ABBR# SUP# Po# REFH OPERATION & MAINTENANCE MANUAL + O0-AT-0301-6-4 MC-503, + 16700-32042, OM) 160A MC-503 PROCESS GAS CHROMATOGRAPH Analytical Instruments 9845 Drysdale REV: -Houston, Texas 77041 PKG:297 Tel: 713-460-5757 FAX: 713-460-1987 February, 1994Ir TABLE OF CONTENTS PRINCIPLES OF GAS CHROMATOGRAPHY 1.1 GAS CHROMATOGRAPHY 1.2 ‘TERMINOLOGY 1.261 Apparatus 1.2.2 Reagents 1.2.3 variables 1.2.4 Presentation of Data 1.3 INSTRUMENT COMPONENTS 1.3.1 Carrier Gas eta Detector 1.3.3 Valves 1.3.4 Temperature Control 1.4 THE CHROMATOGRAPH COLUMN 1.5 PERFORMANCE FACTORS 1.5.1 Resolution 1.5.2 Analysis Time 1.6 GENERAL COLUMN INFORMATION 1.7 COLUMN PACKING 1.8 MULTIPLE COLUMNS AND VALVE CONFIGURATIONS 1.9 APPLICATION ENGINEERING 1.10 THE PROCESS CHROMATOGRAPH 1.10.1 The Analyzer 1.10.2 The Control unit 1.10.3 Outputs 1.10.4 Sample Systems 1,11 PROBLEMS IN CHROMATOGRAPHY INSTALLATION 2.1 GENERAL 2.2. SHIPMENT 2.3 PAYMENT 2.4 WARRANTY 2.5 CONTROL ROOM PANEL MOUNTED COMPONENTS 2.5.1 PC 2.5.2 Monitor 2.5.3 Printer 2.5.4 Analyzer Control Module 2.5.5 Multiplexer 2.5.6 Analog Outputs/Latch 2.6 ANALYZER 2.7 SAMPLE SYSTEM 2.8 INITIAL CHECKOUT 2.8.1 Initial Checkout Carrier Gas Connections Sample Gas Connection Instrument Air Vent Lines Electrical Installation Demon ainBin p 11-2 1-7 11-7 11-8 11-8 II-8 11-8 II-9 II-10 II-10 I-11 II-12 II-13 II-13 II-13 TI-14TABLE OF CONTENTS, CONTINUED III ANALYZER 3.1 ROL 3.8 +9 INTRODUCTION 3.1.1 Carrier Gas Flow System 3.1.2 Instrument Air Flow 3.1.3 Sample Gas Flow and Blocking Valve HEATING SYSTEM THE DETECTOR INDICATING THERMOMETER VALVES AND CONFIGURATIONS 3.541 Sample Valves 3.5.2 Valve Actuation FLOW RATE ADJUSTMENTS 3.6.1 Carrier Flow 3.6.2 Reference Carrier 3.6.3 Precut Carrier Flow ROUTINE MAINTENANCE 3.761 Valve Maintenance ~ 10-Port 3.7.2 Replacing Detector Filaments 3.7.3 Column Maintenance RECOMMENDED SPARE PARTS ILLUSTRATED PARTS IV. CONTROL UNIT 1 INTRODUCTION TO THE MC-503 1.1 THE MC-503 HARDWARE 1.2 MC-503 SOFTWARE GETTING STARTED 2.1 HARDWARE 2.1.1 Installation 2.1.2 Connecting the ACM to an Analyzer 2.1.3 Connecting the MC-503 ACM(s) to PC 2.2 SOPTWARE 2.261 Executing the Menu 2.2.2 A Sample Run with the Default Parameters ANALYZER DEFINITION STREAM DEFINITION COMPONENT DEFINITION NAME VALVE DRIVERS VALVE TIMES ASSIGN SOLENOID DRIVERS SET STREAM SEQUENCE SET LATCH BOARD MODULE Relay Alarm Parameters Analog Output Parameters RUN/STOP ANALYZER ENABLE/DISABLE STREAMS SET/CALIBRATE TEMPERATURE CONTROLLER DISPLAY CURRENT ANALYSIS REPORT ALARM STATUS WUWWYWEUN SYNE ee PEPE PET PREP Pee T Lbaddnhds dost eetodd ‘ i booms wuweUwuL BSSTABLE OF CONTENTS, CONTINUED DETAILED ANALYZER STATUS ACTIVATE DETECTOR PLOT PRINT DETECTOR PLOT FROM RECORDING DISPLAY TREND 3.14 [N] 3.15 [0] 3.16 [P] 3.17 [0] 3.18 [RJ]: DISPLAY STREAM HISTORY 19 [S]: STREAM ANALYSIS TREND 3.20 [T]: VIEW MODBUS REGISTERS THE ANALYZER CONTROL MODULE 4.1.1 1/0 Devices 4.1.2 Operation of Individual 1/0 Devices 4.2 CONSOLE-TO-ACM COMMANDS 4.2.1 ACM Commands 4.2.2 Detailed Command Descriptions 4.3 SWITCH SETTINGS AND STATUS LEDS ‘TROUBLESHOOTING 5.1 HARDWARE PROBLEMS 5.2 SOFTWARE PROBLEMS INSTRUCTIONS TO USE NEW PASSWORD SYSTEM PULSED RELAY OUTPUTS AIC UTILITIES INFORMATION BACKING-UP THE MC-503 DATA INSTRUCTIONS TO COPY ALL ANALYZER SETTINGS LIST OF APPENDICES APPENDIX A: SETTING VALVE TIMES APPENDIX B ACM BOARD CONNECTIONS APPENDIX C MULTIPLEXER BOARD CONNECTIONS APPENDIX D: COMMUNICATION PROTOCOLS LIST OF ILLUSTRATIONS MC 503 FULL CONFIGURATION MC-503 CONNECTIONS PLOT SAMPLE ACM MEMORY MAP ACM BOARD LAYOUT MC-503 ACM/MODEL 600 WIRING ‘MUX BOARD A-1 A-2 A-4 A-6TABLE OF CONTENTS, CONTINUED SAMPLE SYSTEM 5.1 INTRODUCTION 5.2 LOCATION AND MOUNTING 5.3 STREAM CONNECTIONS 5.4 COMPONENTS Filters 041 Separators Pressure Regulator Vaporizer Regulator Liguid valve Steam Tracing Scrubber Water Coalescer Separator Sample Cooler BYPASS FLOW MULTIPLE STREAM SYSTEMS SAMPLE SYSTEM be uabbubh BEM uuu wow LIST OF ILLUSTRATIONS FIGURE DESCRIPTION COMPONENT SEPARATION SYSTEM DIAGRAM DETECTOR FLAME IONIZATION PC FORTRESS CUTOUT OKIDATA PRINTER CUTOUT MC-503 ANALYZER CONTROL MODULE CUTOUT CRT CUTOUT CARRIER GAS FLOW DIAGRAM MODEL 600 ANALYZER, EXTERIOR MODEL 600 ANALYZER, INTERIOR 10-PORT GAS VALVE 20102 10-PORT ROTARY GAS VALVE INSTALLATION OF VAPORIZER REGULATOR SAMPLE PROBE VAPORIZER REGULATOR ASSEMBLY bey bs la is ie ieieieeeiaveratal CO OSSHAUOBUON HE fiitessises vePrinciples Of Gas ChromatographySECTION I PRINCIPLES OF GAS CHROMATOGRAPHY 1.1 GAS CHROMATOGRAPHY Chromatography is defined as a technique for separating the components in a mixture. This separation is performed by distributing the components to be separated between two phases One of these phases, called the stationary or static phase, consists either of a solid adsorbent material (adsorption chromatography) or of a film of liguid 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 mobil phase (carrier) consists of a gas which pushes or carries the gaseous sample through the column. This carrier gas, which most likely will be helium, hydrogen, argon, nitrogen, or carbon dioxide, flows continuously through the column at a constant rate. At a predetermined time, a valve will introduce a measured amount of sample into the carrier gas stream. The carrier will push the sample through the column, where a separation of components results from a difference in the forces by which the column materials tend to hold each of the sample components. Whether the nature of this force is adsorption, solubility, chemical bonding, polarity, or molecular filtration, it detains some components longer than others. Consequently, all components pass through the column at varying speeds and