ATD Tools 5928 Betriebsanweisung

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Inhaltsverzeichnis

Seite 1 - THERMAL DESORBERS

TURBOMATRIX SERIESTHERMAL DESORBERSUser’s GuideGAS CHROMATOGRAPHY

Seite 2

ContentsviAmbient Pressure Calibration ... 259Checking the Pneumatics for the TurboMatrix Series PPC Units...

Seite 3 - User’s Guide

Operation92• set and view current configuration parameters (Status tab)• run analyses using one or multiple methods (Run tab)• view instrument informa

Seite 5

Operation94has been selected, then you only need to enter the tube range. The selected method will be displayed and you will not be able to access the

Seite 6

Operation

Seite 7

Operation96method. The instrument status will be Standby until the instrument reaches all of the set points. If you are using a TD, you must now load

Seite 8

Operation

Seite 9

Operation98The ATD/TD incorporates a packed cold trap to concentrate the volatiles before injection onto the GC column. It is cooled to temperatures b

Seite 11

Operation100Figure 19 Timing TabThe name of the method that is currently loaded on the Run tab is also displayed. The settings displayed here are from

Seite 12

Operation

Seite 13

Contents

Seite 14

Operation102Enter a Loop Load time. This will determine the time interval that ISV1 is open to load the sample loop in preparation to introducing the

Seite 15

Operation

Seite 16

Operation104Figure 22 Options Tab for a TurboMatrix 150 ATDIf you have the Standard Injection option installed, but do not need to use it, then de-sel

Seite 17

Operation

Seite 18

Operation106is when the sample is purged of residual air at ambient temperature. If you enabled the heated purge option, then the tube will be heated

Seite 20

Operation108In this mode, only the cold trap is heated and the contents of the trap are desorbed and vented through the Input Split flow control to pr

Seite 22

Operation110Column Pressure—In the TD/ATD, the Pressure Control system is a manual Pressure Regulator (not a programmable function). Setting a value h

Seite 23

Operation

Seite 24 - About this Manual

ContentsviiiNitrogen Flow Rates...392Index ...395

Seite 25 - Unpacking the Instrument

Operation112ToolsPressing the Tools button opens a pop-up menu of tools that enable you to perform various functions such as creating and editing meth

Seite 26

Operation

Seite 27

Operation114Del key to delete the characters.5. Press OK to enter the new name for your method and then press OK to save the method. Press Done to com

Seite 29 - Electrical Safety

Operation116Maintenance TabYou will use the Maintenance tab to set flows or perform routine maintenance on the instrument. The Maintenance tab contain

Seite 30

Operation

Seite 31

Operation118Figure 28 Preferences Run TabSingle Method Operation—If you select single method operation you can also specify the method to be used. The

Seite 33 - Handling Compressed Gases

Operation120split on. See Setting the Outlet Split Flow on page 80 for details on setting the outlet split flow.Liquid N2 Option—Check this option to

Seite 34

Operation

Seite 35 - Extreme Temperatures

ixFiguresFigure 1 The ATD/TD Input/Output (I/O) Port ...43Figure 2 Connecting the Fail Output Signal in Parallel with the Start Si

Seite 36 - Sample Tubes

To enable and use this option:1. Select the Setup tab.2. Press the Password Protection check box. A check mark will appear in the box to enable the op

Seite 38

Operation124Connect TabKey Clicks— If enabled, this option sounds a tone each time a button is pressed, to confirm that you have pressed a key. Baud R

Seite 40

Operation126groove, and prying them apart. Other techniques, such as twisting the pen-clip from the tube, can cause permanent damage to the pen-clip.

Seite 42 - Installation and Setup

Operation128Single Method Operation on the TDOnce you have set up the TD and entered a method for your application you are ready to begin analyzing yo

Seite 44

Operation130The method can be stopped at any time by pressing the Stop button. A confirmation pop-up window will display, press Ye s to confirm that y

Seite 45

Operation

Seite 46

FiguresxFigure 30 Setup Tab ... 121Figure 31 Password ...

