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Antec Leyden DECADE User Manual

Digital electrochemical amperometric detector
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Antec Leyden DECADE User Manual

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  • Page 1 (217) 352-9330 | Click HERE Find the Antec Decade at our website:...
  • Page 2 DECADE Digital Electrochemical Amperometric Detector user manual Edition 9, 2007 120.0010 Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...
  • Page 3 Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...

  • Page 4: Declaration Of Conformity

    Attention Use shielded cable(s) to connect all I/O’s with other devices. Thoroughly connect the shielding to common. Antec Leyden will not accept any liability for damage, direct or indirect, caused by connecting this instrument to devices which do not meet relevant safety standards.

  • Page 5: Intended Use

    In Vitro Diagnostics Directive. WEEE directive All equipment of Antec Leyden which are subjected to the WEEE directive shipped after August 13, 2005 are compliant with the WEEE marking requirements. Such products are labelled with the “crossed out wheelie”, depicted on the left site.

  • Page 6: Symbols

    The following symbol are used on the rear panel and oven compartment of the DECADE: Consult the manual for further safety instructions Frame or chassis ground terminal The following pictograms are used in the DECADE II manual: Caution Caution, risk of electric shock or other electrical hazard (high voltage)

  • Page 7: Safety Practices

    DECADE user manual, edition 9 Safety practices The following safety practices are intended to insure safe operation of the equipment. Electrical hazards The removal of protective panels on the instrument can result in exposure to potentially dangerous voltages. Therefore, disconnect the instrument from all power sources before disassembly.

  • Page 8: General Precautions

    socket. The power source should exhibit minimal power transients and fluctuations. Replace faulty or frayed power cords. Place the detector on a flat and smooth surface. Do not block the fan located at the bottom of the detector. Blocking the fan will impair the cooling capability of the power supply.
  • Page 9 DECADE user manual, edition 9 Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...

  • Page 10: Table Of Contents

    AUTO mode and time files 37 Introduction 37 Range programming 37 Drift monitor 38 Step by step example (DECADE = Master) 39 Hardware connections: 39 Programming the AUTO mode: 40 Important note when using the drift monitor: 42 Interrupting a time file: 42...
  • Page 11 DECADE user manual, edition 9 Step by step example (DECADE = Slave) 42 Hardware connections: 42 Programming the AUTO mode: 43 Interrupting a time file: 44 Other events 45 Inject/load and inject marker 45 Hold/busy 46 Overload 46 Auto zero 46...

  • Page 12: Decade User Manual, Edition

    Rear panel 71 TTL inputs 71 RS232C 71 Troubleshooting guide 73 No detector response 73 High cell current 73 Noisy baseline 73 Decreased sensitivity (low S/N ratio) 73 Baseline oscillations 74 Saturation of output 74 Pulse damper 75 Dummy cell 76 Index 77 Artisan Technology Group - Quality Instrumentation ...
  • Page 13 DECADE user manual, edition 9 Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...

  • Page 14: Decade Electrochemical Detector

    S/N ratio and therefore you now possess the best possible combination for extremely sensitive EC analyses. To further improve the stability of the DECADE an (electrically actuated, option) injector and a high efficiency pulse damper can be incorporated in the oven compartment.
  • Page 15 DECADE user manual, edition 9 Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...

  • Page 16: Installation Guide

    Installation Please follow the next steps for a successful installation and start-up. 1. To unpack the DECADE, lift it from its transport box by both hands as indicated in Fig. 1A. In any other situation the DECADE should be lifted by both hands under the unit as indicated in Fig.

