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Publication numberUS2977471 A
Publication typeGrant
Publication dateMar 28, 1961
Filing dateSep 25, 1958
Priority dateSep 25, 1958
Publication numberUS 2977471 A, US 2977471A, US-A-2977471, US2977471 A, US2977471A
InventorsWagner Ernest E, Young Howard A
Original AssigneeSocony Mobil Oil Co Inc
Export CitationBiBTeX, EndNote, RefMan
External Links: USPTO, USPTO Assignment, Espacenet
Apparatus for automatically operating a mass spectrometer
US 2977471 A
Abstract  available in
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Claims  available in
Description  (OCR text may contain errors)

March 28, 1961 H. A. YOUNG EIAL 2,977,471

APPARATUS FOR AUTOMATICALLY OPERATING A MASS SPECTROMETER Flled Sept. 25, 1958 5 Sheets-Sheet 1 VALVE CONT/P01.

NIINOME T [R FIN/H YZf TUBE .S/IMPLE 200 HOT BOTTLE SAMPIE 00 RR n2 Ill 226 INVENTORS ErnesTdE/Xwcgner owor oun F I 6. lo g RNEY March 28, 1961 H. A. YOUNG EI'AL 2,977,471

APPARATUS FOR AUTOMATICALLY OPERATING A MASS SPECTROMETER Filed Sept. 25, 1-958 5 Sheets-Sheet 2 Ernest E.Wogner ATTORNEY March 28,1961 H. A. YOUNG ETAL 2,977,471

APPARATUS FOR AUTOMATICALLY OPERATING A MASS SPECTROMETER Filed Sept. 25, 1958 5 Sheets-Sheet 3 P RS UWY Tm. cn EFG STANDBY IIEMILL'JUPPZ) jw ATTORNEY DEF GHJK DE GHJKL March 28, 1961 H A YOUNG r 2,977,471

APPARATUS TOR AUTOMATICALLY OPERATING A MASS SPECTROMETER Filed Sept. 25, 1958 y 5 ShOG'CS-ShGQtA I INVENTORS Ernest E.Wogner Howard .Younq FIG-Id b wa) ATTORN EY FF es HH JJ KK LL March 28, 1961 H YOUNG r 2,977,471

APPARATUS FOR AUTOMATICALLY OPERATING A MASS SPECTROMETER Filed Sept. 25, 1958 5 Sheets-Sheet 5 INVENTO gcsm Ernesr E.W0gner Fl Howard A.Youn% United States Patent APPARATUS FOR AUTOMATICALLY OPERATING A MASS SPECTROMETER Howard A. Young and Ernest E. Wagner, Beaumont, Tex., assignors, by mesne assignments, to Socony Mobil Oil Company, Inc., New York, N.Y., a corporation of New York Filed Sept. 25, 1958, Ser. No. 763,367

3 Claims. (Cl. 250-419) This invention relates to mass spectrometers and, more particularly, to a method and apparatus for automatically operating a mass spectrometer.

Heretodore mass spectrometers have been operated manually in accordance with a programmed sequence of operations which require the constant attention of an operator.

This invention has for its object the provision of means whereby a program of operation for a mass spectrometer may be set up and thereafter the mass spectrometer may proceed through its entire sequence of operation, from taking of sample, through scanning and associated operations, and finally purging and returning to standby condition, all without the intervention of an operator except to make sample material available and to initiate the operation.

In order that the instant invention may be more readily understood it will be described as specifically applied to a mass spectrometer of the type sold by Consolidated Engineering Corporation, Pasadena, California. It is to be understood, however, that by minor adjustments, which become apparent as the description proceeds, this invention finds application to the operation of other types of mass spectrometers.

Figure 1A is a diagrammatic illustration of sample handling apparatus and control elements associated therewith; i

Fig. 1B is a schematic wiring diagram showing the programming elements and electrical circuitry associated therewith; V

Figure 1C is a schematic diagram showing the control panel and the electrical circuitry that is associated with it;

Figure 1D illustrates schematically two portions of a conventional mass spectrometer and novel control circuits forming a part of the present invention applied thereto; and

Figure 1E illustrates two additional portions of a conventional mass spectrometer and additional novel'control circuits applied thereto.

