discharge If you have no way to recycle the empty canisters or are otherwise reluctant to dispose of them you can ship them back to their point of origin for disposal Be certain that they are empty less than 30 psi then package them in a plain cardboard box without any green diamond label Mark the box as Empty Canisters for Destruction Ship them prepaid to Scott Spe...

Page 548: ......

Page 549: ...cator 2 43 no charge 15 58 no indicators 15 57 off indicator 2 44 red indicator 2 44 15 58 compartment 2 41 door 15 55 HAPSITE 2 9 shipping C 1 Begin Time 11 26 blend accuracy B 2 C Calibrate function 12 14 calibration curve 16 1 mix 13 4 B 1 B 3 calibration mix 13 4 calibration report 12 4 canisters empty C 2 shipping C 1 Carbopack concentrator 3 28 5 18 11 19 carrier gas 16 1 Chromatogram Peak W...

Page 550: ...n time 16 2 End Mass 11 25 End Time 11 26 equilibrium time 16 3 Event Log File 10 3 10 10 exhaust 2 6 Extended Standby 3 46 Extended Standby Mode 3 15 F filament 16 3 delay 11 19 16 3 file extension hps 9 3 file transfer 10 11 file types data files 10 3 10 11 event log files 10 3 10 10 Method file 11 1 method files 10 1 10 9 report files 10 11 Tune files 10 4 10 11 Foreflush 11 15 foreline 14 1 14...

Page 551: ...t Component 11 12 Inlet State available 11 15 concentrator 11 16 HSS 11 16 inlet state 11 12 16 4 custom valve state 11 16 integration time 16 2 interconnect plug 14 17 interfaces 1 9 internal standard 1 5 2 7 16 5 B 3 ion 16 5 beam 1 7 energy 16 5 pump 15 3 source filament 15 8 target 16 10 volume 1 7 16 5 ion detector 1 6 ion pump usage 15 1 ionization 1 7 ionized molecules 1 7 ionizer 1 6 1 7 1...

Page 552: ... 4 activation 15 7 safety 15 2 usage 15 1 reactivating 15 14 removal 15 17 troubleshooting 15 11 NIST 6 6 7 1 8 10 12 5 13 1 16 6 analyzing data 9 32 header information 9 25 hits 9 28 library 9 1 16 6 library search 9 23 11 1 Nitrogen 13 4 Canister 13 18 Carrier Gas 2 7 noble gases 1 8 noise check 16 7 Noise Thresholding Level 11 35 O oil vacuum pump 14 3 organic compounds 1 6 gas flow 1 5 gases 1...

Page 553: ...11 6 method 16 9 Survey 11 28 SituProbe 1 1 2 26 16 9 inlet states 11 17 method 3 46 11 10 nitrogen flow pressure 11 20 Skip Mass Range 11 25 SM 1 1 1 8 2 18 14 1 air filter 15 54 15 56 attach to HAPSITE 14 12 batteries 14 3 charger 14 4 charge indicator 14 4 communications 2 22 8 26 14 5 components 1 4 detach 2 26 detaching from HAPSITE 14 17 manifold 14 4 power loss 14 3 14 25 power supply 14 5 ...

Page 554: ... Tune 7 1 16 10 Autotune 7 1 calibration file 11 5 files 10 11 long Autotune 7 3 Manual 7 1 manual 7 25 Report 7 5 7 6 turbopump 1 8 U USB drive 4 13 user access Advanced 8 34 level 8 34 Normal 8 34 V vacuum interconnect valve 1 4 14 1 14 4 16 10 vacuum pump oil 14 3 Valve States 11 13 vent gas pressure 14 3 VI valve 15 22 vials loading 13 6 sample 13 4 VOC free Air B 1 volatile compounds 6 6 vola...

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