TRAINING MANUAL CHROMATOGRAPH MAINTENANCE SCHOOL FOR LABORATORY AND PROCESS SYSTEMSTABLE OF CONTENTS SECTION I PRINCIPLES OF GAS CHROMATOGRAPHY Li 1.1 GAS CHROMATOGRAPHY Ll 1.2 TERMINOLOGY EI 1.2.1 TECHNIQUES El 1.2.2 APPARATUS 13 1.2.3 REAGENTS 13 1.2.4 OPERATING VARIABLES 4 1.2.5 DATA PRESENTATION 14 1.3 INSTRUMENT COMPONENTS 1s 1.3.1 CARRIER GAS 17 13.2 DETECTOR 17 13.3 VALVES 19 1.3.4 TEMPERATURE CONTROL 19 1.3.5 THE CHROMATOGRAPH COLUMN Eu 1.4 GENERAL COLUMN INFORMATION El 1.4.1 COLUMN PACKING 112 1.4.2 MULTIPLE COLUMNS AND VALVE CONFIGURATIONS 13 1.5 PERFORMANCE FACTORS 113 1.5.1 RESOLUTION 4 1.5.2 ANALYSIS TIME kis 1.6 APPLICATION ENGINEERING Lis 1.7 THE PROCESS CHROMATOGRAPH E16 1.7.1 THE ANALYZER 116 1.7.2 THE CONTROL UNIT Ly 1.7.3 OUTPUTS 17 1.7.4 SAMPLE SYSTEMS 17 1.8 PROBLEMS IN CHROMATOGRAPHY 19SECTION I SAMPLE SYSTEM 2.1 INTRODUCTION 2.2 LOCATION AND MOUNTING 2.3 STREAM CONNECTIONS 2.4 COMPONENTS 2.4.1 FILTERS 2.4.2 OIL SEPARATORS 2.4.3 PRESSURE REGULATOR 2.4.4 VAPORIZER REGULATOR 2.4.5 LIQUID VALVE 2.4.6 STEAM TRACING 2.4.7 SCRUBBER 2.4.8 WATER COALESCER 2.4.9 CYCLONE SEPARATOR, 2.4.10 SAMPLE COOLER, 2.5 BYPASS FLOW 2.6 MULTIPLE STREAM SYSTEMS SECTION Il PROCESS ANALYZER 3.1 INTRODUCTION 3.1.1 CARRIER GAS FLOW 3.1.2 INSTRUMENT AIR FLOW 3.1.3 SAMPLE GAS FLOW AND BLOCKING VALVE. 3.2 HEATING SYSTEM 3.3 THE DETECTOR 3.4 INDICATING THERMOMETER 35 AL ES AND CONFIGURATIONS 3.5.1 SAMPLE VALVES 3.5.2 VALVE ACTUATION Il TH m2 m2 2 m4 1-4 14 19 19 1-10 1-10 1-10 1-10 Tu Tell m1 M1 m1 4 ms 16 m6 m7 m7 m7 TL83.6 FLOW RATE ADJUSTMENTS 3.6.1 CARRIER FLOW 3.6.2 REFERENCE CARRIER 3.6.3 PRECUT CARRIER FLOW 3.7 ROUTINE MAINTENANCE 3.7.1 VALVE MAINTENANCE - 10-PORT 3.7.2 REPLACING DETECTOR FILAMENTS 3.7.3 COLUMN MAINTENANCE, 3.8 RECOMMENDED SPARE PARTS. SECTION IV LABORATORY ANALYZER 4.1 INTRODUCTION 4.2 THE INTEGRATOR 4.3 OPERATION 4.3.1 DESCRIPTION OF CONTROLS AND INDICATORS 4.3.2 PRINTED CIRCUIT BOARD PC-1 4.4 START-UP PROCEDURE, 4.5 VALVE MAINTENANCE - LIQUID 4.6 REPLACING HEATER 4.7 REPLACING BLOWER MOTOR SECTION V MC-503 CONTROL UNIT 5.1 INTRODUCTION 5.1.1 THE MC-503 HARDWARE 5.1.2 MC-503 SOFTWARE. 5.2 CONNECTING THE MC-503 ACM(s) TO PC 5.3 SOFTWARE INSTALLATION 5.3.1 EXECUTING THE MENU 5.3.2 A SAMPLE RUN WITH THE DEFAULT PARAMETERS 0-10 1-10 W-11 mil W-11 m-12 1-16 17 1-18 IV-1 IV-10 IV-llSECTION VI MC-503 SOFTWARE VEL 6.1 [A]: ANALYZER DEFINITION VI-2 62 [B]|: STREAM DEFINITION VI-2 6.3 [C]: COMPONENT DEFINITION Vi4 6.4 [D]: NAME VALVE DRIVERS VI-6 6.5 [E]: VALVE TIMES VI-6 6.6 [F]: ASSIGN SOLENOID DRIVERS V6 6.7 [G]: SET STREAM SEQUENCE VL7 6.8 [H]: SET LATCH BOARD MODULE, VET 6.8.1 RELAY/ALARM PARAMETERS Vi7 6.8.2 ANALOG OUTPUT PARAMETERS VES 6.9 [I]: RUN/STOP ANALYZER V8 6.10 (JJ: ENABLE/DISABLE STREAMS VEO 6.11 [K]: SET/CALIBRATE TEMPERATURE CONTROLLER VES 6.12 [L]: DISPLAY CURRENT ANALYSIS ‘I-10 6.13 [M): REPORT ALARM STATUS VEIL 6.14 [N]: DETAILED ANALYZER STATUS Vi 6.15 [O}: ACTIVATE DETECTOR PLOT Vi-12 6.16 [P]: PRINT DETECTOR PLOT FROM RECORDING Vi-13 6.17 (Q|: DISPLAY TREND VI-IS 6.18 IR]: DISPLAY STREAM HISTORY VL-16 6.19 [S]: STREAM ANALYSIS TREND VEIT 6.20 [T]: VIEW MODBUS REGISTERS VI-I7 SECTION VIL THE ANALYZER CONTROL MODULE Va-1 7.1.1 YO DEVICES Vo-1 7.1.2 OPERATION OF INDIVIDUAL I/O DEVICES VI-3 7.2 CONSOLE-TO-ACM COMMANDS vu-4 7.2.1 ACM COMMANDS Vo-S7.2.2 DETAILED COMMAND DESCRIPTIONS Vo-6 7.3 SWITCH SETTINGS AND STATUS LEDs VO-1i SECTION VII TROUBLESHOOTING V1 8.1 MC-503 HARDWARE PROBLEMS VI-1 8.2 MC-503 SOFTWARE PROBLEMS Vm-2 8.3 MC-502 PROBLEMS ‘VI-3 8.4 PROCEDURE TO ZERO THE CHROMATOGRAPH BRIDGE vul4 8.5 RECENT UPDATES TO MC-503 SYSTEM. VuIL-S 85.1 INSTRUCTIONS TO USE NEW PASSWORD SYSTEM ‘VII-6 8.5.2 PULSED RELAY OUTPUTS VuL-7 8.5.3 AIC UTILITIES INFORMATION ‘VII-8 8.5.4 BACKING-UP THE MC-503 DATA ‘VI-10 8.5.5 INSTRUCTIONS TO COPY ALL ANALYZER SETTINGS VO-11v n 12 13 14 15 16 7 18 19 20 MC-503D INTRODUCTION THEORY/ PHILOSOPHY CALIBRATION CALCULATIONS GENERAL EDITING [A]: ANALYZER DEFINITION [B]: COMPONENT LIBRARY (Cl: METHOD PARAMETERS [DI-METHOD COMPONENTS [E]-METHOD EVENTS [F|‘STREAM DEFINITION [G]:STREAM SEQUENCE [H]-ALARM REGISTERS (U;UTILITIES [1]: RUN/STOP ANALYZER [J]: STREAM ON/OFF METHOD IK]: ANALOG OUTPUTS [LI: CURRENT REPORTS [M]: ANALYZER ALARMS [IN]: ANALYZER STATUS [0]: DETECTOR GRAPH Ix-1 Xl IX-1 IX5 X-8 1X10 TX-11 IX-13 IX-15 IX17 1X18 1X21 1-22 1X-24 1X25 1X27 1X28 1X30 1X32 1X-339.22 9.23 9.24 9.25 9.26 9.27 9.28 929 9.30 9.30.1 9.30.2: 9.30.3: 9.21.1 SCALES IP}: PLOT [Q]: GRAPHIC TEND 9.23.1 GRAPHIC TREND VIEW DIFINATION (SETUP) [R]: HISTORY [S]: LAST FIVE ANALYSIS [7]: SERIAL DATA REGISTER ANALYZER ALARM STATUS ENVIRONMENT VARIABLE, COMMUNICATIONS APPENDIX EXAMPLE: RATIO EXAMPLE: SUMMATION EXAMPLE: MODBUS, GLOSSARY/ DEFINITION O F TERMS 1X40 1X33 1X35 1X36 1X37 1X39 IX-41 1X43 1X44 X45 1X47 X48, X49 1X50 1X51SECTION I PRINCIPLES OF GAS CHROMATOGRAPHY 11 GAS CHROMATOGRAPHY Chromatography is a technique for separating the components in a mixture. This separation is performed by distributing the components between two phases. One of these phases, called the stationary or fixed phase, consists either of a solid adsorbent material (adsorption chromatography) or of a film of liquid on an inert support (partition or absorption chromatography). Whichever is used, it is packed into a tube of small diameter resulting in a column. The mobile phase (carrier) consists of a gas which carries the gaseous sample through the column. This carrier gas flows contimnously through the column at a constant rate. At a predetermined time, a valve will introduce a fixed amount of sample into the carrier gas stream. The cartier gas will push the sample through the column, where separation of components results from the difference in the affinity between column material and each of the sample components. Whether the nature of this affinity is adsorption, solubility, chemical bonding, polarity, or molecular filtration, column material detains some components longer than others. Consequently, all components flow through the column at different rates and emerge in the inverse order of their affinity for the column material. At the end of the column, a detector measures the amount of each component. Since each component progresses through the column at a predictable rate, the elution time identifies each component qualitatively. This process is demonstrated in Figure I-1. 12 TERMINOLOGY Following are definitions of the terms frequently used in this manual: 12.1 TECHNIQUES Gas-Liquid Chromatography - A description for all chromatographic methods where the mobile phase is gas and the stationary phase is a liquid distributed on a solid support.Figure J-1 Components separation in a column. RECORDER outputGas-Solid Chromatography - All chromatographic methods where the mobile phase is a gas and the stationary phase is an active solid such as alumina, activated carbon, silica gel, or molecular sieves. Gas Chromatography - All chromatographic methods where the mobile phase is gas. It is the collective name for gas-liquid and gas-solid chromatography. 122 APPARATUS Sample Valve - Device for introducing a fixed volume of liquid or gaseous sample into the column. Switch Valve - A valve which routes the gases in the chromatograph through alternate channels according to the needs of the analysis. ‘The sample valve often performs this function. Column - A tube packed with stationary phase which separates components of a sample. Detector - A part of the analyzer which detects the separated components. The detector continuously measures the change in composition of the carrier gas as it emerges from the column. A change in composition is indicative of the amount of sample component mixed with the carrier gas. 123 REAGENTS Carrier Gas - The mobile phase of a chromatograph system. It is a gas that is used to move the sample through the column. Liquid Phase - A non-volatile liquid coated on a solid support which constitutes the packing for a gas-liquid (absorption) column. The sample components are dissolved in this liquid phase as the sample moves through the columm and the separation of the components depends I-3on their vapor pressure (volatility) in liquid phase. Solid Support - An inert porous solid such as diatomaceous earth. The column efficiency is influenced by particle size and surface area of the solid support. Active solids may be modified to serve as solid support. It is also possible to use the inner wall of a capillary tube for the same purpose. ‘Active Solid - A porous solid which is capable of separating sample components without any liquid coating. In this case, the separation mechanism is adsorption rather than absorption. 