BASIC INSTRUMENT INSTRUCTIONS PART NO. 70304-91 Series 100 and Series 400 Analytical Gas Chromatographs‘Table of Contents Section 1 — Background Information: System Design Approeh, Tstrument Characteristics and General Installation and Operating Requirements Section 2 — AGC-111 Step-By-Step Installation and Operating Procedure Section 3 — AGC-211 Step-By-Step Installation and Operating Procedure ......-... ++ 5 Section 4 — AGC-311 Installation and Operation... . - « Berane eeriae Section 5 — AGC Shutdown . . . Section 6 — Understanding AGC Subsystem Operation ‘A. Flow Subsystem — Carrier Gas and FID Fuel Gases... . peaereernte, B. Heating Subsystem 9 C. Temperataure Controller Subsystem sso ee et. D. Inlet Subsystem... 6. it iW E. Column Subsystem... 2... ss sae eae eee eee ret Seer Section 7 — TCD Design and Operation... 2.0.0 0e ee eves eee ee eee 12 Section 8 — TCD Electronics Design and Control Functions... . . - pores eHas Section 9 — FID Design and Operation... 022000000005 15 Section 10 — FID Flectrometer Design and Control Functions 16 Section 11 — Using the AGC with Valves ce 18 Section 12 — Owner Service: Interchanging TCD Sensors and General Troubleshooting Guide . 19 Section 13 — Factory Service: Module Removal for Factory Repair»... - 0. ++++++ 23 Section 14 — Replacement Parts aes . Section 15 — Instrument Schematics and Wiring Diagrams Soe eee te aECerat29. PRINTED IN USA.Section 1: Background Information System Design Approach All models of the Analytical Gas Chromatograph (AGC) are compact, convenient instraments designed to give high quantitative accuracy with years of trouble free service. ‘The heating system of each instrument features a solid- state, full-proportional temperature controller capable of responding to temperature changes of less than 0.001°C, ‘This controller operates high wattage heaters carefully matched with conductive thermal mass £0 give precise temperature control of columns, inlets, detectors and valves from ambient to 399°C with only a single digital temperature control. Allelectronics, including the electrometer for the flame ionization detector (FID), the bridge/power supply for the thermal conductivity detector (TCD) and the tem- perature controller, are modular for user convenience, Bach electronic module is removable as @ unit so that factory exchange or service can be conducted promptly and economically. Particular features of the FID are very high sensitivity, unusually wide dynamic range, and location of high impedance connections and insulators to minimize the need for cleaning. The low volume TCD is designed for either thermistors or filaments, and the bridge power supply adapts to either at the push of a switch, Tlets are designed to confine samples in the column and allow for both flash vaporization and on-column injection. ‘Mounting brackets are provided for up to three valves, fone at ambient and two at controlled temperature Ready accessibility of the column, detector, inlet and valve area are provided by the flip-open top. In every case the design engineers have attempted to provide an instrament to work with, ratber than work on. All AGC models are dual-column, dual-inlet instru- ments. Standard columns are ‘A-inch in diameter. However, through the use of accessory inlets and fit- tings, the design provides for Yie-, Yie- and Yinch columns. Columns are heated with an air bath sur- rounded by and uniformly heated with a conductive metal enclosure. Detectors, valves and inlets are heated conductively through contact with aluminum plates — permitting operation of these components at stable, differential temperatures above column temperature. Characteristics of AGC-LLL ‘This model of the AGC is provided with a filament or thermistor thermal conductivity detector. The two dif- ferent sensing elements are interchangeable and the power supply adapts to cither with the push of a switch ‘The use of thermistors is advantageous for highest sensitivity below about 70°C and in those cases where oxidation by sample components may be a problem ‘with filaments. Filaments give higher sensitivity at temperatures above 70°C and also permit hydrogen to be used as carrier gas. The power supply provides constant current to maximize the dynamic range of the detector and to keep sensitivity constant under particu- lar operating conditions. Attentition is in binary steps ‘and has a range of 1 to 1024 to provide an optismum interface with modem data handling equipment, Characteristics of AGC-211 ‘The AGC-211 comes with a flame ionization detector ‘and a high sensitivity electrometer, Single-burner, dual-input detector design gives column choice ver satility as well as the same sensitivity with either col- umn. Wide dynamic range and improved sensitivity are provided because ofthe Larger flame and optimiza- tion of the eartier gas and hydrogen ratio. ‘The varactor bridge electrometer gives a sensitivity of 10°"? amps full scale. Range attenuation is in steps of 10 from to 10°, Output attenuation is in binary steps from 1 to 1024, giving a total attenuation range of slightly more than 107 while maintaining the flexibility of selecting the optimum range for maximunn signal-to-noise ratio and best linearity. Characteristics of AGC-311 ‘The TCD of the AGC-11 Land the FID of the AGC-211 are combined in this instrument, Detectors can be op- ‘erated independently or simultaneously. This gives the capabilities of either or both of the single detector instruments. Simultaneous operation gives the addi- tional capability of a more complete analysis with a single sample injection than is possible with two sepa- rate single detector instruments. General Installation Requirements A little care and preparation on initial instalation will help increase long-term, high-quality performance of the AGC. Carrier and fuel gases of adequate purity are particularly important. Organic contamination inthe carrier gas or hydrogen fuel gas at a level of no ‘more than 50 ppm may give a background of full scale ‘ata range attenuation of 10° with the FID. This would make trace analyses impossible. Carrier gas and hydro- gen with an organic contamination level of I ppm or less are readily available and should be used. Cleanliness of tubing, regulators and fittings is very important, particularly with the FID. One drop (about 50 mg) of oil or organic solvent in any of these areas provides sufficient contamination to give a full scale background with the FID at a range attenuation of 10° for 1.5 hours. All connections and cylinders should be leak-free. This is important to obtain stable flow rates and prevent waste of gases. It is even more important to Keep ait out of the carrier gas. A small leak of about 10-* mL/see could permit an inward air leak sufficient to contaminate the carrier gas to a level of 10 ppm. (Large carrier gas leaks aetually pose less ofa problem because they tend to prevent inward air leaks.) In addition to being clean, all regulators used on cartier ‘gas and fuel gas cylinders should give a constant outlet pressure at a given setting. In most cases flow rates are controlled from the outlet pressure. The outlet pres- ‘sure range should be adequate for pressure: drops ex- pected, but too much range is undesirable because it limits precision when setting the regulator. Column pressure drops rarely exceed 70 psig. ‘The range of outlet pressure of the carrier gas (usually helium) reg- lator should be « minimum of 0-50 psig and, except special cases, a maximum of 0-100 psig. Pressure drop for hydrogen fuel gas is provided with fa builtin restrictor fitting. ‘The outlet of the hydrogen regulator usually will be operated at 20-25 psig with Yéeinch columns and 45-50 psig with Yi-inch columns, ‘Therefore, a maximum of 100 psig for the second stage of the hydrogen regulator is adequate. Pressure drop for air fuel gas also is provided