  • Page 17: Hplc Connections

    For 110 V (AC) ± 10%, use two 3.2 AT fuses (slow, ¼” x 1¼ ”, UL/CSA). For 220 V (AC) ± 10%, use two 1.6 AT-fuses (slow, 5 x 20 mm, IEC127). 4. Switch ‘on’ the DECADE by the mains switch on the rear panel. HPLC connections Use proper eye and skin protection when working with solvents.
  • Page 18 CHAPTER 2 Installation guide Fig. 2. Installation of the DECADE. 8. If a manual injector is applied, it is only part of the Faraday shield if the yellow wire from the cell cable is clamped on a metal part of the injector.
  • Page 19 DECADE user manual, edition 9 If the ISAAC reference electrode is used, add 2 mmole/l chloride ions (e.g. KCl or NaCL) to the mobile phase. Equilibrate HPLC and continue installation. 12. Before connecting a new column read the manufacturer’s instructions.
  • Page 20 CHAPTER 2 Installation guide The DECADE has been developed for continuous operation. For maximum stability it is advised to leave the system ON continuously. If preferred, the flow cell may be switched OFF at night. Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...
  • Page 21 DECADE user manual, edition 9 Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...

  • Page 22: The Decade Controller

    The DECADE controller Introduction The DECADE has been designed for maximum functionality and ease of use. The control of ECD parameters is such that without reading this chapter, it should be possible to operate the detector. This chapter is intended as a reference guide in case questions arise during operation.

  • Page 23: Overview Of All Decade Screens

    DECADE user manual, edition 9 Overview of all DECADE screens Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...
  • Page 24 CHAPTER 3 The DECADE controller Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...

  • Page 25: Parameters

    DECADE user manual, edition 9 Parameters Actor (AUTO) PRGR control Controls the electrically actuated injector, during execution of a time file. Forces this valve to load (‘LD’) or inject (‘INJ’) (see page 37). (AUTO) PRGR function Adds the current data line to the time file. Confirmation is asked for if an existing time is overwritten.
  • Page 26 AUTO SET control (master) Controls the number of times a time file has to be repeated. If the DECADE is master this number can be 1 - 99 or continuous. If the DECADE is slave the number of cycles is 1 (see page 37).
  • Page 27 DECADE user manual, edition 9 time file when the baseline is drifting. The available drift monitor settings depend on the range selected at time 00:00 in the time file (see page 37). Can be set between 0.1 pA/min and 10 nA/min.
  • Page 28 CHAPTER 3 The DECADE controller Interrupts the execution of a time file or scan. Toggles between 1 and 0. Pressing the hold button again continues the time file or scan were it was stopped (see page 37). Icell DC STAT, PULS STAT, SCAN STAT status Displays the true, non-compensated cell current, i.e.
  • Page 29 AUTO SET function Starts the execution of a time file (master/slave). If the DECADE is slave, the system waits for the ‘START’ input trigger to start the next run (see page 37). Software 3.00 and higher: In the slave mode the RUN command initialises the AUTO RUN screen, the system waits for the ‘START’...
  • Page 30 CHAPTER 3 The DECADE controller (AUTO) PRGR function Scrolls through a time file (see page 37). DC STAT, AUTO RUN, PULS STAT, SCAN STAT) function Returns to the previous (xx SET) screen. SET1, SET2 PULS SET2, PULS STAT function Returns to PULSE SET screen 1 or 2...
  • Page 31 DECADE user manual, edition 9 Time (AUTO) PRGR control Controls the time to execute a data line in a time file, can be set with one second resolution. Maximum time is 999 min and 59 s. The time to stop the execution of a time file must be programmed by the CycleTime in the AUTO SET screen (see page 37).

  • Page 32: Data Acquisition

    I/E converter which is as close as practically possible to the working electrode (WE). The recorder signal is manipulated by the CPU of the DECADE. The details on data acquisition in the various ranges will be discussed for both output channels.

  • Page 33: Integrator Output

    These are the three DECADE integrator ranges that can be set in the ‘Range select’ screen. Fig. 5. The DECADE ‘Range select’ screen. The 10 nA/V corresponds to 100 nA full scale on the integrator output (=10V). The integrator range selection is the first step in the signal pathway (Fig. 4). It affects both the integrator and the recorder output and has several important consequences for data acquisition (Table I).