1.2.4 OPERATING VARIABLES Column Pressure - Column pressure affects the carrier and sample gas flow rates. It depends upon the column selected and the carrier gas pressure. Column pressure is controlled by the Carrier Gas Pressure Regulator and indicated by a pressure gauge mounted on the regulator. Carrier Gas Flow Rate - The volume flow rate of cartier gas at column outlet measured at ambient temperature. It is controlled by the metering valves mounted on the carrier regulator. Column Temperature - Column temperature is of prime importance to the sample analysis and depends on the oven temperature. 125 DATA PRESENTATION Chromatogram - A time plot of the detector response to sample components as they elute from the column. This plot can be obtained from @ computer. Printer - It provides the print-out of normalized and non-normalized analysis, and chromatogram of a sample. Component Peak - A response from the detector at the time of elution of the component I-4from the column, Peak Height - The distance between the baseline and the top of a peak. The peak height commonly used as a quantitative measure of the component concentration. Resolution - The degree of separation between two adjacent peaks. Elution Time - Elapsed time between the injection of a sample and the detection of the maximum peak height for each sample component by the detector. Since, for a given column, every component has a characteristic elution time, it is used as a means of component identification. Baseline - The portion of a chromatogram between two peaks when no sample component is being eluted. The detector output is normally adjusted to make the baseline coincide with the electrical zero of the recording/printer unit. Integrated Area - The area under a peak. This area is proportional to the quantity of the ‘component and is usually measured with an integrating device. 13 INSTRUMENT COMPONENTS ‘The industrial applications of the principles discussed in this section are the foundation of the Process gas chromatograph. Basically, a process chromatograph needs a sample inject valve to repeatedly inject fixed quantities of sample into the system, a regulated supply of carrier gas to move the sample, a column to separate the sample into its individual components, a detector to detect the components, temperature control to regulate the heater, and air for the heater and valves actuation. The AIC Process Chromatograph incorporates these requirements and is designed to provide automatic and continuous monitoring of process streams. Its design incorporates the use of three modules: an analyzer, the MC-503 ACM, and 2 IBM compatible PC. The essential elements of an AIC instrument are shown schematically in Figure 1.2.“squouungsuy OY J0y WUT UWLOISKS om, Z-] ANB L = {| | $0 (ATER) | fainanon NOW! IG Fn | sap9 ens oqo roe A, “| doo =f in sing yu py —L_ [a | wean) oe a I} , (i ni] ny i (myes suas exdwog : | 01 OL al tL _ 1 INA va Seve | has —P-— | Laas — oar <4 Sa 1 way + at mu oa] au a oy a of I-613.1 CARRIER GAS Since the carrier gas is the mobile phase, its selection is very important to achieve optimum results from Gas Chromatograph. The carrier gas must be inert. It should not react with column materials or the components. Since most systems utilize a thermal conductivity detector, the carrier gas should have thermal conductivity properties different from those of the gases to be analyzed. The majority of organic compounds have a thermal conductivity of 3 to 7 thus hydrogen or helium with thermal conductivity of 50 and 40 respectively, should give the best results. However, because of safety factors, helium is generally preferred. It is a colorless, inert gas, and will not bum. Nitrogen, argon, and carbon dioxide are less frequently used as carrier gas because they decrease the sensitivity of the thermal conductivity detector. For hydrogen flame ionization detector, any gas is acceptable as a carrier gas. 132 DETECTOR Two types of detectors are normally used in process work: a thermal conductivity detector and a hydrogen flame ionization detector. The thermal conductivity detector may use either themnistors or hot wire filaments as the sensing element. Detectors with the hot wire filament are arranged in a wheatstone bridge configuration with each of the four filaments located in separate chambers within a metal block. Two of the detectors are continuously exposed to the carrier gas only (reference side), while the other pair (active) are exposed to column effluent comprised of carrier gas plus separated components (Figure F-3). A highly regulated voltage, supplied by the detector power supply, is placed across the bridge which causes a current to flow through the filaments. The heat produced by this current is carried away by the cartier gas flowing across the filaments. As long as the detectors detect carrier gas only, the bridge is balanced and no electrical output is produced. The light gases, such 2s helium, Temove heat more efficiently than heavy gases. When sample mixed with cartier gas elutes from the column and passes across the active detectors, the temperature of the filaments increases. Since he Slaments have « positive temperature coefficient of resistence (hei resistance increases with increasing temperature) and the voltage across the bridge is constant, the current through the filaments should change, which causes an unbalanced bridge.-[ Power’ SUPPLY RECORDER [ OF FILAMENTS NATCHED SET REFERENCE ER WwW caRRi couse: eFriuent 7 REFERENCE CARRIER OUT Figure J-3 The thermal conductivity detectors with hot wire filaments.The unbalanced bridge produces a signal which is proportional to the amount of sample moving across the detector. Sensitivity of the detector can be varied by changing the voltage impressed across the bridge. Generally thermal conductivity detector is used for high parts- per-million (ppm) concentration range. The second detector is hydrogen flame ionization type, in which the sample components are ionized by combustion which produces a current. Column effluent is mixed with hydrogen and bumed in a Teflon chamber. Combustible materials containing carbon atoms produce ions which are collected by impressing a voltage between the bumer tip and the collector (Figure I-4). The small current set up by flow of ions is measured by an electrometer amplifier and sent to the ACM. The flame ionization detector is sensitive to the parts per billion (ppb) concentration range of sample. Since this detector measures ion current, it is only sensitive to components which produce ions on combustion. This selectivity sometimes can be used to advantage such as in the measurement of acetylene in oxygen or air with a full scale of only 10 ppm acetylene and with almost complete insensitivity to the oxygen or air. 13.3 VALVES ‘The sample valves used in AIC instruments are multi-port rotary type operated by a pneumatic air cylinder. The valve parts which are wet with sample are constructed of 400 series stainless steel and glass filled Teflon, making them resistant to corrosive materials present in the sample. The multi-port configuration of the valve serves the dual function of sample introduction and column switching. Only complex applications will require a second valve. 13.4 TEMPERATURE CONTROL A column is the heart of a chromatograph’s ability to do the job for which it is designed. ‘Consequently, factors which affect the functioning of a column are of primary interest. One such factor is temperature. Resolution, sensitivity, and elution time are functions associated with column which are affected by temperature. For example, if the column temperature is too low, the sample will move through the column slowly resulting in a prolonged analysis 1-9Stack Collector Cathode anc Ignitor tector Air In Figure 1-4 Flame ionization detectortime and very low sensitivity since the recorded peaks will spread out in width. If the column temperature is too high, the components will elute quickly and the recorded peaks will crowd together, making resolution difficult. It is also essential that the column temperature be such that the components of the sample remain in the vapor state when passing through the column. ‘The high column temperature reduces the life of a partition column because of evaporation of the liquid phase. Evaporation will cause the column to deteriorate and produce a decrease in the component retention times. The stability of the temperature is also very important during the column operation. Because of unattended operation of a process gas chromatograph for long periods of time, it is vital that there exist a method of temperature control. In the AIC Gas Chromatograph, various column configurations are installed in a hot air bath. The air bath consists of an insulated oven, a heater above which a stteam of air is constantly flowing, and an electronic control system which automatically compensates for any temperature shifis. Such system eliminates the necessity of placing different components of the analyzer at equal distance from the heater. The temperature in the air bath analyzer is maintained at +.1° centigrade. 