with a built-in restrictor fitting, The outlet of the air regulator usually will be operated at about 20 psig. However, since air flow is not particularly critical, the more common 0-100 psig outlet pressure range regulator generally is used. AIL AGCs require 118 VAC, 50/60 Hz and can draw ‘a maximum of up to 7 amps. A three-wire cord is provided and a good earth ground is necessary. The ‘common side of the circuit should not be more than one volt away from ground. AGCs are designed to work with a line voltage of 100-130 VAC. Best per- formance will be obtained when line voltage has rela- tively good short-term stability. Recorders and other ancillary equipment used with the AGC should have the same ground, A good practice is to use the same circuit (wall receptacle). ‘Some AGCs have internal or external 220 VAC, 50/60 Hz step-down transformers which are factory-installed. ‘This option may be requested for a fee at the time of order.Section 2: AGC-111 Installation, Operation AGC-111 Installation 1, Carefully unpack instrument and remove all in- ternal packing material 2. Place instrument on table or bench where itis to bbe used. Turn on back so that bottom is facing forward. Remove hold-down straps to frec carrier gas line and power cord, CAUTION: Do not plug in instrument at this point. 3. Attach a carrier gas line to a source of pressurized carrier gas through an adequate regulator. 4. Install the valves and columns to be used if they differ from standard columns shipped in the instrument. 5. Set carrier gas to proper flow rates. (See Section 6A and 6B.) 6. Connect recorder cable to a I-mV recorder, red to +, short black to —, long black to recorder ground, At AGC, connect red to terminal No. 3 and black to terminal No. 2 on barrier strip at back of TCD bridge power supply. 7. Free reference thermocouple (back of bridge power supply). For accurate temperature meas- ‘urements, place in an ice slush before reading termperature on the recorder. 8, Make sure the push-push switch for filaments or thermistors (back of bridge power supply) is in proper position for sensing elements to be used. ‘Thermistors, installed when shipped, may be re- placed by the user with the filaments shipped ‘with the instrument if desired. (See Section 12.) 9. Make sure COLUMN TEMP (digital switch) is set t0 000. INLET ATT switch is off. BRIDGE SETTING switch is off, POWER switchis off. 10. Plug power cord of AGC into three-wired recep- tacle which supplies 118 VAC, 50/60 Hz and will deliver a minimum of 10 amperes. Ground should be a real carth ground. The neutral side of the line should not be more than 1 volt away from ground. 11. Plug recorder in. Power ground must be same as that of the AGC. It is preferable to operate both from the same circuit AGC-LL1 Operation (Filaments) Instrument is installed and carrier gas flow rate is set. Push POWER switch on. NOTE: Do not tun INLET AT switch on unless additional inlet heat is needed, (See Section 6B and 6C.) Set COLUMN TEMP switch to column temper- ature desired. Turn OUTPUT switch to TEST. Tum recorder ‘on. Recorder pen should be at zero after recorder has had a few minutes to warm up. If pen is not at zero, recorder should be zeroed according «0 recorder instructions, Place reference thermocouple in ice slush. If an ice reference is not used, the ambient temperature rust be added to the temperature read on the re- corder and measured temperature will be subject to ambient fluctuations, Turn OUTPUT switch to COL. Monitor column temperature on recorder (1 mV = 400°C, I div = 4°C). Occasionally tum OUTPUT switch to INLET and check inlet temperature. (NOTE: Inlet temperature will rise mote rapidly than column. See Section 6B.) Place BRIDGE SETTING switch at 1, 3, 6 oF 8 Always use lowest setting that will give required sensitivity. (NOTE: See Section 7.) Place READOUT switch at LEFT or RIGHT de- pending on column and inlet to be used for the samples. When columns have reached set temperature as indicated on the recorder and inlet temperature is stable, tum OUTPUT switch to 128, Zero recorder with COARSE ZERO control. Then place OUT- PUT switch at 1 and zero with FINE ZERO. (NOTE: See Section 8.) COARSE and FINE ‘ZERO may be used together and interchangeably, but it is more convenient to usc FINE ZERO at tow attenuations and COARSE ZERO at high attenuations. When adequately stable, the instrument is ready for sample injection. Inject sample and attenuate as necessary with OUTPUT switch to keep peaks on scale,AGC-L11 Operation (Thermistors) ‘Steps 1 through $ are the same as Steps | through 5 for filaments. Make sure the FILAMENT- HERMISTOR switch at back of TCD elec: tronic module is in ‘THERMISTOR position. Place READOUT switch to CURRENT posi- tion. Place BRIDGE SETTING switch to ‘THERMISTORS. Place OUTPUT switch to 1. Measure thermistor current on recorder. (1 mV = 50 mA or 1 div = 0.5 mA) Set desired thermistor current by turning screwdriver CURRENT control clock wise to increase, counterclockwise to decrease. NOTE: Current is pre-set at the factory and may 10. ML. not need adjustment. (See Section 7 and 8.) ‘Turn BRIDGE SETTING to OFF. Turn READ- OUT switch to LEFT or RIGHT depending on column to be used for samples. ‘Tur OUTPUT switch to 1024, Turn BRIDGE SETTING to THERMISTORS. ‘When column has reached set temperature, adjust coarse zero for the mid-point of its range, and then zero recorder with screwdriver BALANCE control When adequately stable the instrument is ready for sample injection. Inject sample and attenuate as necessary to keep peaks on scale,Section 3: AGC-211 Installation, Operation AGC-211 Installation 1. Carefully unpack instrument and remove all in- ternal packing material. 2, Place instrument on table or bench where itis to toe used. Tum on back so that bottom is facing forward. Remove hold-down straps to free gas Fines and power cord. (CAUTION: Do not plug in instrument at this point.) 3, Attach carrier gas line ('4-inch Tine going to tee inside instrument) to a sourve of pressurized car- rier gas through an adequate regulator. 4. Attach hydrogen line (A-inch Tine going to re~ strictor fitting inside instrument) to a source of pressurized hydrogen through an adequate reg- ulator. (CAUTION: Do not put hydrogen through air line.) Attach air line (V/-inch line going to a restrictor fitting inside instrument) to a source of pres- surized air through an adequate regulator. 6, Install the valves and columns to be used if they differ from the standard columns shipped in instrument. 7. Set carrier gas to proper flow rate, (See Section 6A and 6B.) 8. Connect recorder cable to a 1 mV recorder, red to +, short black to —, long black to recorder ground. AC AGC connect red to terminal No. 3 ‘and black to terminal No, 2 on barrier strip at back of FID electrometer. 9. Free reference thermocouple (back of electrome- ter). For accurate temperature measurements, place in an ice slush before reading temperature on recorder. 10, Make sure COLUMN TEMP (digital switch) is set to 000. INLET AT switch is off. ZERO SUPPRESSION toggle switch is off. POWER switch is off. 11. Plug power cord of AGC into three-wire recepta- le which supplies 118 VAC, 50/60 Hz and will deliver a minimum of 10 amperes. Ground should be a seal earth ground and the neutral side of the Tine should not be more than 1 volt away from ground, 12. Plug recorder in. Power ground must be the same as that of the AGC. It is preferable to operate both from the same circuit AGC-211 Operation 1. 