  • Page 34: Recorder Output

    CHAPTER 4 Data acquisition When data are obtained from the integrator output, it is obvious that the pA range allows the highest sensitivity. Each range has a different maximum zero compensation (Table II). For example, in the nA range a current of 100 nA full scale can be managed.
  • Page 35 DECADE user manual, edition 9 There is much overlap in the recorder range settings offering flexibility as to maximum zero compensation (Table IV). For example, if a chromatogram is acquired at 10 nA, the nA or µA range can be selected (Table IV). With a high background current the µA is chosen (max.

  • Page 36: Integrator Vs. Recorder Output

    CHAPTER 4 Data acquisition Fig. 7. A ‘stepwise’ pattern after magnification of a chromatogram. This phenomenon will not occur at the integrator output because this output is purely analog and therefore, in principle, with infinite resolution. Integrator vs. recorder output In the pulse and the scan mode, only the recorder output is suitable for data acquisition.

  • Page 37: Offset

    DECADE user manual, edition 9 Fig. 8. The clean signal from the integrator output (A) is smoothened by integrator software using a running average filtering (C). This results in a similar chromatogram as obtained from the recorder output using a rise time filter of 1 s (B).
  • Page 38 CHAPTER 4 Data acquisition Table V. Effect of recorder range on the offset of the 10 V integrator output. Range Offset µA 0.01 0.02 0.05 0.10 0.20 0.50 1000 10.0 1.00 2000 20.0 2.00 1000 5000 50.0 5.00 1000 1500 2000 2500 1000...
  • Page 39 DECADE user manual, edition 9 Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...

  • Page 40: Auto Mode And Time Files

    Fig. 9. Programming a time file using the '(AUTO) PRGR' screen. The file is made using the ‘(AUTO) PRGR’ screen on the DECADE (Fig. 9) or, when the DECADE is equipped with the RS232 option, by using the time file editor in ‘DECADE Dialogue for Windows’.

  • Page 41: Drift Monitor

    Cycle Time (end of run) Drift monitor The AUTO mode of the DECADE is equipped with a drift monitor, which puts the detector on ‘hold’ when the baseline is drifting. The drift monitor is only active at the beginning of a time file, both in the master and slave mode. After starting a time file the baseline is monitored during one minute and the ‘wait..’...

  • Page 42: Step By Step Example (Decade = Master)

    Step by step example (DECADE = Master) In this step-by-step guide the example from Table VI will be programmed. In this example the system consists of an HPLC system, a DECADE with an electric valve, an integrator, and an on-line microdialysis set-up.

  • Page 43: Programming The Auto Mode

    DC mode (and 4 in the Pulse mode). The number of times you want to repeat this time file is set with ‘Cycles’. Because the DECADE will give the integrator and switching valve the starting signals, it is set at ‘Master’.
  • Page 44 CHAPTER 5 AUTO mode and time files Data acquisition’, page 29, for specific details on differences between both modes. In our example the nA range is chosen, and confirmed with ‘ACCEPT’. The message ‘New time is saved’ is displayed. Choosing ‘SCROLL’ allows you to scroll through your time file. With ‘DEL’ an existing line in your time file can be deleted (after confirmation).

  • Page 45: Important Note When Using The Drift Monitor

    HPLC system with autosampler, a DECADE and an integrator. The DECADE is slave which means that a run is started by an external contact (i.e. from autosampler). Also the number of automated runs is controlled externally.

  • Page 46: Programming The Auto Mode

    Connect your integrator to the REC output at the rear panel of the DECADE. Fig. 13. Input contacts needed for external control of the DECADE (slave mode) A: until DECADE software version 3.00 and B: from version 3.00 and higher . Prepare the LC-EC system for analysis.

  • Page 47: Interrupting A Time File

    DECADE user manual, edition 9 ‘RESET’ of the DECADE is required. This is necessary to be ready for the next run. In our example the following line has to be programmed: This activates the ‘relay1’ output (‘0100’) for 1 second, just before ending the time file.

  • Page 48: Other Events

    A manual injector with position sensor has an internal relay which is connected by a cable connection in the oven cabinet of the DECADE to the inject/load of the rear panel. The relay is open when the valve is in ‘load’...