13.5 THE CHROMATOGRAPH COLUMN, ‘The column is the single most important factor affecting the ability of a chromatograph to handle a specific application. It generally consists of an 1/8, 3/16 or 1/4 inch outside diameter tube packed with a resolving material which may be either an adsorbing agent or a Partitioning liquid on an inert support. The column is usually fabricated from stainless steel, though Teflon due to its inert chemical characteristics, is enjoying increased use. Small plugs of glass wool in either ends of the column retain the packing. Length of the column may vary from a few inches to 30 ft. depending on the application. 14 GENERAL COLUMN INFORMATION As previously mentioned, there are two types of column packing materials: active solids and inert solids covered with a liquid. The common adsorption-type columns are activatedalumina, silica gel, activated carbon, and molecular sieves. They are nommally used for separation of fixed gases and light hydrocarbons. Adsorption columns are susceptible to contamination. The commonly used adsorbents can be contaminated by water, oxygenated compounds, and in some cases, carbon dioxide. These contaminants reduce resolution and sensitivity by reducing the amount of surface area available for sorption of sample components. The contamination can be reversed by purging the column with dry carrier gas. This procedure is a reactivation process and allows the column to be reused. Partition columns are considerably more versatile than adsorbent types and have a much wider range of application. They are also less susceptible to contamination. Some examples of partition columns are: * Dow Coming Silicon Oil on Firebrick * Carbowax on Firebrick ° — Oranite on Teflon 14.1 COLUMN PACKING While a column supplied with an AIC process chromatograph can be obtained on short notice from AIC, occasionally a customer desires to produce his own columns. For an adsorbing type column, all that is required is to pack the column tube with the correct mesh of the proper material and then bake the column out for about 24 hours before installing it in the analyzer. With partition columns, it is sometimes necessary to prepare the liquid phase and apply it to the solid support before the column may be packed. The procedure for applying the liquid phase is as follows: + The important factor in preparing a partition column is the ratio of liquid to solid support. This value is generally known so all that is required is to weigh the comect amount of liquid and solid support. + Add sufficient amount of solvent (acetone, methanol, ether, etc.) to the liquid phase to produce 2 mixture which will completely wet the solid support.+ Pour the solid support into the liquid mixture and stir thoroughly. + Evaporate the solvent from the mixture by warming and stirring. Do not use high temperature as this might cause the liquid phase to boil off. Once the material is completely dry, pack it in a suitable tubing. While the tube is being filled, it should be vibrated or tapped to ensure that the material settles correctly. ‘The appropriate fittings are then attached and the column is installed in the instrument. It should be purged with carrier gas at operating temperature until the recorder baseline is stable. 142 MULTIPLE COLUMNS AND VALVE CONFIGURATIONS It is often impossible to find a single column which will separate all of the desired components. The solution most often adapted is to use two or more columns and, occasionally, an additional valve. For many analyses, two columns are used when analysis with a single column is too slow or has other disadvantages. For example, if the sample from the process stream contains components which are harmful to the main column, it is advisable to use a second column which will separate the harmful components from the primary components before they reach the main column. The harmful components then can be backflushed to vent. There are literally hundreds of column packing materials available today, with additional ones coming into use every year. The resulting possibilities in valve and column configuration are staggering in their number. Yet, out of these complexity of columns, the best configuration for the analysis desired must be determined. AIC personnel, with years of experience, are qualified to deal with the problems of column selection. Consequently, AIC offers a wide variety of column systems as standard modifications. 15 PERFORMANCE FACTORS Once a column for a patticular application is chosen, its actual performance with respect to resolution, analysis time, and sensitivity must be matched to the customer's requirements by I-13suitable variation of the operating parameters. Predicting the actual performance frequently presents difficulties because the desired performance factors are often mutually incompatible. ‘The measurements usually made on the basis of peak area, often require a different degree of resolution than deemed necessary in non-industrial applications. Minor components of low peak area must be resolved from the tail of 2 major component, if they are to be measured quantitatively. Stability and rapid analysis times required for industrial applications dictate that tailing effects must be kept to a minimum. This may exclude the use of certain desirable partition liquids with excessive vapor pressures which are rapidly lost from the column. Also, the inert support should be chosen to eliminate surface effects that introduce tailing or non-linearity. Some general rules which might assist in determining the best column for a given application are as follows: 15.1 RESOLUTION ‘Within limits, resolution is increased by increasing the length of a column, reducing the oven temperature and, to a lesser extent, reducing the carrier flow rate. These factors increase the retention time and generally reduce the sensitivity. Further, the point of diminishing returns is reached rapidly because diffusion effects assume greater significance. If resolution between two components is poor, it might be improved by decreasing sample size. However, if sensitivity is a problem, small samples may not provide sufficient peak height for trace components. Generally, when resolution between two components is poor on a column, it is better to look for another column that is more suited to the application, 152 ANALYSIS TIME Generally, the conditions of an application should be such that the analysis time is as short as, possible. This procedure results in narrower peaks, greater sensitivity, and more sample cycles per unit time. Diffusion effects is also minimized which results in better reproducibility of peak height. Analysis time decreases with higher temperatures and, to a lesser extent, with greater carrier flow rates. Unfortunately, both of these factors may have damaging effects on resolution and column life. If column size (length and volume) is kept I-14to a minimum, then analysis time can be shortened. 