10, Instrument is installed and cartier gas flow rate is set. Push POWER switch on. (CAUTION: When power is on, 300 volts are supplied to polarizing electrode of FID.) (NOTE: Do not turn INLET AY switch on unless additional inlet heat is needed. See Section 6B and 6C.) ‘Set COLUMN TEMP switch to column temper ature desired. ‘Turn OUTPUT switch to TEST, Turn recorder ‘on. Recorder pen should be at zero after recorder has warmed up for a few minutes. If pen is not at zero, recorder should be zeroed according to recorder instructions. Place reference thermocouple in ice stush. If an ice reference is not used, ambient temperature rust be added to temperature read on recorder ‘and measured temperature will be subject to am- bient fluctuations. Turn OUTPUT switch to COL. Monitor column ‘temperature on recorder (1 mV = 400°C). Ocea- sionally tum OUTPUT switch to INLET and check inlet temperature. (NOTE: Inlet tempera ture will rise more rapidly than column. (Sec Section 6B.) ‘Turn RANGE switch to BAL. OUTPUT switch to 1. Then with AMPLIFIER BALANCE con- trol place recorder to zero, (NOTE: The elec- trometer is now zeroed. Repetition of this adjust ment should not be required unless AGC has been tumed off. Never usc AMPLIFIER BAL- ANCE to zero output of FID. ZERO SUPPRES- SION is used for this purpose.) Start hydrogen flow. Initially set outlet pressure of regulator 10 psig above pressure to be used. (NOTE: See Section 6A). ‘After allowing one to two minutes for hydrogen Tine to purge, depress IGNITE button for about ‘two seconds. Burner should make a slight pop ‘when lit, Confirm flame is on by holding a mirror or shiny metal plate over the burner exhaust; the mirror will fog if flame is on. Start air flow by setting outlet pressure of reg- ulator to desired pressure, usually 15 to 20 psig. (NOTE: See Section 6A.) Reduce hydrogen regulator to proper operation outlet pressure.11, Allow columns and inlets to reach set temperature as indicated on the recorder. 12, Tum OUTPUT switch to 1. Flip ZERO SUPPRESION toggle switch on, Turn RANGE switch to 10°, Recorder pen should be on scale unless background signal from flame is unteason- ably high. (NOTE: See Sections 6A and 6E.) Bring recorder pen to zero with COARSE and FINE ZERO SUPPRESSION control. Sequen- tially turn RANGE switch to 10°, 10 and 1, using COARSE and FINE ZERO SUPPRESSION controls to zero at each stage. Electrometer and output from flame are now zeroed. It should be possible to change RANGE settings from 1 to 10* and OUTPUT settings from 1 to 1024 without Section 4: AGC-311 Installation, Operation 1. For TCD operation, refer to installation and operat- ing procedure for AGC-111 2. For FID operation, refer to installation and operat- ing procedure for AGC-211. NOTE: It is assumed the AGC-311 normally will be used with a nwo-pen recorder (one channel for each detector). The tem- perature readout on the recorder is controlled by Section 5: AGC Shutdown ‘A gas chromatograph performs best when iti left on, ‘Time is required for temperatures to equilibrate, Gas flows equilibrate according to pressure drops, which are temperature-dependent, Column vapor pressure must stabilize and the whole system must be purged to remove impurities and atmospheric contamination, In deciding what to turn off, the time required to re- establish adequate stability must be weighed against the cost and possible danger (if unattended) of leaving the instrument on, a significant offset of zero. Flame will not be operable at a RANGE setting of 1 and possibly 10 until background signal from the flame is low and stable. 13. When adequately stable the instrument is ready for sample injection. Set OUTPUT switch to 1 and RANGE switch to position dictated by sam- ple, As rule of thumb use a RANGE of 1 for picograms, 10 for nanograms, 10°-10° for micro- grams and 10°-10* for milligrams of sample com- ponent. Inject sample and attenuate as necessary to keep peaks on scale. Whenever possible leave RANGE switch at set position and attenuate with OUTPUT switch, the FID output switch. However, if a single pen recorder is being used, the column and inlet ther- ‘mocouples can be moved for control at the output switch of the module being used (ie., to the FID electrometer or TCD bridge). Each module has its ‘own terminal strip, and the thermocouple connee- tions on each strip are numbered 5, 6 and 7. Suggested Guidelines Overnight 1. Tum BRIDGE SETTING off. 2. Turn hydrogen off. 3. Reduce carrier flow. 4. Reduce air flow Weekend 1-4 Same as above. 5. Place POWER SWITCH off. Longer Than Weekend Complete shutdown. Carrier gas flow should not be turned off until columns have cooled,Section 6: AGC Subsystem Operation Even though it is possible to operate the AGC without referring to this and subsequent sections, the user is urged to read them carefully when time permits. Infor- ‘mation presented makes operation of the instrument simpler and more understandable, permits saving of time and helps achieve peak performance. A. Flow Subsystem:Carrier Gas, FID Fuel Gases ‘The carrier gas for all AGCs is brought into the instru- ‘ment through a clean ‘4-inch copper line toate fitting. Flow is divided at the tee fitting according to the pres- sure drop of the columns to supply each inlet and column. (See Figure 1.) Provision is made at the tee for front panel mounting of two accessory needle valves, one for each column, if desired. A single needle valve can be used for addi- tional pressure drop to balance flows between columns of significantly unequal pressure drops. The second needle valve can be added both to balance flows and increase the pressure drop of the column system. This may be desirable to achieve better flow control when Tey short low pressure colums are wed, or when igure 2 — Optional needle valve resicion eat be large liquid samples are injected. Mounting of needle added to one or both columns for additional flow con- valves is shown Figure 2. trol and column balancing. LEFT INLET 10 { LEFT COLUMN a3) VagIARLe [ RESTRICTORS RIGHT INLET To ior couumn | {7319 CARRIER ‘GAS AIR Figure 1 — AGC Flow System: Valves and restritors are optional accesories and can be installed in different configurations than the one shown.Carrier Gas Pare helium is the most commonly used carrier gas, particularly with the thermal conductivity detector. Helium, inert and nonflammable, has high thermal conductivity (the highest except for hydrogen). Nitro- gon and argon are used frequently with the flame ioni- zation detector and may be used with the TCD. How- ‘ever a large loss in sensitivity occurs when used with the TCD (except when measuring hydrogen or neon). Hydrogen may be used with the TCD with no loss in sensitivity (not recommended with thermistors). Hydrogen also may be used as carrier gas with the FID under certain conditions, When hydrogen is the carrier gas with the FID, the column flow becomes: ‘one of the required fuel gases. Therefore column flow rate must be adjusted to be within the limits of the hydrogen flow satisfaptory for the burner, With '4-inch ‘columns, this is not difficult because the desired col- ‘umn flow of about 40 mL/min (20 mL/min through ‘each column) is well within the capabilities of the burner, If hydrogen is used as a cartier gas, remember hydr0- genation of partition liquid and sample components can occur at elevated temperatures. Also, it is highly flammable, and all necessary precautions should be observed. With hydrogen as carrier gas, nitrogen or ‘argon should be put through the normal hydrogen line to serve as diluent gas in the flame. “The viscosity of all carrier gases increases with temper- ature, Therefore, when the column is the controlling, pressure drop in the system, flow rate will decrease with an increase in column temperature at a fixed car- rier gas pressure. Carrier gas pressure must be in- creased at the rate of factor of 2 for an increase in column temperature of about 200°C to obtain the same volume flow rate. ‘With the AGC-111, carrier gas flow from each column ‘can be measured at the detector exhaust lines with a bubble meter (Cat. No. 72506-50). The right column ‘exhaust is on the right side. With AGC-211 and 311, carrier gas from both columns is combined and exhausts