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Gow-Mac 580 series, Руководство по эксплуатации

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Series 580 TCD Gas Chromatograph
September 2017, Rev. 5

29

Section 5

Operation

A.  General

 

The chromatographer should be familiar with the techniques of chromatography, the function of 
all controls, the operation of the recorder, and the characteristics of the columns used prior to 
running samples.

B.  Operation

 

1.  Gas Flow

 

 

a.  Make sure that ALL switches are in the “OFF” position.

 

 

b.  Set helium or other carrier gas pressure regulator to 40 psig.

 

 

c.  Adjust fl ow of carrier gas to: 30 mL/min. for 1/8” columns 60 mL/min. for 1/4” columns.

 

 

d.  Check for leaks as described in Section 3, Paragraph I.

 

 

e.  Disconnect fl owmeter.

 

 

f.  Allow 5 minutes to purge the system before turning power “ON”.

 

2.  Temperature Controls

NOTE

 

)

 TEMPERATURE CONTROL KNOBS are locking type. Push locking 

ring “IN” to turn knob.

 

 

a.  Turn the DETECTOR CURRENT CONTROL fully counterclockwise (CCW). 

THIS STEP

 

 

IS EXTREMELY IMPORTANT!

 

 

b.  Plug in the instrument to the appropriate ac outlet. Switch the instrument “ON”.

 

 

 

Charts 5-1 thru 5-5 illustrate the maximum current for specifi c cell temperature

 

 

and carrier gases helium, nitrogen, and argon for single and dual carrier detectors.

 

 

 

THESE SHOULD NOT BE EXCEEDED!

 However, for longer fi lament life and a more

 

 

stable baseline, lower detector current is recommended. Reference recommended

 

 

starting bridge settings (pg. 26).

Содержание 580 series

Страница 1: ...l Series 580 TCD Isothermal Gas Chromatograph Series 580 120 V 50 60 Hz Series 582 230 V 50 60 Hz September 2017 Rev 5 READ INSTRUCTIONS BEFORE OPERATING 277 Brodhead Rd Bethlehem PA 18017 8600 U S A Tel 610 954 9000 ...

Страница 2: ...GOW MAC Instrument Co 2 ...

Страница 3: ... Co assume responsibility for any injury or damage which may result directly or indirectly from the use of such information This document contains proprietary information which is protected by copyright All rights are reserved No part of the document may be photographed reproduced or translated into another language without the prior written consent of GOW MAC Instrument Co The warranties made by ...

Страница 4: ... be binding upon GOW MAC unless reduced to writing and approved by an officer of the Company 11 This warranty shall be governed by the laws of the Commonwealth of Pennsylvania LIABILITY Buyer assumes all responsibility for warning and protecting its employees and independent contractors with respect to all hazards to persons and property in any way connected with the Equipment and the use thereof Se...

Страница 5: ...al A sample of each statement appears below Within each sample a definition of the statement type and its purpose is given DANGER DANGERS alert you to an immediate hazard that causes serious injury or death and requires special precautions to be taken WARNING WARNINGS alert you to a potential hazard that causes serious injury or death under certain conditions CAUTION CAUTIONS alert you to a non imm...

Страница 6: ...GOW MAC Instrument Co 6 ...

Страница 7: ...ations 13 Section 2 Safety 15 Section 3 Installation 17 Section 4 Operating Controls 25 Section 5 Operation 29 Section 6 Valves 37 Section 7 Maintenance 43 Section 8 Options Accessories 51 Section 9 Troubleshooting 55 Section 10 Replacement Parts 63 Section 11 Drawings Schematics 65 ...

Страница 8: ...GOW MAC Instrument Co 8 ...

Страница 9: ...hly read the appropriate sections of this manual before operating your instrument Certain sections of this manual apply to specific options you may have chosen for your instrument The information contained within concerns itself with a standard hotwire detector GC If you have Options 204 or 218 Capillary installed make sure to read Section 8 Operate the Series 580 GC according to these instructions...

Страница 10: ...GOW MAC Instrument Co 10 ...