Seite 47 - Electrical Connections

Operation132NOTE: Before powering up the TD/ATD again, ensure thata) Carrier Gas supply and Dry Air to the TD are restored,b) Wait 20 to 30 minutes to

Seite 49 - Chromatograph

Operation134and stop tubes. The tube range will default to 1 to 50. Press the first entry box to enable the option. If you are using a TD, the tube ra

Seite 50

Operation

Seite 51 - TD Output Signals

Operation136Editing a SequenceTo delete an entry from the sequence, select the entry in the list and press the Del button. To change the tube range, y

Seite 52

Operation

Seite 53 - TurboMatrix I/O Port

Operation138Heat Rate—Once the volatiles are transferred from the sample tube, the trap is heated. Set the heating rate to any value between 5, 20, 40

Seite 55 - Connecting the ATD/TD to the

Operation140Figure 36 Timing TabThe name of the method that is currently loaded on the Run tab is also displayed. The settings displayed here are from

Seite 58

Operation142being chromatographed. This setting is intended to ensure that the current run has finished in time for the trap desorption of the next sa

Seite 59

Operation

Seite 60

Operation144Figure 39 Internal Standard Popup for the TurboMatrix 650 ATDThe Options TabThe Options button at the bottom of the Status screen provides

Seite 61

Operation

Seite 62

Operation146Inlet Split and Outlet Split Options—Two split points are provided on the ATD/TD: one before and one after the cold trap. By using either

Seite 64

Operation148Operating ModesNOTE: The screen above shows operating modes for a TurboMatrix 650 ATD.The ATD/TD can operate in any one of five modes. A b

Seite 66

Operation150Load Internal Standard (ISTD) on TubeIf the instrument has been equipped with the Internal Standard option, a metered volume of an analyti

Seite 67

Operation

Seite 68

FiguresxiiFigure 101 Open Loop Purging Apparatus with Removable Adsorbent Tube...334Figure 102 S

Seite 69 - Panel of the GC

Operation152Inlet Split- Set the Inlet Split flow rate by accessing the entry field and incrementing or decremented the displayed value with the plus/

Seite 70

Operation

Seite 71 - Good Cut

Operation154Pressure or the Trap Desorb Flow Time is set to zero, the system will default to the Isobaric Pressure Injection Mode.To set the Trap Deso

Seite 72

Operation

Seite 73

Operation156also contain the date and time the sequence was started and when the sequence was completed.ToolsPressing the Tools button opens a pop-up

Seite 75

Operation158complete the selection and return to the Run tab.Activate Command—This command makes the currently selected method active. The method is l

Seite 77

Operation160Maintenance TabYou will use the Maintenance tab to set flows or perform routine maintenance on the instrument. The Maintenance tab contain

Seite 79 - Gas Connections

xiiiTable 1 ATD/TD Shipping Kit...19Table 2 Electrical Protection ...

Seite 80

Operation162Preferences TabYou will use the Preference tab to set the configuration options for the TD. The selections you make here will enable or di

Seite 81

Operation

Seite 82

Operation164Figure 48 Config TabNOTE: Integrity Testing button is grayed out for all models except the TurboMatrix 650 ATD. See the section on Integri

Seite 84 - Connecting the Dryer Assembly

Operation166Liquid N2 Option-Check this option to enable it on the Status tab. The option allows you to cool the cold trap down to -100°C. This option

Seite 86 - Series 100 TD and 150 ATD

Operation168Monitor Trap Impedance-Selection of the check box enables the input boxes for Lower and Upper Limits. The measured pressure will be report

Seite 87

Operation

Seite 88

Operation170Protection” and the pop-up Password box will appear in the figure above. If you wish to create a new password, touch each box and the alph

Seite 89

Operation

Seite 90

TablesxivTable 34 Column (0.32 mm) Flow Rates with Helium Carrier Gas ...389Table 35 Column (0.53 mm) Fl

Seite 91 - Operation 3

Operation172Connect TabKey Clicks— If enabled, this option sounds a tone each time a button is pressed, to confirm that you have pressed a key. Baud R

Seite 92

Operation

Seite 93

Operation174The pen-clip can be removed from a sample tube by inserting a wide-bladed screwdriver between the clip and the tube, close to the groove,

Seite 94

Operation

Seite 95

Operation176tab.3. If you are running with a pre-selected method you only need to load the tube. 4. If the method has not been selected, select it now

Seite 97

Operation1783. Enter the desired end tube.4. From the method drop-down box, select the method to be used for the selected range of tubes.5. Press the

Seite 98

Operation

Seite 99

Operation180

Seite 103

Accessories

Seite 104 - Status Tab

Accessories184window.8. If you are using the Method Editor, save your method. If you are using the Status tab, you must enter all of the other method

Seite 106

Accessories186Tubes and CapsThe ATD/TD uses industry standard, patented stainless steel tubes. The stainless steel tubes are compatible with pumped an

Seite 108

Accessories188Capped Sample Tubes (with PTFE Analysis Caps)Stainless SteelGlass Glass Lined Stainless SteelQtyM041-3595 M041-3598 M041-3597 10M041-359

Seite 109

Accessories

Seite 110

Accessories190(140 to180 kPa).To conserve liquid nitrogen, the accessory will be turned off automatically under the following conditions: • when the A