Referring to the drawings, the various sheets, when placed side by side in their proper order, will show schematically, as though in a single figure, the entire control circuitry for rendering a mass spectrometer fully automatic in its operation and enough of the circuitry of a mass spectrometer to show the points of vapplication of the control circuitry.

In Figure 1A there is shown schematically sample handling apparatus for use in conducting both coldbottle" analysis and hot bottle" analysis. By cold bottle analysis is meant an analysis of a sample which, at normal temperature and pressure, is in gaseous form, such as hydrogen, helium and hydrocarbons involving one to seven carbon atoms. A hot bottle analysis will be used in reference to type analyses of hydrocarbons which are liquid at normal temperature and pressure, such as, gasoline, fuel oil, kerosene, gas oils, or anything, having six or more carbon atoms, which must be heated to vaporize itbefore analysis;

- sample for analysis. Switch 18 provides means whereby ice A sample which, at normal temperature and pressure, is in gaseous form contained in the sample flask 200, is metered into the constant volume and constant pressure chamber 201 and the cold bottle 202 by a solenoid operated valve 203, which is controlled by manometer 204.

Valve 201A is then closed manually. The sample, which is undergoing analysis, passes through the solenoid op-,

erated valve 82 and leak 205 into the analyzer tube 206. The control of the operation of valve 82 will be described later in connection with the main spectrometer control circuitry. When the sample, which is normally in gaseous form, is undergoing analysis, solenoid operated valves 207 and 208 and valve 209 are closed, thereby confining the sample to the constant volume and constant pressure chamber 201 and the cold bottle 202. Valves 207 and 208 are automatically operated after the analysis has been completed to evacuate the constant volume and contion of valve 213 is controlled by the manometer 214.

The vaporized sample passes from the manifold 212 through the solenoid operated valve 215 into the hot bottle 216 and valve 212A is manually closed. Then manually operated valve 209 is opened and the sample passes through valve 209 and the leak 217 into the analyzer tube 206. All of the solenoid operated valves are supplied with power from the power busses 83 and 218 by means of double pole, double throw switches, which are shown in the positions that they would occupy during automatic operation of the spectrometer.

As shown in Figure 1C, the control panel consists of four switches and five pilot lights, a power pilot light'10, associated with the power on-oif switch 11, which, in turn,

is supplied with power from a conventional alternating shown schematically in' Figure 1A, is underway. Pilot light 16, when lighted, signals that a scanning operation is underway. Pilot light 17 signals the completion of the pump-out of the sample manifold and indicates to the operator that the system is in condition to receive a new any one of six analyses may be selected. Although switch 18 is shown as a three-deck, three-pole, twelve positionswitch, only the first six positions of each deck are used.

When'the contactors are in the position shown, on the first contact points, molecular masses H through C 'will tion, masses C through C will automatically be scanned;

when rotated to the third position, masses C through C will be scanned; when advanced to the fourth position, masses C through C will be scanned; when in the fifth position, masses C through C are scanned; and when in the sixth position, a type analysis is automatically made. By type analysis is meant the analysis of hydrocarbons. such as gasoline, fuel oils, kerosene, gas oils, or anything C or heavier that is normally in liquid form, and must be heated to vaporize it for analysis. The manner in which this novel control circuit performs automatically the se-;

quence of steps to scan a sample H through G; will first be described.