Страница 11: ... 5 IN THIS MANUAL FAILURE TO REMAIN WITHIN THE STATED LIMITS WILL CAUSE FILAMENT BURN OUT RECOMMENDED STARTING BRIDGE SETTINGS FOR HELIUM WX filaments 100 mA AuW filaments 100 mA Ni filaments 100 mA WX7 filaments 80 mA FILAMENT OPERATING NOTES 1 Filament life may be extended by operating at low current and low cell temperatures The cell temperature should only be as high as needed for samples used and...

Страница 12: ...a CR in the part number take note CAUTION CAUTION This instrument was designed for DRY sample applications only Care must be taken to make sure only moisture free samples are introduced into the system GOW MAC Instrument Company is not responsible for damage to equipment caused by exposure to hydrolyzed samples ...

Страница 13: ...rature Range ambient to 400 C Temperature Readout 3 1 2 digit LED digital meter Temperature Control solid state time proportioning RTD sensors direct reading ambient to 400 C Column Oven Temperature Protection Circuit shuts the column oven off if the temperature rises to 30 C over the set point Oven Fittings accommodates 1 8 or 1 4 o d metal 6 mm glass or capillary columns Oven Capacity can accommo...

Страница 14: ...Temperature Readout 0 400 C 3 1 2 digit LED digital meter Injection Method direct on column or gas sample valves GAS FLOW conditions may vary depending upon the options chosen for your instrument Dual column with dual injection ports and exits Two metering valves for separate control of each column Exit ports allow easy collection of effluent Filament protector pressure switch in carrier inlet line ...

Страница 15: ...NOT overload the ac outlet with other electrical equipment 4 Adhere to the color coding descriptions when hooking up electrical connections 5 Repair or replace faulty or frayed wiring C COMPRESSED GAS CYLINDERS Compressed gas cylinders are potential sources of serious accidents injuries and even death if proper precautions and safety practices are not followed Therefore during handling and use of ...

Страница 16: ...ERAL 1 Perform periodic leak checks on all fittings 2 Store organic solvents away from the GC in fireproof vented labelled cabinets 3 DO NOT allow flammable and or toxic wastes to accumulate 4 Keep combustibles away from gas cylinders and eliminate ignition sources 5 DO NOT place papers charts samples etc on top of the GC 6 Maintain adequate ventilation 7 Dispose of wastes properly ...

Страница 17: ...s 580 1100 W at 115 V 60 Hz Series 582 550 W at 230 V 50 Hz CAUTION OPERATING INSTRUCTIONS FOR BOTH MODELS ARE THE SAME EXCEPT FOR LINE VOLTAGE REQUIREMENTS TO PREVENT DAMAGE TO THE INSTRUMENT MAKE SURE THAT THE AC ELECTRICAL OUTLET IS THE CORRECT VOLTAGE FOR YOUR INSTRUMENT BEFORE PLUGGING IT INTO THE OUTLET 5 GOW MAC Installation Kit Part no 59 400 or 1 8 o d copper tubing and Swagelok fittings 6...

Страница 18: ...lectrical outlet ac should be near the location where the Series 580 GC is to be installed If the outlet is not a 3 pin type make sure that a good ground connection is available since a good ground is necessary for proper operation The ac outlet should be connected to a circuit that is not heavily loaded with other electrical equipment because input voltage to the instrument should be steady for o...

Страница 19: ...als located at the rear of the G C Figure 3 1 Connection should be made as follows Black to black Red to red Silver to green 2 Connect the other end of the recorder cable to the proper terminals on the recorder GND INLET RECORDER GND I O Figure 3 1 Recorder Cable Connection G Integrator Connection The same cable referred to above can be used for connecting an integrator to the GC H Chromatography ...

Страница 20: ...of your own connect a 1 8 o d piece of clean copper tubing from the gas outlet located on the regulator of the carrier gas cylinder to the CARRIER GAS INLET on the back of the GC Swagelok fittings are recommended NOTE PLASTIC TUBING IS NOT RECOMMENDED SINCE ALL PLASTICS ARE PERMEABLE TO AIR To prevent contamination of your GC by grease oil or chemical residue the following procedure should be follo...