Seite 114

Accessories192Figure 59 Flow Diagram of the TurboMatrix 350 ATD (PPC) with Internal Standard Accessory The standard addition accessory is kept at ambi

Seite 116

Accessories1944. 4. In the same dialog box you can set the Inject Time (in minutes) to the amount of time you want helium to go through the loop onto

Seite 118 - The Log Tab

Accessories196upon and set.This function is available by selecting the Preferences entry on the Tools menu and then selecting the Config tab and the I

Seite 119

Accessories

Seite 120 - Method Editor

NOTE: Use a clean sample tube that does not contain a sample for the set-up procedure. The sample tube should contain the type of packing material tha

Seite 121

Accessories

Seite 122

Accessories200Figure 61 Sequential Tube Sampler with monitoring pump.Contact PerkinElmer for further details about this accessory. Online Sampling Acc

Seite 126

Method Development 5

Seite 128 - Setup Tab

Method Development

Seite 129

Method Development206The process of developing thermal desorption methods can be greatly simplified by keeping the principles given below in mind when

Seite 130

Method Development

Seite 131

Method Development208Setting System ParametersTemperature TabThere are five temperature settings for the TD: tube oven temperature, the transfer line

Seite 132 - Connect Tab

Method Development

Seite 133 - Loading Tubes

Method Development210time but may be required for the analysis of thermally labile analytes.Trap High Temperature—The trap is heated to the high tempe

Seite 134

Method Development

Seite 135

Introduction14TurboMatrix 100 TD: Single-tube, manual-pneumatics model, can be upgraded to the automated version. Also includes a separate trap-clean-

Seite 136

Method Development212overlapping tube desorptions and analyses to maximize throughout. For example, if the CYCLE TIME is 42 minutes after the previous

Seite 137

Method Development

Seite 138

Method Development214If you have enabled this option, then you must enter a Standard Inject time on the Timing tab. The standard addition valve is act

Seite 139 - Shutdown

Method Development

Seite 140 - Status Line

Method Development216degrade rapidly and leak. You may also want to install high temperature o-rings into the fixed seal assembly. The high temperatur

Seite 141 - The Run Tab

Method Development

Seite 142

Method Development218Upon completion of each flow adjustment an entry of its value can be made in the respective field of the Status/Pnu tab. These se

Seite 143

Method Development

Seite 144

Method Development220Carbotrap™Carbopack B ™(n-C4) n-C5 to n-C14400 100 Wide range of VOCs including ketones, alcohols and aldehydes (bp>75°C), and

Seite 145

Method Development

Seite 146

Introduction

Seite 147

Method Development222temperatures, up to 300°C and more, for efficient thermal desorption.1As a general policy it is a good idea to use similar sorben

Seite 148

Method Development

Seite 149

Method Development224Compound Boiling Point (°C) Retention Volume at 20 °C (l/g)Heptane 98 170Octane 125 780*Benzene 80 62Toluene 111 360Xylenes 138-1

Seite 150

Method Development

Seite 151

Method Development226Figure 65 Glass or Stainless Steel Sample Tubes Containing Adsorbents of Increasing Strength Linked Together in Series In this ca

Seite 152

Method Development

Seite 153

Method Development228All forms of Tenax are susceptible to decomposition since they are polymer based, so there is always some background (artifacts)

Seite 154

Method Development

Seite 155

Method Development230your trap loading and column capacity and flow, figure out how much sample you need on the trap and therefore what the outlet spl

Seite 156

Method Development

Seite 157

Introduction16About this ManualThis manual is an integral part of your thermal desorber. It begins with unpacking and general safety information in Ch

Seite 158

Method Development232 Outlet Split = 8 mL/minIn the above example, the trap desorption flow of 10/mL/min is barely suffic

Seite 159

Method Development

Seite 160

Method Development234The percentage of components from the sampling tube which reach the analytical column is:Equation 10Example: In this example 10%

Seite 161

Method Development

Seite 162

Method Development236Four major techniques are commonly used to introduce standards into desorption tubes.Vaporizing a Liquid StandardIn the first met

Seite 163

Method Development

Seite 164

Method Development238Internal Standard Addition AccessoryThe Internal Standard Addition accessory is required for the third method. A gaseous calibrat

Seite 165

Method Development

Seite 166

Method Development240Desorb-Rec-Same: This method will inject a sample but instead of loosing the sample to outlet split the split flow is directed to

Seite 167

Routine Maintenance 6

Seite 168

Introduction

Seite 170

Routine Maintenance

Seite 171

Routine Maintenance244Table 17 Maintenance ScheduleCleaning the InstrumentExterior surfaces may be cleaned with a soft cloth, dampened with a mild de