at the burner jet. ‘Total flow is measured at the jet with the special Teflon-tipped tube (Cat. No. 72090-30) provided with the instrument and a bubble meter. Hydrogen flow must be off. Indi- vidual column flows with both the 211 and 311 may be determined by removing the column at the detector fitting and measuring at the exit end of the columns. FID Fuel Gas — Hydrogen Hydrogen flow to the FID is controlled by regulated pressure and a built-in restrictor fitting connecting the hydrogen line to the burner, The pressure drop of the restrictor fitting gives a hydrogen flow of approxi- mately 25 mL/min when the inlet pressure is 20 psig. Because sensitivity and noise level of the FID are both 1 function of the hydrogen-carrier gas ratio, the flow rate of hydrogen should be set carefully. This relation- ship of hydrogen with helium carrier is shown in Figure Figure 3 — FID sensitivity relative to Hy/HH, ratio Maximum sensitivity occurs at a H,/He ratio of 0.6. ‘A similar relationship holds with H,IN2, except the curve is steeper and maximum sensitivity occurs at a somewhat lower ratio of Ha/Nz. In some cases it will bbe desirable to operate the flame hydrogen-tich. The "upper limit of the linear range of the burner is a function ‘of the amount of sample component relative to hydro~ gen, Linearity will be maintained only up to about 3% by volume (gaseous) of sample component relative (0 volume of hydrogen. ‘Also remember column bleed counts as sample compo- nent, Flow rate of hydrogen should be measured at the flame jet with the special Teflon-tipped tube provided with the FID instraments. Carrier gas flow should beoff, but itis possible to first measure carrier gas with hydrogen off and then measure total flow. FID Fuel Gas — Air Air flow to the FID is controlled by regulated pressure and a built-in restrictor fiting connecting the air line to the burner. The pressure drop of the restrictor fiting, gives a flow rate of approximately 500 mL/min when the inlet pressure is 20 psig. Air flow rate is not par~ ‘ticularly critical and normal flow is about 400 mL/min or 16 psig. Sensitivity will decrease and noise will increase at both excessively low and high flow rates. Measurement of air flow rate normally is not required; just set pressure at 16-17 psig. B, Heating Subsystem ‘The beating system of the AGC consists of a column’ detector heater, inlot'valve heaters, platinum resistance thermometer (PRT), full-proportional temperature con- troller, thermal burn-out link, and thermocouples for ‘measuring column and inlet temperatures, ‘The column-detector heater is clamped underneath the ‘aluminum detector plate/column box enclosure. Col ‘umns are evenly heated to the desired set temperature in the air bath formed by the column box. Dectector(s) are mounted directly to the plate and heated to a tem- perature which is relative to but always slightly higher than column temperature. Inlets and valves are contact-heated with an aluminum inleUvalve plate tightly coupled to the inlet heaters. ‘Instrument on, Col. set to 6 EEE 20 EFL S0 THEE 40] Figure 5 — Typical temperature rise time Figure 4— Inlet and detector temperatures relative to column temperature “The inlet heater has two windings. One winding is for normal inlet/valve heating and is controlled proportion- ally from the temperature controller. The other wind- ing, the INLET AT heater, provides additional inlet heat when desited. It is operated from the INLET OT switch on the temperature controller. Normal inlet! valve temperatures are relative to column temperature ‘and always higher than the column. Typical tempera~ ture relationships relative to column temperature are shown in Figure 4. Saket aT on “1 fete Bgutlibrated At Now Temp.With the exception of INLET AT, all temperatures are set with the digital switch which is numerically equal fo column temperature, Temperature profiles be- tween columns, detectors and inlets have been selected carefully for high performance, trouble-free chroma- tography while maintaining simplicity of operation. A typical temperature rise and equilibration pattern for columns and inlets is shown in Figure 5. Even though the INLET AT heater does not signifi- cantly affect measured column temperature, some of the additional heat applied is conducted down part of the column length and slightly affects retention times. Magnitude of these retention time changes will be greater with short metal columns than with glass or Jong metal columns. For best repeatability of retention times with a given application, the INLET AT heater should always be either on or off. ‘The PRT in the heating system supplies the signal to the temperature controller, causing it to control output voltage to heaters for precise temperature control. If the PRT should short for any reason, full heat will be applied. However, 2 burn-out link is provided (acces- sible from the base) to turn off power to the heaters if the instruments reach 425°C, If the PRT should open, the temperature controller will not supply power to the heaters. The PRT has a resistance of about 07 hins at 25°C. In the event that a PRT must be replaced, the replacement unit will match so closely that no readjustment of the temperature controller should be necessary. ‘Thermocouples in the AGC electrically float and should not be grounded. Grounding of a thermocouple ‘will result in erroneous temperature measurements, ‘The thermocouples are chromel-alumel. Output vol- tage is divided at the OUTPUT attenuator to give @ I-mV signal at the recorder for 400°C. Room temper- ature must be added to the recorder reading unless the reference thermocouple is placed in an ec slush. C, Temperature Controller Subsystem ‘This is a completely solid-state, full-proportional con- troller, As shown in Figure 6, power to the instrument is controlled by the POWER switch, Column temper- ‘ature is set on the digital dial (COLUMN TEMP) which is settable in 1°C increments up to 399°C. 10 Figure 6 — Power switch, the digital column temper~ ‘ature control and the INLET AT switch of the temper- ature controller When a temperature higher than ambient is sot on the COLUMN TEMP dial, an inbalance signal from the PRT occurs at the input of the high-gain integrated circuit differential amplifier of the temperature control- Jer. ‘This imbalance signal is amplified and converted to a train of pulses which fire a triac at the correct phase angles to apply the precise amount of required power to the heaters. As the temperature of the AGC Increases, the PRT increases in resistance until the input to the amplifier is balanced (the AGC reaches the desired set temperature). ‘The closed loop system then maintains the instrument at set temperature. The INLET AT switch tums power on or off to the auxiliary winding of the inlet heater to supply addi- tional heat to the inlet, if desired, Screwdriver control 1 adjusts the span ofthe temperature controller to match the characteristics of the PRT. Serewdriver control 2 sets the zero of the temperature controller. Both of these controls are faetory-set and should aot require readjustment even if a PRT (Cat, No, 72090-11) must be replaced. Electrical connections to the temperature controller are made through an edge connector facilitat- ing removal of the unit if necessary.D. Inlet Subsystem Dual inlets for “-inch ©.D. columns are standard with the AGC. Optional inlets for 14-inch O.D. columns and Ye-inch O,D. columns are available. The “is-inch 0.D. columns are sleeved to fit into the standard inlets. Glass column dimensions which require the inlets for Vcinch columns are available. Spring-loaded septurn exp ste Stow in J passage Cairn WN Cohum Figure 7 — Schematic diagram of inlet ‘When a sample valve is being used, carrier gas is first brought to the inlet, then through an inlet stub to the sample valve and then to the columns. This flow