Страница 21: ...y fully clockwise then opened 1 2 turn counterclockwise CCW CAUTION THESE ARE PRECISION NEEDLE VALVES NOT SHUT OFF VALVES CARE SHOULD BE EXERCISED IN MAKING ADJUSTMENTS 7 Using Tygon tubing connect the two OUTLET PORTS together located on the left side of the GC 8 Adjust the PRESSURE REGULATOR on the gas cylinder to a gauge pressure of 30 psig then shut OFF the gas at the cylinder 9 If the system ...

Страница 22: ...psig may be required for longer 1 8 packed columns 10 or longer 3 A bubble type flowmeter can also be used with a stopwatch Gently squeeze the reservoir of the flowmeter until a stream of soap bubbles emerge Allow several bubbles to rise and wet the sides of the glass meter START the stopwatch when a bubble reaches the 0 mark on the meter STOP the stopwatch when the bubble reaches the 10 mark on the...

Страница 23: ...marked restrictor found in either the front or back of the Accessory Housing to equal flow rate set in Series position 30 mL min or 60 mL min NOTE Flows in series and by pass position should be equal to each other as well as equal to B side setting When setting flows on S B P Valve allow sufficient time for flows to stabilize 2 5 minutes M Installation Check List 1 Electrical _____ Correct voltage and ...

Страница 24: ...GOW MAC Instrument Co 24 ...

Страница 25: ...tector current reading to appear on the PANEL METER e SET IN ACTUAL OUT selects either actual or set point parameters for any of the functions a d above This button should be left in the ACTUAL OUT position EXCEPT when settings are being changed 3 COLUMN TEMPERATURE CONTROL Selects the temperature of the column oven Temperature is indicated on the DIGITAL PANEL METER when the COLUMN TEMP BUTTON is...

Страница 26: ...tarting bridge settings Section 5 NOTE DUAL CARRIER TCDs Controls to set the TCD temperature and bridge current are as described above Special attention is required when setting the TCD temperature and bridge current on a dual carrier detector Helium is normally one carrier gas while either nitrogen or argon is the other To determine the operating limits of the TCD current and temperature refer to...

Страница 27: ...0 GC is complete with four Swagelok fittings for 1 8 o d columns Unless otherwise specified The oven is designed to accept twenty 20 feet of 1 4 column tubing Correspondingly longer lengths of 1 8 tubing can be wound on a mandrel of 4 o d a standard 1 lb coffee can is about 4 in diameter This technique SHOULD NOT BE USED with 1 4 tubing Figure 4 2 illustrates column B An appropriate column or bypass ...

Страница 28: ...GOW MAC Instrument Co 28 Your Series 580 GC has been supplied with one 1 4 x 1 8 stainless steel column packed with 5 OV 101 on Chromosorb P AW DMDCS 80 100 mesh 4 50 dia max Figure 4 2 Column B ...

Страница 29: ...described in Section 3 Paragraph I e Disconnect flowmeter f Allow 5 minutes to purge the system before turning power ON 2 Temperature Controls NOTE TEMPERATURE CONTROL KNOBS are locking type Push locking ring IN to turn knob a Turn the DETECTOR CURRENT CONTROL fully counterclockwise CCW THIS STEP IS EXTREMELY IMPORTANT b Plug in the instrument to the appropriate ac outlet Switch the instrument ON C...

Страница 30: ... mA When maximum sensitivity is not required the current should be reduced to 100 mA Single Carrier TCD Chart 5 1 0 100 200 300 400 500 0 100 200 300 Bridge Current mA Cell Temperature C W WX W2 W2X AuW AuW2 Ni Ni2 Filaments Oxygen Argon Nitrogen Helium Chart 5 2 10 952 Cell with Wx7 Filaments 0 100 200 300 400 500 0 100 200 300 Bridge Current mA Cell Temperature C 400 Helium Nitrogen Argon ...

Страница 31: ...ll with Wx7 Filaments 0 100 200 300 400 500 0 100 200 300 Bridge Current mA Cell Temperature C 400 Helium Recommended Starting Current Dual Carrier TCD 0 0 100 100 200 200 Cell Temperature C Bridge Current mA 300 275 Dual TCD WX or W2B Filaments Argon Nitrogen Maximum Chart 5 4 ...