Seite 172

Routine Maintenance

Seite 173

Routine Maintenance246Sample Tubes and Storage CapsWhen samples have been collected, the tubes should be analyzed as soon as possible. If the tubes ca

Seite 174

Routine Maintenance

Seite 175

Routine Maintenance248Figure 69 ATD Arm HousingTo gain access to the top of the heated valve, you must further remove the transfer line cover.8. Remov

Seite 176

Routine Maintenance

Seite 177

Routine Maintenance250and 0920-0093) are intended for operation up to 300 °C. See High Temperature Operation on page 215 for further details.We recomm

Seite 178

Routine Maintenance

Seite 179

Introduction18the side.3. Lift out the instrument using the two lifting straps.4. Check that all ordered parts have been supplied undamaged.The follow

Seite 180

Routine Maintenance252NOTE: Do not over tighten the seal.Table 18 Fixed and Mobile Seal Replacement O-RingsChanging the O-Rings and Filter Disk in th

Seite 182

Routine Maintenance2544. Remove the carousel and bottom cover.Figure 71 Automated Mobile Seal5. Turn the mobile seal cap counterclockwise to remove it

Seite 183

Routine Maintenance

Seite 184

Routine Maintenance256inserting the end of the column into a silicone septum. 1/8” packed columns may be capped using a 1/8” Swagelok® cap (P/N 0496-7

Seite 185

Routine Maintenance

Seite 186

Routine Maintenance258select Maintenance and select Column Leak Test. The following screen will appear. Press OK to start the test.If your GC fails th

Seite 187

Routine Maintenance

Seite 188

Routine Maintenance260Checking the Pneumatics for the TurboMatrix Series PPC UnitsYou may need to check the pneumatics on the three available units wi

Seite 189 - Accessories 4

Routine Maintenance

Seite 190 - <>

Introduction

Seite 191 - Options Board

Routine Maintenance262Where: Fa is the measured flow rate under ambient conditions (mL/min). Fs is the flow rate entered/display

Seite 192 - Accessories

Routine Maintenance

Seite 193 - BCD Interface

Routine Maintenance2644. Set the Valve temperature to the value required for the analysis. NOTE: For the best accuracy, the calibration procedure shou

Seite 194 - Tubes and Caps

Routine Maintenance

Seite 195

Routine Maintenance2666. Place a clean and empty glass or stainless steel tube into Position 1 (see the following figure) of the carousel and press th

Seite 196

Routine Maintenance

Seite 197

Routine Maintenance2688. Manually transpose the average Actual values into the corresponding Offset fields.

Seite 198

Routine Maintenance

Seite 199 - Internal Standard Accessory

Routine Maintenance270Removing the Cold TrapNOTE: Always have one or two spare traps on hand in case of breakage before proceeding.To remove the cold

Seite 200

Routine Maintenance

Seite 201 - Operation of the IS Accessory

Introduction20Symbols Used on the InstrumentFurther information is available in this safety section.Safety InformationThis manual contains information

Seite 202

Routine Maintenance272Figure 76 Cold Trap8. Remove the Desorb line and slide it to the back. See the following figure.CAUTIONBefore shutting off both

Seite 204

Routine Maintenance27410. Carefully remove the o-ring from the trap by removing the nut and removing the brass ring. See the following figure.Figure 7

Seite 205

Routine Maintenance

Seite 206

Routine Maintenance2762. Also on the left side of the trap, reattach the brass nut and tighten. Figure 81 Trap O-Ring, Brass Ring and Nut 3. Put the

Seite 208 - Online Sampling Accessory

Routine Maintenance278When specifying a Trap Clean method in a sequence, the method must have a tube assigned to it. An empty tube is best suited for

Seite 209 - Clarus 500 GC

Routine Maintenance

Seite 210

Routine Maintenance2802. Using the cold trap packing tool (P/N L427-1203), remove the old packing. Insert the tool into the cold trap and gently push

Seite 212

Introduction

Seite 213 - Analytical Objectives

Routine Maintenance282Under normal operating conditions, the filter disks do not require changing. However, they must be changed if the packing of the

Seite 214

Routine Maintenance

Seite 215

Routine Maintenance28413. Connect the supply of purge air and carrier gas and begin purging the cold trap enclosure. Wait for 30 minutes before poweri

Seite 217

Routine Maintenance286When tubes are packed with more than one adsorbent in series, the different beds of packing are usually separated with glass woo

Seite 218

Routine Maintenance

Seite 219

Routine Maintenance288conditioning stages until it is finally close to, or at, the maximum temperature limit for the packing material. Where possible,

