A SCENT OF FUTURE. Master DHS. Dynamic Head Space Sampler. Operating Manual

Transcription

1 A SCENT OF FUTURE Master DHS Dynamic Head Space Sampler Operating Manual

2 Edition Master DHS - Operating manual rev. 1.0 Warnings The information contained in this document can be updated by DANI Instruments S.p.A. at any time without prior warning. DANI Instruments S.p.A. shall not be held liable for any errors in this manual or improper use of the information contained in it or of the instrument. It is advisable for users to carefully read all the information contained in this manual before using the instrument. Safety information The Master DHS and the Master AS are in compliance with Safety standards EN and CSA C22.2 EN The instruments are in compliance with electromagnetic compatibility standard EN , and The products have been designed and tested in accordance with safety standards for the use in closed environments (Indoor use, Pollution degree 2, Installation category 2). If the instruments are used in a manner not indicated by the manufacturer, the protection devices on the equipments could be damaged. If this occurs, disconnect the units from the electrical power supply and make sure they cannot be started up by accident. The machines should only be serviced by professionally trained personnel. Do not replace parts or make modifications on the instruments unless authorized too do so. Always disconnect the power supply cord before lifting the lid. Users cannot replace the internal fuses. Safety symbols The warnings in the manual and on the instrument must be observed both during operating phases and when servicing the instrument. Failure to observe these rules violates the design and instrument use safety standards. DANI Instruments Spa bears no liability for user failure to observe these rules. Attention!!! Warning Warns of a condition or possible situation which could cause damage or harm the user. Warns of a condition or possible situation which could damage or destroy the product or the operator s work. Indicates a grounded terminal. Indicates a hot surface. Attention! Refers to attached documentation. Indicates hazardous voltages.

3 Table of Contents Technical specifications iii Descriptions 1 Oven 1 Sampling system 1 Dew Stop 1 Trap 2 Transfer line 2 External connections 2 Pneumatics 3 Installation 4 Environmental conditions 4 Positioning 4 Pneumatic supply 4 Connection to gas chromatograph 5 External connections 6 Leak test 6 Operating principle Analytical Cycle 7 Incubation 7 Stripping 8 Trap dry step 9 Injection 10 Baking 11 User Interface 12 Status bar 12 Desktop 16 Tool bar 17 Devices status and ready conditions 19 Status 20 Operation 22 Loading/unloading vials 22 Control of analysis 23 i

4 Cycle 24 Method 27 Sequence 30 Options 36 Setup 37 Maintenance 38 Temperatures 38 Valves 39 Gases 39 Movements 40 Trap Cleaning 41 Calibration 42 Parts and replacement 43 Removing the trap 43 Filling the trap 43 Assembling and conditioning the trap 44 Replacing the transfer line needle 44 Replacing the sampling needle 45 Cleaning the instrument 46 Handling precautions 46 Leak test 46 Diagnostics 49 Diagnostic 49 Alarms 50 Master AS 54 Introduction 54 Description 54 AS parameters 58 AS sequence 61 AS status 62 Maintenance 62 Consumables 64 ii

5 Technical specifications Master DHS is an automatic sampler for dynamic headspace analysis able to automatically sample up to 65 vials. The system uses the principle of a dual needle and a packed focusing trap: compatible with the standard gas chromatographs (GC) and GC/mass spectrometry (GC/MS) systems and with both packed and capillary columns. Master DHS unit CONFIGURATION Hardware configuration Capacity Samples Stand alone 18-place electrically driven carousel standard 20 ml headspace vials with crimped or screw magnetic caps and PTFE coated silicone rubber septa ANALYTICAL SYSTEM Methods up to 25 methods stored Oven temperature: 40 to 300 C, increment 1 C time: 0 to 999 min, increment 0.1 min shaking: no, slow, fast Switching valve Focusing trap Dew Stop Transfer line Sample pathway Sampling needle 10 ports, electrically actuated temperature: 40 to 300 C, increment 1 C packed focusing trap stripping temp.: 10 C above ambient to 40 C, increment. 1 C (-10 C to 40 C with optional cooling device) dry step temp.: 10 C above ambient to 40 C, increment. 1 C (-10 C to 40 C with optional cooling device) injection temperature: 40 to 450 C, increment 1 C baking temperature: 50 to 450 C, increment 1 C direct resistive heating 900 C/min heating rate to 450 C material: quartz programmable Dew Stop device temperature: 0 to 225 C, increment 1 C water removal stainless steel internally coated with inert material, inner diameter 0.80 mm length: 0.80 m temperature: 40 to 300 C, increment 1 C stainless steel coated with inert material dual needle design dynamic headspace mode (standard) purging mode (optional) iii

6 Technical Specifications PNEUMATICS Carrier gas Auxiliary gas digital pressure reading safety control on carrier gas presence max. inlet pressure: 9 bar electronic flow control flow rate: 10 to 150 ml/min precision +/- 0.1 ml/min maximum inlet pressure: 9 bar OPTIONS Optional trap cooling device electrical cooling device COMMUNICATIONS Input/Output signal Communication Interface LAN, USB, n 1 RS232 for service, n 2 RS232 to autosampler start out: contact closure at start injection ready in: contact closure from GC at sample sequence ready to start and trap ready to inject TOUCH SCREEN GRAPHIC USER INTERFACE Display LCD TFT, 5.7 Resolution 240x320 pixel Colors 65,536 POWER SUPPLY Power supply automatic selection: / V~, 60 Hz, 1300 VA / V~, 50 Hz, 1300 VA DIMENSIONS Size (W x H x D) Weight 450 x 490 x 560 mm 55 kg iv

7 Technical Specifications Master AS unit CONFIGURATION System type XYZ robot Vial volume 20 ml crimped or screw magnetic cap vials Vial capacity 65 Solvent 2 (10 ml vials) Waste 2 (10 ml vials) Standard solution 6 (10 ml vials) Syringe 5, 10, 25, 100, 250, 500 μl Injection volume range 0.1 μl 500 μl Priority sequence yes Sample overlapping with constant incubation time Parameter control pre standard addition solvent washing post standard addition solvent washing standard rinse standard addition vial depth syringe stroke before standard addition plunger sampling and standard addition speed viscosity delay solvent volume internal standard volume Sample washing up to 25 Pre standard adding washing up to 25 Post standard adding washing up to 25 Standard addition per vial up to 4 different standards User interface Master DHS touch screen graphic user interface Data communication 1 RS232 port 1 start out signal 1 ready in signal Power supply V (Autoranging) Size (W x H x D) 455 x 750 x 650 mm Weight 13 kg v

8 Description The Master DHS is an automatic sampler for analysis of volatile and semi-volatile compounds in liquid or solid samples. The samples are directly placed into the Dynamic Headspace Sampler in standard 20 ml vials that can be heated at a chosen temperature, if necessary. An inert gas flow is used to purge the sample in order to carry out the volatile compounds; then the purged gas passes through a cooled trap where the compounds are concentrated. The trap is quickly heated in backflush to a high preset temperature transferring the compounds to the chromatographic column in a narrow band and a reduced volume of gas. The Dew Stop device removes humidity from the desorbed gas before entering into the GC or GC/MS system. The Master DHS is able to automatically sample up to 65 vials. It can be easily connected and synchronized to any gas chromatograph for an automatic and reliable management of the entire analytical system. Oven The DHS oven contains the carousel for the vial housing and incubation. The sample carousel, able to hold up to 18 vials, can be heated from 40 C to 300 C. Vials can be automatically inserted in the carousel by using the Master AS autosampler or manually by the operator that moves the Carousel and the Insertion and Sampling Lifters in the Load/Unload page. The carousel can be moved in both directions using the buttons in the Movement page of the Maintenance. In this page it is also possible to move up and down the Insertion and Sampling Lifters. Sampling system Switching Valve The sampling system is composed of an electrically activated 10 port valve that can switch between two positions in order to concentrate the compounds into the trap in one step and let the carrier gas pass through the trap in the other. It can be heated from 40 C to 300 C. Sampling needle The sample stripping is managed through a dual needle. In the dynamic headspace needle (standard) the stripping gas flows from an orifice at the middle of the needle and is recollected through the two orifices in the upper part. In the purging needle (optional) the orifice in the lower part allows the liquid purging to be performed directly in the sample solution. Dew Stop The Dew Stop is a device especially designed to remove humidity from the desorbed gas before entering the GC or GC/MS system. It is kept at low temperature during the injection phase and is heated during the baking step to eliminate retained water. It can be cooled to 0 C using a Peltier cell electric system and can be heated up to 225 C. 1