Страница 32: ...tric type 1 mV 10 mV or other For best results and maximum sensitivity the GOW MAC Model 70 150A 1 mV Recorder is recommended An adjustable chart drive is also recommended 40 20 10 4 2 and 1 cm min and hour After the recorder is properly connected to the instrument it may be turned ON At this time the electrical zero on recorder should be established Proceed as follows 1 Set the GC ATTENUATOR to t...

Страница 33: ...rence should be made to the software operating manual F Sampling Procedure 1 After a stable baseline is established change the GC ATTENUATOR to a setting of 8 then 4 etc until a straight line trace is obtained at the selected temperatures 2 INJECT the sample 3 Observe the developing peaks Set POLARITY to the setting either or which will give an upscale deflection for emerging peaks NOTE If your Ser...

Страница 34: ...NTS MAY BURN OUT OXIDIZE 5 Elute all samples from the column BEFORE the columns cool down 6 Turn ac power OFF 7 Turn helium or other carrier gas OFF when detector temperature is 80 C CAUTION IT IS MOST IMPORTANT THAT ELECTRICAL POWER BE TURNED OFF BEFORE THE HELIUM IS TURNED OFF AS LONG AS THE CELL AND FILAMENTS ARE HOT THE HELIUM SHOULD BE FLOWING THE FLOW RATE CAN BE REDUCED TO CONSERVE HELIUM C...

Страница 35: ...tional instrumentation is connected properly 2 Pneumatic _____ Gas cylinder pressure is sufficient _____ Cylinder pressure regulator set properly _____ Gas flow rates are adjusted properly _____ Appropriate columns are installed _____ Carrier gas flow pressure at 40 psig _____ Leak check made 3 Front Panel _____ All temperature settings are set BELOW the recommended circuitry maximum limits See Charts...

Страница 36: ...GOW MAC Instrument Co 36 ...

Страница 37: ... to three 3 valves They must be treated with care CAUTION VALVES HAVE UPPER TEMPERATURE LIMITS WHICH IF EXCEEDED CAN PERMANENTLY DAMAGE SLIDERS UPPER TEMPERATURE LIMIT FOR VALCO VALVES IN THIS GC 175 C UPPER TEMPERATURE LIMIT FOR ACTUATORS IN THIS GC 150 C All valves may be fitted with pneumatic actuators which are available from GOW MAC Air pressure of 50 60 psig is required for proper operation B...

Страница 38: ...y be taken from a static system or from a flowing stream Valves are also used to back flush column column selection sample selection and detector switching Since the most common use of the valve is for sample injection only that application will be discussed here in general terms The valve may be installed in place of or in series with the injection port The valve may be permanently connected to a s...

Страница 39: ... psi is recommended to fully drive the valve Option 411 Interface PCB is used to activate auto valves from a TTL closure generated by an external source i e computing integrator Option 411 will time a maximum of three 3 valves Option 412 accepts up to two 2 valves in a separate heated oven assembly located in the accessory housing G Automatic Valve Operation Interface PCB Opt 411 The interface PCB...

Страница 40: ...ll allow the separation of H2 O2 N2 CH4 CO and CO2 with one injection and one valve change First an injection of certified standard of H2 O2 N2 CH4 CO and CO2 is made with the S B P Valve in the B P position The porous polymer column will separate this standard into four components H2 Air O2 N2 or CO CH4 and CO The separation of the Air and CH4 may not be baseline on a 1 8 column but this is not im...

Страница 41: ...2 x8 Typical Chromatogram Analysis of Furnace Gases Instrument Series 580 Detector TCD Column See Note A Carrier Gas Helium Carrier Flow 40 cc min Temperature Column 59 C Detector 100 C Bridge Current 150 mA Attenuation Noted Sample Gas Mix Sample Size 2 cc Note A Column 1 7 x 1 8 Porapak Q 80 100 mesh Column 2 8 x 1 8 Molecular Sieve 5A 80 100 mesh ...

Страница 42: ...GOW MAC Instrument Co 42 ...