Seite 220

Routine Maintenance

Seite 221

Routine Maintenance290Once the packed tubes have been thoroughly conditioned in this way, subsequent conditioning runs (for example, after storage) wo

Seite 222

Routine Maintenance

Seite 223 - High Temperature Operation

TurboMatrix Series Thermal DesorbersUser’s Guide

Seite 224 - Carrier Gas Flow Rates

Introduction22.Line Cord—Use only approved line cords with a protective ground conductor (green or green/yellow) to ensure safe operation. The line co

Seite 225

Routine Maintenance292To replace fuses:1. Ensure that the power cord is disconnected from the power entry module on the rear left side of the instrume

Seite 226 - Phase Sampling

Routine Maintenance

Seite 227

Routine Maintenance294

Seite 228

Theory of Thermal Desorption 7

Seite 230

Theory of Thermal Desorption

Seite 231

Theory of Thermal Desorption298or decrease the carrier-gas pressure during trap desorption to improve desorption efficiency and give better recoveries

Seite 232

Theory of Thermal Desorption

Seite 233 - Aniline 184 2200

Theory of Thermal Desorption300Figure 86 Standby ConfigurationNOTE: SV is a solenoid valve, and PR is a pressure regulator in this section.In standby,

Seite 234

Theory of Thermal Desorption

Seite 235

Introduction

Seite 236 - Setting Sample Split Ratios

Theory of Thermal Desorption302Start of the Tube Conditioning Sequence—When the tube conditioning sequence is started, the carrier gas pressure is tes

Seite 237

Theory of Thermal Desorption

Seite 238 - Single Split Operation

Theory of Thermal Desorption304Upon finishing the leak test, SV1 and SV3 open and the sample tube is purged with carrier gas for the duration of the p

Seite 239 - SplitOutlet 2

Theory of Thermal Desorption

Seite 240 - Double-Split Operation

Theory of Thermal Desorption306If SV4 is open, it will remain open for the three minutes and switch with SV2. SV2 and SV4 (if selected) will switch th

Seite 241

Theory of Thermal Desorption

Seite 242

Theory of Thermal Desorption308Figure 90 Pressurize Sample TubePrimary and Secondary Leak Test of the Sample TubeIf no large leaks are detected, SV1 i

Seite 243

Theory of Thermal Desorption

Seite 244 - Vaporizing a Liquid Standard

Theory of Thermal Desorption310The number of retries can be set to between zero and two (0-2); the default value is two (with two retries, a total of

Seite 245 - Sample Tube

Theory of Thermal Desorption

Seite 246 - Atmosphere

Introduction24Mechanical HazardWhen working with the instrument, please observe the following:• Keep your hands, clothing and other objects away from

Seite 247 - Sample Archiving

Theory of Thermal Desorption312adsorbent to strong adsorbent. Any volatiles purged out of the weak adsorbent will land on the strong adsorbent (see th

Seite 248

Theory of Thermal Desorption

Seite 249 - Routine Maintenance 6

Theory of Thermal Desorption314Single-Stage versus Two-Stage DesorptionSingle Stage (Non-PerkinElmer)If the volatiles extracted from the sample by the

Seite 250

Theory of Thermal Desorption

Seite 251 - Routine Maintenance

Theory of Thermal Desorption316in the environmental field where samples frequently contain a significant amount of water.Packed cold traps can functio

Seite 252 - Cleaning and Decontamination

Theory of Thermal Desorption

Seite 253 - Adsorbent Storage

Theory of Thermal Desorption318

Seite 254 - Spectrometer

Sampling Techniques 8

Seite 256 - Door Latch

Sampling Techniques

Seite 258

Sampling Techniques322Figure 96 Principles of Diffusive SamplingUnder these conditions, components will migrate to the adsorbent or reactive surface a

Seite 259

Sampling Techniques

Seite 260 - TD Mobile Seal

Sampling Techniques324If the concentration is required in ppm, then the formula is modified to include the molecular weight of the compound of interes

Seite 261 - ATD Mobile Seal

Sampling Techniques

Seite 262

Sampling Techniques326Alternatively, the uptake rate can be determined experimentally. One quick experiment that can be used either to determine appro

Seite 263 - Leak Testing

Sampling Techniques

Seite 264

Sampling Techniques328placed over the front of the tube to reduce the ingress of particulate material if required. (P/N L407-0208)The flow rate range

Seite 265 - Column Leak Test

Sampling Techniques

Seite 266 - GC Temp Calib

Sampling Techniques330Table 25 Mass of Component Collected on a Sample TubeDuring Pumped Air Monitoring The data in Table 26 is based on a sampling t