When switch 18 is on its first position, as shown, and switch 14 turned to the automatic position, power is then turned on by switch 11. Moving switch 14 to the automatic position, one step in a clockwise direction, simultaneously operates the solenoid valve 82, shown in Figure 1A, to bleed a hydrocarbon sample through a magnetic field to ionize it. The circuits employed to open the solenoid valve 82 includes the conductor QQ, which is connected to the power supply bus 83, the contacts on switch 14C, conductor PP, the bottom points 108 of relay XIII, conductor MM, contacts on switch 148, conductor NN, conductors 220 and power bus 218. Switch 19, a double pole, single throw, push button type, that normally remains in an open position, is pressed to close position to start the operation of the control circuits. The depression of this switch energizes timing motor M1 through switch 11, conductor A, switch 14C, conductor 20, switch 19, conductor 21, switch 13B, conductor D and conductor B. Timing motor M1, a one r.p.rn. motor, drives a rotatable drum which actuates switches 22, 23, 24, 25, 26 and 27 in a predetermined timed sequence to energize other circuits to be described hereafter. Timing motor M1 is one of five similar motors. Each of these motors drives a rotatable drum having switch actuating means carried thereby. The drum driven by timing motor M2, a one r.p.m. motor, operates switches 28, 29, 30, 31, 32 and 33. The drum driven by timing motor M3, a rpm. motor, operates switches 34, 35, 36, 37, 38 and 39. The drum driven by timing motor M4, a rpm. motor, operates switches 40, 41, 42, 43 and 44. The drum driven by timing motor M5, a /6 rpm. motor, operates switches 45, 46, 47 and 48.

Switch 19 is held in its depressed position until timing motor M1 has rotated its switch actuating drum sufliciently far that the switch 22 is closed to provide another power circuit for timing motor M1 which does not depend for completion upon switch 19. This new power circuit for timing motor M1 includes the switch 11, conductor A and the switch 22. At the same time that the timing motor M1 was started, relay I was energized by means of switch 19, conductors 49 and 50, switch 18C and conductor C to open contact points 51 to break a circuit to turn oif the standby pilot light 17. This circuit includes switch 11, conductor B, the standby pilot light 17, conductor 52, switch 14C, conductor G, conductor 53, switch 35, conductor 54, switch 41, conductor 55, switch 45 and conductor 56 which connects with the auxiliary power circuit completed by switch 22 during the first rotational movement of timing motor M1. At the same time that the points 51 on relay I are opened, points 57 are closed to complete a holding circuit for relay I so that it will not knock-out when the push button 19 is released. This holding circuit includes the conductors 73 and 74, the switch 45 and conductor 56, which connects with the power supply conductor A at switch 22. This holding circuit also maintains the scanning light 16. which is in parallel with the coil of relay I, lighted. Since the scanning pilot light 16 is connected in parallel with the actuating coil of relay I, it will be turned on at the same time that the relay is actuated and will remain on until this relay is de-energized. The scanning light circuit includes the switch 19, conductor 49, switch 14A, conductor 114, the scanning light 16 and conductor B. As timing motor M1 continues to drive the switch actuating drum, switch 23 Will be opened to open a shunt comprising conductors P and Q, which shunts a resistance 94, shown in Figure 1D of the drawings, that is in the circuit which supplies current to energize the electromagnet in the mass spectrometer. Opening switch 23 in effect removes this shunt and the resistance 94 becomes operative to reduce the magnetic field so that masses, including hydrogen and helium, may be scanned. Further rotation of the switch actuating drum by timing motor M1 will close switch 24 to energize relays VI, V11 and VIII. With switch 24 closed, actuating coils of relays VI, VII and VIII receive power through switch 11, conductor A, conductor 75, points 68 of relay XI, conductor 84, conductor 85, switch 24, conductor 86, the respective windings of relays VI, VII and VIII, conductors '87, 88 and 89 respectively, which connect to conductor B, which returns to the switch 11 and the power supply. Relay VI will close points 58 to complete holding circuits for these relays. Points 59 of relay VI will close to complete a mass marker circuit in the mass spectrometer through conductors DD and 11. Relay VII will close points 60 and 61 to turn on the galvanometer in the mass spectrometer. The closing of points 60 completes a circuit which involves conductors W and X while breaking the manual operating circuit which includes conductors X and Y which circuit is used when switch 14 is turned to the manual operation position. Points 61 close a circuit which involves conductors T and U while opening a circuit involving conductors U and V, the latter circuit being needed for manual operation when switch 14 is turned to the manual operation position. Relay VIII will close points 62 and 63, to, in effect, close mass marker switches in the mass spectrometer. Closing of points 62 completes a circuit which involves conductors GG and HH while closing of points 63 completes a second circuit through conductors EE and FF. Further rotation of the switch actuating drum, driven by timing motor M1, will next close switch 25 to energize relays IX and X. The bottom point of switch 25 receives power through conductor in the same way that the bottom point of switch 24 received it. The other side of switch 25 is connected by conductor to the windings of relays IX and X. The other side of the windings are connected respectively to conductors 87 and 88, which return to the power supply by way of conductor B. Relay IX will close points 64 to complete holding circuits for these relays. Since switch 18 is on its first position, the opening of points 65 serves no purpose. However, the closing of points 66 by relay X will turn on the camera or recorder in the mass spectrometer by completing a circuit involving conductors R and S. Relay IX opens contacts 67 to remove the charging potential from the scanning voltage condenser 97 within the mass spectrometer. This, in effect, disconnects conductors CC and Z, which complete the power circuit for charging the sweep condenser 97. Removing the charge potential from the sweep condenser 97 permits it to discharge through a resistance to produce a decaying scanning voltage that is applied to the analyzer tube electrodes. This operation starts the scan of hydrogen through helium. After the elapse of a period of time that is sufliciently long to scan mass #2, switch 26 will be closed by the actuating drum driven by timing motor M1 to complete a circuit through the coil of relay XI to supply power thereto to actuate it. This circuit includes the conductor A, conductor 92, switch 26, condoctor 91, the coil of relay XI and conductor 87, which returns to the power supply through conductor B. The actuation of relay XI opens the switch points 68 to deenergize relays VI to X inclusive and return all switches controlling the mass spectrometer to their normal position. In the meantime, switch 23 will have closed to again shunt the resistance 94 in the electromagnet circuit of the mass spectrometer. Further rotation of the switch actuating drum, driven by timing motor M1, will close switch 27 to energize relay II and start timing motors M2 and M3. Power will be supplied to timing motor M2 by the conductor A, switch 22, conductor 92, switch 27, conductor 93 and conductor B. Simultaneously with the supplying of power to timing motor M2 to initiate its operation, a circuit is closed to energize relay II. This circuit includes the conductor 77, which is connected to conductor 93 at one terminus and to the points 65 of relay X at its other terminus. From these points,