Страница 43: ...utes which are exhibited under different requirements of analysis such as corrosion resistance oxidation resistance catalytic reactions and sensitivity CHEMICAL RESISTANCE BEHAVIOR OF VARIOUS GOW MAC FILAMENTS Gold Sheathed Tungsten Nickel Tungsten Substance W WX Ni HR AuW Oxygen Good Good Very Good Water Good Good Good Steam Good below 700 C Good Good Ammonia Amines Good Poor in presence Poor of H...

Страница 44: ...tings c Replace the columns with lengths of CLEAN copper tubing Refer to Section 3 paragraph H and Figure 7 1 d Inject 100 mL of acetone through the septum and leave overnight e Purge the sampling system of the entire GC with helium at a flow rate of 20 mL min for one hour f With DETECTOR CURRENT at 100 mA observe 1 completion of acetone purge and 2 correction of detector contamination WARNING If y...

Страница 45: ... GLOVES IS RECOMMENDED To remove the detector use the drawings provided and proceed as follows a Remove the columns using 9 16 open ended wrenches for 1 4 fittings or 7 16 wrenches for 1 8 fittings b Remove the two 2 screws located just above and below the OUTLET PORT c Remove the SEPTUM NUTS d Remove the six 6 screws from the FRONT OVEN PANEL e CAREFULLY remove insulation so as to expose the DETECT...

Страница 46: ...emoving the four 4 screws l Remove the DETECTOR HOUSING front panel by removing the four 4 screws m Remove the DETECTOR HOUSING rear panel by removing the four 4 screws n CAREFULLY lift the DETECTOR out of cell housing 4 Filament Replacement To replace filaments proceed as follows a Place cell in a vise b Using a 1 2 wrench remove each of the four 4 bushings holding each of the four 4 filaments in p...

Страница 47: ... ceramic is properly installed in the small hole in the DETECTOR HOUSING bottom This is only held in place by the insulation B Columns NOTE When ordering new columns please specify the instrument model number and serial number whether the column is for side A or B length diameter material liquid phase loading solid support and mesh size 1 Supplied Column Care should be exercised to ensure that the...

Страница 48: ...d the bevelled end of the injection port Then back off about 1 4 to allow carrier gas to sweep into the column By using this technique on column injections can be attained CAREFULLY tighten nuts with a 9 16 wrench or 7 16 wrench for 1 8 fittings CHECK FOR LEAKS 1 4 o d Column 1 8 o d Column with Glass Adapter 1 8 o d Column Standard Optional Optional Figure 7 2 Injection Ports C Septums The septums ...

Страница 49: ...ure gradients The blower also provides rapid cool down when needed E Column Oven The column oven is heated by a 500 W tubular heater controlled by a proportional control The solid state control incorporates a platinum RTD Resistance Temperature Detector and a 3 3 4 turn set potentiometer Built into the circuitry is a fail safe feature which disables the controller s triac output in the event of sh...

Страница 50: ...perature Control The injection ports are heated by 60 W heaters mounted inside the injector block The temperature control sensor is also located in the block The injection port temperature is controlled in the same manner as the column oven ...

Страница 51: ...a constant upstream pressure flow is varied by changing the pressure drop across the stratified flow element Once the differential pressure is set it is maintained regardless of changes in the down stream pressure C Capillary System Capillary chromatography provides the utmost in GC performance Advantages to using capillary techniques include high efficiencies about 4000 plates per meter versus about 50...

Страница 52: ...MPERATURE READOUT AND TEMPERATURE SHOULD BE DETERMINED BY EXPERIMENTATION 2 The column adapter is attached to the column exit port of the GC instrument which is located directly after the hotwire detector front left The heated exit port is threaded to match the 6 32 adapter MOST IMPORTANT The threads of the exit port must extend sufficiently along the exit port section of the column so that the end ...

Страница 53: ...Tube 12 mL Centrifuge Tube Cotton Plug 100 μL Conical Vial Sample Collects Here GC Collection Tube GC Connection Adapter Vial Conical Reaction Threaded Figure 8 1 Microscale Prep Kit E Dual Carrier TCD With a TCD helium is usually used as the carrier gas In order to achieve high sensitivity the samples should have a different thermal conductivity than the carrier gas Most of the components we want ...

Страница 54: ...GOW MAC Instrument Co 54 ...