9 Description Trap The trap consists of a 90 mm long quartz tube with a 4 mm outside diameter. The ends are connected to special fittings with PTFE seals. The trap included in the instruments standard accessories is filled with Tenax GR mesh for approximately 4 cm. It is possible to purchase other pre-filled traps, single or multi-layer, or empty traps to fill according to the instructions described in the Maintenance chapter. The pneumatic configuration is designed in order to desorb the trap in counter current to the collection. This condition facilitates desorption of compounds at a high boiling point and is compatible with use of a multi-layer trap. Trap heating and cooling devices In the Master DHS standard configuration cooling is achieved using an electrically controlled fan and the minimum temperature reached is 10 C above ambient temperature. It is possible to install an optional Peltier cell electric cooling device. The minimum temperature reached in this case is -10 C. In both cases heating occurs through a spiral heating element and the maximum desorption temperature is 450 C (according to the sorbent material) or 400 C when the cooling device is installed. Transfer line The transfer line connects the headspace sampler to the gas chromatograph. It is a 0.80 mm inner diameter, 80 cm length stainless steel tube internally coated with inert material. It can be heated from 50 up to 300 C. A needle is screwed at the end of the transfer line to be introduced into the gas chromatograph injector (see Installation chapter). External connections The Master DHS has the following external connections: power supply LAN port USB port two RS232 serial outputs remote control output The connections are located on the rear of the instrument (see Installation chapter). 2

10 Description Pneumatics The instrument is equipped with two separate inlets on the rear for carrier gas (CARRIER IN) and auxiliary gas (AUX IN). The carrier gas is supplied and regulated by the gas chromatograph. However inside the sampler there is a digital pressure control which detects the presence of gas (PM). If the carrier gas pressure is lower than 50 mbar, the instrument signals an error condition and the sequence can not be started. The carrier gas flows to the injector through the transfer line. The auxiliary gas is used to strip analytes from the sample and concentrate them into the trap. It is possible to use a different gas rather than the carrier gas (usually Nitrogen). The auxiliary gas is regulated by an electronic flow control (EFC). It is possible to set different auxiliary flow values for the stripping, dry step and baking steps (see Operation chapter). 1: AUX EV 3: VENT 1 EV : CARRIER EV 9 8 SWITCHING VALVE 3 4 TRAP DEW STOP 4: VENT 2 EV Figure 1 Pneumatics. 3

11 Installation Environmental conditions The Master DHS must be installed in an environment with suitable temperature and humidity conditions for best operation and long life. The Master DHS can operate in a temperature range from 0 to 40 C and in a relative humidity range from 5 to 95 %. Maximum altitude is 2000 meters. However, the instrument performs best at C room temperature and relative humidity of 40 % to 50 %. Exposure to corrosive, gaseous, liquid or solid substances can damage the material used in Master DHS and therefore must be avoided. Positioning A laboratory bench with a free surface space of approximately 75 cm deep and 55 cm wide (80 cm deep and 100 cm wide with the autosampler) and able to support at least 60 kg (75 with the autosampler), is suitable for installing the Master DHS. It is also important to leave a space of at least 20 cm behind the instrument to allow the electronic parts to cool properly. The instrument is approximately 55 cm high (110 cm with the autosampler); the area above must be free from shelves or other obstacles which would limit the access to the upper part of the instrument and suitable air circulation. The instrument is normally installed on the left side of the gas chromatograph. The maximum distance from the gas chromatograph must consider the length of the transfer line which is approximately 80 cm. Pneumatic supply Choosing the gas type The Master DHS is equipped with two distinct inlets for carrier and auxiliary gas. The maximum inlet pressure allowed is 9 bar (130.5 psig). It is better to use a two stage pressure regulator upstream from the lines and a single stage regulator near the instrument. The gas must have a high level of purity because volatile organic compounds in the gas could contaminate the trap and be released during desorption. It is better to install filters on the gas lines to eliminate hydrocarbons, oxygen and humidity and to achieve the best performance. The choice of carrier gas is primarily based on the analysis and the type of detector installed on the gas chromatograph. The auxiliary gas can be different from the carrier gas because the inlets are separate. Usually Nitrogen is used because of its density and low cost. Attention!!! When using Hydrogen as carrier gas, be very careful to avoid the formation of explosive Air/ Hydrogen mixtures. Carefully check the seal on the lines which supply the Hydrogen. Hydrogen must not be used as auxiliary gas! 4

12 Installation Choosing the gas type Connect the instrument to the supply line using preconditioned steel or copper tubing with the minimum number of connections possible. Do not use plastic tubing as it is permeable to Oxygen and other substances and could contaminate the column or detector. Do not ever clean the tubing with organic solvents as any remaining solvent could build up in the trap. The tubing diameter is based on the distance between the instrument and the gas supply source and the total gas flow rate required. A 1/8" tubing, as the one supplied with the instrument, is suitable for most cases. The gas inlets, located on the back of the instrument, consist of 1/8SW male bulkhead connectors. To connect the pipes proceed as follows: Cut the tubing to the desired length. Always leave it slightly longer for minor movements of the instrument. Fit a 1/8SW ss nut (cod ) on the tubing and a brass seal (cod ) with the conical part facing outwards. Both pieces are equipped with the instrument. Insert the tubing to the bottom of the gas inlet connector and finger-tighten the nut With a 7/16" wrench tighten the nut 1 and 1/4 turns. Check the seal on the pneumatic line. Connection to Gas Chromatograph Connecting the transfer line Connect the Master DHS sampler to the gas chromatograph by inserting the end of the transfer line in the gas chromatograph injector. The needle has dimensions of 0.7 mm outer diameter and 0.4 mm inner diameter (cod ) and can be used on injectors for packed and capillary columns. To prevent the transfer line needle from blocking during insertion, unscrew the injector septum holder and insert the needle in the septum. Then screw the septum holder again with the needle inserted. In addition, to prevent the needle from bending, replace the capillary injector flat septum holder with the high septum holder available for DANI gas chromatographs or use the proper strain relief available for other gas chromatographs. Connecting carrier gas In the standard configuration, the instrument is setup to use the gas chromatograph carrier gas regulation system and thus the standard configuration is not equipped with any pressure or flow rate regulator. Effectuate the connection as described below: Intercept the gas chromatograph carrier gas line near the injector. Connect the carrier gas supply tubing to the CARRIER inlet on the back of the instrument using an 1/8SW adapter. Close the line towards the injector (by using for instance a union and a nut). Regulate the pressure or gas flow rate directly from the gas chromatograph. Note: adding an external circuit to the carrier gas line causes additional pressure drop which cannot be calculated. Thus may be possible that the carrier gas flow rate calculated by the gas chromatograph (when this option is available) is much higher than that actually demonstrated. 5

13 Installation External connections Remote control DANI Master DHS communicates with the gas chromatograph via two remote controls: A connection for receiving the signal from the gas chromatograph when it is in Ready condition (Ready in). Note: in standard conditions, the instrument is configured to receive the Ready IN command as a closing contact, this mode is used by DANI gas chromatographs. If the instrument is to be connected to a gas chromatograph which produces an opening contact, the configuration in the Setup page has to be modified (see "Setup" chapter). A connection to send to the gas chromatograph the start signal (Start out). Note: in standard conditions, the instrument is configured to send the Start out command as a closing contact, this mode is used by DANI gas chromatographs. If the instrument is to be connected to a gas chromatograph with a normally closed contact, the configuration in the Setup page has to be modified (see "Setup" chapter). To connect the remote controls, insert the remote connection cable (Cod ) in the RMT connector on the back of the instrument. Connect the wires to the DANI gas chromatograph as follows: Master DHS Start OUT (orange/brown wires) - GC Start IN Master DHS Ready IN (gray/green wires) - GC Ready OUT If connecting to other gas chromatographs, refer to the instructions provided for each system. Leak test After Master DHS has been assembled and connected to the gas chromatograph, it is advisable to effectuate a leak test on the entire pneumatic circuit, from the carrier gas inlet to column outlet. This procedure should be repeated every time a modification is being made on the system, for example column or transfer line replacements. Proceed as follows: Disassemble the detector head and close the main body with the specific cap or disconnect the column from the detector; in case a capillary column is used insert a silicone rubber septum in its end; when a packed column is used close it with a cup nut Leave the Master DHS in stand-by conditions, and regulate the carrier gas pressure to approximately 2 bar (30 psig). Wait a few minutes for the pressure to stabilize in the entire system and check the value of the current pressure. Turn off the pressure supply and check the value reading. After a minimum decrease, the pressure value has to be constant. In case, after approximately 5 minutes, the pressure drop is less than 0.04 bar, the system is sealed. If the pressure decrease is more than 0.04 bar, it means that there is a leak in the system. Repressurize the system and find the leak by using a soapy solution. Find the leak, tighten the fitting until it is eliminated and repeat the leak test. Replace the detector or remount the column. 6

14 Operating principle - Analytical cycle Incubation In the first step of the analysis the vial is inserted into the oven, which is kept heated at a preset temperature (Oven Temp). This operation can be managed using the Automatic Sampler or directly by the operator. If the Automatic Sampler is enabled, the vial is moved from the tray to the DHS while the carousel rotates bringing the chosen position to the insertion lifter, which is moved up. When the vial is to be removed with the Master AS, the carousel rotates and the insertion lifter is consequentially moved to allow the automatic sampler to bring the vial back to the tray. Using the Automatic Sampler allows to keep a constant incubation time. Without the Automatic Sampler all vials must be inserted in the carousel before the sequence is started (See chapter Operation - Loading/Unloading vials ). EFC 1: AUX EV 3: VENT 1 EV : CARRIER EV 9 8 SWITCHING VALVE 3 4 TRAP DEW STOP 4: VENT 2 EV Figure 2 Incubation. 7