points 70 completes a power circuit for timing motor M3. 7

This circuit includes the switch 11, conductor B, timing motor M3, conductor 81, points 70 of relay II, points '80 of relay III, conductors 79 and 84, points 68 of relay XI, conductor 75 and conductor A, which is connected to switch 11 and the power supply mains.

The initial rotational movement of timing motors M2 and M3 will close switches 28 and 34 to complete auxiliary power circuits for these motors so that they will not be turned off when timing motor M1 completes its cycle. These auxiliary circuits include the conductors 56, 92 and A. At the same time that the switches 28 and 34 are closed, switch 35 is opened to break the circuit which supplies power to the standby pilot light so that it will not be turned on when relay I is tie-energized. Further rotation of timing motor M2 will close switches 29 and 30 substantially simultaneously to energize relays IV and V. The coil of relay IV is energized through a circuit which involves conductor A, conductor 75, conductor 99, points 100 of relay III, conductor 101, switch 29, conductor 102, the winding of relay IV, conductor 1 87 and conductor B. Relay V is energized through a circuit which involves conductor B, conductor 88, the coil of relay V, conductor 103, switch 30, conductor 104, conductor 93, switch 28, conductor 56, conductor 92 and conductor A, which leads to switch 11 and the power supply mains. These relays serve to select the desired scanning voltage that is used to charge the sweep voltage condenser 97 in the mass spectrometer. Closing of the top switch points of these two relays complete holding circuits for them. The actuation of relays IV and V .will move the armatures 71 and 72 to their up position, thereby breaking the low voltage charging circuit which was used to charge the sweep condenser 97 for the hydrogen through helium scan and select the highest voltage used to charge the sweep condenser for the C through 0; mass scan. Armature 72, when moved to the up position, produces no effect since its circuit is completed through the bottom points of relay IV, which were opened when armature 71 was moved to its up position. Further rotation of timing motor M2 will close switch 31 to energize relays VI, VII and VIII to turn on mass marker switches and galvanometer switches in the mass spectrometer in the manner described above in connection with the hydrogen through helium scan. The energizing circuit for these relays includes conductor A, conductor 75, points 68 of relay XI, conductor 84, conductor 105, switch 31, conductor "36, the windings of relays VI, VII and VIII. The other side of these windings are respectively connected by conductors 87, 88 and 89 to conductor B, which leads back to switch 11 and the power supply mains. Switch 32 is next closed momentarily to reset the mass marker in the spectrometer. This operation is carried out through a circuit which includes conductors KK and LL. Further rotation of timing motor M2 closes switch 33 to energize relays IX and X. The actuation of relays IX and X, in the manner described above, completes their holding circuits, turns on the camera and opens the sweep condenser 97 charging circuit to start the C through C scan. Timing motor M3, being a 1/10 revolution per minute motor, next closes switches 36 and 37. However, since switch 18 is on its first position, the operation of these switches produces no eiiect. At the end of a period of time that is sufficiently long for scanning masses C through C switch 3 8 is closed by timing motor M3 to end thescan by energizing relay XI to knock out relays IV to X inclusive to, in effect, return all mass spectrometer switches to their normal position.