Страница 55: ...tructed carrier gas lines Injector septum leaking Replace septum Column connections leaking Tighten connections Carrier gas connected to Provide correct carrier gas wrong injector connection to injector Recorder not properly Check recorder connections connected recorder see recorder manual defective Syringe leaking or Replace syringe plugged Insufficient carrier gas Check carrier gas pressure pressu...

Страница 56: ...ncreased retention time too low for depleted carrier gas supply obstructed carrier gas lines Carrier gas leaking at Locate and correct leak injector septum column fittings etc Column temperature too Increase column temperature low Negative peaks Polarity switch in wrong Select correct polarity for position location of analytical column Sample injected into Inject sample into wrong column correct co...

Страница 57: ...ontroller to ensure proper operation Poor grade of carrier Replace cylinder Carrier gas gas or contaminated should be zero grade or cylinder better Consult local gas supplier Sinusoidal a baseline drift Detector oven temp Check temperature sensing controller or sensor defective probe for resistance approx or improperly installed 100 at room temp and proper installation Column oven temperature Same...

Страница 58: ... without difficulty This symptom may occur even on well conditioned columns in which carrier gas flow rates have been carefully optimized High background noise Column contaminated Recondition column or excessive column bleed Contaminated injector Clean injector and replace septum Contaminated detector Clean detector Defective recorder Set GC Attenuator to infinity If noise continues check recorder See...

Страница 59: ... stepping Instrument and or recorder Make sure instrument and Baseline does not return not properly grounded recorder are connected to to zero attenuation is good earth ground incorrect peaks are flattopped Recorder gain and or control Adjust recorder gain and or improperly adjusted damping control Refer to recorder manual Baseline cannot be properly set Adjustable recorder zero not Set detector co...

Страница 60: ...n in flow lines Heat lines to remove regular intervals causing carrier gas to bubble condensation while purging through with dry gas Leading peaks Column overloaded Sample Decrease sample size size too large for column diameter and length Sample condensed in system Check that injector and detector settings are correct Unresolved peaks Column oven temperature Reduce column oven too high temperature ...

Страница 61: ...time for eluting from previous previous sample injection to sample injection elute chromatogram I Chrom I Air peak chromatogram II Normal when making syringe injections Desorption from column Make several solvent packing when solvent is injections and recondition injected chromatogram II column Chrom II Sample decomposition Reduce injector temperature chromatogram II Use different column if packing...

Страница 62: ...GOW MAC Instrument Co 62 ...

Страница 63: ...upply 123 191 240 Temperature Controller PCB 123 177 240 Display Switch Interface PCB before S N C38001 123 185 Display Switch Interface PCB after S N C38002 123 194 Mechanical Assemblies Injection port assembly 069 86 1 Electronic Parts Zero potentiometer 20K 111 178 and Controls Receptacle power switch w line filter 115 230 V 129 152 10A Fuse 10 A 115 V 121 162 Fuse 5 A 230 V 121 177 Attenuator b...

Страница 64: ... 10 580 04 1 TC cell s s capillary w 1 8 fittings 10 955 WX7 205 10 580 05 2 TC cell s s prep w 1 8 fittings 10 077 WX 206 10 580 06 1 TC cell s s prep w 1 8 fittings 10 077 AuW 207 10 580 08 1 TC cell s s prep w 1 8 fittings 10 077 Ni 209 10 580 09 1 TC cell s s nanokatharometer w 1 8 fittings 10 952 WX 210 10 580 10 1 TC cell s s nanokatharometer w 1 8 fittings 10 952 AuW 211 10 580 11 1 TC cell s s n...

Страница 65: ...Series 580 TCD Gas Chromatograph September 2017 Rev 5 65 Section 11 Drawings Schematics Flow Diagram Wiring Schematic ...

Страница 66: ...GOW MAC Instrument Co 66 ...

Страница 67: ...e boxes are checked the following statements and or questions must be answered 1 Specifically describe where on or in the instrument device part there could be any residual contamination for example blood spill on the surface ____________________________________________________________________________________________ _________________________________________________________________________________...

Страница 68: ...GOW MAC Instrument Co 68 ...

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