16 APPLICATION ENGINEERING Since each process chromatograph is designed to fit a specific application, it is necessary to coordinate or blend the various elements which are involved in order to achieve the desired results. This process is called application engineering. Generally, when a customer orders an instrument from AIC, he will request that we custom build the columns, select a valve configuration, and determine the operating conditions necessary for each specific task. When the chromatograph is delivered, all that is required to place it into operation will be the installation procedure. Occasionally, a customer will purchase only the “hardware” of a chromatograph system. ‘Under these conditions, the column selection and determination of operating parameters, such as peak sequence and time cycle, will be customer's responsibility. In other words, customer will perform the application engineering. While it is impossible to provide a complete discussion of variables affecting the operation of a chromatograph, we will nevertheless consider some of the basic principles of the operating ‘process. ‘Once the different elements of an instrument have been interconnected and are operating properly, the temperature of the analyzer must be adjusted to some arbitrary value. Other parameters, such as flow, are adjusted according to information given in the operating ‘manual, and the instrument is ready for a manual run. A sample is injected into the column and a chromatogram is produced on the recorder. Depending on the results of this chromatogram, adjustments are made to the various parameters to improve performance. For instance, if the peaks of the chromatogram are too much apart then the temperature of the analyzer can be raised and/or the cartier gas flow rate can be increased. If the resolution is poor, then temperature and flow rate should be decreased. Another area of possible adjustment is sensitivity. If peak height is inadequate, then the ‘bridge voltage can be increased. The normal operating voltage range of the bridge is 8 to 12, volts, but higher voltage is permissible. However, very high bridge voltage will increase noise and decrease the filament lifespan from overheating. An altemative is to increase the I-15sample size by changing the sample loop on the gas sampling valve or the sample disk in the liquid sampling valve. When a multi-column and/or a multi-valve configuration is used, it is necessary to determine, by experimentation, the best time to energize and de-energize the valve(s). For example, a single and precut configuration is designed to precut or remove certain components of the sample and prevent them from entering the main column by de-energizing the valve when the components of interest have eluted from the precut column. If the valve is not de-energized quickly enough, components which might damage the main column are permitted to elute. Early precutting, on the other hand, might prevent a peak of interest from eluting. Several manual chromatographic analyses are performed to determine the complete cycle time, precutting or column switching time, and automatic zeroing point. Once these parameters have been fixed, an automatic sequence may be programmed, regulating the operation of the entire chromatographic system. 1.7 THE PROCESS CHROMATOGRAPH A process chromatograph must be mgged, resistant to corrosion, and suitable for use around explosive gases, because of the environment in which it is often situated. Also, because it is often operated for long period of time unattended, it should be completely automatic. ‘The purpose of a gas chromatograph is to analyze a process stream. The unit should be located close to the sample source for increased efficiency. But, most process plants are actually operated from a control room which may be some distance from the process stream. In order to fulfill these conflicting requirements, the process chromatograph consists of three basic units: the analyzer, control unit, and data acquisition and presentation unit. 17.1 THE ANALYZER Just as the column is the heart of an analyzer, the analyzer can be considered the heart of gas chromatograph. The system components which are primarily responsible chromatographic r-16analysis: sample valve, columns, and detector, are located in the analyzer. In addition, flow and temperature controllers, which affect these primary components, are situated at the analyzer. Electrical components are installed in explosion proof enclosures for operations in hazardous area. Also, the analyzer is designed to accommodate additional valves and columns, thereby increasing the number of applications for which it can be used. 1.7.2 THE CONTROL UNIT The unit is solid state and microprocessor controlled with a crystal time base and no relay contacts. It is capable of the simultaneous operation of up to ten analyzers, with up to 10 streams per analyzer and up to 20 components per stream. The programmed functions incorporated with the MC-503 are slope sensitivity, component detection, peak area determination, internal elution time determination of each component, automatic component elution time adjustment, continuous base-line zero tracking, and auto zero to compensate for Jong term drift. Input to the MC-503 can be from thermal conductivity, flame ionization, or flame photometric detector. There are 4 status alarm inputs from each analyzer, and an RS-232 input from another computer or CRT terminal. Power requirements are 115V 10A, 50/60 Hz, 150 watts, plus analyzer load. 173 OUTPUTS ‘The MC-503 interfaces with an IBM compatible PC through a standard RS-232 port or ‘current loop serial port A hard copy of all analysis may be obtained through a parallel Ftinter. Also available are up to thirty two (32) 4-20 ma outputs for trend recording or closed loop control. = )) SAMPLE SYSTEMS In order for the accurate and reliable analysis with a chromatograph, it is necessary that the I-17sample delivered to the analyzer be representative of the process stream being monitored. ‘This requirement places the sample system on a level of importance equal to that of the analyzer. Some of the operations which a sample system may be called on to perform are: + Take a representative sample from vessel to process line. + Transport it to the instrument without excessive delay. + Remove particulate matter. + Filter mists and aerosols. + Vaporize liquid samples. + Prevent vapor samples from condensing. + Measure and control flow and pressure through the analyzer. + Remove unwanted components. + Accommodate introduction of calibration standards. + Accommodate analysis of more than one stream with one analyzer. The AIC sample conditioning system is designed to assist analyzer in performing the specific job for which the chromatograph system, was designed. Basically, each sample system regulates pressure, filters and controls the flow of streams to the analyzer, and introduces a calibration standard either manually or by means of a valve controlled by the programmer. Generally, AIC sample system is mounted on a rack with the analyzer directly above it. I-1818 PROBLEMS IN CHROMATOGRAPHY ‘As might be expected with an instrument of enormous application possibilities, problems are sometimes encountered. Generally, these difficulties are results of inadequate information. For example, occasionally, when a process analyzer is connected to a plant stream, the stream is found to contain components which were not known to be present. These unexpected components in the sample may cause problems by eluting from the column at the same time as a peak of interest or by interfering with the operation of the sample system. To correct this problem, it may be necessary to substitute a different column, or to adjust the flow, pressure and temperature parameters. If a plant sample is available at the time of original application engineering, it is possible to minimize such problems. ‘A gas chromatograph must be calibrated with a sample of known composition. The improper standard sample will result in incorrect chromatographic analysis. Another factor which greatly affects instrument accuracy is the physical state of a sample. A chromatograph column accepts only vapor samples. However, since the chromatograph is required to monitor both gas and liquid process streams, it is important to vaporize the liquid sample so that it is acceptable to the column. The partial vaporization of samples will result in different sample volume, from one sample to another, hence large inaccuracies in analysis of sample will result. The similar difficulties can occur with a vapor stream. If condensation of vapor samples occurs, the sample will not be in vapor phase and measurement errors will again result. To facilitate vaporization and prevent condensation, it may be necessary to heat the sample lines. Steam tracing normally provides the heat source. However, the incorrect tracing may develop cold spots, resulting in condensation of sample.SECTION IL SAMPLE SYSTEM 2.1 INTRODUCTION It is generally recognized that a comectly designed and built sampling system is as important as analyzer for proper analysis of the sample. This section will provide the necessary information for operation and maintenance of the Sample System. Each sample system is designed for the specific application, so the customer is assured of receiving the correct system for his needs. However, certain basic components are used in every sample system. A discussion of the various components utilized in the AIC sample system is included in this section. ‘The function of the sample system is to prepare the sample for analysis. This preparation includes controlling and measuring flow, regulating