15 Operating principle - Analytical cycle Stripping In this step the vial is pierced by the double needle and flushed with a flow of inert gas for a certain period of time. The stripped compounds are then concentrated in the cold trap. At the beginning of this phase the carousel rotates bringing the vial to the sampling lifter position. The flow regulator of the auxiliary gas (EFC) opens and brings the flow to the preset value (Stripping Flow). The AUX EV is activated to allow the passage of auxiliary gas through the needle and the VENT 2 EV closes. The SWITCHING VALVE rotates to enable the trapping on the auxiliary gas line and the sampling lifter is moved up. The sample is purged with the auxiliary gas flow for the preset time (Stripping Time) and the compounds are concentrated in the trap, which is kept at the Stripping Trap Temperature. EFC Stripping flow 1: AUX EV 3: VENT 1 EV : CARRIER EV FROM GC TO GC 9 8 SWITCHING VALVE 3 4 TRAP : VENT 2 EV DEW STOP Figure 3 Stripping. 8

16 Operating principle - Analytical cycle Trap dry step In order to remove part of the humidity from the trap prior to GC injection, a trap dry step can be performed. During the trap dry step the AUX EV is not activated and VENT 1 and VENT 2 EV are closed. The auxiliary gas is regulated to the trap dry step setpoint and the SWITCHING VALVE is rotated to enable the trap on the auxiliary gas line. The auxiliary gas flows directly to the trap, kept at the Trap Dry Step temperature, and then to the needle. EFC Stripping flow 1: AUX EV 3: VENT 1 EV : CARRIER EV FROM GC TO GC 9 8 SWITCHING VALVE 3 4 TRAP : VENT 2 EV DEW STOP Figure 4 Trap dry step. 9

17 Operating principle - Analytical cycle Injection At the end of the Stripping (or Dry Step) phase the SWITCHING VALVE rotates and the trap is disabled from the auxiliary gas circuit. The Carrier EV activates to allow first the passage of carrier gas through the trap, heated to the set temperature (Injection Trap Temp), and then to the Dew Stop device, kept at low temperature (Injection Dew Stop Temperature) to remove humidity. The trap desorption phase starts and persist for the time established by the method (Injection Time). At the same time, the sampler sends a start signal to the gas chromatograph to initiate the chromatographic analysis and the auxiliary gas regulator closes. At the end of this phase the CARRIER EV returns in its previous state. EFC 1: AUX EV 3: VENT 1 EV : CARRIER EV FROM GC TO GC 9 8 SWITCHING VALVE 3 4 TRAP DEW STOP 4: VENT 2 EV Figure 5 Injection. 10

18 Operating principle - Analytical cycle Baking In this step all the system is cleaned at high temperature in order to condition the trap and remove traces of condensed water or sample. At the beginning of this phase the auxiliary gas is regulated to the Baking setpoint, the VENT 1 EV is closed (while the VENT 2 EV is kept open) and the SWITCHING VALVE rotates to enable the Trap and Dew Stop to be on the auxiliary gas circuit. For the first 3 seconds the AUX EV is activated to clean the lower hole of the needle and then it returns to its previous state. The auxiliary gas flows to the trap and the upper hole of the needle and to the Dew Stop and Vent 2. (Trap and Dew Stop are both heated to their Baking Temperatures). 1: AUX EV 3: VENT 1 EV : CARRIER EV FROM TO GC 9 8 SWITCHING VALVE 3 4 TRAP : VENT 2 EV DEW STOP Figure 6 Baking. 11

19 User interface All Master DHS functions, including autosampler programming, can be managed by the innovative touch screen interface. The display allows to access to every parameter by no more than four touches on the touch screen. The display can be divided in three blocks (Figure 7): Status Bar Desktop Tool Bar Figure 7 Display. Status bar The Status bar is on the bottom of the screen. In this section you can find Menu, Status and Time Clock. Menu This section allows to gain access to many functions and to select the submenu (Figure 8). Refer to each specific chapter for details. 12

20 User interface Figure 8 Menu. Menu and Submenu items are reported in the table below together with the chapter of the manual where you can find detailed information. MENU SUBMENU REFERENCE CHAPTER Cycle - Operation - Cycle Devices Status - Devices status and ready conditions Load/Unload - Operation Loading/Unloading vials Master AS Sequence Master AS AS sequence Parameters Master AS AS parameters Setup Master AS - Setup Maintenance Master AS - Maintenance Tools Setup Operation - Setup Diagnostic Diagnostic Maintenance Maintenance Calibration Calibration Options Operation - Options Lock/Unlock Status This section is able to show in real time the DHS status. A different inscription is shown depending on the actual status of the system: READY, WAITING GC READY, WAITING GC (min:s), CONDITIONING (min:s), WAITING, AUTORUN, RUNNING, PAUSE, ABORT, ABORT & BAKING (see Chapter Devices status and ready conditions ). If you press on this bar a window Status will appear. This window consists of five pages: DHS, Sequence, Vial, Alarms and Log. 13

21 User interface DHS When a component of DHS is not in the ready condition (Oven, Switching Valve, Trap, Dew Stop and Transfer Line), the red inscription Not Ready will be visualized (Figure 9). Figure 9 Ready - Not Ready status. Figure 10 DHS Status. When the analysis is running, six blue bars are displayed which describe the progress of the cycle and of the single steps of the analysis and the remaining times (Figure 10). Sequence The Sequence page shows a frame where you can follow the parameters of the sample sequence: sequence row, vial and current repetition (Figure 11). If the Master AS is setup the AS Status frame is also shown by means of a label with the current status of the Automatic sampler. Figure 11 Sequence status. 14

22 User interface Vial In the Vial page 18 circles representing the positions in the DHS carousel are shown. During the run the number of the vial (or a V in case of AS Sequence control OFF) located in the corresponding position of the carousel appears in the middle of the circle (Figure 12). Figure 12 Vial status. Alarms In the Alarms page (Figure 13) you can find all the messages concerning problems or advices. To gain access to this page, press the exclamation mark blinking on the right of the status bar (see Alarms in the chapter Diagnostics ). Figure 13 Alarms page. 15

23 User interface Log This page contains information on problems that may have occurred during the sampling sequences. Time clock and date This section allows to read time and date. If you press here, the window Time & Date will appear. Open the page Time (Figure 14) and enter hours, minutes and seconds in the three boxes to set the time. To set the date, open the page Date (Figure 15) and select month, day and year. Figure 14 Clock. Figure 15 Date. Desktop The desktop is the central portion of the display. Here you can find five buttons that allow to gain access to the following components: Cycle, Devices Status, Start/Stop, Carousel Sequence/AS Sequence and Trap Cleaning. CYCLE (see chapter Operation/Cycle) DEVICE STATUS (see chapter Device status and ready conditions) CAROUSEL SEQUENCE/AS SEQUENCE (see chapter Operation - Sequence) These buttons are alternatively displayed on the toolbar depending on the kind of sequence that is selected. In both cases this shortcut key opens the sequence table window. 16

24 User interface TRAP CLEANING (see chapter Maintenance Trap cleaning). START/STOP These two buttons are alternatively displayed on the desktop. When the instrument is out of an analysis, the START button is displayed. If an analysis is in progress, the STOP button is available. (see Control of analysis in the chapter Status ). Tool bar The Tool bar (Figure 16) is positioned on the top of the display and consists of three parts: the upper left side, where the name of the current method is shown. If you press on this inscription, the Manage Methods page will be available. (see the chapter Method ) the upper right side, where the name of the window opened is displayed. the lower rows where seven shortcut keys allow to start an application (Start, Stop, X for window closing) or to alternate between windows corresponding to Cycle, Device Status, Carousel Sequence/AS Sequence and Load/Unload. Figure 16 Tool bar. START STOP (see Control of analysis in the chapter Status ). (see Control of analysis in the chapter Status ). CYCLE Press the shortcut key in order to open the Cycle window and set all the analytical parameters. The cycle consists of six pages (see chapter Operation - Cycle): Incubation Stripping Dry Step Injection Baking Others DEVICE STATUS This shortcut key opens the Devices Status windows, with the Temperatures and Press/Flow pages. (see chapter Devices status and ready conditions). CAROUSEL SEQUENCE/AS SEQUENCE These buttons are alternatively displayed on the toolbar depending on the type of sequence that is selected. In both cases this shortcut key opens the sequence table wind window (see chapter Operation - sequence). 17

25 User interface LOAD/UNLOAD This button opens the load/unload page, where you can move the carousel and the Insertion and Sampling lifter in order to load vials without using the Automatic sampler (see chapter Operation Loading /unloading vials). This page is disabled when AS sequence control is ON. The last button represents an X and allows to close the windows and to return to the desktop. How to enter a value? In order to set a parameter you have to press on the corresponding box and a numeric keypad will appear (see Figure 17). Digit the value and press OK. Figure 17 Numeric keypad. 18