pattern retains the capability for injecting samples by syringe (© the inlet and minimizes the pre-column volume required for valve injection. All inlets have the general design shown schematically Figure 7. ‘The syringe needle enters the column immediately after puncturing the septum. Because in- jection is directly into the column, sample width is ‘minimized. There are no imegular geometries or un- swept areas to cause spreading, The inlets are used for both on-column and flash-vaporization-type injection. For on-column injection, the column is packed close enough to the end so that the syringe needle deposits the sample onto the packing. For flash vaporization, about three inches at the end of the column ace not packed. ‘On-column injection generally is used when the sample is relatively small (usually 1 mg or less) and when some or all of the sample components have a boiling point above column temperature. This is the usual case for samples which boil above about 150°C. In most cases better efficiency will be obtained if the inlet is operated at a relatively high temperature. The AGC temperature system always maintains the inlets at a higher temperature than the columns. Also, the normal temperature differential can be increased by adding additional heat with the INLET AT beater. Flash vaporization is used for larger samples and where the boiling point of the sample is at or near column temperature, In this case, the INLET AT heater may bbe needed to achieve rapid vaporization, particularly for large samples. Septum caps for the inlets are spring-loaded. This as- sures proper pressure on the septa over wide tempera- ture ranges, prolongs septa life and minimizes the troublesome problem of plugging syringe needles. Proper tension on the spring is achieved by making the caps full-tight and then backing off a half to one turn. E, Column Subsystem ‘The importance of columns in gas chromatography ‘cannot be overemphasized, For good results with the thousands of different types of applications for which 1 gas chromatograph may be used, the AGCs aecom- rrmodate columns of different diameters and lengths. ‘Metal columns with an O.D. of Yie inch, Ye inch , %ie inch and “% inch can be used in the AGC by proper choice of standard and accessory inlets. Glass columns equivalent to Yé-inch 0.D. also may be used Dual columns are utilized to increase the capability of the instrument. Each of the ‘Arinch columns may be up to 24 feet in length. Two Yinch columns up to 12 feet cach in length easily fit in the column compart- ment, The type of column in terms of active material (absorption or partition packing) is dictated by the sam- ple to be separated, Diameter also should be considered Section 7: TCD Design and Operation “The low-volume (240 pL) TCD is made from stainless stect for inertness towards sample components and to make it sufficiently rugged for high temperature oper- ation, Aluminum plates are used on the sides to provide high heat conductivity and the mass needed to obtain precise temperature control. Good thermal coupling is made by tightly clamping the machined surfaces of the detector and aluminum plates to each other and then bolting to the aluminum heater plate ‘The standard detector accepts either filaments or ther mistors, Care should be exercised in removing or changing these sensing elements. (See Section 12.) ‘Thermistors are recommended for highest sensitivity below about 70°C and/or for oxidizing or reactive sam- ples. Sensitivity of thermistors is a function of both thermistor current and detector temperature as shown in Figure 8. [A thermistor current of 20 mA, recommended as a fixed setting, is a reasonable compromise for the usual range of detector temperatures. If needed, the sensitiv- ity of the detector can be peaked at any detector tem- perature by adjusting current in increments and inject- ing samples to determine sensitivity at each current setting. For convenience, small sample which elutes from the column quickly is recommended. A 10-wl, air sample usually is a good choice. Filaments are recommended for higher temperature op- tration (greater than 70°C). Filaments also are neces- sary if hydrogen is used as carrier gas. The sensitivity of filaments increases slightly with increasing detector R carefully because, either directly or indirectly, diame- ter determines sainple size and bleed rate (background to flame detector). With the typical packing, sample ‘ize should not be greater than about 1 mg with Yi-inch columns and 6 mg with Minch columns if good effi- ciency is to be maintained, Column diameter also determines the use rate of earrier gas. For best efficiency with packed columns, the av- trage carrier gas velocity should be 7-9 emsee. This translates to a flow rate of 15-20 mL/min for “-inch columns, 50-65 mL/min for Yis-inch columns, and 110-120 mL/min for ‘A-inch columns, SOS ee eee Figure 8 — Sensitivity relative to thermistor bridge cutrent and detector temperature temperature and exponentially with filament current. ‘The AGC does not require that the filament current be read and carefully adjusted. Four discrete settings, rol- lative to each other, are provided to permit selection of fixed sensitivities. Filaments should always be oP crated at the lowest BRIDGE SETTING which gives adequate sensitivity, if oxygen is present in the sample, the BRIDGE SET- TING should be low enough so that an oxygen peak is not more than full scale with an output attenuationof 16. If the oxygen is eluted as part of an air peak, the air peak can be full scale at an output attenuation of 64. The BRIDGE SETTING used with filaments also should be reduced if nitrogen is used as carrier {gas and as the temperature of the detector is increased. Maximum BRIDGE SETTINGS relative to detector temperature and type of carrier gas are summarized in ‘Table No. | Section 8: TCD Electronics Functions ‘The TCD electronic module consists of two power supplies and the bridge circuitry and controls necessary to operate the detector with filaments or theimistors. ‘The + 15-volt power supply is all solid state and utilizes state-of-the-art integrated cireuits which regu- late the full-wave rectified AC input voltage. As an added feature, the regulated + 15V is fed back and used as a reference for the regulator, substantially re- ducing sensitivity 10 line voltage fluctuations. This regulated + 15V supply provides a fixed reference for the current supply and the temperature controller ‘The other power supply provides selectable constant ‘current up to 200 mA and 50 volts to the bridge. This supply utilizes a high-gain differential operational amplifier which compares the voltage selected with the front panel BRIDGE SETTING switch against the voltage gonerated by the current flowing through the detector bridge. Any imbalance creates a differen- tial signal which is amplified and applied as a correction voltage to the series current regulator transistor. Reg ‘lation and stability of tis supply is better than 0.005% of set current Operating the bridge at constant current rather than at constant voltage extends the linear dynamic range to higher sample concentrations. The bridge-power sup- Table No. 1 Bridge Settings Relative to Detector Temperature ‘and Carrier Gas Temp. GAC FHT OTC WIFE He-H recone 3 1 NA 3 eee i ply is adapted to filaments or thermistors with a push- push switch operable from the back of the module, Output Switch A 14-position OUTPUT switch selects the function displayed on the recorder and attenuates the output signal from the detector in binary steps from { to 1024. ‘TEST position provides a shorted input to the recorder so that the recorder can be zeroed properly. The COL position is for measuring column temperature on the recorder (1 mV = 400°C). The INLET position is for measuring inlet temperature on the recorder (1 mV = 400°C). Bridge