emerge in the inverse order of their affinity for the column materials. At the end of the column, a detector based on the principle of thermal conductivity measures the amount of each component. Since each component progresses through the column at a predictable rate (column temperature and pressure must remain constant) the travel time (or elution time) identifies each component qualitatively. This process is demonstrated in FIGURE 1-1.saWPLe cyrens wien recone SWHPCE-VaGie 16 ACTORED ournut coun DETECTOR { 4 x A ExT a ein caRnien Gas. FIGURE COMPONENT SEPARATION 1.2 TERMINOLOGY Following are definitions of the terms frequently used in this manual: TECHNIQUE GAS-LIQUID CHROMATOGRAPHY - a description for all chromatographic methods where the moving phase is gas and the fixed phase is a liquid distributed on a solid support. GAS SOLID CHROMATOGRAPHY - All chromatographic methods where the moving phase is a gas and the fixed phase is an active solid such as alumina, activated carbon, silica gel, or molecular sieves.GAS CHROMATOGRAPHY - All chromatographic methods where the moving phase is gas. It is the collective name for gas-liquid and gas- solid chromatography. 1.2.2 APPARATUS SAMPLE VALVE - Device for introducing a repeatable fixed volume of liquid or gaseous sample into the column. COLUMN SWITCHING 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 length of tubing packed with separating agents which separate the sample into its individual components. DETECTOR - That part of the analyzer which detects the components after they have been separated. 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. 1.2.2 REAGENTS CARRIER GAS - The mobil phase of a chromatograph system. It is the gas that is used to move the sample through the column. LIQUID PHASE - Consists of an appropriate liquid, essentially non-volatile at the operating temperature of the column, coating a solid support which constitutes the packing for a gas-liquid (absorption) column. The sample components are dissolved in this liquid as the sample moves through the column and the separation of thecomponents depends on their differences in volatility in the solution. SOLID SUPPORT - Usually an inert porous solid such as diatomaceous earth. The efficiency of the column is influenced by the particle size and the surface area of the solid support. Active solids may be modified to serve as solid support and it is also possible to use the inner wall of a capillary tube for this purpose. ACTIVE SOLID - A porous solid which is capable of separation of the sample components without liquid coating. In this case, the action of the column is one of adsorption rather than absorption. 1.2.3 VARIABLES: PRESSURE - Column pressure effects the carrier and sample gas flow rate. It is dependent upon the column used and the carrier gas pressure. Pressure is controlled by the Carrier Gas Pressure Regulator and indicated by a gauge mounted on the regulator. FLOW RATE - The volume flow rate of carrier at column outlet as measured at ambient temperature. It is controlled by the metering valves mounted on the carrier regulator. TEMPERATURE - Column temperature is of prime importance to the analysis and is dependent upon the oven temperature. 1.2.4 PRESENTATION OF DATA CHROMATOGRAM - A time plot of the detector response to components as they elute from the column. This plot may be obtained from the computer.PRINTER - Provides the print out of normalized, non- normalized analysis, and chromatograms. PEAK - The recorded response from a detector, indicating the elution of a component from the column. PEAK HEIGHT - The distance from the baseline to the top of a peak. The peak height commonly used as a quantitative measure of the component concentration. RESOLUTION - The degree of separation between adjacent peaks. ELUTION TIME - Elapsed time between the injection of the sample and the detection of each component by the detector. Since, for a given column, every component has a characteristic elution time, this measure is used as a means of identification. BASELINE - The portion of the chromatogram between 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 recorder. INTEGRATED AREA - The area under a peak. This area also is proportional to the quantity of the component and is usually measured with an integrating device. 1.3 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 I-5sense the sample, temperature control to regulate the heater, and air for the heater and actuation of valves. The AIC Process Chromatograph incorporates these requirements and is designed to provide repetitive and automatic monitoring of process streams. Its design incorporates the use of three modules, an analyzer, the MC-503 ACM, and a IBM-PC compatible PC. Additional design features provide for easy modification, thereby making the instrument adaptable for most applications which are normally encountered. The essential elements of the AIC instrument are shown schematically in FIGURE 1-2. 