and measuring pressure, filtering the streams to remove particulate matter, vaporizing liquid samples, and maintaining the ‘temperature of vaporized samples. The unit also handles selection of the stream to be analyzed and introduction of a standard sample upon instructions from the controller. ‘The components of the sample system are housed in a heavy duty steel cabinet (3 standard sizes available for AIC sample system) with a latched and gasketed door. If required, an air bath heated system can be incorporated. The unit may be rack or wall mounted, and is suitable for installation in almost any area of a plant. This characteristic is extremely advantageous when one considers that the unit should be located as near the sample point as possible, 2.2 LOCATION AND MOUNTING Several factors should be considered before positioning the sample system at a location. It should be positioned as close as possible to the analyzer to minimize the response time. At II-1the same time, it should be located near sample points so that a constant supply of fresh sample can be assured. In both cases, placement should be in either an instrument room or house set up for that purpose, or in a semi-protected area. Once the location for the sample system has been determined, it will be necessary to mount the unit. Generally, when the sample system is shipped, it has already been mounted, by AIC, in a house or on a rack with the analyzer. If this is not the case, then the cabinet should be mounted vertically against a panel or wall and secured with four 7/16 bolts. 23 STREAM CONNECTIONS ‘The sample system should be located near sample points and a rapid flowing stream from sample probe (Figure II-1) should be piped to the immediate vicinity with a side stream directly to the conditioner. Sample lines are generally 1/4” SS, and there is a sample inlet and bypass for each stream. Since the unit is capable of analyzing eight streams per analyzer, there can be as many as sixteen stream connections. When a calibration standard is utilized, there will be one 1/8” connection to be made. All of the aforementioned comnections are made at the side of the sample box. A vent line is located at the bottom of the unit which should be connected to a suitable vent and should not be returned to the process stream. 24 COMPONENTS As previously stated, each AIC sample conditioner is custom built for its particular application. A functional description of these components follows. 2.4.1 FILTERS A suitable filter is the Swagelok bypass unit provided with most sample systems furnished by AIC. This filter has two flow paths. The main path is tangential to the filter elements. This flow helps to sweep away particulates accumulated on filter elements and minimizes the tendency of plugging of filter element. A side stream is taken through the filter element. qI-2aqoud aidueg 1 03 wy p “74 “Tamdyy ye Rie ‘BAN CROWS SNA CD) HON ous ment] vag ORD al a To mana! || Ho -od_fe L- zhy—e} Pan2.4.2 OIL SEPARATORS oe eS Often the sample might contain entrained mist, such as sulfuric acid, absorption oil, compressor lubricant, or heavy ends. Since these materials are difficult to vaporize, they might collect and cause line plugging or damage to the chromatograph column. They should ‘de removed using a suitable oil separator or other knockout device. 2.4.3 PRESSURE REGULATOR ‘The chromatograph accepts a vapor or liquid sample, depending on the of type of sample valve used, at a pressure between 1 and 300 + 1 psig. Vapor samples should be provided to the analyzer at a pressure of 1 to 10 psig regulated to + 0.5 psig. Liquid samples up to 2 maximum of 800-1000 psig can be analyzed. A special all-stainless pressure regulator, AIC Part No. 12125, or equivalent, is recommended for vapor sample regulation, This regulator can also be used for liquid samples when a liquid sample valve is provided. Brass or aluminum regulators can be used depending on the nature of the sample. A filter should always be used up-stream of the regulator to protect the seat. Most regulators have built in filters ahead of the seat. 24.4 VAPORIZER REGULATOR The AIC Vaporizer Regulator is a combination of vaporizer and pressure regulator designed to vaporize liquid samples with boiling points up to 300°F and to regulate the pressure of vaporized samples precisely to within + 0.1 psig. The unit can be mounted at the sample point, but is generally installed in the sample conditioning box. Heat for vaporization of liquid sample is provided by steam (maximum steam pressure 300 psig) or an electrical heating clement. The unit is weatherproof and a spring loaded design allows mounting in any Position, since gravity has no effect on its operation. Maximum up-stream pressure range is 2000 psig, and an automatic vent eliminates the possibility of downstream pressure exceeding the preset value. The downstream pressure can be set to any value between 8-30 psig by tuming the adjusting screw at the top of the regulator. rI-4Specifications + Stability: For input pressure between 50 and 700 psi, the regulator will maintain the output pressure within 0.5 psi with an upstream pressure change of 50 psi, or within 0.1 psi with upstream pressure variation of 10 psi. For input pressure between 20 and 50 psi, the regulator will maintain output pressures within 0.1 psi for upstream pressure variations of 5 psi. + Flow Capacity: Maximum flow capacity of regulator, while maintaining the stability as stated above, is approximately 2200 co/min. A variation of flow rate from 10-2000 ce/min. will not change the outlet pressure more than 1 psi. + Pressure Ranges: Maximum inlet pressure 700 psig, outlet pressure 8-30 psig. : ‘Vent Flow Rate: Varies with downstream pressure but should be less than 300 ccfmin. + Maximum Steam Pressure: 300 psig. + Size: Space clearance required for mounting, 4 1/2 inches width x 7 3/8 inches height. + Weight: Approximately 10 pounds. . Construction Materials: Components wetted by the sample are made of AISI ‘Types 302, 420, and 440 stainless steel, Monel and Teflon. Installation Figure IL-2, shows the mounting dimensions and sizes of connectors required for installation of vaporizer regulator. It is recommended that a valve be installed in the sample line between TI-5ADJUSTING ALLEN CAP SCREW aq| o 738" Ft VENT OUT 1/8" NPT VAPOR QUT 1/8" “NPT vate, STEAM WOR CONDUTT FoR USE __ TTI ai foes OE Nee eden WITH ELECTRICAL HEATER hpi LUN HEATER 15 USED 1/4" NPT. v2" NPT Lup SAMPLE We" wer HTT NOTES - MATERIAL WEIGHT AIST Types 302, 420 and 440 Stainless Steel, Monel, and Teflon TO Lbs. Max. Steam Pressure 300 PSIG Sample Inlet Pressure 700 PSI Sample Outlet Pressure 8-30 PSI Flow Capacity 0-2,000 cc/min. Figure IL? Installation drawing for AIC vaporizer regulator.the regulator and the sampling point to shut off the sample for periodic cleaning of the porous metallic filter in the vaporizer regulator. ‘The regulator is rugged and corrosion-resistant and designed to withstand the environmental conditions of outdoor locations. If the downstream sample line is to be steam-traced, the steam should be brought first to the regulator, then into the tracing line. If the user desires, a downstream pressure gauge, flow meter, and flow control valve can be installed. Operation After the installation of regulator, turn on the steam supply and allow a few minutes for warm-up. Unscrew the adjusting screw on the top of the regulator all the way and open the sample valve to admit sample. Adjust the regulator to give the desired output pressure as indicated by the downstream pressure gauge. Set the sample flow through the analyzer to the desired value with the downstream flow control valve, and re-adjust the regulator output pressure if required. The regulator will now operate without further attention. Maintenance ‘The vaporizer regulator should require litle servicing except for occasional cleaning of the porous metallic filter. To access the filter, remove the bottom cap and the screw in the center of the filter. If the unit is to be dis-assembled (Figure II-3), it should be done only by a qualified instrement technician. Great care must be taken to avoid buckling the metal diaphragm during disassembly. The unit may be retumed to AIC for reconditioning when required. I-7Ayquiasse s0yvjnBo1 sozpodes E11 82n3}yVaporizer Regulator Recommended Spare Parts List DESCRIPTION PART NO. ory Filter 2010 1 Gasket 2018 2 Gasket 2017 1 Gasket 2019 i Gasket 2020 i Spring 2016 1 Ring, Retainer 13005-2 1 Diaphragm 2007 1 Pin Ball Release 2008 1 Ball, Precision 2009 1 Spring, Retention 2006 1 2.45 LIQUID VALVE ‘When samples are introduced through a liquid valve to the analyzer, no vaporization facilities are required, but the sample must be completely liquid. 