Setting Switch A six-position BRIDGE SETTING switch helps select filamients or thermistors and selects sensitivity (related to current) for filaments. This switch should be in the OFF position if the instrument is not being used with either thermistors or filaments, Itis in THERMISTORS position when the thermistor sensors are used. With filaments, itis either in 1, 3, 6, or 8, depending on sensit spond to relative sensitivity. Po: eight times the sensitivity of position 1 1BScrewdriver Balance Control The screwdriver BALANCE control is used for ther- mistor operation. It is a continuous control with 15 active tums which change bridge resistance to balance the thermistor detector. Adjustment is relatively coarse and should not be used unless the ZERO control does not have sufficient range to zero detector output. If it is used for initial detector balance, the OUFPUT switch should be at a setting of 128 or above. Serewdriver Current Control ‘The screwdriver CURRENT control is used with the thermistor detector to set thermistor bridge current. It is a continuous control with 15 active tums. When adjusting the bridge current with this control, read the current on the recorder with the BRIDGE SETTING switch at the THERMISTOR, the OUTPUT switch at 1 and the READOUT switch set to CURRENT (1 mV = 50 mA), (NOTE: When making this adjustment, always place the BRIDGE SETTING switch to OFF before turning the READOUT switch 0 or from CUR- RENT. This prevents putting excessive current on the ‘thermistors.) Readout Switch A three-position READOUT switch permits selection of the correct polarity for the column being used. When in the CURRENT position, it permits the thermistor current to be measured on the recorder. Fine Zero Control ‘The continuous FINE ZERO control (10 active turns) is used to zero the output to the recorder. It is used in combination with the COARSE ZERO control. FINE ‘ZERO has a restricted range and usually is used at an OUTPUT switch position of 16 or less Coarse Zero Control The continuous COARSE ZERO control (10 active turns) is the wide range zero control. It is used at the higher OUTPUT switch positions Computer Output A three-position computer output barrier strip at the ‘back of the electronic module allows connection of a ‘computer interface or integrator to an unattenuated out~ put signal. This 0 to L volt signal is equivalent to the XI position of the OUTPUT attenuator. Push-Push Filament-Thermistor Switch ‘The push-push filament-thermistor switch at the back of the electronic module adapts the power supply and bridge for filaments or thermistors. It should always be in correct position for the sensors used. Require ‘ments for filaments and thermistors are quite different, In order to operate both correctly, the push-push switch ust be used to change the current and bridge config uration as shown schematically in Figure 10, — ee 2003 200s THERMISTOR FILAMENT (BALANCE RECCRDER ‘OUTPUT FiLaweNt FILAMENT Figure 10 — TCD bridge configuration with thermistor sensing elements (left) and filament sensing elements Gight). 4Section 9: FID Design and Operation ‘A dual-feed, single-burner flame ionization detector is used in the AGC-211 and 311, Sample is directed to the burner from one column. The other column pro- vides additional carrier gas giving improved sensitivity because of a more optimized flame. In addition, it permits the flame to be fed with an increased hydrogen flow and this extends the linear dynamic range. The burner is shown in Figure 11 Parallel, large arca plates make up the collector and polarizing electrodes. The polarizing plate also carries the igniter. Mounting the igniter on the plate gives several advantages. It places the igniter in a protected area so the risk of damage is minimal. The igniter is not a competitive collector because it is part of the polarizing electrode (j.e., at the same voltage as the polarizing electrode except when igniter button is de- pressed). Additionally, the igniter wire is out of the flame and, therefore, there isno thermionic emission. Insulators are placed outside the burner and there are no high impedance feedthroughs with the open slot design. This greatly minimizes electrical leakage which ‘may be caused by acid gases and carbon (soot) condens- ing on insulators or feedthroughs. ‘The quartz jet is a polarized insulator. However, con- tact is provided (o the polarizing plate, ensuring that the jet does not become a competitive collector from contamination or high temperature. Handle the jet care~ fully so that it does not become conductive. Always used cotton gloves or plastic tweezers (Teflon if the jet is hot). CAUTION: Because of heat and danger- ‘ous voltage, use only thespecial Carle® Teflon probe provided to measure flow through the jet. To prevent damage to the polarizing tab, the probe should be low- ‘ered carefully until just touching the jet and then gently pushed no more than Y% inch to seal on the jet. The probe is of sufficient length to allow measuring flows with the instrument closed. Dust and impurities in the burner will cause noise spikes if the burner has been opened or has not been used for a period of time. Removal of dust can be accelerated by using a higher-than-normal airflow. To help prevent dust from getting info the burner, always operate the bumer with the dust eap in place. Proper \stment of the gas flows for the FID is described in Section 6A. Figure 11 — The FID bumer has a single quart jet with parallel plates surrounded by a cylindrical enclosure to provide an insulating air gap between plates and high impedance connections. 15Section 10: FID Electrometer Functions ‘The electrometer module consists of a dual + and ~15 volt power supply, a solid-state 300V supply, a varac- tor bridge amplifier and front panel controls for attent- ation, background suppression (burner zero) and amplifier (electrometer zero). ‘The +15 volt power supply is all solid state and utilizes state-of-the-art integrated circuits which regulate the full-wave rectified AC input voltage. As an added fea- ture, the regulated +15 volt power is fed back and used as a reference for the regulator, substantially re- ducing sensitivity 0 line voltage fluctuations. The +15 volt power supply is a reference for the temperature controller and the clectrometer amplifier. The ~15 volt power supply is a reference for the electrometer amplifier and tracks the +15 volt power supply 10 significantly improve common and normal mode noise rejection. Polarizing voltage to the burner is supplied from a closely regulated 300-volt power supply made insensi- tive (0 line voltage fluctuation with an RC network, ‘This system gives all the capabilities of a battery with- out any replacement requirements. The signal-measuring part of the electrometer ul fa state-of-the-art varactor bridge axnplifier which bas extremely high input resistance (Jow input current) and very low noise. It converts the low current at is input {produced by generation of ions in the flame and the polarizing voltage) to a voltage which is applied to the OUTPUT attenator. The electrometer produces a full scale signal (1 mV) with a current of 1 107"? am- peres. The noise level under proper conditions is only 1x 10-4 amperes. j NOTE: Pin 4 of the barrier strip on the tear of the module carries an output for connection of a computer interface or integrator. This 0 to | volt output signal is not affected by the OUTPUT attenuator butis sealed by the RANGE switch ((.c., equivalent to 1 X 1, 10 x 1, 10? X 1, ete). Output Switch ‘The 14-position OUTPUT switch selects the function displayed on the recorder and attenuates the output from the flame detector in binary steps from 1 to 1024 ‘The TEST position shorts the recorder so that the re- corder can be properly zetoed. COL, position is for ‘measuring column temperature on the recorder (1 mV = 