ti Further rotation of the switch'actuating drum, that is driven by timing motor M3, will close switch 39 to actuate relay XII. The closing of switch 39 completes a power circuit for the Winding of relay XII, which includes the conductor 116, the winding of the relay conductor 87 and conductor B which returns to switch 11 and the power supply mains. The bottom points of relay XII complete a power circuit to start timing motor M5, which is connected in parallel with the evacuating pilot light 15. The circuit includes conductor A, conductor 75, the bottom points of relay XII, conductor 106,.timing motor M5 and conductor B. The power circuit for the evacuating pilot light 15 includes conductor B, pilot light 15, conductor 107, points on switch 14C and conductor N. The initial rotational movement of the drum, driven by timing motor M5, actuates switch 45 to complete a holding circuit for relay XII so that it will not be de-energized when timing motor M3 reaches the end'of its cycle. The actuation of switch 45 also breaks the holding circuit for relay I. Knocking out relay I turns 01f the scanning pilot light 16 and completes a circuit through the points 51 whereby the standby pilot light 17 can be turned on at a later programmed time. The switch actuating drum, which is driven by timing motor M5, simultaneously with the actuation of switch 45, opens switch 46 to pump out the sample manifold. Opening switch 46 breaks a power circuit that controls the manifold solenoid actuated valve 207 shown in Figure 1A. This circuit includes bus 83, conductor QQ, contact points on switch 14C, conductor PP, points 108 on relay XIII, conductor 109, conductor 110, switch 46, conductor 111and conductors 22.1. Approximately fifteen seconds thereafter, switch 47 is closed to pump out the sample bottle 202 shown in Figure 1A. This completes a power circuit for opening the solenoid valve 208 shown in Figure 1A. This circuit includes the bus $3, conductor QQ, points on switch 14C, conductor PP, points 108 on relay XIII, conductor 109, switch 47, conductor 112, conductor 222, conductors 223. and the power bus 218. The switches actuated by timing motor M5 remain in this position for a period of approximately five minutes and 45 seconds, this being the time required to pump out the cold bottle 202. At the end of this period, the switch actuating drum, driven by timing motor M5, opens switch 47 and, five seconds thereafter, switch 46 closes. This allows the manifold to be pumped out to accommodate a new sample which can be metered and trapped in the constant volume and constant pressure chamber 201 ready to be expanded into the cold bottle 202, from which it can be discharged through the leak 205 pro: vided and be ionized for analysis. Further rotation of the timing motor M5 to close switch 48 has no effect on the circuit since relay XIII has not been actuated to complete this circuit. When timing motor MS has completed its cycle, all switches actuated thereby, which have not already been returned to normal position, will constant volume and constant pressure chamber 201;

all switches in the mass spectrometer, which were operated during the scanning period, have been returned to their normal position; and the system is ready to start a new analysis.