1.3.1 CARRIER GAS Since the carrier gas comprises the mobile phase of chromatography, its selection is of the utmost importance if optimum results from the Gas Chromatograph are to be achieved. The carrier gas, first of all, must be inert. It cannot react with the column materials or the components in the process stream. Secondly, because most systems utilize a thermal conductivity detector, the carrier gas should have thermal conductivity properties different from those of the gases to be measured. Since the majority of organic compounds have a thermal conductivity of 3 to 7, hydrogen or helium, with thermal conductivity factors of 50 and 40 respectively, should give the best results. However, because of safety factors, helium is generally preferred. it is a colorless gas, one of the nobel or inert gases, and will neither burn nor explode. Nitrogen, argon, and carbon dioxide are less frequently used in process work since they will cause a decrease in thermal detector sensitivity. In the case of the hydrogen flame ionization detector, almost any gas is acceptable as a carrier.Sod \\ syndyng asnsojg yaD,U0g — —— | a lOW WT nO yu Gz~F < WuDS OL dn SSvdAd | WVAYLS —P¢—, TIN LOIN | Wvaa1s —3—L}-— op IdNWS GNVONVIS sania ‘S5VdAR VEOVIC. WAISAS- [WSS * yun uu09 owes lwaoauNoo]_| £0S-OW1.3.2 DETECTOR Two types of detectors are commonly used in process work; a thermal conductivity detector and a hydrogen flame ionization detector. The thermal conductivity type may use either thermistors or hot wire filaments as the sensing elements. Detectors using the hot wire filament are arranged in a wheatstone bridge configuration with each of the four filaments supported in separate chambers within a metal block. Two of the detectors are continuously exposed to the carrier gas (reference side), while the other pair (active) are exposed to a column effluent comprised of carrier plus separated components (FIGURE 1-3). A highly regulated voltage, supplied by the detector power supply, is placed across the bridge, causing a current to flow through the filaments. The heat produced by this current is conducted away by the carrier gas flowing across the filaments. As long as the detectors see only pure carrier gases, the bridge is balanced and no electrical output is produced. at this point, it is helpful to know that light gases, such as helium, remove heat more efficiently than heavy gases Consequently, when sample mixed with carrier elutes from the column and passes across the active detectors, the temperature of the filaments increases. Since the filaments have a positive temperature coefficient of resistance (their resistance increases with increasing temperature) and since the voltage across the bridge is constant, then the current through the filaments must change, causing an unbalance of the bridge. The unbalance produces a signal which is proportional to the amount of sample crossing the detector. Sensitivity of the detector may be varied by changing the voltage impressed across the bridge. Generally, however, thermal Conductivity detection is used for percentage and highPOWER [+ ‘SUPPLY 4 RECORDER | MATCHED SET OF FILAMENTS conn EFFLUENT N {REFERENCE CARRIER IN FIGURE _I-3 DETECTOR REFERENCE CARRIER OUTparts-per-million range measurements. | The second detector is the hydrogen flame, or ionization detector, in which the sample components eluting from the column are ionized by combustion, and thus produce a current which is then measured. Column effluent is mixed with hydrogen and burned in a teflon chamber. Combustible materials containing carbon atoms produce ions, which are collected by impressing a voltage between the burner tip and a collector. (FIGURE 1-4) The small current set up by this flow of ions is measured by an electrometer amplifier and sent to the ACM. A flame detector is sensitive down to the parts per billion level, while still proving useful in the percentage range as well. Since the device measures ion current, it is sensitive only to those components which produce ions in 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 ten parts per million acetylene, and with almost complete insensitivity to the oxygen or air. 1.3.3 VALVES The sample valves used in AIC instruments are multi-port rotary types operated by a pneumatic air cylinder. Sample wetted parts are constructed of 400 series stainless steel or glass filled teflon, making it resistant to attack by any corrosive materials present in the process stream. The multi-port configuration on the valve permits it to serve the dual function of sample introduction and column switching. Only the more complex applications will require a second valve.Stack Mounting Bracket Collector Cathode and Ignitor Hydrogen In Detector Air In Heater Detector Base Thermostat Detector Heater Block Sample In FIGURE 1-4 FLAME IONIZATION DETECTOR1.3.4 TEMPERATURE CONTROL It is acknowleged that a column is at the heart of a chromatograph's ability to do the job for which it was 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 all column associated functions 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 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 in quick succession and the recorded peaks will crowd together, making resolution difficult. Yet 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. Another consideration is that high column temperatures reduce the life of partition columns because of evaporation of the liquid phase. Such an evaporation will cause the column to deteriorate and produce a decrease in the component retention times. As critical as temperature level is for a column, even more important is the stability of the temperature throughout its operation. Because a process gas chromatograph is often operated unattended for long periods of time, it is vital that there exist a method of temperature control. In the AIC Gas Chromatograph, the various column configurations are installed in a hot air bath. The air bath consists of an insulated oven (analyzer), a heater over which a stream of air is constantly flowing, and an electronic control systemwhich automatically compensates for any temperature shifts. The advantage of such a system is that it eliminates the necessity of placing the various components of the analyzer at equal distances from the heater. The temperature in the air bath analyzer is maintained at +.1° centigrade. 