  • Page 49: Hold/Busy

    Output: the ‘BUSY’ output is active (low) when during operation in the master or slave mode the DECADE is put on ‘hold’ by the drift monitor. The ‘HOLD’ command from the keyboard does not affect the status of the ‘BUSY’ output! Overload Activated when a recorder overload occurs.

  • Page 50: Ttl Contacts

    1000 TTL contacts The DECADE uses TTL input contacts for START, RESET, AUTO ZERO, TO POS. A and TO POS. B. These contacts require a minimum TTL-low pulse duration of 100 ms to be activated. If multiple activations are required the next pulse must be given after 100 ms TTL-high.
  • Page 51 (see Fig. 13, ‘RESET’ command). In the latter case it is important that the status of the external contact is known, and that the apparatus is connected to the same ground (by the mains power supply) as the DECADE. Table VIII. I/O contacts, upper 12 pins connector. Default status of output connections is low (0 V).
  • Page 52 Resets the AUTO mode triggered Auto zero always level Auto zero command, always triggered accessible when ‘I-Cell’ is in DECADE display Overload always status: low Active when recorder overload occurs (‘REC OVLD’) not conn. Inject marker always status: low In combination with electric valve, high: ‘load’, low: ‘inject’.
  • Page 53 DECADE user manual, edition 9 Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...

  • Page 54: Pulsed Amperometric Detection

    Pulsed amperometric detection Introduction Several advanced features are implemented in the DECADE. One of these features is the so-called pulse mode. In pulsed amperometric detection (PAD) the working electrode (WE) is regenerated at a frequency of 0.5 - 3 Hz by the application of a series of potential changes.
  • Page 55 (160 nA). Therefore, only the µA range is available in the pulse mode. If the RS232 option is installed, the pA and nA range can be used via the ‘DECADE Dialogue’ software.

  • Page 56: Pulse Settings

    CHAPTER 6 Pulsed amperometric detection chromatography. The CO -free sodium hydroxide is available from several suppliers as a 50% solution (19.2 mol/l). NaOH pellets are not recommended because of their high CO content. • The accuracy of certain pH-electrodes is poor at high pH. For applications at high pH it is sometimes better to calculate the pH from the OH concentration.

  • Page 57: Optimisation Of Wave Forms

    DECADE user manual, edition 9 Optimisation of wave forms LaCourse and Johnson [2-4] have published several papers on optimisation of wave forms in PAD. Several considerations are important for the choice of the pulse duration. Optimisation is depending on the working electrode material, the sample constituents and the required detection frequency.

  • Page 58: Peak Width And Integrator Frequency

    CHAPTER 6 Pulsed amperometric detection of the pulse. Once every cycle, the ts signal is sent to the output. This can be visualised by magnification of a peak in the chromatogram (Fig. 19). Fig. 19. A magnified view of a chromatogram obtained with PAD. The integrator frequency is 5 times higher than the detector output frequency resulting in a typical stepwise signal.

  • Page 59: Working Electrode Material

    DECADE user manual, edition 9 Fig. 20. A detailed part of a chromatogram acquired at different integrator frequencies. The integrator frequency is (A) 5x, (B) 2.5x, (C) 1.2x, (D) 0.6x and (E) 0.3x the frequency of the pulse. In case of PAD the duration of the pulse should also be taken in account.
  • Page 60 CHAPTER 6 Pulsed amperometric detection different from the noble metals. The capacitance of the electrode material is very high, such that the charging current is not stabilised before start of the next potential step. This pattern makes detection impossible. Fig. 21. Change in cell current during PAD. The cell current of the noble metals gold (Au) and platinum (Pt) is stabilised faster than the cell current of glassy carbon (GC), due to a much lower capacitance of the noble metals.

  • Page 61: References

    DECADE user manual, edition 9 Table XI. Potential settings for PAD of glycols, alcohols, aldehydes at a platinum working electrode. t (ms) E (mV) +200 +1300 -100 Table XII. LC-EC conditions for PAD of carbohydrates. detector DECADE, Antec Leyden column...