26 Device status and ready conditions In the Device Status window you can control the actual value and the set value for the listed parameters. Besides, you can find the Ready conditions - Rdy function. When all the parameters checked for the Ready Conditions satisfy the set conditions, the instrument reaches the Ready status. The Device Status window contains two tabs: Temperatures and Press/Flow. The parameters available in the Temperatures page (Figure 18) include all the devices that have a temperature regulation, that is Oven, Switching Valve, Trap, Dew Stop and Transfer Line. The tolerance on the ready condition is different for each device, depending on its characteristics and the type of heating/cooling systems. In the Default method, the Ready conditions for the oven, switching valve, Dew Stop and transfer line temperatures are active. To eliminate a parameter from the ready condition, press on the corresponding check box and cancel the check. To include a parameter in the Ready conditions, press on the corresponding check box to display the check. When a parameter, selected for the Ready condition, has not reached its setpoint yet, it will be visualized in red. Figure 18 Temperature page. In the Press/Flow page (Figure 19) you can find the Auxiliary Gas Flow and Carrier Gas Press parameters. For the auxiliary gas flow the current actual and set values are visualized. When a sequence is started a control of the auxiliary gas presence is performed: if the auxiliary stripping flow setpoint of the current method is not reached (or if the control fails) the sequence is automatically aborted. A control of the auxiliary gas presence during the run is also performed; if the auxiliary gas is too low the sequence will be aborted. In both cases a new message will be displayed in the log file. 19

27 Device status and ready conditions Carrier Gas Press visualizes the pressure of carrier gas coming from the gas chromatograph. If there is no carrier gas it is not possible to start the analytical sequence. Status Instrument condition Figure 19 Pressure/Flow page. The status of the instrument is shown on the Status Bar where the operative steps of the DHS are reported. READY READY indicates that all the devices selected as ready conditions (see Ready conditions) have reached the values initially set in the method in the Cycle pages. The Status bar will show the message READY. The Oven, Switching Valve and Transfer Line Temperatures are set in the Incubation and Others pages and remain constant during all the analytical cycle. The Trap and Dew Stop Temperatures considered for the ready condition are the values set in Stripping and Injection pages, respectively. The instrument can only accept the START command after all conditions are shown as Ready. WAITING GC READY When the gas chromatograph is not in the ready condition at the end of a sequence line and the following line has to be started, the instrument passes to the WAITING GC READY step. The instrument will remain in this condition until the gas chromatograph reaches the ready condition and the following line is started. WAITING GC (min:s) When the DHS cycle on one vial is ended and the instrument is waiting before starting the cycle on the next vial, in order to respect the GC ready interval, the label WAITING GC, with the corresponding countdown is shown. The cycle on the next vial will start at the end of the countdown. 20

28 Device status and ready conditions CONDITIONING (min:s) When the DHS cycle on one vial is ended and the instrument is waiting before starting the cycle on the next vial, in order to respect the DHS cycle and cooling time, the label CONDITIONING, with the corresponding countdown is shown. The cycle on the next vial will start at the end of the countdown. WAITING When one or more DHS components are not in the ready condition, for instance at the end of the cooling step, when Dew Stop and Trap temperatures reach the values set for the standby condition, the instrument passes to the WAITING step. The instrument will remain in the WAITING condition until all the parameters reach the initial condition set in the method (See Ready conditions). AUTORUN When a sequence is started and the instrument is not in Ready condition the inscription AUTORUN will appear on the Start icon (see Method and Sequence in the chapter headed Method ). Pressing this shortkey, the DHS passes in Autorun condition. In this case when all ready conditions are reached, the sequence will start automatically. RUNNING This label is shown while the analysis is running. PAUSE This label will appear after a sequence is stopped, remaining until one of the possible options is selected to continue. ABORT This label will appear when the Abort option is selected and will be displayed until the Abort procedure is ended. ABORT & BAKING This label will appear when the Abort & Baking option is selected and will be displayed until the Abort & Baking procedure is ended. 21

29 Operation Loading/Unloading vials Master AS enabled If a Master AS sequence is started the vials will automatically be inserted from the tray in the carousel at the requested time, according to the set parameters. When the stripping on a vial is ended (according to all the repetitions) the vial is ready to be removed by the Autosampler. The use of Master AS allows sample overlapping with constant incubation time. Master AS disabled If the Master AS is disabled the vials have to be inserted by the operator before any sequence is started. Enter the Load/Unload page pressing the Menu, Load/Unload or the shortkey on the tool bar (this page will be disabled when a Master AS sequence is selected). A Warning pop-up will automatically appear to remind that vials can be hot. Pressing Ok the Load/ Unload page will be accessible (Figure 20). In this page, 18 circles representing the position of DHS carousel are shown: the slot corresponding to the insertion lifter position will be marked in blue (Figure 21). Select the position where the vial has to be loaded: the carousel will automatically move to bring the chosen position to the insertion lifter; press on the arrow to move the insertion lifter up (Figure 22). Insert the vial, then press on the arrow to bring the lifter down (Figure 23). Repeat these operation lo load all vials. Figure 20 Warning pop-up. Figure 21 Load vial: lifter up position. 22

30 Operation Figure 22 Load vial: lifter up position. Figure 23 Load vial: lifter down position. Control of analysis Start of analysis The analysis starts by pressing START positioned in the middle of the desktop or the shortkey on the tool bar. The START command determines the start of the sequence and will only be accepted if the instrument is in READY condition. If the instrument is not in Ready condition and a sequence is activated the inscription AUTORUN will appear instead of the START icon. Pressing this shortkey, the DHS passes to AUTORUN condition (See AUTORUN in the chapter headed Instrument condition ). In this case, when all ready conditions are reached, the sequence will start automatically. End of analysis The analysis will end automatically when the analytical cycle for the vials in the sequence is completed. However, the analysis can be stopped before completion of the program by pressing STOP in the middle of the desktop or the shortkey on the tool bar. When you press STOP the Master AS will enter the Pause state and a pop-up will appear (Figure 24). Selecting Resume the sequence will restart from the point it was stopped. Selecting End cycle the sequence will be stopped but the cycle on the current vials (or the vials still present in the carousel in AS sequence) will be completed. Pressing Abort or Abort & Baking both analysis and sequence will be interrupted; in the case of Abort & Baking a Baking step with the conditions set in the current method will be executed. When you press STOP the Master AS will immediately stop in its current position. The Master DHS will stop or go on with the analysis when one of the four options is selected. 23

31 Operation Attention!!! If you press stop when the Master AS is removing one vial from the DHS and other vials are still present in the carousel, it is possible that the vial is kept in that position until the analysis on the vials in the carousel are ended. Finally all the vials will be removed. In all cases, all the operations necessary to preserve the correct handling of the vials and do not influence the correct overlapping of the analysis times will be taken. Figure 24 Sequence stop. At the next START, the sequence will start from the first repetition of the first level. In case the sequence is interrupted, the instrument will return to the conditions of the first method of the sequence. Cycle The analytical Cycle is composed of five steps: Incubation, Stripping, Dry Step, Injection and Baking. The Cycle window consists of five pages, one for each step, and an additional page Others, where all method parameters can be set. In the lower part of each Cycle page the analysis times information is displayed. The DHS Cycle Time label indicates the sum of the duration of the five steps: Incubation, Stripping, Dry Step, Injection and Baking. The Cycle Total Time indicates the time between one injection and the following one, according to the GC ready interval parameter (see paragraph Others for details). In order to set a new value for any parameter press on the correspondent textbox and use the numeric keypad to type the value (Figure 25). If you enter a value out of the allowed range the message Out of range with the indication of the correct range will be shown (Figure 26). The minimum or maximum value allowed will be automatically saved by pressing OK. 24

32 Operation Figure 25 Numeric keypad. Figure 26 Out of range. Incubation The parameters associated with this step are Incubation Time, Oven Temperature and Shaking. The incubation time is the time during which the vial is conditioned in the oven at a fixed temperature before the stripping is started. The use of the Master AS automatic sampler allows the incubation time to be kept constant for all samples. If the shaking option is enabled the carousel will be kept moving, clockwise and counter-clockwise, during the incubation in order to keep the samples stirred. To select the shaking option press on the dropdown menu and chose one of the two options. In the table below units of measurement, interval range and default values for all parameters are shown: Parameter Measurement Unit Interval Default value Incubation Time min from 0,0 to 999,00 0,0 Oven Temp C from 25 to Shaking - NO, slow, fast NO Stripping The parameters associated with this step are Stripping Time, Stripping Flow and Trap Temp. In the table below units of measurement, interval range and default values for all parameters are shown: Parameter Measurement Unit Interval Default value Stripping Time min from 0,00 to 999,00 10,00 Stripping Flow ml/min from 10,0 to 150,0 30,0 Trap Temp. C from -10 to