1.4 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. This material may be either an adsorbing agent or a partitioning liquid on an inert support. The column is usually fabricated from stainless steel, though teflon, with its inert chemical characteristics, is enjoying increased use. Small plugs of glass wool in either end of the column retain the packing. Length of the column may vary from a few inches to 30 £t., depending on the application. 1.5 PERFORMANCE FACTORS Once the proper column for a particular application is chosen, its actual performance with regard to resolution, analysis time, and sensitivity must be matched to the customer's requirements by suitable variation of the operating parameters. Predicting the actual performance frequently presents difficulties because the desired performance factors are often mutually incompatible. The fact that measurements are usually made on the basis of peak area often necessitates 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 a major component, if they are to be measured quantitatively. Stability and rapid analysis times, which are required for industrial applications, dictate that tailing effects must be kept to a minimum. This may preclude the use of certain otherwise desirable partition liquids which, because of an excessive vapor pressure, are rapidly lost I-13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 which column is best for a given application follows: 1.5.1 RESOLUTION Within limits, resolution is increased by lengthening the column, reducing the oven temperature or, to a lesser extent reducing the carrier flow rate. ‘These methods 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 a pair of components is poor, it might be feasible to improve it 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 a pair of components is poor on a given column, it is better to look for another column that is more suited to the application. 1.5.2 ANALYSIS TIME Generally speaking, 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 of time. Diffusion effects also tend to be minimized, which results in better reproducibility of peak height. Analysis time decreases with higher temperatures and, (to a lesser extent) with faster 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 to a minimum, then analysis time can be shortened.1.6 GENERAL COLUMN INFORMATION As previously mentioned, there are two types of column packing materials: active solids or inert solids covered with a liquid. The more common adsorption-type columns are activated alumina, silica gel, activated carbon, and molecular sieves. They are normally used for separation of the fixed gases and light hydrocarbons. Unfortunately, adsorption columns are somewhat susceptible to contamination. The commonly used adsorbents strongly adsorb and 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 available for sorption of sample components. Fortunately, the contamination can be reversed by purging the column with dry carrier gas. This procedure is, in effect, 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 Corning Silicon Oil on Firebrick * Carbowax on Firebrick + Oranite on Teflon 1.7 COLUMN PACKING While any original column which is used on an AIC process chromatograph is obtainable on short notice from AIC, occasionally a customer desires to produce his own columns. ‘The degree of difficulty involved ranges from almost none in the case of an adsorption column, to considerable when packing teflon columns with certain partitioning substances. In the case of 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 I-15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 follows: * The importance factor in preparing a partition column is the ratio of the liquid to the solid support. This value is generally known so all that is required is to weigh out the correct amount of liquid and solid support. + Add sufficient solvent (acetone, methanol, ether, etc.) to the liguid phase such that a mixture is produced 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. Be careful not to let the temperature get too high as this might cause the liquid phase to boil off. Once the material is completely dry, it can be packed into a suitable length of 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 stabilized. 1.8 MULTIPLE COLUMNS AND VALVE CONFIGURATIONS With the increasingly complicated separations which process chromatographs are being called upon to perform, 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 a single column is too slow or I-16has other disadvantages. For example, if the sample from the process stream contains elements which are harmful to the column which is responsible for separating the components of major interest, it is advisable to use a second column which will separate the contaminating elements from the primary components before they reach the first column. The contaminates can then be backflushed to vent. There are literally hundreds of different types of column packing materials available today, with additional ones coming into use each year. The resultant possibilities in valve and column configuration are almost staggering in their number. Yet, out of this 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. 