Seite 268 - TurboMatrix Series PPC Units

Introduction26• Do not heat the cylinders or expose them to direct sunlight. The cylinders may rupture at high temperatures.• Do not mutilate cylinder

Seite 269

Sampling Techniques332obtained from regular monitoring for individual analytes will vary considerably.Figure 99 Probability of a Result Occurring vers

Seite 270

Sampling Techniques

Seite 271 - Figure 73 Filter in Place

Sampling Techniques334Purge and TrapOne of the variations of vapor phase sampling is the purge and trap technique. In this method, an inert gas is use

Seite 272

Sampling Techniques

Seite 273

Sampling Techniques336Table 28 GC Certified Standards on PerkinElmer TubesThese analytical results were in agreement with the values calculated from

Seite 274

Sampling Techniques

Seite 275

Sampling Techniques338Figure 104 Sampling Resins and Ointments Sampling SolidsIdeal solids for analysis by thermal desorption have a large surface are

Seite 276

Sampling Techniques

Seite 277

Sampling Techniques340If a 1 µL injection of standard solution is to be used, the concentration of the solution must be approximately 25% by volume. 1

Seite 279

Introduction

Seite 281

Troubleshooting

Seite 282

Troubleshooting344Status DescriptionEconomy Mode The instrument is in the economy mode. The heaters have been switched off and the carrier gas flow ha

Seite 284

Troubleshooting346Status DescriptionARM TO DECAPPERContact your PerkinElmer Service Representative if you get this message.ARM TO DESORBContact your P

Seite 286 - De-Icing the Cold Trap

Troubleshooting348Status DescriptionDECAPPER CLOSECheck the air pressure, the valve could be leaking or failing, check for a mechanical obstruction. I

Seite 288 - DesorbAdsorb

Troubleshooting350Status DescriptionOVEN FAIL AT IDLE POSITIONContact your PerkinElmer Service Representative if you get this message.OVEN FAIL AT TUB

Seite 289

Troubleshooting

Seite 290

• Secure the Dewar vessel so that it cannot fall over. • Protect the Dewar vessel from any damage and from sources of heat. The Dewar vessel must be f

Seite 291

Troubleshooting352Table 30 TurboMatrix Status and Error Messages SummaryInstrument Fault ConditionsIf there is more than one fault occurring at a tim

Seite 293 - Stainless Steel Tubes

Troubleshooting354Fault: Carousel Motor StalledCause: An obstruction has caused the carousel to halt rotation.Action: Turn the ATD off and disconnec

Seite 295

Troubleshooting356the gripper arm has dropped a tube.Action: Turn the ATD off and disconnect the power cord from the AC mains. Remove the case as out

Seite 296

Troubleshooting

Seite 297

Troubleshooting358Action: Ensure nothing is touching the carousel. Action: Ensure all of your tubes have been installed correctly. If pen clips are

Seite 298

Troubleshooting

Seite 299 - Cleaning the ATD Sample Tray

Troubleshooting360Re-orient the tube on the carousel. Touch the Tools button, press Reset in the menu and answer Yes to the pop-up question.The instr

Seite 300

Troubleshooting

Seite 302

Troubleshooting362must be inserted into the carousel with the pen clip facing in, toward the center of the carousel. Re-orient the tube on the carouse

Seite 303

Troubleshooting

Seite 304

Troubleshooting364Fault: Valco-A, B, C or D Valve FailedCause: A Valco valve cannot be initialized. Valco valve A is the heated valve used for normal

Seite 305

Troubleshooting

Seite 306 - Theory of Thermal Desorption

Troubleshooting366should be replaced as described in Installing the Heated Transfer Line on page 51.Cause: A poor connection between the transfer lin

Seite 308

Troubleshooting368Cause: There is ice forming on the cold trap. Action: De-ice the trap as outlined in De-Icing the Cold Trap on page 278. Ensure th

Seite 310

Troubleshooting370matrix is not escaping from the tube or trap and migrating into the rest of the system. Use glass wool plugs in the tubes and trap,

Seite 311 - Analysis

Troubleshooting

Seite 312

Introduction30A label with a crossed-out wheeled bin symbol and a rectangular bar indicates that the product is covered by the Waste Electrical and El

Seite 313

Troubleshooting372diffuse back into the system if the filters become overloaded.Action: The inlet and outlet split and desorb charcoal filters must b

Seite 315 - Automated Leak Testing

Troubleshooting374The following conditions are particularly important:• at least 10 mL/min flow is passing through the tube during primary desorption•

Seite 316

Troubleshooting

Seite 317 - Number of Leak Test Retries

Troubleshooting376Discrimination of Compounds Over a Wide Boiling RangeCause: The packing material contained in the trap or in the sample tube is not