33 Operation Trap Dry Step The parameters associated with this step are Dry Step Time, Dry Step Flow and Trap Temp. In the table below units of measurement, interval range and default values for all parameters are shown: Injection Parameter Measurement Unit Interval Default value Dry Step Time min from 0,00 to 999,00 0,00 Dru Step Flow ml/min from 10,0 to 150,0 30,0 Trap Temp. C from -10 to The parameters associated with this step are Injection Time, Trap Temp and Dew Stop Temp. In the table below units of measurement, interval range and default values for all parameters are shown: Parameter Measurement Unit Interval Default value Injection Time min from 0,00 to 15,00 1,0 Trap Temp. C from 40 to Dew Stop Temp. C from 0 to Usually an injection time of 1 minute is enough to transfer all the compounds to the GC. Baking The parameters associated with this step are Baking Time, Trap Temp and Dew Stop Temp. In the table below units of measurement, interval range and default values for all parameters are shown: Parameter Measurement Unit Interval Default value Baking Time min from 0,00 to 30,00 5,00 Baking Flow ml/min from 10,0 to 150,0 80,0 Trap Temp. C from 50 to Dew Stop Temp. C from 50 to The baking parameters are to be chosen according to the analysis conditions. Others In this page you can find all the parameters that remain constant during the whole analytical cycle. In the table below units of measurement, interval range and default values for all parameters are shown: Parameter Measurement Unit Interval Default value Transfer Line Temp. C from 40 to Switching Valve Temp. C from 40 to Trap Max. Temp. C from 40 to GC Ready Interval min from 0,00 to 999,00 10,00 26

34 Operation The Trap Max Temperature is the highest temperature to which the trap can be heated and any damage to the sorbent material can be prevented. If any of the trap temperature setpoints in the cycle is higher than the trap maximum temperature, a blocking alarm will be displayed and the start will be disabled. The GC Ready Interval indicates the minimum time interval between one injection and the next (analysis time plus cooling time); it is suggested to insert a value slightly higher to ensure that the GC will be ready at the end. The Master DHS will automatically calculate the time between one injection and the other (indicated as Total Cycle Time in the lower part of all Cycle pages), in order to respect both the GC ready interval time and the DHS cooling time. In this way, the second vial, as also the following ones, can undergo incubation and stripping before the previous analysis has been completed and the GC is in Ready condition. Method How to create a method? A method controls the functioning of the instrument during the analytical runs. To create a method is necessary to specify all the parameters of the analytical cycle (See Cycle Chapter for details). If the Master AS is setup all the AS parameter will be included in the method. Pressing on the method name, the "Manage Methods" window will appear. Figure 27 Manage methods. 27

35 Operation In the area of dialog "Active Method" of the "Manage Methods" page (Figure 27), you can find three options: to save the modification preserving the same name of the loaded method. This function is active if: The current method has been modified. The active method is different from the Default method. to save the parameters entering a new method name. This key is not active when: The instrument is running. The maximum number of stored methods is used. In order to enter a new method name an alphanumeric keypad will appear. Insert the name and press OK to confirm (Figure 28). to create a new method starting from the Default method. This function is not active if: The instrument is running. The maximum number of stored methods is used. All saved methods are listed in the frame "Stored Method" (Figure 29). Figure 28 Keypad. Figure 29 Stored methods. 28

36 Operation Pressing on the name of method you want to select, four options will be activated. allows to load a method. This function is active if : The current method has been modified. If the current method has been modified and not saved, before loading the selected method, the pop-up "Save Active Method" will open (Figure 30); by answering "Yes", the changes to the current method will be saved, answering "No" they will be lost. allows to copy a memorized method and to save it with a new name. This key is not active when: The maximum number of stored methods is used. allows to eliminate a method. This function is not active if: The instrument is running. Pressing Delete a pop-up "Delete Method" (Figure 31) will be displayed. If you are sure you want to eliminate the method, reply "Yes" to the question. Figure 30 Save active method pop-up. Figure 31 Delete method. allows to change the name of the method. The function is available when: The current method has been modified. 29

37 Operation Sequence Carousel and AS Sequence The "Sample Sequence window allows to set all parameters concerning the sampling sequence. The sequences can be run using the Master AS or by inserting the vials directly into the carousel using the Master DHS interface in the load/unload page (See Operation chapter for details). The Carousel Sequence/AS Sequence buttons are alternatively displayed both on the toolbar and on the desktop depending on the kind of sequence that is selected. When Master AS is setup you can gain access to the Sequence Table also pressing Menu, Master AS, and then Sequence. In the "Sample Sequence" window you can choose between Master AS and Carousel Sequence by pressing one of the two buttons, that are alternatively activated. Attention!!!! When you change from a carousel sequence to a Master AS sequence the Check vials in oven window will appear (Figure 32). This reminds that any vial still present in the carousel must be removed before a Master AS sequence is started, so that no vial is inserted in an occupied slot. Pressing OK, the Load/Unload window will automatically be opened (Figure 33), to allow vials to be removed (see Loading/Unloading chapter for details). Figure 32 Check vials in oven. Figure 33 Loaf/Unload window. How to create a sequence Press Add to create a new row in the table: then, enter the position of the first and the last vials to be sampled in the cell "First" and "Last" respectively (see Figure 34). If the number of the first vial is higher than the last vial, the alarm "First vial > Last vial" will be shown. The allowed vial number range is 1-18 for carousel sequence and 1-65 for Master AS sequence. If you enter a value out of the allowed range the message Out of range with the indication of the correct range will be shown. The minimum or maximum value allowed will be automatically saved by pressing OK. 30

38 Operation Figure 34 MASTER AS sample sequence. Specify the number of repetitions for each vial in the cell "Rep". The number of repetitions ranges from 1 to 20. All the repetitions for the same vial will be processed before moving to the next. Clicking on the column "Method", all the stored methods will be shown. Select the method to be used for each sequence row. Up to five different sequences can be stored as Sequence A, B, C, D or E (according to the selection on the dropdown menu (Figure 35). In order to eliminate a line, click on the row to select it and press "Delete". Figure 35 MASTER AS sample sequence - drop down menu. 32

39 Operation If the current method is different from the first sequence method a pop up "Load First Sequence Method" will appear (Figure 36). Figure 36 Load first sequence method. By pressing "Yes" the first sequence method will be loaded, selecting "No" the first method will be loaded after pressing START. Changing method parameters during run It is possible to modify some of the method parameters while a sequence is running. In order to set the new value you have to press on the corresponding box and a numeric keypad will appear (see Figure 37). Digit the value and press OK. If the value cannot be modified during the run the corresponding box will be coloured in grey. If you change the time of one of the five steps of the cycle, the modification will be active for the next vial inserted in the carousel. If you modify a temperature or a flow rate, the modification will be active for the next vial in the sequence. The change in the shaking mode will be performed immediately. If the GC ready interval is modified the change will be considered for the insertion on the next vial in the carousel. Figure 37 Changing method parameters during run. 33

40 Operation Changing sequence parameters during run It is possible to modify some of the sequence parameters while the instrument is in running condition. In order to set the new value you have to press on the corresponding box and a numeric keypad will appear (see Figure 38). Digit the value and press OK. The first vial cannot be modified during the run. If you change the last vial, the new value will be immediately considered. If you change the repetition number, the new value will be active for the next vial inserted in the carousel. The method selected for the current row cannot be modified while the sequence is running. If you press on the corresponding box the Select Method window will appear. Figure 38 Changing sequence parameters during run. Priority sequence The "Priority sequence" allows you to setup a sequence during the analysis. This sequence will start immediately after the end of the current analysis. In order to program the priority sequence press the "Priority Seq" button. A pop-up will appear (Figure 39). Insert the first and last vial to be urgently sampled in the corresponding boxes, the number of repetitions and the method to be used. 34

41 Operation Figure 39 Priority sequence. Sequence interrupted In case a problem occurs during a sequence and the Master DHS is switched off, when the instruments is switched on again a message will be displayed. If an AS sequence is stopped and some vials are present in the oven the Oven contains vials popup will appear; a message will be displayed: The sample sequence has not been completed. Do you want the Master AS to automatically recover vials from the oven?. Selecting Yes the vials will be removed by the Master AS; selecting No the operator will have to remove the vials manually from the load/unload page, as in the case of carousel sequence. If a carousel sequence is stopped the Check vials in oven pop-up will appear. The following message will be displayed: The sample sequence has not been completed. Please manually remove any vial from the oven. Pressing Ok the load/unload page will be opened. If the Master AS is switched off during an AS sequence an hardware error will appear. Changing AS parameters during run All Master AS parameters can be modified while the sequence is running. The changes will be considered for the next sampling step. 35

42 Operation Options In this page you can find information on different options. Gas In this page you can select the options related to the auxiliary gas (Figure 40). Auxiliary Gas The auxiliary flow rate displayed depends on the type of gas used (Nitrogen or Helium). Pressure Unit In this text box you can select the pressure measurement unit. The units available are: bar, psi and kpa. The default unit is bar. All set values will be automatically converted. Figure 40 Options - Gases. Handshake In this page you can select the option related to the communication between Master DHS and the gas chromatograph (Figure 41). The Master DHS features a control on the ready condition of the gas chromatograph: the first control is performed at the start of a sequence; a second control is then performed prior to any subsequent injection. By selecting Abort (that is the default option) a sequence can only be started if the gas chromatograph is in the Ready condition ; otherwise if you press the Start button the sequence will automatically be aborted. At the same time if the GC is not in the ready condition at the moment of all subsequent injections the sequence will be aborted. If you select Ignore, the Not ready condition of the gas chromatograph both at the start of the sequence and prior to any injection will not be considered and the started sequence will be completed. 36