400°C). INLET position is for measuring inlet tem perature on the recorder (1 mV = 400°C). Range Switch ‘The six-position RANGE switch changes input to the electrometer in steps of 10 and in BAL position permits yeroing the electrometer. The RANGE attenuation positions of 1 to 10* are true attenuations and may be tised in combination with the OUTPUT attenuator for an attenuation range of 1.024 x 10". However, when possible, itis always preferable to set RANGE at a Single position and use the OUTPUT switch as the aitenuator, This is not always possible, with a sample where trace components and major components must both be measured. Using the RANGE switch at the highest range possible is recommended to minimize noise. Figure 12 — FID electrometer control panel 16Amplifier Balance Control A continuous contro (10 active turns), the AMPLI- FIER BALANCE control is used to balance o zero the amplifier. ‘This adjustment should be made after the electrometer has warmed up for a few minutes and before the flame is lit. The RANGE switch must be at BAL, the OUTPUT switch should be at 1, and the ZERO SUPPRESSION toggle switch should be off. ‘Then turn the amplifier BALANCE control to place the recorder at zero. It should not be necessary to repeat this adjustment unless the electrometer is turned off. Igniter Button ‘The IGNITER BUTTON switch energizes the igniter and lights the flame when sufficient hydrogen is present to support a flame. It should not be necessary to hold the button down more than two to three seconds to light the flame ‘Zero Suppression Toggle Switch ‘The ZERO SUPPRESSION toggle switch actuates the COARSE and FINE ZERO SUPPRESSION con- trols, making it possible to suppress or zero the back- ground signal from the lane detector when the fame is on, A suppression of slightly more than 10° peres can be applied. Fine Zero Suppression Control A continuous control (10 active tums), the FINE ‘ZERO SUPPRESSION contro! is used in combination with the COARSE ZERO SUPPRESSION control to zero out the background signal from the flame and place the recorder at zero. It has the sensitivity of control needed at a RANGE attenuation of 10 or less and an OUTPUT attenuation of 8 or less. Coarse Zero Suppression Control ‘The COARSE ZERO SUPPRESSION control (10 active tums) provides the range needed to zero the coutput (background) of the flame dotector at higher RANGE and OUTPUT attenuations. wSection 11: Using The AGC With Valves Valving is a necessity for many applications in a gas chromatograph. In other situations, valving is a con- venience or a way to increase versatility and perform- ance of the instrument. A valve is required for repeat- able injection of gas samples. Valves also must be used when it is necessary to backflush part of the sample to vent or through the detector. Valves used in the Series/Bypass configuration make it possible to achieve separations with two columns which cannot be made with either column alone or in fixed series operation. This particular technique saves time in ap- plications typically requiring a long column and a long, separation time between eatly-cluting and later-eluting ‘components. Other important applications in gas chromatography include switehing detectors and cutting out unwanted components so they do not reach the detector, In all these applications, an important advantage of valving js that the instrument is always operated in an equili- brated condition. Valving is a preplanned feature of the AGC. As shown in Figure 13, it has space allocated and mounting holes pre-drilled for up to three Carle valves. Any of the Carle 2000 (Micro Volume), 5600 (Mini, Volume) or 2900 (Hastelloy C) Series Valves fit into the mounting areas provided. With the mounting provided, two valves are temperalure-controlled and one is held at ambient temperature. The valves may be actuated man- ually or automatically with actuators. With the ac- tuators, an accessory base providing mounting and ac- cess is available. ‘The temperature-controlled valves are mounted in the same temperature area and in close proximity to the columns, inlets and detectors. This ensures keeping ‘connecting lines short and hot enough to prevent con- densation. Mounting for two restrictor valves also is provided in the temperature-controlled area. These are tused primarily to control the bypass column pressure drop in a Series/Bypass configuration Figure 13 —‘The photo at lefl shows the instrument with no valves installed; a right the instrument has three rmanvally acwated valves, series/bypass restrictors and all necessary plumbing, No separately heated ines are necessary; all mounting holes are provided. 18Section 12: Owner Service Every effort has been made in design and check-out procedures for the AGC to minimize the need for serv- ice. However, there will be infrequent occasions when the instrument requires service. Minor service can be performed more expeditiously and economically by the user than by servicemen or factory personnel, In most cases the source and then the cure for a mal- function can be ascertained by referring to the follow- ing table on symptoms, causes and corrections and to the appropriate wiring schematic and description sec- tion in this manual Interchanging TCD Sensors To remove and change sensors, first turn the instrument power off. Liftoff the top of the insulated box around Figure 14 — Care must be exercised when removing and inserting thermistor and filament sensing clements. ‘Always replace the gasket. the TCD, Remove sensor feads at the barrier strip. Straighten lead wires for about one inch directly above header nuts, Now, unscrew the header nuts (coun- terclockwise). When heater nuts are free of threads, remove the sensor by carefully fing straight up, hold- ing the lead wire at the top of the header mut. (See Figure 14.) Be careful not to damage the filament or thermistor. Remove the aluminum gasket from the de~ tector chamber. (NOTE: Do not permit insulation to fall down into the detector and always use a new gasket when installing sensors.) ‘To install replacement sensors, reverse the above pro- cedure. Make sure leads are connected to the barrier strip properly, Right filament leads go to terminals 4 and 5. Left filament leads go to terminals I and 2 Right thermistor leads go to terminals 6 and 7. Left thermistor leads go to terminals 1 and 3. Removing Inlets ‘To remove inlets, first turn off instrument power and cartier gas flow. Remove the spring-loaded septum caps. Then remove the spacer nuts which clamp the inlets to the inlotivalve plate with a Y%-inch socket wrench. Remove the inlet feed lines from the tee or accessory needie valves. Inlet(s) ate now free and are removed by pushing or pulling toward the back of the instrument. To install inlets, reverse the above proce- dure, making sure the spacer nuts are reasonably tight. Installing New FID Jet ‘To install a new jet (Cat. No. 72090-29), first remove the burner assembly by taking out the two base screws Cables are freed by removing the two screws (top front of the instrument) which keep the cables in their ehan- nel. Both the electrometer cable and the polatizi cable disconnect inside the AGC. CAUTION: Always turn off the instrument power or disconnect the polarizing cable before opening or removing the burner. With the instrument on and the polarizing cable connected, 300V are present at the polarizing, electrode and at insulator connections outside the burner.) When installing a new jet, be careful in tightening the jet nut, The sealing system uses a Swagelok mut, @ compression ferrule and an aluminum sleeve to provide sealing without breaking the jet. The nut should be ‘made just tight enoiigh so that the jet will not pull out “of the sleeve when gently tugging with plastic tweezers, 19Heater Replacement ‘The inlet heater is accessible from the base of the AGC. Refor to Figure 15. To remove the inlet heater, tum the power off and unplug the power cord. Remove leads atthe barrier strip (terminals 13, 14, 16). Remove the wiring cover from the AGC base ‘Tam off carrier gas flow and remove inlet septum caps. Then loosen inlet spacer nuts with a Y%-inch socket wrench. Loosen four base screws holding the inlevvalve plate. Push the inlev/valve plate toward the of the instrument. Then the inlet heater can be pushed out with a screwdriver, To install an inlet heat- cr, reverse the above procedure. (NOTE: If glass col- tumns are installed in the AGC, they should be removed before replacing an inlet heater.) ‘The column heater is mounted under the detector plate column box. To remove or replace this heater, first remove the detector plate/column box Figure 15 — The inlet heater is removed easily after the inlet/valve plate has been loosened and slid toward the rear of the instrument. 