1.9 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. Then, 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 technology and other operating parameters, such as peak sequence and time cycle, will be his responsibility. In other words, he will perform the application engineering. I-17While it is impossible in this brief section to provide a complete discussion of the variables affecting the operation of a chromatograph, we will nevertheless consider some of the basic principles of the operating process. Once the units of the 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 this manual, and the instrument is made 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 have too much separation then the temperature of the analyzer may be raised and/or the carrier gas flow rate increased. If, on the other hand, resolution is poor, then temperature and flow rate might be decreased. Another area of possible adjustment is sensitivity. If peak height was inadequate, then it might be desirable to increase the bridge voltage. The normal operating voltage range of the bridge is between 8 and 12 volts, but high values are permissible. There is a limit, however, in that too high a bridge voltage will increase noise and decrease the filament lifespan from overheating. an alternative is to simply increase the sample size. This is accomplished by changing the sample loop on the gas sampling valve or the sampic 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 instance, a single and precut configuration is designed to precut or remove certain components of the sample and prevent them from entering the main I-18column. In order to accomplish this function, the valve is de- energized when the components of interest have eluted from the precut column. The importance of timing is obvious. If the valve is not de-energized quickly enough, components which might clog up or damage the main column are permitted to elute. Precutting too soon, on the other hand, might prevent a peak of interest from eluting. Several manual chromatographic analyses are run 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 accordingly, regulating the operation of the entire chromatographic installation. 1.10 THE PROCESS CHROMATOGRAPH Because of the environment in which it is often situated, a process chromatograph must be rugged, resistant to corrosion, and suitable for use around explosive gases. Also, because it is often operated for long periods unattended, it should be completely automatic. The purpose of a gas chromatograph is to analyze a process stream, so, for increased efficiency, the unit should be located as close as possible to the sample source. Yet, 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 presentation system. 1.10.1 THE ANALYZER Just as the column is the heart of an analyzer, the analyzer might be considered the heart of the gas chromatograph. The components which are primarily responsible for performing the chromatographic analysis, the sample valve, columns, and detector, are located in the analyzer. In addition, methods of controlling theparameters of flow and temperature, which affect these primary elements, are situated at the analyzer. Because the analyzer is designed to operate in hazardous areas, it's electrical components are installed in explosion proof enclosures. Also, the analyzer is designed to accommodate additional valves and columns, thereby enlarging the number of applications for which it might be suitable. 1.10.2 THE CONTROL UNIT The unit is microprocessor controlled with a crystal time base, all solid state, 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. Programmed functions incorporated into 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 long term drift. Input for the MC-503 may be from either 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. 1.10.3 ourpurs The MC-503 interfaces with an IBM PC-AT compatible through a standard RS-232 port or current loop serial port. A hard copy of all analysis may be obtained through a parallel printer. Also available are up to I-20thirty two (32) 4-20 ma outputs for trend recording or closed loop control. 1.10.4 SAMPLE SYSTEMS In order for the accurate and reliable analysis of which a chromatograph is capable, it is necessary that the 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. There are often more considerations to the design of satisfactory sample system than meets the eye. 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 dirt or other particulate matter. + Filter out fogs, mists, or aerosols. * Vaporize liquid samples. + Prevent vapor samples from condensing. * Measure and control pressure and flow through the analyzer. + Remove an unwanted component. * Provide means for introduction of calibration standards.+ Provide means for analyzing more than one stream with one analyzer. The AIC sample conditioning system is designed to assist the analyzer in performing the specific job for which the chromatograph system, of which it is a part, was sold. Various degrees of sophistication are available, but basically, each sample system regulates pressures, filters and controls the flow of the streams to the analyzer, and admits a calibration standard either manually or by means of a valve controlled from the programmer. Generally, the AIC sample system is mounted on a rack with the analyzer directly above it. 1.11 PROBLEMS IN CHROMATOGRAPHY As might be expected of an instrument with such numerous application possibilities, problems are sometimes encountered. Generally, these difficulties are the result 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 there. These unexpected elements 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 the problem, it may be necessary to substitute a different column, or to adjust the parameters of flow, pressure and temperature. If, when the original application engineering is performed, a plant sample is available, it is possible to minimize the possibility of such problems occurring. A gas chromatograph is not an absolute standard, and hence must be calibrated against a sample of known composition. If the standard sample is in error, then obviously the