43 Operation Figure 41 Options - Handshake. If you select Wait, when the gas chromatograph is not in ready condition at the moment of the start of a sequence or at the moment of every injection a popup GC not ready will appear, where a blue time bar is displayed. If the gas chromatograph reaches the ready condition within 10 minutes the sequence will go on automatically, otherwise the sequence will be automatically aborted. Setup This window allows to set the specific configuration of each instrument (Figure 42). This task is performed at factory or by the DANI Instruments Technical Assistance personnel during the instrument installation. All setup parameters are accessible through a password, and preferably managed by technical assistance personnel, to avoid unintentional modifications. Figure 42 Setup window. 37

44 Maintenance The Maintenance window includes five pages to support the instrument maintenance: Temp, Valves, Gas, Mov. and Trap Cleaning. In these pages it is possible to enable or disable some of the electrical and pneumatic devices to be controlled in manual mode separately from each other. The options selectable in this window are particularly useful for diagnostic operations or for analysis setup. All these options will be disabled during running status. To gain access to the "Maintenance" section, press Menu, Tools, then Maintenance. When you close this window the system will automatically return in the standby status. Temperatures In this page it is possible to test the temperatures of the following devices: Oven, Switching Valve, Trap, Dew Stop and Transfer Line (Figure 43). When you enter this page all the temperatures are set to the standby condition. Insert the requested setpoints in each textbox; then press Test to activate the heating or cooling devices. When you press Test a timeout control is activated: after 30 minutes all the temperatures will be automatically set at the default values, in order to prevent the devices to be kept at high temperature for a long time. Figure 43 Temperature page. In the table below units of measurement, interval range and default values for all parameters are shown: Parameter Measurement Unit Interval Default value Oven C from 40 to Switch. Valve C from 40 to Trap C from -10 to Dew Stop C from 0 to

45 Maintenance Valves In this page it is possible to test the movements of all valves: Aux EV, Vent 1 EV, Vent 2 EV, Carrier EV and Switching Valve (Figure 44). When you enter this page all the valves are in the standby status; press ON / OFF buttons to change the status of each device. Figure 44 Valves page. The function Switching Valve Counter visualizes how many times the valve has been activated. This information is used by the DANI Instruments technical assistance personnel to evaluate the use of the instrument. This is an actual value and cannot be modified. The Reset button is accessible through a password and preferably managed by technical assistance personnel, to avoid unintentional modifications. Gases In this page you can control the actual of carrier gas pressure value and test auxiliary gas flow: this option allows you to control the pneumatic circuit. Insert the requested setpoint in the corresponding textbox; the press Test to activate the flow regulator (Figure 45). 39

46 Maintenance Figure 45 Gases page. Movements In this page you can test the movements of the carousel and lifters. Use the UP / DOWN buttons to move up and down the vial insertion lifter and the vial sampling lifter. (Figure 46). Figure 46 Movements page. Use the two arrows to rotate the carousel of one slot in the two directions (clockwise and counterclockwise); pressing Home the carousel will return to the position with slot number 1 corresponding to the insertion lifter. The Slow Shake and Fast Shake buttons activate the shaking of the carousel (at slow and fast speed respectively); press Home to stop shaking and return in the original position. When you exit the maintenance window, the carousel and the lifter will automatically return to the standby position. 40

47 Maintenance Trap cleaning You can gain access to this page by pressing Menu, Tools, Maintenance, then Trap Cleaning or directly by pressing the trap cleaning icon on the desktop. In this page you can start a procedure of trap and Dew Stop cleaning. When you enter this page the system is in the standby status; set the chosen values for cleaning time and flow, as also for the trap and Dew Stop temperatures (Figure 47). The trap conditioning temperature should be based on the sorbent type. In the table below units of measurement, interval range and default values for all parameters are shown: Parameter Measurement Unit Interval Default value Cleaning Time min from 0,00 to 999,00 10 Cleaning Flow ml/min from 10,0 to 150,0 50 Trap Temp C from 40 to Dew Stop Temp C from 0 to In the default condition the Dew Stop is kept at low temperature during trap cleaning, because the Dew Stop is cleaned up during the baking step and no additional cleaning is normally requested for this device. In any case the auxiliary gas will automatically flow also through the Dew Stop during trap cleaning and it can be heated at the requested temperature. Figure 47 Trap cleaning page. Press Start to begin the procedure. When the trap cleaning is running a label TRAP CLEANING will appear in the status bar; if you press on this label a status window with a blue bar which describes the progress of the trap cleaning procedure and the remaining time will be displayed. If you want to end the procedure before the set cleaning time is finished, press Stop to abort it; otherwise the procedure will automatically stop at the end of the time. 41

48 Maintenance Calibration This window includes three pages to support the instruments calibration. The Gas calibration and Alignment pages are accessible only through a password, and preferably managed by service people, to protect from unintentional modifications. Note: The gas calibration is performed at factory or by the DANI Instruments Technical Assistance personnel during the instrument installation, using Nitrogen as auxiliary gas. The Touch page is available to the user. Touch screen calibration In order to make the touch screen suitable to your finger touch, you can calibrate it. Open the page "Touch" and press the button "Calibrate touch screen". A series of circles will be displayed. Press at the centre of each circle (Figure 48). Figure 48 Touch screen calibration. At the end of this procedure the message "Congratulation, your touch screen has been calibrated" will appear. Press the touch screen again to continue. 42

49 Parts and replacement Attention!!! Always disconnect the power supply cord before opening the instrument Removing the trap To disassemble the trap proceed as follows: Switch off the instrument. Withdraw the power cord. Turn the carrier gas off. Uncover the right upper part of the instrument by unscrewing the two front screws located on the two sides and gently moving the lid backward. Attention!!! To prevent accidentally breaking the trap, absolutely avoid touching it when it is under tension. The slightest pressure or twisting can cause it to break. Immobilize the fitting connected to the gas line and use a 12 mm wrench to loosen the hex screw at each end. First unscrew completely the front hex head screw and remove the fitting from its position by slightly shifting it to the side and being careful to retrieve the seal. Remove the fitting from the opposite end without taking out the trap. Slightly push the trap towards the bottom to retrieve the seal at the other end. Retrieve the trap by completely removing it from the front part Filling the trap DANI has different types of pre-filled traps and it is highly recommended to use these traps. To fill a trap proceed as follows: Get a new empty trap or empty the one being used, after disassembling it from the instrument, gently push the filling with a rigid tube of approximately 1 mm diameter (for example a glass rod or a stainless steel tube). Insert a glass wool plug of approximately 10 mm length and push it until it is 15.5 mm from the end of the trap. Place the trap vertically on a work surface with the open end facing up. Insert a small funnel in the open end. Add enough sorbent so that a length of approximately 40 mm is filled, settle the sorbent by gently and frequently hitting the trap. Do not compress the filling. Insert another glass wool plug of 10 mm length and push it until it is in contact with the filling. If the trap needs to be filled with more than one sorbent, insert the strongest material at first, and then the weakest, separating the sorbents with a minimum quantity of glass wool (approximately 1 mm). Add the amount of the various materials in the desired proportions so that the total length is equal to 40 mm. 43

50 Parts and replacement Assembling and conditioning the trap To assemble a new trap proceed as follows: Gently insert the trap from the front part of the instrument following the alignment of the holes. If the trap is filled with more than one sorbent, insert the trap with the strongest material in the front end. Gently push the trap towards the bottom so that it slightly comes out from the hex head screw. Put on the Teflon seal with the cone part facing the end of the trap. Secure the back fitting by screwing the hex head screw with a 12 mm wrench. Before finishing the seal, gently press the trap to the bottom and then tighten until the hex head screw offers a slight resistance. Insert the Teflon seal with the cone part facing the end of the trap at the front end and secure the fitting by gently screwing the hex head screw until it offers a slight resistance. Attention!!! To obtain a pneumatic seal for the trap just tighten until there is a slight resistance. Too much tightening can easily break the trap. Reinsert the power supply cable and turn on the instrument. Supply the carrier gas. Start leak test procedure in the stripping status as described in the Leak Test paragraph. If the system is not sealed gently tighten the fitting ¼ of a turn and repeat the procedure. If necessary, check the vial. If the system is sealed, you can start conditioning the trap. Enter the Trap Cleaning page and start trap cleaning procedure setting the conditioning temperature based on the type of sorbent. (See chapter Maintenance trap cleaning). Put the cover back on the front part and secure it with the two screws located on both sides. Replacing the transfer line needle The transfer line needle is connected to the line by a fitting and a stainless steel ferrule. To replace the needle: Use a 7 mm wrench to support the fitting and with another 7 mm wrench unscrew the needle. Replace the needle and tighten the fitting until sealed. It is not necessary to replace the stainless steel ferrule on the tube. Check the seal by closing the tube outlet, for example with a septum, and pressurizing the carrier gas line. 44