Seite 318

Troubleshooting

Seite 319

Troubleshooting378

Seite 320

Appendices 10

Seite 323

Installation and Setup 2

Seite 324

Appendices382Appendix B Warranty Exclusions and LimitationsThe following consumable items are excluded from your instrument warranty agreement:• Fused

Seite 326

Appendices384A Method for the Determination of Personal Exposure to Atmospheric Nitrous Oxide...TDA-17 D

Seite 328

Appendices386International Standard Methods Relating to VOC Air Monitoring using Thermal Desorption... GCA-77Bibliography

Seite 329

Appendices

Seite 330 - Sampling Techniques

Appendices388Appendix D Carrier Gas PressuresThe flow rates listed below are approximations only. In order to accurately determine the column flow rat

Seite 332 - Zx 24.45

Appendices390Table 35 Column (0.53 mm) Flow Rates with Helium Carrier GasHydrogen Flow RatesTable 36 Column (0.22 mm) Flow Rates with Hydrogen Carri

Seite 333

Appendices

Seite 334

Release HistoryUser AssistancePerkinElmer, Inc.710 Bridgeport AvenueShelton CT 06484-4794email: [email protected] information contained i

Seite 336

Appendices392Table 39 Column (0.53 mm) Flow Rates with Hydrogen Carrier GasNitrogen Flow RatesTable 40 Column (0.22 mm) Flow Rates with Nitrogen Car

Seite 338 - Component

Table 43 Column (0.53 mm) Flow Rates with Nitrogen Carrier GasNitrogen Flow Rates (mL/min)Column Diameter: 0.53 mm Optimum Flow: 0.79 ml/minInletPres

Seite 339 - Concentration

395IndexAAC Line Connections 40Accessory 200BCD Kit 186Caps 186Gauze-Loading 286Internal Standard 104, 145, 191, 213Liquid Nitrogen (LN2) 189STS-25 19

Seite 340

Index396BBackflush Configuration 281Baud Rate 124, 172BCDData Logic 185Bend Dimensions of Transfer Line 56Benzene, Sampling 328Binary Coded Decimals (

Seite 342 - Soil Probes

Index398ComplianceEMC Directives 23FCC 23CompoundsSafety Information 24Sampling Emulsions, Liquids 337Sampling Resins, Ointments 338Sampling Solids 33

Seite 344

Index400No Tubes in First-Last 356Oven Fail at Cool Position 362Oven Fail at Idle Position 362Oven Fail at Tube Position 361Robot Arm 354Sealer Fail a

Seite 346 - Sampling Solids

Installation and Setup

Seite 347

Index402GC 47TD/ATD to HP6890 GC 49Transfer Line 51Tubing Requirements 71InstrumentContamination 370Dimensions 37Fault Conditions 352Input Signals 46L

Seite 349 - Troubleshooting 9

Index404In this Manual 16Number of Injections 105, 146, 213OOintments, Sampling 338Open Command 113, 157Open Loop Purging 334Operation 85Double Split

Seite 351 - Status Messages

Index406Purge Time 100, 140RRate, Heat 98, 138, 209ReadyIn Signal 46Out Signal 43Ready/StartCable Assembly 47HP6890 Cable Assembly 49Redesorbing 339Re

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Index408Contacting 381Customer 381SettingAnalysis Options 103, 144Analysis Temperatures 97, 136Analysis Times 99, 139Carrier Gas Flow Rates 77Date 125

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Index410Calculator 115, 158Exit Method Editor 114, 158Log Out 158Reset Command 115Tools Menumaintenance options 160Touch ScreenBrightness 124, 172Inte

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Installation and Setup34Operating Environment on page 35. 2. Read in Safety in the Introduction chapter and ensure that you have complied with the req

Seite 360 - Instrument Fault Conditions

PerkinElmer Life and Analytical Sciences710 Bridgeport AvenueShelton, CT 06484-4794, U.S.A.Internet: http://www.perkinelmer.comemail: info@perkinelmer

Seite 361

Installation and Setup

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Installation and Setup36Table 5 Required Laboratory ConditionsAltitude(operating)Sea level (0 metres) to 2000 m (6,562 feet)Storage(non-operating)You

Seite 363

Installation and Setup

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Installation and Setup38Allow at least 94 cm (3’) on either side of the TD/GC to accommodate additional equipment (for example, the computer).The labo

Seite 365

Installation and Setup

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Installation and Setup40It should be checked by a qualified electrician before you connect the instrument.To avoid interference caused by ground loops

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Installation and Setup

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iContentsIntroduction ...11Introduction...