  • Page 62: Optimisation Of Working Potential

    Both peak height and background current are plotted against the working potential. A scanning voltammogram is obtained in the so-called scan mode of the DECADE: the voltage runs between two pre-set values and the current is measured.

  • Page 63: Hydrodynamic And Scanning Voltammogram

    DECADE user manual, edition 9 electrons are transferred at the WE resulting in an electrical current that is amplified by the controller. Hydrodynamic and scanning voltammogram A hydrodynamic voltammogram is constructed when the pure analyte is not available and separation over an analytical column is required. Furthermore,...
  • Page 64 CHAPTER 7 Optimisation of working potential Fig. 24. Scanning voltammetry of 1.0 µmol/l nor epinephrine (A) at a glassy carbon working electrode, at a scan speed of 10 mV/s. Scan (B) is the blank solvent. As peak heights are used, the signal in Fig. 23, line A is only due to the analyte.

  • Page 65: Optimisation Using A Voltammogram

    DECADE user manual, edition 9 Optimisation using a voltammogram Sometimes, when interfering peaks appear in the chromatogram, it is possible to optimise the method with regard to selectivity. If the interfering compound has a higher oxidation potential, a working potential is chosen that gives the best selectivity, i.e.
  • Page 66 CHAPTER 7 Optimisation of working potential Fig. 26. At a higher pH the I/E curve of nor epinephrine is shifted to the left. Reaction kinetics predict that electrochemical detection is mass flow dependent. When the LC flow is stopped in LC-EC, the analyte will be oxidised completely and the signal decreases rapidly.

  • Page 67: Construction Of A Hydrodynamic Voltammogram

    Construction of a scanning voltammogram The scan mode is programmed in the ‘SCAN SET’ screen of the DECADE. Depending on the data acquisition software that is used and the experimental set-up, a full, half or continuous scan cycle can be chosen.
  • Page 68 CHAPTER 7 Optimisation of working potential Fig. 29. The scanning voltammograms of 2,4-dimethylphenol (DMP), phenol (P), 2-chlorophenol (2-CP) and 4-nitrophenol (NP). The following procedure is used to obtain the voltammograms in Fig. 24 and Fig. 29: 1. The column is removed from the LC system. The voltammogram is recorded in the flow injection analysis (FIA) mode.
  • Page 69 DECADE. 7. The analyte is injected and the scan is started by pressing the ‘START’ in the ‘SCAN STAT’ screen of the DECADE at the time the analyte plug enters the flow cell (see 4). 8. A background scan is obtained by scanning the HPLC buffer.

  • Page 70: Specifications Decade

    CHAPTER 8 Specifications DECADE C H A P T E R Specifications DECADE General specifications Power 110-120/220-240 VAC, 50/60 Hz Operating modes DC, Pulse and Scan Potential range between +2.00 and - 2.00 V in 10 mV increments Recorder output between +0.1 and - 0.1 or between +1.0 and -1.0 V...

  • Page 71: Auto Mode

    DECADE user manual, edition 9 AUTO mode DC mode (5 files) and pulse mode (4 files), master/slave mode, cycle time, number of cycles, drift monitor Time-based control of 20 time points as to sensitivity, filter settings, output contacts (2 open collector, 2 relays), auto zero, offset, inject/load position of electrically actuated injector (option) and E-cell (DC only).

  • Page 72: Error Messages

    CHAPTER 9 Error messages C H A P T E R Error messages Error Message Error 1 Current overload, maximum current + maximum compensation has been exceeded. Advise: use less sensitive range in ‘Range select’ screen. Error 2 A ROM failure has been detected. Please contact supplier. Error 3 A RAM failure has been detected.
  • Page 73 DECADE user manual, edition 9 Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...