51 Parts and replacement Replacing the sampling needle The sampling needle is located in the manifold in the upper part of the instrument, within the thermally insulated aluminum box that contains also the switching valve. Removing the sampling needle To remove the sampling needle proceed as follows: Uncover the right upper part of the instrument by unscrewing the 2 front screws located on the two sides and gently moving the lid backward. Unscrew the screw located in the left side of the aluminum box that contains the manifold and the switching valve. Then open the cover of the aluminum box by sliding it gently up toward the back part. Use a 8 mm wrench to support the fitting in the upper part of the manifold and with a 7 mm wrench unscrew the fitting of the tubing entering the manifold from the upper part. Unscrew the fitting from the manifold with a 8 mm wrench. Use a 7 mm wrench to unscrew the fitting of the tubing entering the manifold from the right side. Unscrew the 2 screw that block the needle lodging to the manifold and remove all the lodging. Pull out the needle from the upper part of the lodging. In case the Kalretz O-ring remains in the needle lodging, remove it. Replacing the sampling needle Insert the Teflon seal in the upper part of the new needle and the Kalretz O-ring in the lower part. Insert the new needle in the lodging pushing it from the upper part. Replace the lodging in the manifold, paying attention the needle must enter in the guide positioned in the lower part of the manifold. Replace the 2 screw that block the needle lodging to the manifold and tighten them. Replace the tubing entering the manifold from the right side. (Use a 7 mm wrench to tighten the fitting). Replace the fitting in the upper part of the manifold and tighten it with a 8 mm wrench. Replace the tubing entering the manifold from the upper part and use a 7 mm wrench to tighten the fitting. Close the cover of the aluminum box that contains the manifold and the switching valve and tighten the screw located in the left side of the box. Put the cover back on the front part and secure it with the two screws located on both sides. 45

52 Parts and replacement Cleaning the instrument Only the smooth external surfaces of the instrument should be cleaned. Turn off the instrument, remove the power supply cable from the outlet and let any hot parts cool down. Only use a slightly damp cloth. Do not use alcohol or other solvents. Handling precautions If it is necessary to move the instrument, the following precautionary measures should be taken: Remove the vials from the carousel Remove the quartz trap following the instructions in the Removing the trap paragraph in this chapter. Remove the needle from the transfer line. Use the original packing to transport the instrument. Do not turn the instrument upside down. Leak test The Master DHS is able to perform an automatic leak test procedure. The leak test should be made every time the trap is disassembled and reassembled. In order to start this procedure press Menu Tools Diagnostic Leak Test. Before starting the procedure you have to wait until all the temperatures stabilize to the requested values. The leak test can be managed with the switching valve in the two different states. Select Incubation Status if you want to make a leak test on the auxiliary line excluding the trap and Dew Stop or select Stripping Status if you want to include the Dew Stop and trap in the leak test (Figure 49). The carousel and the two lifter will automatically move to allow the insertion of the vial. Insert an empty sealed vial in the carousel and press Next (Figure 50): the leak test will start automatically. The leak test procedure is demonstrated with the switching valve in Stripping Status. In the first step the system is pressurized at 1,5 bar for 2 minutes (Figure 51); then the auxiliary gas supply is turned off to find leaks (Figure 52). If the pressure decrease is less than 0,04 bar the system is sealed and the message Leak test in stripping status successful will appear (Figure 53). 46

53 Parts and replacement Figure 49 Leak test. Figure 50 Leak test in stripping status. Figure 51 Pressurization step. Figure 52 Leak check. 47

54 Parts and replacement Figure 53 Leak test status. Figure 54 Leak test finalization. In the pressurization and leak check step or when the leak check is completed, a button Cancel or Close will be displayed. Pressing it the procedure will be interrupted and the carousel and the lifter will automatically move to allow the removal of the vial. Remove the vial, then press Close to exit the procedure (Figure 54). Figure 55 Leak test failed. Figure 56 System pressurization. In case a leak is detected the corresponding message will be displayed (Figure 55); if you press Next the system will be repressurized in order to find leaks (Figure 56). It is suggested to check first the vial and the trap, then all fittings, particularly those carried out most recently. Finally press Next. 48

55 Diagnostics Diagnostic Hardware When the instrument is switched on, a Self test is performed to check the correct functioning of the instrument. During this procedure, all the configured devices are checked one by one. At the end, the Hardware tab of the diagnostic page will show all the devices in a list (Figures 57 and 58). Figure 57 Self test. Figure 58 Self test alarm. If the device passes the test, a symbol " " will be showed. If a device fails the test, an alarm (exclamation mark) will be visualized. Pressing on the device's name, a pop-up will appear. Here detailed information about the device and/or the malfunctioning are reported. The Diagnostic page can be entered in any moment after the self test. To gain access to Diagnostic page press Menu, Tools and then Diagnostic. The first item in the list is "System". Here you can read the serial number of the instrument and the firmware version of the Main Board and the other controllers (Figure 59). 49

56 Diagnostics Figure 59 System information. Alarms When the control unit diagnoses an error condition, an exclamation mark will blink on the status bar near the time clock. Press the icon to display the "Alarms" page (Figure 60), where the alarm messages are listed. Press on the row and a pop-up will appear containing details on the problem and, in most cases, the instructions to solve it. Figure 60 Alarms. 50

57 Diagnostics The errors can be divided in: Red hand alarms: this indicates an error that could cause serious damages. In this case the START of the analysis is blocked. Blue hand alarms: this indicates an error concerning a wrong setpoint. In this case the START of the analysis is not blocked. Hardware Errors indicate a malfunction of the instrument. They are alvisualized by a red hand, with the message Hardware error. Refer to the diagnostic page for details. If these problems occur, it is preferable to refer to the technical assistance (see "Diagnostic" in this chapter). BLUE HAND ALARMS MESSAGE ERROR DESCRIPTION HOW TO SOLVE IT Load Method A method parameter wasn t found in the flash memory: the corresponding default value has been loaded. Parameter default value has been loaded Modify the parameter value in the method (see Cycle chapter). Load Sequence A sequence parameter wasn t found in the flash memory: the corresponding default value has been loaded. Sequence Nr Seq, column [Row] default value has been loaded Modify the sequence parameter in the analysis table (see Sequence chapter). 51

58 Diagnostics RED HAND ALARMS MESSAGE ERROR DESCRIPTION HOW TO SOLVE IT Sequence: First Out Of Range The First vial in a sequence row is out of range, because you switched between AS sequences and carousel sequences. Rows: 1, Range Modify the First vial in the Analysis Table. (see Sequence chapter). Sequence: Last Out Of Range The Last vial in a sequence row is out of range, because you switched between AS sequences and carousel sequences. Rows: 1,... Range Modify the Last vial in the Analysis Table (see Sequence chapter). Sequence: First vial > Last vial You selected a first vial > than last vial. Rows: 1, First vial > Last vial Modify the First and Last values in the Analysis Table (see Sequence chapter). Analysis table is empty There are no entries in the analysis table. No entries in analysis table Insert at least a line in the analysis table (see Sequence chapter). Stripping Trap Temperature Dry Step Trap Temperature Injection Trap Temperature Baking Trap Temperature Cleaning Trap Temperature Std. Rinse Volume too large You selected a stripping trap temperature > trap max temperature. You selected a dry step trap temperature > trap max temperature. You selected an injection trap temperature > trap max temperature. You selected a baking trap temperature > trap max temperature. You selected a cleaning trap temperature > trap max temperature. You set a rinse volume larger then the syringe volume. Trap Temp. > Trap Max Temp Trap Temp. > Trap Max Temp Trap Temp. > Trap Max Temp Trap Temp. > Trap Max Temp Trap Temp. > Trap Max Temp. Std. Rinse Volume > Syringe Volume Modify the stripping trap temperature value in the method (see Cycle chapter). Modify the dry step trap temperature value in the method (see Cycle chapter). Modify the injection trap temperature value in the method (see Cycle chapter). Modify the baking trap temperature value in the method (see Cycle chapter). Modify the cleaning trap temperature value in the method (see Cycle chapter). Insert the correct value in the Std. Handling page (See the Master AS chapter). 52

59 Diagnostics RED HAND ALARMS MESSAGE ERROR DESCRIPTION HOW TO SOLVE IT Washing Volume too large You set a rinse volume larger then the syringe volume. Washing Volume > Syringe Volume Insert the correct value in the Solv. Wash. page (See the Master AS chapter). Carrier Gas Pressure too low The carrier gas pressure is below the 50 mbar threshold. Carrier Gas Pressure below threshold Check carrier gas supply and check for possible leaks. AS Disconnected Log message Hardware error Carousel Error Insertion Lifter Error Sampling Lifter Error Switching Valve Error Master DHS lost communication with Master AS or Master AS was shut down during a sequence. A problem occurred during a sequence and a new message was displayed in the log file. It indicates a malfunction of the instrument. Carousel lost its position or a hardware failure occurred. Insertion lifter lost its position or a hardware failure occurred. Sampling lifter lost its position or a hardware failure occurred. Switching valve lost its position or a hardware failure occurred. AS Sampler is disconnected, check wiring and power cycle it Log file has a new message See diagnostic page Carousel lost pos. or hw failure Insertion Lifter lost pos. or hw failure Sampling Lifter lost pos. or hw failure Switching Valve lost pos. or hw failure Check Master AS wiring and power cycle it. Check the log file in the Status page (see Status in the User interface chapter). See diagnostic page for details and in case call the technical assistance. Power cycle Master DHS and if problem persists call the technical assistance. Power cycle Master DHS and if problem persists call the technical assistance. Power cycle Master DHS and if problem persists call the technical assistance. Power cycle Master DHS and if problem persists call the technical assistance. 53