20o ‘Table 2: Trouble-shooting Guide for AGC Wiring ‘Symptom Cause Correction Zero offset with attenuator and ‘With TCD and FID: electrical Place OUTPUT switch in TEST {allure to attenuate property zeroofrecordet notat chartze10 position andmake recorder electrical oro agree with chart zero according to recorderinstructions. Eitherorboth AGC andiecorder Ground AGC and recorderto same not adequately grounded (also ground may have noise) With FID: amplifier balance Adjust notagjusted properly Output noise (TCD) With flamonts: BRIDGE Reduce SETTING toohigh AGC andiorrecorder not Ground AGC and recorder to same ‘adequately grounded round. Filaments badly oxidized Inspectand replace if necessary. Output noise (FID) Excessive column biewd Reduce temporature or wait for (eackgroundiis high) equilibration System notcloanodup ‘Waitor clean-up (may accelerate (backgrounds high) by raising temperature). HyiHe ratlotoo rich ‘Adjust ows. Airflow too ow orhigh Adjust. Dustin burner (usually spikes) Clean outby raising airflow forabout onehalfhour. Leakyjet Tighten. Contaminated jet Replace. Contaminated insulators loan with pure ethanot. Output rit Temperaturenot equilibrated Monitor temperature and waitfor (TCD and FD) equilibration. Excessive column bleed Leaks Impure gases Gas flow variations Waitor reduce temperature (may raise temperature to accelerate clean-up). Check fittings and valves. Replace septa. Use adequate quality gases for sensitivity required. May need bottercylinderregulator a‘Trouble-shooting Guide for AGC Wiring (continued) ‘Symptom Cause Correction Output “Thermistors may be drifting. ‘Workat higher output attenuation {thermistors) cor wait or ditto diminish. When thermistors have not been used for ‘sometime they may drit. Drift may be corrected faster by heating detectorto 135°C and running at 20mAcurrent. Lossofsensitivity Leaks atiniets Tighten inlet fitings. Replace septa. (FIDand TCD) (FID) ‘Too lowortoo high HalHe ratio Adjustflows. Retention time change “Temperature change Check column temperature. Significant change indicates problems with heaters or PRT. ‘Substantialieak Cheok tings andleaktestit {flowrate change) necessary. ‘Temperature willnotrise (Open PRT. Replace, ‘Thermal fuse out Replace, ‘Column orinlet heater out Replace. ‘Temperature keeps rising PRT shorted Replace. utputwillnotzer0 (TOD) ‘Thermistors notbalanced Use balance control, Try higher ‘current. Replace thermistors. Filaments damaged Replace filaments. (FID) ‘Backgroundtohigh Reduce column temperature or walt forciean-up. No power Blownfuse Replace with 10 amp fuse. (Cat. No.72090-13) 2ry Section 13: Factory Service Major service is done at the factory where complete check-out equipment, fully trained service personnel and a stock of spare parts are maintained, If the need for major service does occur, itis likely that it will be one of the electronic modules. These modules are made to be removable as individual units to make return for factory service convenient. If an electronic module is returned for service, it should be packed carefully to prevent damage in shipment, NOTE: When packing, ddo not place styrofoam in direct contact with the mod- ules. Static electricity could cause damage to electronic components Electrometer Module 1. Turn instrument power off. 2. Disconnect polarizing and electrometer input ea- bles at connections inside AGC. 3. Remove barrier strip cover at back of electrometer. 4. Disconnect harness at barrier strip on back of elec~ trometer, Retighten barrier strip screws. Remove two screws at each end of back panel of the electrometer. 6. Pull electrometer straight back to remove from outer housing, 7, Fold polarizing and electrometer input cables into ‘electrometer and tape down 8. Place electrometer in a plastic bag. Then place in center of an oversized carton, putting adequate packing insulation completely around the elec- trometer. If possible, use the box-in-a-box packing technique. ‘TCD Module 1, Tum instrument power off. 2. Remove barrier strip cover at back of TCD module, 3. Disconnect harness at batrier strip on back of TCD module. Retighten barrier strip screws 4, Remove two serews at each end of back panel of the TCD module 5. Pull TCD module straight back to remove from outer housing. Place TCD module in a plastic bag. Then place in center of an oversized carton, putting adequate packing insulation completely around the module. If possible, use box-in-a*box packing technique. ‘Temperature Controller Module 1. Unplug AGC power cord. 2. Disconnect leads from Temperature Controller to PRT at positions 8 and 9 on barrier strip (located beside oven). 3. Remove the four TC Module mounting screws: one at base back, two at base front and one near the top. 4, After noting how the PRT wires are routed, remove the TC module by lifting it up and rocking front-to- back to unplug it from the edge connector. Be ‘careful not to damage the two PRT wires. 5. For shipment, place TC modale in plastic bag and put in oversized cardboard carton, Surround with. ample packing insulation. If possible use the box- in-a-box packing technique. 23Section 14: Replacements, Diagrams Replacement Parts 24 Cat. No. 7100-12 72090-05 72090-06 72090-07 72990-08 72090-11 72090-13 7290-14 72090-15 72090-16 7290-18 72090-23 72090-24 7290-25 72090-26 7290-27 72090-28 72090-29 72090-30 72090-31 72090-32, 72090-33 72090-34 72090-35 7250-01 7250-09 Deseription ‘Thermostat Assembly ‘Thermistors, 8-10K Filaments, matched Header Sealing Gaskets, Header Nuts Platinum Resistance Thermometer (PRT) Fase, 3AB, 10A, 250V ‘Thermistors, 1.2K, matched AGC Inlet Heater AGC Column Heater AGC Power Transformer ‘AGC Column Oven Temperature Controller AGC Detector Bridge Power Supply AGCFID Electrometer Septum Caps, spring-loaded Inlet Assembly Kit, Ye-inch Inlet Assembly Kit, Y-inch, Quartz Jet Assembly Probe, flow measuring ‘AGC PID Dust Cap Polarizing Plate with Ignitor for AGC Collector Plate for AGC AGC FID Bummer Assembly AGCFID Chimney Silicone Septa Electrical Fuse, L.Samp Unit pair pair box/10 pair box/S pair each each each each, each, each, pair each pair each, each each each, each each box/50 box/Sfra 3 TD Ra as a “sojsuoyosoqui ujexe senyea eoueonpul lye “eparnjoroqus ulase senjensounijoedeo IY "Z “eunjo Ul o1e SOnveA @DUEts}s0 MY “L poyoeds asymuouno ssojun :s10N \ Figure 16 — Temperature Controller SchematicBridge Power Supply Schematic 17—TCD FigureFigure 18 — FID Blectrometer SchematicBRIDGE POWER SUPPLY Figure 19 — AGC-111 Wiring Diagram 28TEMPERATURE CONTROLLER Figure 20 — AGC-211 Wiring Diggram 29VBR BRN 2 ra | & ie ouo> aa : ange 20% aatt| at Srey coal als rae 99 M3 tll] § aot ca 9 98 sa) aie eovewssnases oo owe (23 Sano (2s BSTIOWINGD SHALVUSSMSL pan TSaS BSNS si soaua cxousnoe | 31 Fo Figure 21 — AGC-311 Wiring Diagram 30TEMPERATURE CONTROLLER BRIDGE POWER SUPPLY au | 2 13h] rca ino | & 5 ELECTROMETER : i i af ad Figure 21 — AGC-311 Wiring Diagram 30