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Installation and Setup42injector or detector port at the top can be used. This may be the case if you have an older GC or a GC equipped with PPC. Anot

Seite 370

Installation and Setup

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Installation and Setup44The contacts remain closed for 6 seconds. The Start signal is normally used to start a GC run, by connecting it to the GC Star

Seite 372 - Fatal Errors

Installation and Setup

Seite 373 - Edition, (Glasgow, 1996), p27

Installation and Setup46The Fail signal can be generated at a number of points in the sequence, including detection of an empty tube position or an er

Seite 374

Installation and Setup

Seite 375 - The Cold Trap Does Not Cool

Installation and Setup48Connect the opposite end to the GC EXT START pins 3 and 4.Figure 3 Connecting the ATD/TD to the AutoSystem XL GC using the Rea

Seite 376 - Sample Carryover

Installation and Setup

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Installation and Setup502. Locate the I/O port on the rear panel of the ATD/TD.3. Connect the white wire of the cable assembly (P/N N610-0402) to the

Seite 378 - System Contamination

Installation and Setup

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ContentsiiInstalling the Heated Transfer Line... 51Capillary Analytical Column Directly connected to the TD...

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Installation and Setup52Figure 5 Installing the Transfer Line on the AutoSystem XLCAUTIONThe stationary phase of your column must be able to withstand

Seite 381

Installation and Setup

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Installation and Setup54back of the oven outer wall should be visible. See Figure 9.6. Remove both of the PVC end caps from the oven entry insulation

Seite 383

Installation and Setup

Seite 384 - Wide Boiling Range

Installation and Setup56Figure 7 Bend Dimensions for Connecting the ATD/TD Transfer Line to an AutoSystem GC or Clarus 500 GC 4. Remove the cap from t

Seite 385

Installation and Setup

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Installation and Setup589. From the GC end, pass the fused silica transfer line, or the front end of the GC column (as you prefer), through the instal

Seite 387 - Appendices 10

Installation and Setup

Seite 388

Installation and Setup60Figure 8 Connect the Transfer Line to the TD Instrument Vespel FerruleGraphitzed Vespel FerruleStainless SteelSleeveHeatedValv

Seite 391 - Appendix C References

Installation and Setup62Figure 9 Installation of the Transfer Line through the Rear Panel 2. Install a union (P/N 0497-2073 for capillary columns or P

Seite 392 - Appendices

Installation and Setup

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Installation and Setup64are not included in the kit.We recommend that you use the 0.53mm ID Retention Gap kit, Part No. 0497-8449.Installing the Trans

Seite 394

Installation and Setup

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Installation and Setup66(35 kPa), better carrier gas control can be achieved by inserting a length of narrow bore, fused silica tubing, between the co

Seite 396 - Helium Flow Rates

Installation and Setup

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Installation and Setup680497-2066) or the graphite ferrule supplied with the union (not for ECD or MS). After passing the column end through the ferru

Seite 398 - Hydrogen Flow Rates

Installation and Setup

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Installation and Setup70should be installed at every gas line connection. The carrier gas connections require 1/8” tubing with 1/8” parallel compressi

Seite 400 - Nitrogen Flow Rates

Installation and Setup

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ContentsivRun Tab ...162Config Tab...

Seite 402

Installation and Setup72Use only carrier gases with a purity of 99.995% or better. Only top quality gases are suitable; typical laboratory supplies ar

Seite 403

Installation and Setup

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Installation and Setup74compression fitting with which to connect the regulator to the TD. The delivery pressure must be adjustable to 90 psig (620 kP

Seite 405

Installation and Setup

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Installation and Setup76Column Leak Test1. To perform the column leak test, cap one end of the column and/or transfer line with a rubber septa. Connec

Seite 407

Installation and Setup

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Connect the gas supply line to the carrier in port on the rear panel of the TD. 1. Ensure the transfer line has been connected correctly to the GC. Se

Seite 409

Installation and Setup

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Installation and Setup807. Allow a few minutes for the flow to stabilize before disconnecting the flow meter.8. To set the desorb flow, connect a flow

Seite 411

Installation and Setup

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Contents

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Installation and Setup82

Seite 414

Operation 3

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Operation

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Operation86TurboMatrix 350 ATD: Automated sampling of up to 50 tubes, incorporating PPC. Supports pressure, flow and velocity control of the carrier g

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Operation

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Operation88Attention:Before attempting to disconnect the TD/ATD from the GC or to shut off the carrier gas supply, ensure that:• The GC oven and detec

Seite 420

Operation

Seite 421

Operation90Figure 16 Dimensions of the Automated Thermal Desorber (example shown here is the TurboMatrix Series 300 TD) To begin operation of the ATD

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