24.6 STEAM TRACING It is necessary to maintain some sample lines at higher temperatures to prevent condensation. One effective method of accomplishing this is to employ steam tracing or jacketing. If steam tracing is employed, the steam lines should be close-coupled to the sample lines and components to assure good heat transfer, and the two lines lagged. When multiple stream manifolds are supplied, all the solenoid valves and other components should be steam traced and lagged. Care should be taken to leave no cold spots. If vaporizing regulators are not utilized, the sample cabinet should be heated. qI-92.4.7 SCRUBBER It is sometimes required to remove certain materials from the sample prior to analyzer, such as large amounts of water or acid. An effective method of removing these materials is to pass the sample through a stainless steel, or Monel scrubber. The scrubber is packed (usually by the customer) with 2 material suitable for the specified application. A scrubber can be made from a length of two or three inch pipe with end caps and sample IN and OUT fittings at both ends. The end caps are removed to replace the packing. 24.8 WATER COALESCER The water coalescer removes free water or water vapor from Hiquid or gaseous samples which contain 10% or less free water and no solid particles. When water coalescer is used with a sample which is heavier than water, it should be installed in an inverted position. As the water and gas mixture flows through the polymer membrane, the water separates from the gas and flows down the outside of the membrane and vent out with the bypass flow. 24.9 CYCLONE SEPARATOR ‘The cyclone separator is used to remove entrained water in a gas stream. The cyclone separator separates water from gas by centrifugal force, the water collects on the sides of the separator and drains at the bottom of the separator. Inlet and outlet comnections are 1/4" NPT. 2.4.10 SAMPLE COOLER The sample cooler is a counterflow heat exchanger for cooling of high temperature samples. It is used to drop temperature of liquid samples to prevent the liquid sample from affecting analyzer temperature and becoming two-phase. It can also be used to separate moisture in a hot gaseous sample. II-1025 BYPASS FLOW Sample lines should be kept as short as possible to maintain rapid instrument response. For liquid samples, a speed loop should be connected to a tee and the inlet port of the vaporizer regulator (if used) with a bypass flow at this point. For either gas or liquid samples, additional bypass flow is desirable at either the stream selection manifold or the analyzer unit. The bypass flow can be vented or recycled to a low pressure point in the process. Bypass flow should be chosen so that the transit time of the sample is minimal. 2.6 MULTIPLE STREAM SYSTEMS ‘The sampling techniques described previously apply to each individual stream in multiple stream installations. In addition, there are special considerations relating to operation of the sample system for multiple stream instruments. The system uses the backflush system, where the sample, from the stream being analyzed, flows not only through the valve to the analyzer, but also circulates through the other solenoid valves, to purge the lines. If a solenoid fails to seal completely after a period of use, any leakage will be purged out the vent line. The system includes for each stream a tee, for sample bypass, a stainless steel 3-way solenoid valve, and a needle valve in the vent port of the solenoid valve. The needle valve can be used to adjust the bypass flow. For proper conditioning of sample, these components can be mounted in an insulated oven for electrical or steam heating. I-11SECTION DL PROCESS ANALYZER 3.1 INTRODUCTION ‘An analyzer is generally considered to be the heart of a process chromatograph system. As stated in Section I, it is the analyzer’s components: the sample valve, columns, and detector, which are primarily responsible for performing the chromatographic analysis. The sample valve repeatedly injects a fixed quantity of sample into the column. A carrier gas carries the sample through the column, where it is separated into its individual components. These ‘components then elute in the inverse order of their affinity to the column packing and flow across the detector where they are measured. ‘While the sequence of component elution is dictated by the chemical and physical properties of the column, the time of elution is determined by carrier flow rate and column temperature. Since elution time identifies each component qualitatively, and since all automatic programming functions are based on this information, the importance of precisely controlled carrier flow and oven temperature is obvious. Basically, an analyzer (Figure IN-1 and Figure I1J-2) consists of an air bath unit with precise temperature control, a detector, and columns and valves for a specific application. On AIC Model 600 analyzer, the regulators and pressure gauges are mounted outside where they are readily available for monitoring and adjustment. The detector, valve and columns are located inside the analyzer where they benefit from a constant temperature environment. All automatic functions regulating the operation of the analyzer are controlled from the PC. 3.L1 CARRIER GAS FLOW In theory, any gas which is not a component of the sample may be used as a carrier. However, only very few gases make efficient carriers. Helium, because of its inertness and high thermal conductivity, is the most frequently used. Carrier gas flow rate must be III-1Carrier Regulator Carrier In Hester Air Press Gauge Carrier Pressure Gauge Heater Air Reguiat Thermometer Column Out Figure IIL1 Exterior of AIC model 600 Analyzer.oaueg wanquseduey,adjustable over a wide range in order to control the elution rate. At the same time, it is important that the flow should be constant throughout sample analysis. Carrier gas is supplied to the analyzer from the cylinder at a constant pressure, generally 100 psig. It first enters the analyzer at the carrier regulator (Figure I-1). The carrier gas regulator is provided with three outputs. Two of these, marked secondary, are adjustable from 0 to 100 psig, while the third supplies carrier gas at the primary unregulated pressure. From one of the secondary ports, the gas goes through the sample valve and to the main column. A 0-100 psig pressure gauge is also attached to this port and it measures carrier gas pressure at the column. Gas from the other secondary port passes through a metering valve (mounted on the regulator) and goes to the reference side of the detector. The unregulated port is in service only when a precut column configuration is utilized. In this case, the carrier ‘gas passes through a metering valve and is used to backflush the precut column. The port is plugged when the precut operation is not used. 3.1.2 INSTRUMENT AIR FLOW An air supply at 40-50 psig to the analyzer is required. The air is used for heating and valve actuation for sample introduction and column switching (Figure Il-1). It enters the analyzer through 1/4” tubing and is connected to a tee on the four-way solenoid used to actuate the sample valve. From the tee, the air is piped to the inlet of a single stage regulator. A Pressure switch is connected to one port of the regulator. The air going to the regulator is used to heat the analyzer. The output of this regulator is adjustable from 0 to 15 psig, and is normally set at 8 psig. From it, air travels to the heater condulet, over the heater, and out into the analyzer. The safety pressure switch is an electrical switch which is set to cut the voltage to the heater if air pressure should fail. It is normally set for about 3 psig, but can be increased or decreased by turning the adjustment serew on the top of the switch. No adjustment should be attempted until the set screw securing the adjustment screw has been loosened. TII-4The sample inject valve (and column switching valve, when used) is operated by air supplied by the four-way solenoid. When this solenoid is de-energized, air is applied to the rear chamber of the air cylinder, causing the shaft or piston arm of the cylinder to be extended. If the solenoid is energized, air is shifted to the front of the cylinder, causing the piston arm to retract. The sample inject valve assumes a new position for proper operation of the chromatograph sequence. 