chromatographic analysis will be in error.Another factor greatly affecting instrument accuracy is what might be called sample condition. A chromatograph column is designed to accept only vapor samples. However, since the chromatograph is obliged to monitor both gas and liquid process streams, it is necessary to vaporize the liquid sample so that it is acceptable to the column. If this vaporization process is incomplete, then the volume of the samples will not be repetitive and large inaccuracies in measurement will result. The same difficulties can occur with a vapor stream. If any condensation occurs, the sample will not be in a single phase and measurement errors will again be the result. To prevent vaporization or condensation, it may be necessary to cool or heat the sample lines. Steam tracing normally provides the heat source. However, if the tracing is not done correctly, cold spots may develop, with the resulting condensation of sample.InstallationSECTION IT INSTALLATION 2.1 GENERAL This section contains information pertaining to the installation procedure for the AIC Model MC-503 Chromatograph System consisting of: PC, Monitor, Printer, Analyzer Control Module(s), Requested Analog Output(s), Multiplexer, Model 600 Analyzer and Model 700 Sample System. Also included are standard terms and conditions 2.2 SHIPMENT 2.2.1 Estimates as to shipment are based on conditions prevailing at date of quotation. Shipment will be scheduled after acceptance of order in conformance with Customer's requirements as far as possible, but may require adjustments. All agreements as to shipment are subject to the contingency of strikes fires or other causes of delay beyond AIC's control. 2.2.2 Shipments made F.0.B. AIC's plant shall be at the risk of the Customer who shall make all claims to the carrier in the event of damage to shipped material or losses in transit. Customer shall notify AIC in writing of any shortage within ten (10) days from receipt of shipment. 2.3 PAYMENT Net payment is due on date of shipment and payable within thirty (30) days thereof, unless otherwise specified. Price is F.0.B AIC's plant, unless otherwise agreed. Interest will be charged at the rate of 1.5% per month on overdue accounts. II-12.4 WARRANTY AIC warrants the articles delivered hereunder will be merchantable, of good material and workmanship, free from defect at the time of shipment, and that AIC will repair or replace, at AIC's option, any defect in material or workmanship proved defective within a period ef one (1) year from shipment with the following exception + Peripheral equipment (PC's, printers, etc.) is subject to standard warranty of the manufacturer. The terms of our purchases provide for such warranties to be extended to our Customers. + Expendable items (detector filaments, valve seats, filter elements, regulator diaphragms, lamps, etc.) are not warranted and AIC does not agree to replace these. All claims under Warranty are subject to written notice within the warranty period to AIC. AIC reserves the right to make changes in design of its products at any time without incurring any obligation to make equivalent changes to existing equipment. 2.5 CONTROL ROOM PANEL MOUNTED COMPONENTS The AIC Model MC-503 is designed for panel mounting in a non- hazardous location, such as a plant control room. For optimum performance, the environment should be non-corrosive, dry and dust- free. Temperature should be reasonably constant, but it is not necessary that the room be air conditioned. Testing of the units, before shipment, has been carried out at the environmental conditions existing in Houston, Texas throughout the year. The mounting procedure is as follows: * Make Panel cutouts in accordance with the shape and dimensions specified on Figures 2-1, 2-2, 2-3 and 2-4.¥608-¥ | 1nO-1ND SSRUNOI Id 1-@ 3unold mlacd = “a seo SHER —__ val “wisn ronan svowasn wana | LV (SAIL 9 “dAL) cf-Ol SS¥d peewee denne ee eee eee b-------2------2-+ 1 ——#. @ i w/t =22 Band “TaNVd ONIH39 O3YINORY SONVAVSTO 2 sow (SAWIL 8 “dAL) ‘vid SZ" NO YSLNIYd VLVGINO GSLNNOW TANWdTheue g auatvusaus a 8008-V ABY| waenan onmvuo| —— 40-19 SINGOW IOLNOD HAZATVNY £0S OW suosnouuy] B/E, 809 senmvual _srv2¢] SVX3L NOLSNOH Orv NOIVYOdOD — SLNSWNYISNI AVOILATVNY, “LHOIM BLVWIXONddY $8122 > <8/2 © 2dOL 316UL' ,b/1 Y= ANNOW NOVY -Y “W3ACO LNON4 WOW JO SNOISN3WIO 'E “ZONVAVEIO NV3Y 61 LSV37 LY MOTI 2 (91/3 S310H TAv1 :S310N € 3LON 33S 61 Lf INO-iN9 8-2 gandu 11-5 € 3LON 2A P/ BI| een) —_LNOLND 140 re nar i a [al wes F—— ‘(SINIL 9 WOldAL) “WIG SZ’ STIOH Thy “ALON 00'| —~| | oo ot 00'S ot ood 1 00°C ns ose +} 001. ———+| LAOLAD INNON TAN¥d LYo+ Upon completion of panel cutouts, proceed to slide the cabinets into the panel from the front. + Secure cabinets to panel as indicated. When locating the panel cutout, it should be remembered that electrical connections to the various units are made at the rear of the instruments, consequently, sufficient room should be left around the rear of the various components for working and interconnecting. 2.5.1 PC The MC-503 PC is provided in a fortress cabinet for panel mounting. The cabinet comes with a key for the user's Protection. The MC-503 PC/Programmer Unit is capable via a multiplexer of the simultaneous operation of up to ten (10) analyzers, with simultaneous presentation of information via a monitor and printer. Dimensions of the panel cutout and mounting information are given in Figure 2-1. The electrical interconnection of the various components of the system is depicted by the interconnecting wiring diagram B-200202 located in the modifications section of this manual. Careful attention to this schematic will ensure correct interconnection of the unit. Additional information on electrical installation will be found in part 2.10 of this section. 