  • Page 74: Rear Panel

    Windows, and another DECADE EPROM with R-extension. DECADE Dialogue for Windows is a multi-functional control bar which handles all important settings of the DECADE via the RS232C port. The program runs simultaneously with your favourite Windows-compatible Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...
  • Page 75 DECADE output contacts for control of external equipment. For users of integration software running under DOS DECADE Dialogue may still offer an attractive option. A time file can be transmitted from a PC to the DECADE and executed from in the auto mode of the DECADE, independently from the computer.

  • Page 76: Troubleshooting Guide

    CHAPTER 11 Troubleshooting guide C H A P T E R Troubleshooting guide No detector response Possible cause Remedy No power Check line voltage setting, plug in power cord Power switch off Turn this switch ‘on’ (at the rear panel) Faulty fuse Replace fuse Divergent mains voltage...

  • Page 77: Baseline Oscillations

    DECADE user manual, edition 9 Possible cause Remedy Cell potential too low Optimise potential Contaminated buffer (high I Replace buffer, do not recycle the buffer cell Baseline oscillations Possible cause Remedy Malfunctioning pump (regular Check pump (seals, valves) pattern) Overtightened cell bolts...

  • Page 78: Pulse Damper

    CHAPTER 12 Pulse damper C H A P T E R Pulse damper The current version of the SSI pulse damper is SSI part no. 12-0625. This damper is ready for use, as supplied. The older version of the SSI damper (part no.

  • Page 79: Dummy Cell

    DECADE user manual, edition 9 C H A P T E R Dummy cell A successful dummy cell test confirms that the controller, including the cell cable, functions properly. If the result of the noise measurement with the dummy cell is within specs, the controller is excluded in a trouble shooting procedure.

  • Page 80: Index

    CHAPTER 14 Index C H A P T E R Index Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...
  • Page 81 DECADE user manual, edition 9 +24 V, I/O contact, 46 Actor, control, 20 ADD, function, 20 AUTO mode example, 37; 40 range programming, 35 AUTO, function, 20 autozero accessibility, 42 signal processing, 28 Autozero I/O contact, 44; 47 AUX1, I/O contact, 46...
  • Page 82 CHAPTER 14 Index DEL, function, 21 dipswitch settings, 67 drain, 13 drift monitor, 36 busy output, 44 events at t=0.00, 40 example, 38; 39 'wait...' message, 39 Drift, control, 21 dummy cell test, 74 E1, control, 22 E2, control, 22 E3, control, 22 Ec, control, 22 Ecell, status, 22...
  • Page 83 DECADE user manual, edition 9 I/E relationship, 57 I/O contacts 0000-string TimeFile, 44 accessibility, 47 rear panel, 69 specifications, 46 I-cell display, 28 Icell, status, 23 INJ=I/L function/status, 23 inject marker trigger, 43 Inject marker example, 37 I/O contact, 47...
  • Page 84 CHAPTER 14 Index master accessible functions, 40; 43 example, 37 maximum current, 29 maximum zero compensation, 30 messages, 67 NEXT, function, 23 noise, 14; 50; 52; 62; 65; 71 air bubbles, 14 Offs., control, 23 Offs., status, 23 offset, 29 affected by recorder range, 32 signal processing, 28 Outp., control, 23...
  • Page 85 DECADE user manual, edition 9 recorder ranges, 29 Range control, 24 REC, 27 recorder output, 27; 29 frequency, 52 pulse mode, 52 resolution, 29 stepwise ‘bit’ profile, 30; 35 vs. INT output, 31 RECOVLD, 67 reference electrode pulse mode, 50...
  • Page 86 CHAPTER 14 Index upgrade info, 20; 24; 25; 40; 41; 43; 46; 50 spare parts, 4 specifications DECADE, 65 Start I/O contact, 47 START function, 25 STATUS, function, 25 STOP, function, 25 t1, control, 25 t2, control, 25 t3, control, 25...
  • Page 87 DECADE user manual, edition 9 zero compensation resolution, 30 Artisan Technology Group - Quality Instrumentation ... Guaranteed | (888) 88-SOURCE | www.artisantg.com...

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