3.13 SAMPLE GAS FLOW AND BLOCKING VALVE Generally, by the time the sample reaches the analyzer, it has already been filtered, vaporized, or condensed, reduced in pressure, etc., and no further preparation is necessary. Occasionally, however, as in the case of a fairly uncomplicated sample, the sample handling equipment will be attached to the side of the analyzer. Whichever is the case, the sample system drawing in the modification section of this manual, gives a schematic presentation of the sample system. Sample flow through the analyzer is usually on the order of 200 cofmin. for gas, and 100 cc/min. for liquids. It flows continuously through the sample valve, and leaves the analyzer through the sample out port. Sample pressure of gaseous or vapor samples at the inlet of the analyzer should be reduced to a value (about 5 psig) just sufficient to move the desired flow through the analyzer. Liquid samples, on the other hand, must be under sufficient pressure to ‘prevent them from flashing, To achieve accuracy and reproducibility in the sample size, the flow in the sample loop is blocked by the blocking solenoid just before sample introduction. ‘This action allows the pressure of the sample trapped in the sample loop to stabilize. When the sample is a vapor, the blocking solenoid is located before the sample loop, and its actuation allows the trapped sample to bleed to atmospheric pressure. Since this pressure is essentially constant, the sample volume will be repetitious. In the case of a liquid sample, the blocking solenoid is located after the sample loop. When the solenoid is energized, flow through the sample loop is stopped, and the sample assumes the sample in pressure. Since this pressure is held constant by regulators, a consistent sample volume is assured. This also allows any gas bubbles to go back into solution at full sample pressure thus minimizing the chances of a two phase sample. rII-53.2 HEATING SYSTEM ‘An important feature of the AIC analyzer is the control of its temperature by a solid state temperature controller. The system consists of an electronic controller, a sensor, and a heater. ‘The electronic controller portion is located in the MC-503 controller. Any adjustments to the temperature of the analyzer are made at the console. The sensor is a solid state probe located out of the stream of hot air from the heater assembly that distributes the air flow through the oven. The heater is an air-flow-through type and is enclosed in a condulet mounted at the bottom of the analyzer. Maximum power consumption of the heater is 800 watts and the temperature control within the analyzer is approximately 20.1°C. A high temperature limit thermoswitch is located in the detector condulet, and is designed to remove power from the heater if the analyzer temperature exceeds 300°F. Any time this switch is used, an investigation of the heater system should be undertaken to determine the cause for high temperature. 33 THE DETECTOR ‘The standard detector used in the AIC Model 600 analyzer is in the form of a four element bridge. Each of the filaments has a resistance value of approximately 30 ohms at 25°C. Current is supplied to the bridge by a highly regulated power supply, located in the control unit. This power supply is adjustable from 7 to 20 volts with the nomal range being between 8 and 12 volts. The filaments are mounted in a metal block, called the detector block, which is in tum mounted in an explosion proof condulet known as, you guessed it, the detector condulet. ‘These filaments are constructed from 2 combination of nickel and iron, and enjoy the following advantages over other types of filaments: + They maintain good sensitivity at high temperature. III-6= By operating hot, they discourage coating. + They are capable of surviving long periods of operation without a carrier gas. In fact, some filaments of this type have remained operable after 24 hours without carrier. Despite their ruggedness, however, filaments eventually become mismatched, and it becomes necessary to replace them. 3.4 INDICATING THERMOMETER Each analyzer is equipped with a thermometer located on the door. It indicates the temperature of the oven. 3.5 VALVES AND CONFIGURATIONS ‘The components which we have discussed so far in this section, detectors, heaters, etc., are the same in almost every analyzer. It is the addition of the valves and columns which makes a chromatograph uniquely able to perform a specific analysis. ‘There are literally hundreds of columns available for the separation of specific components, and up to four of these columns normally can be installed in the Model 600 analyzer. The direction of flow of carrier gas and sample through these columns is determined by the valves and the way they are interconnected. AIC uses two types of valves; the standard 10-port rotary valve, and the liquid valve. A total of two valves, in any combination, can be mounted in the analyzer. The various ways in which the valves can be interconnected results in ammerous column configuration possibilities. 3.5.1 SAMPLE VALVES As previously indicated, AIC utilizes two types of valves, a ten port gas valve and a liquidvalve of 4, 8 or 10 ports. The gas valve is the more common, and a picture of the assembly can be found in Figure III-3. ‘The lower section of this valve is constructed of 440 stainless steel, and the upper rotary body is made of aluminum surfaced with fluorogold. No lubrication between the mating surfaces is required. The valve cap contains an arrangement which allows the pressure between the rotary and the lower body to be vatied by tightening or loosening the cap. This construction pemmits the use of high carrier and sample pressures. A general explanation of its operation follows. The upper surface of the lower body contains 10 equally spaced ports in a circle. The fluorogold surface of the upper rotary contains 5 ‘grooves machined into it. Each groove is designed to cover two ports simultaneously. When the valve is de-energized (the shaft on the air cylinder is extended) ports 1 and 2 are covered by a single groove and hence are common to one another. The same is true of ports 3 and 4, 5 and 6,7 and 8, and 9 and 10. When the valve is energized, a different set of ports are common. In this case 2 and 3, 4 and 5, 6 and 7, 8 and 9, and 1 and 10 are the connected pairs. ‘The second type of valve is the liquid valve. AIC uses the Valco air-actuated 4 port. The Valco valve is constructed of 303 SS and has pressure and temperatute ratings of 3000 psi and 300°F. Multiple sample sizes (2 to 5 sl) are available by exchanging the shaft and seal assembly. This valve is used primarily in conjunction with the AIC 10-port valve. 3.5.2 VALVE ACTUATION Actuation of the liquid sample valve and the ten-port rotary valve is essentially identical in Principal and mounting details. In both cases, actuation is accomplished through linkage connected to a conventional air cylinder operated by air supplied from a four-way solenoid valve. Pressure is applied alternately to opposite ends of the air cylinder (depending on whether the four-way solenoid valve is energized or de-energized) with the other end vented to atmosphere. When the solenoid valve is de-energized, pressure is applied to the rear of the air cylinder and the cylinder piston arm or shaft is extended. When the coil is energized, pressure is applied to the front chamber and the piston arm or shaft is retracted. rII-83.6 FLOW RATE ADJUSTMENTS As previously indicated, the flow of carrier gas through the system is one of the major Parameters in proper operation of the analyzer. If accurate and repeatable results are to be obtained, then this flow must be carefully controlled and regulated. Sensitivity, resolution, and elution time are all critically affected by the cartier flow rate. Furthermore, each column will have an optimum flow rate which will depend largely on the type of sample being run, and the type and length of the column. ‘There are several methods of measuring the carrier flow rate, the most convenient being the rotameter. Another, and a more accurate method, is to observe a moving soap bubble. With this method a soap solution is placed at the bottom of a burette, and the carrier gas is permitted to flow into the burette. The amount of time required for a soap bubble to move ‘over a measured volume will provide the necessary information for determining the flow rate of the carrier gas. The procedures for adjusting carrier flow through the column, reference flow, and precut carrier flow follow: 3.6.1 CARRIER FLOW Carrier flow through the column should be set the first time before the analyzer is turned on. If application