2.5.2 MONITOR It should be installed as close as possible to the PC, preferably right above it. Dimensions of the panel cutout and mounting information are given in Figure 2-4. The electrical interconnecting details are found in Drawing B-200202. I-72.5.3 PRINTER The printer used with the NC-503 is the Okidata 320. Dimensions of the panel cutout and mounting information are given on Figure 2-2. The electrical interconnecting details are found in Drawing B-80116-1. 2.5.4 ANALYZER CONTROL MODULE The Analyzer Control Module(s), up to ten (10) without analog output board(s), up to nine (9) with analog output boards, should be installed as close as possible to the PC, preferably next to it. For remote locations of the ACM's, the maximum permissible distance is 1000 feet with 4 wire link connection to the multiplexer. For optimum performance, the environment should be non-corrosive, dry and dust-free. | Temperature should be reasonably constant, but it is not necessary that the room be air conditioned. Optional recorder plug at each ACM provides for recording of detector output chromatograms in the event the PC is down. Normal operation and storage of data take place while PC is not in operation. Dimensions of the panel cutout and mounting information are given on Figure 2-3. 2.5.5 MULTIPLEXER The Multiplexer and 5 feet of interconnecting cable are provided for mounting in the vicinity of the PC. 2.5.6 ANALOG OUTPUTS/LATCH The latch board(s), up to two (2), providing up to thirty-two (32) analog outputs, should be installed as close as possible to the PC, preferably next to it. For remote locations of the latch board(s) the maximum permissible distance is 1000 feet with 4 wire link connection to the multiplexer. This allows the latch board(s) to be apart a maximum distance of 2000 feet away TI-8from the ACM's. For optimum performance, the environment should be non-corrosive, dry and dust-free. Temperature should be reasonably constant, but it is not necessary that the room be air conditioned. Dimensions of the panel cutout and mounting information is the same as the ACM's and are given on Figure 2-3. 2.6 ANALYZER The AIC Model 600 Analyzer is contained in a weatherproof housing, but shelter should be provided to protect the analyzer from direct exposure to weather elements. The mounting site should be as free from vibration as possible, and as close as practical to the process stream in order to ensure rapid instrument response. Attach the analyzer to any sturdy support (such as a rack or wall), in accordance with the installation recommendations drawing. Make certain to leave sufficient clear area around the unit to permit easy access for adjustment and maintenance. The following utilities are required for operation of the analyzer: Electrical Power: 115 VAC, 60 cycles, 10 amps Instrument Air: 50 psig at the analyzer. 4 CEM Supply. Carrier Gas: Standard 1A cylinder of the appropriate gas. It is vital that the gas be absolutely dry and of chromatograph grade/quality. Sample Preparation If the AIC sample system is not used, then the customer must arrange for proper sample preparation between the process stream and the analyzer. II-92.7. SAMPLE SYSTEM The AIC Model 700 Sample System is generally mounted on the rack or frame which contains the analyzer. It should be located as close as possible to the process streams, and each sample line led to the sample box must have a bypass loop. The sample in and bypass lines are 1/4" SS tubing, and the pressure differential between the two should be at least 10 psig. Maximum permissible sample-in pressure to the sample box is based on the Sample System design. Refer to the sample system drawing in the Modification Section. 2.8 INITIAL CHECKOUT 2.8.1 Each AIC Analyzer is carefully checked out before it leaves the plant. However, during shipment, especially if over a long distance, it is possible for damage to occur. Consequently, after the analyzer has been uncrated and mounted, the following checkout procedure should be observed: + Make certain that the heater condulet, detector condulet, sample valves and regulator(s) have not vibrated loose during shipment. + Check all tubing fittings for tightness. + Check that the wires connected to terminal board TB-201 and B-202 are all securely fastened. If any have some loose, refer to the analyzer schematic B-200202 for proper connections. * Check all sealing unilets for chico packing. + Ascertain that all pressure gauges are reading zero. TI-102.8.2 CARRIER GAS CONNECTIONS When helium is used as the carrier gas, high purity (reactor grade) with a dew point of -60°F is recommended. If nitrogen or argon are used, a purity of 99.99% is required. Whatever carrier gas is used, the cylinder should be located in a shaded area, and attached to a post or column to prevent it from being knocked over. A 1A cylinder is often pressured to 2500 psig and the results of a hard impact could be catastrophic. + Equip the carrier gas cylinder with a dual stage regulator. The primary side of the regulator should have a pressure range from 0 to 3000 psig, and the secondary stage a range of 0 to 300 psig. + It is recommended that a molecular sieve dryer be installed between the carrier gas cylinder and the carrier in position on the analyzer. This device is often included in the order, but if not, it should be considered. only pipe thread and Swagelok fittings should be used since quick-disconnect and hose fittings are susceptible to leaks. + Connect the carrier gas cylinder to the analyzer. Figure 2-5 depicts a standard flow diagram for a carrier