60 MASTER AS Introduction The MASTER AS Automatic Sampler, mounted on the left side wall of the Dynamic Headspace Sampler, allows to automatically move vials in the Dynamic Headspace Sampler and to add standard solutions directly into the samples. It can operate using normal headspace vials with magnetic caps and standard syringes for liquids. Description Master AS includes: The moving block (1) consisting of three moving axes X, Y and Z. The vertical axes Z includes the syringe housing and provide the vertical movement of both the syringe and the plunger. The block moves along three axes (X,Y and Z) to carry the vials from the tray to the Mater DHS and back to the tray at the end of the analysis and to carry the syringe to the standard, solvent and waste vials. A 65 sample tray for 20 ml vials that can also contains up to six internal standard vials, up to two solvent vials and up to two waste vials (10 ml) (2). These removable trays are seated in the base of the autosampler and blocked by the position keys. The electrical connections are available on the back of the instrument. Syringe block The syringe is lodged in an interchangeable support (1) and is held in place by a retainer(2). The plunger head is set in an adjustable holder(3) and fixed by a blue screw(4). The syringe needle is inserted in a retractable guide (5) protecting it from possible bends. A transparent sliding cover protects the block (6) (Figure 61). Figure 61 MASTER AS syringe block. 54

61 MASTER AS Electrical connections The electrical connections, available on the back of the instrument (Figure 62) are: the supply socket (1), the main switch (2), RS232 serial output (3) for the control of the instrument. Figure 62 MASTER AS connections. Attention!!! If the touch screen is not used for at least 10 min and, in case, the instrument is not in the running condition, the motors power supply automatically goes in stand-by mode. Setup The "Setup" window consists of two pages, "Vial & Syringe" and "Standards", and allows you to select the syringe volume and the position of solvent, internal standard and waste vials. To gain access to this section, press three times on the corresponding short cut key or select "Menu", "Master AS" then "Setup". Vial & Syringe In the "Vial & Syringe" page (Figure 63), the following settings are available: Vial: the Master DHS can only be used with 20 ml headspace vials. Syringe: seven different syringes are available through a dropdown menu: 5, 10, 25, 50, 100, 250 and 500 μl (The default syringe volume is 10 μl). If you do not add internal standards to the samples it is suggested not to install the syringe. 55

62 MASTER AS Figure 63 Vials & Syringe. Syringe Replacement Pressing this button makes the vertical arm of Master AS to move in a useful position to replace the syringe. The Syringe replacements popup will appear. Open the transparent sliding cover. Keeping the needle guide completely lifted, insert the syringe into its seat by inserting the needle through the holes on the seat and on the needle guide. Keep the syringe with the graduated side in front. Insert the syringe in the interchangeable support and the plunger head into its seat on the adjustable holder and regulate the height by loosing the two front screws, then fix the plunger head by the blue screw. Close the retainer to block the syringe. The standard syringe support is suitable for 5 and 10 μl syringes. For syringe from 25 to 500 μl a different support is available as an option. To remove the syringe support, pull it towards you. To install the other support insert the four pins into the corresponding holes. 56

63 MASTER AS Press "Done" after the syringe replacement: the vertical harm will move to its home position (Figure 64). Figure 64 Syringe replacement. Standards Master DHS has two positions, A and B, for solvent and waste vials and six positions, from 1 to 6, for the standard solutions vials. In this page you can select all the positions that contain an internal standard and for each standard you can select the corresponding solvent/waste position (Figure 65). Figure 65 Standards. 57

64 MASTER AS AS Parameters To gain access to this section you can press twice on the corresponding short cut key or select "Menu", "Master AS" then "Parameters". Standard volumes Master AS is able to add up to four standards for each sample. In this page you can select the standards that will be added to the samples and choose the corresponding volume (range from 0.1 to 100 μl; default value 1 μl). Pressing on each of the four dropdown menu you can choose one of the standards that have been selected in the Setup page. Enter the chosen volume and select the checkbox for the requested standard (Figure 66). Figure 66 Standard volumes. If a volume higher than the current syringe volume is selected, the standard sampling will be performed with multiple additions. The standards will be added in the order of the four lines. Standard Handling In this page you can setup the options related to the internal standard addition (Figure 67). Master AS is able to rinse the syringe with the internal standard (if selected). 58

65 MASTER AS The following parameters are available: Volume: this is the volume used for the internal standard rinse (if selected). This value is expressed in μl and can range from 0.1 to 500 μl; the default value is 2 μl. If you set a internal standard rinse volume higher than the capacity of the syringe, an alarm "Standard rinse volume too large" will be shown in the "Alarms" page. Number: this value represents the number of repetitions (up to 25; default value: 3) of the internal standard rinse. Figure 67 Standard handling. Plunger strokes number : the plunger is able to move up at the speed set in "Plunger speed (μl/s)" and down at a fixed speed, before the selected standard volume is taken. The strokes are very useful to eliminate air bubbles present inside the syringe. You can select up to 25 strokes (the default value is 3). Plunger speed: This is the speed, expressed in μl/sec, at which the plunger moves up during the strokes. It can range from 0.1 to100 μl/sec (default value: 5 μl/sec). Standard Injection Height: It is the needle distance from the bottom of the vial during the standard adding. This value is expressed in millimetres and can range from 35 to 65 mm (the default value is 35 mm). Viscosity delay: This function is important when viscose standards are used and allows to be sure that the correct volume is taken. It is the time, expressed in seconds and considered from the moment in which the plunger stops at the chosen volume, during which the needle remains inside the standard vial before the standard sampling. This value can range from 0 to 25 seconds and the default value is 0. 59

66 MASTER AS Solvent Washing It is possible to carry out the syringe washing with one of the two solvents at the beginning and/or at the end of each standard sampling, with the Pre Solvent Washing and the Post Solvent Washing respectively (see Figure 68). To do this, the syringe block lowers on the solvent position, the syringe takes a set volume of solvent and discharges it into the waste vial. This operation is repeated for the number of washings with solvent set in the method. Figure 68 Solvent wash. The washing volume, expressed in μl, can range from 0.1 to 500 μl (default value 2 μl). If the washing volume is higher than the capacity of the syringe, an alarm "Washing volume too large" will be shown in the "Alarms" page. The number of washings (up to 25; default 5) can be selected separately for both the "Pre solvent Washing" and the "Post solvent washing". 60

67 MASTER AS AS Sequence The "Sample Sequence" window (Figure 69) allows to set all parameters concerning the sampling sequence. Figure 69 AS sample sequence. To gain access to this section, press once on the corresponding short cut key or select "Menu", "Master AS" then "AS Sequence". See chapter Sequence for more information on how to create a sequence. 61

68 MASTER AS AS Status A detailed description of the AS status is available in the page "Sequence" of the Status window (Figure 70). In the lower frame "AS Status", all the steps are monitored in real time. Figure 70 AS sequence status. Missing vials Before sampling, the syringe block moves to the position of the current vial and goes down to check the presence of the vial. In the AS status frame of the page Sequence of the Status window, "Checking Vial" will be displayed. If the instrument does not find the vial, it moves to the next vial. The information of missing vial will be reported in the Log page of the Status window. Maintenance To open the "Maintenance" window press Menu, select "Master AS", then "Maintenance". This window contains two page: Syringe cleaning and Axes. Syringe Cleaning This option allows you to manually wash the syringe. Select the solvent/waste through the dropdown menu "Position solvent" and insert the number of washing in the corresponding box (Figure 71). 62

69 MASTER AS Figure 71 AS Maintenance. Pressing "Start", the washing procedure will begin. During the Syringe cleaning, "SYR. CLEANING" will be reported both in the Status bar and in the "AS Status" page. To stop the syringe washing press "Abort". Axes This window allows to save the Master AS alignment along the three axes X, Y, Z on the tray and DHS position. This task is performed at factory or by the DANI Instruments Technical Assistance personnel during the instrument installation. It is accessible through a password and is preferably managed by technical assistance personnel, to avoid unintentional modifications. The Master AS is equipped with a sensor to check the presence of the vials on the tray. The sensor has to be calibrated on the height of the vial to ensure the checking of the vial to be managed correctly. Insert a vial in the position number 1 of the tray and press on the Sensor button in order to start the automatic calibration. Attention!!! The calibration of the sensor has to be repeated every time the vial type is changed, for instance from screw cap vials to crimped vials and vice versa, because their heights might not be identical. 63