engineering was done by AIC, simply adjust the carrier regulator until the Pressure is the same as the column pressure for the specific application. Tum the analyzer on and allow it to reach operating temperature. Attach a rotameter or bubblemeter to the “column out” port and measure the flow. If it differs from the value given, adjust the carrier regulator until the values are the same. When using a rotameter, make certain it is the correct type. For example, if helium is the carrier, be certain to use a helium meter. Since helium is such a light gas, an air oxygen rotameter would indicate that the cartier flow was much lower than it really is. III-103.6.2 REFERENCE CARRIER ‘The reference carrier is that portion of the carrier which flows across the two reference detectors. is rate is adjusted by the metering valve located on the carrier regulator. As in the case of the main carrier flow, the reference carrier should be adjusted the first time while the analyzer is off. Adjust the main carrier flow first, then, making certain that the precut metering valve is shut off, attach a rotameter to the vent port on the analyzer and adjust the reference carrier valve until the rotameter indicates a flow of about 15 cc/min. Anytime the main carrier flow is adjusted, it will be necessary to readjust the reference flow. 3.63 PRECUT CARRIER FLOW A precut carrier is needed only when a single and precut column configuration is used. In this case, the precut carrier's function is to backflush the precut column and push the ‘unwanted components to vent. As a result, it is necessary to measure the precut cartier flow rate at the same vent port where the reference flow rate is measured. To accomplish this, simply set the reference cartier flow rate, and then adjust the precut metering valve attached to the carrier regulator until the sum of the reference and precut flow rates is the desired value. For example, if reference flow is 15 cofmin., and the desired precut flow is 30 ccc/min., then the flow at the vent port should be 45 cofmin. As a matter of fact, this is the flow which will normally be measured at the vent port since 30 cc/min. is the correct precut cartier flow rate. 3.7 ROUTINE MAINTENANCE ‘There are no requirements for periodic maintenance on the Model 600 Analyzer. Whenever convenient, however, the operator should make the following general checks in order to ascertain that everything is functioning properly. * Check the pressure on the carrier cylinder. If it is at or below 200 psig, then the cylinder should be changed. TIt-11+ Occasionally, check fittings for tightness. + The 10-port vaive is mounted on an aluminum channel which is, in tum, secured to the analyzer mounting pan. ‘The operating of the valve could loosen the mounting and it should be checked occasionally for tightness. + About once 2 month, check the pressure switch by dropping the pressure below the pre-set point. The heater will go off. Then retum the air pressure to 50 psig; the heater will come on. ‘When, by abnormal functioning of the instrument, the need for more specific service becomes evident, one of the following procedures should be observed. 3.7.1 VALVE MAINTENANCE - 10-PORT A picture of the valve assembly and a detailed drawing of the rotary valve is given in Figure IL-3 and Figure III-4, respectively. The valve cap assembly can be removed for inspection of the valve surfaces by turning it in a counter clockwise direction. After the cap has been lifted off, remove the upper rotary by pulling it straight out and off the shaft. The surface of the lower valve is 440 stainless steel and the upper rotary is surfaced with glass filled Teflon. Should cleaning be required they can be washed with a suitable solvent not harmful to these materials, Buffing The Upper Rotary After long use (several months), the surface of the upper rotary becomes somewhat rough. In order to prevent leaks, it becomes necessary to refinish the fluorogold surface. The procedure is as follows: * Obtain a sheet of 800 grit sandpaper. I1I-12200A en ae fe Oia] set NOs NBL ova as “oaqea sed Aawjox wod woy, p11] aunty on sua ayes on wa paren Tornoe shaman sate OLY (1) aw @ 4960 G Cy — =» TL NE yee lt cooo-fLay the sandpaper, grit side up, on a hard, smooth surface. Place the fluorogold surface on the paper and make about four figure eights. Do not press down hard. ‘Tum the paper over so that the grit side is down, and buff the upper rotary until it is smooth. Removing The Lower Valve ‘Tum off the instrument air. Disconnect the two fittings to the air cylinder. Disconnect all fittings to the lower valve. Undo the four screws securing the aluminum channel to the analyzer pan. Remove the assembly from the analyzer. Remove the four screws securing the valve to the channel and lift the valve off. ‘Make certain to note the positioning of the valve before removing it. Port 1 should be located at the top of the bracket (Figure III-3). Unscrew the cap and lift off the upper rotary. If the lower valve is to be cleaned, remove all the fittings. Reassembly Replace the fittings in the ports of the lower valve. Make certain each port has a Teflon gasket in it. III-14Reattach the lower valve to the channel. Port 1 should be at the top. Place the upper rotary on the valve. Make certain that one of the marks in the rotary line up with the scribe above Port 1 on the valve. Screw on the valve cap assembly. Hand tighten or until the bottom of the cap is about 1/32” off the valve body, plus 1/4 tum with wrench. Replace the assembly in the analyzer and reattach all lines according to the column configuration diagram for the specific application. Replacing The Air Cylinder (Figure H11-3) ‘Tum off the instrument air going to the analyzer. Disconnect the two fittings to the air cylinder. Loosen the set screw in the clevis. Unscrew the pivot mount bolt. The cylinder will be free of the channel and attached only by its shaft. ‘Tum the cylinder in a counter clockwise direction until the shaft is unscrewed from the clevis. Remove the cylinder from the analyzer. Pop off the snap ring and remove the pivot mount from the cylinder. Secure a new cylinder and attach the pivot mount to it. III-15Screw the shaft of the cylinder into the clevis until the end of the shaft is flush with the surface of the clevis. Screw in the pivot mount bolt. Make certain the cylinder is positioned as shown in Figure III-3. Remove the valve cap assembly, leaving the upper rotary on the shaft, with the air shaft of the cylinder extended. If the line on the upper rotary does not line up to the scribe on the valve body, then the pivot bolt must be removed and the shaft screwed into or out of the clevis as necessary. Once the adjustment is correct, tighten the clevis set screw. Replace the valve cap. 3.7.2 REPLACING DETECTOR FILAMENTS Depending on the current and temperature to which they are subjected, detector filaments eventually become mismatched. This condition is revealed through baseline drift and inability of the zero controls to adjust the baseline. The four filaments must be replaced as a set (AIC Part # 10331-1). To replace the filaments, proceed as follows: Tum the power off at the analyzer. Remove the detector condulet cover. Undo the four 1/16 Swagelok fittings from the bulicheads in the condulet Disconnect the two shielded cables from the terminal board. Note where each. III-16connects so that they can be reconnected properly. Loosen and remove the two retainer screws in the front of the detector block. Remove the detector block assembly. ‘Remove the filament leads from the terminal strip to which they are connected. Loosen and remove the retaining mut on one of the filaments. Replace the old filament with a new one, making certain to take the Teflon sleeving off the Jeads of the old filament and put them on the new filament. Tighten down the retaining mut. Repeat for the other three filaments. With a meter, check the leads for shorts to the detector block. Attach the filament leads to the correct positions on the terminal board. Consult the analyzer schematic if there is any doubt. Replace the detector block in the condulet. Connect the two cables and the ‘Swagelok fittings. Replace the detector condulet cover and place the unit back in operation. 3.73 COLUMN MAINTENANCE A contaminated or failing column normally manifests itself as a drifting baseline, a high baseline, or an unstable baseline. Once a malfunctioning column has been detected, it can be regenerated by flushing with carrier gas at the operating temperature, or, this failing, it can be replaced. The procedure for replacement follows: III-17