gas hook up. + Open the main valve on the carrier gas cylinder. Adjust the regulator until the secondary stage pressure is 100 psig. Check the system thoroughly for leaks. I-11CARRIER REGULATOR (MOUNTED ON ANALYZER) REVISED 10/9/06 ANALYZER, ---- STREAM SAMPLE THREE WAY (SOLENOID ACTUATED FOR AUTOMATIC WALVE CALIBRATION ONLY) PRESSURE, GAGE SHUTOFF NEEDLE VALVE VALVE CALIBRATION SAMPLE SHUTOFF VALVE DUAL ,STAGE REGULATOR. beeen 3000" Primary DUAL 300# SECONDARY STAGE, REGULATOR 3000* Primary SUTOFF 3008 SECONDARY VALVE CARRIER CARRIER, CYLINDER CYLINDER FIGURE 2-5 CARRIER GAS FLOW DIAGRAM Dual Manifold Automatic Switch Over II-122.8.3 SAMPLE GAS CONNECTION ‘The type of sample gas connections made to the analyzer are dictated by the type of application and the specific installation. For example, if the chromatograph includes an AIC sample system, then the sample connection to the analyzer will require only that a length of tubing (generally 1/8" Ss) be run from the sample box to the analyzer. Normally, the two units are ordered mounted together on a rack, and the interconnecting is done by AIC at the factory. If use of a calibration gas is desired, and there is not a sample system, then connect a cylinder of this gas to a manifold (not supplied by AIC). 2.8.4 INSTRUMENT AIR Instrument air at a pressure of 50 psig into the analyzer is required for actuation of the sample valve and for analyzer heating. Small amounts of moisture in the air will not affect the instrument, but corrosive gases (such as H,S, SO,, or CL,) must be removed. The air-in fitting is 1/4" Swagelok, and is on the side of the analyzer. (Refer to the analyzer drawing in the modification section of this manual.) 2.8.5 VENT LINES The analyzer will generally have three vent lines, depending upon the application. ‘hese are column out, vent and sample out. The first two, column out and vent, are 1/4" tubing and are generally allowed to flow to atmosphere unless a flammable carrier is used. When a vent is utilized, extreme care should be taken to see that it is large enough to avoid back pressure. If there is a chance of condensation, then steam tracing or a trap should be incorporated. II-13The third exhaust is the sample out connection, and it is also essential that this exhaust be connected to a vent of sufficient capacity to minimize back pressure. 2.8.6 ELECTRICAL INSTALLATION The control unit and analyzers are interconnected by wiring that is normally run through conduit, and which must be installed in accordance with local code requirements. Instructions for the interconnection are given by the interconnecting wiring diagram B-200202, located in the modification section of this manual. This wiring is not supplied by AIC unless ordered at the time of instrument purchase. The following recommendations should be observed when performing the electrical installation: + Refer to B-200202, interconnecting wiring schematic before installing conduit or wire. + Note that all detector bridge, signal and proportional temperature control wiring is shielded, and observe instructions for connection of shields. + It is recommended that the chromatograph be installed on its own 15 amp circuit. + If line voltage fluctuations are expected, it is advisable to use a SOLA regulation transformer. I-14AnalyzerSECTION III ANALYZER 3.1 INTRODUCTION The analyzer is generally considered to be the heart of a process chromatograph system. As stated in Section I, it is the analyzer 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 pushes the sample through the column, where it is separated into its individual components. these components then elute in the inverse order of their affinity for the column packing material (whether it is adsorbent or absorbent) and pass 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 the parameters of carrier flow and column temperature. © Since elution time identifies each component qualitatively, and since all automatic programming functions are based on this information, then the necessity of precisely controlling carrier flow and oven temperature is obvious. Basically, then, an analyzer (FIGURE 3-1 and FIGURE 3-2 at the end of this Section) consists of a box type air bath unit with precise temperature control, a detector, and columns and valves for a specific application. On the AIC Model 600 analyzer, the regulators and pressure gauges are mounted outside where they are readily available for adjustment and viewing. The detector, valve and columns, on the other hand, are located inside the analyzer where they may benefit from a constant temperature environment. All automatic functions regulating the operation of the analyzer are controlled from the PC. III-13.1.1 CARRIER GAS FLOW SYSTEM In theory, any gas which is not a component of the sample being monitored may be used as a carrier. Actually, however, only a few gases make efficient carriers with Helium, because of its inertness and high thermal conductivity, being the most frequently used. Whatever gas is used, its flow rate must be adjustable over a wide range in order to control the elution rate. At the same time, it is necessary that the flow be kept constant throughout an 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 3-1), where it is controlled to within about 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 pound pressure gauge is also attached to this port and hence measures carrier gas pressure on 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 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 of 40-50 psig at the analyzer is required. The air is used for heating and actuation of sample introduction and column switching valves (FIGURE 3-1). III-2