When it is desired to analyze a sample for hydrocarbons having masses 0, through C switch 18 is advanced one step in a clockwise direction to its second position. The power is turned on "by switch 11 and switch 14 is again turned one step in a clockwise direction to its automatic position. In the manner described above in connection with the hydrogen through C scan, the manipulation of switch 14 will open the solenoid valve 82, shown in Figure IA, to allow the sample to leak into the ionization chamber where it will be ionized. Switch 19 is then momentarily depressed to complete a circuit through relay II and the scanning pilot light 16. With switch 18 in its second position, power is supplied to relay II and the scanning pilot light 16 through the circuit, which includes switch 11, conductor A, switch 14C, conductor 2%, switch 19, conductors 4-9 and 5G, switch 18C, conductor 113, switch 133, conductor E, the winding of relay II, con: doctor 83, conductor B and the switch 11. It can be seen, by means of conductor B, scanning pilot light 16, conductor ill-i, switch 14A, conductor 50, switch 18C and conductor 17.3, that the scanning pilot light is connected in parallel with the coil of relay II. Depression of switch I9 also completes a circuit to switch 37, which, when actuated at a later programmed time, Will energize relay XI to knock out other relays in a manner to be described later. This circuit includes switch 11, conductor A, switch 14C, conductor 20, conductor 115, switch 18A and conductor L. The depression of switch 19 and actuation of relay II serve to start timing motors M2 and M3. Timing motor M2 receives its power through conductors E and 76, relay points 65 which are closed, and conductor 77. Timing motor M3 is energized through conductor E, points 69 which are closed by relay II, conductors 78 and 79, points 80 on relay III which are closed, points 70 on relay II and conductor 81. The operation of timing motors M2 and M3 will perform in their predetermined programmed time the sequence of operations described in connection with the hydrogen through C scan with one exception. For the C through C analysis, switch 37 will be closed in its proper order ahead of switch 38 to energize knock-out relay XI to return the circuits to normal condition at t e end of the C scan. Further rotation of the drum driven by timing motor M3 will close switch 38. But, since switch 13 is in its second position, closing switch 33 will not complete a power circuit and, therefore, this operation will not be effective. Still further rotation of the drum driven by timing motor M3, in completing its cycle, will close switch 39 in the manner described above in connection with the hydrogen through helium scan to energize relay XII to initiate the pump-out cycle by starting timing motor M5.

When it is desired to make an analysis of a sample for hydrocarbon C through C switch 18 is turned clockwise to its third position, switch 14 is again turned to its automatic position and switch 11 operated to turn the power on. The operation of switch 14 will again open the solenoid valve 82 to allow the sample to leak from the cold bottle 202 into the analyzer ionization chamber. With the switches so set, the momentary depression of switch 19 will again energize relay II and turn on the scanning pilot light 16. Relay II, in the manner described immediately above, energizes 'timing motor M2. The depression of switch 19 also establishes a circuit which includes the conductor E, the points 69 of relay II, conductors 78 and 79, points 30 of relay III, points 70 of relay II and the conductor 81 to start the timing motor M3. These motors operate switches in the same predetermined program as before with the exception that timing motor M3 will now operate switch 33 to terminate the scan at the end of mass C Since switch 37 is in a dead circuit with the switch 18 set on position three, its actuation by the drum driven by timing motor M3 will not be effective to stop the scan at the end of C Operation of switch 38 will, in the manner described in connection with the hydrogen through C scan, energize relay XI to knock-out previously actuated relays and return the circuits to their normal condition. Further rotation of the drum driven by timing motor M3 will close switch 39 to energize relay XII to initiate the sample evacuation step by starting timing motor M5 in the manner described above.

When it is desired to analyze a sample for hydrocarbon having masses C through C switch 18 is rotated clockwise to its fourth position, power is turned on by switch 11 and switch 14 turned to its automatic position. The operation of switch 14, as pointed out above, completes a circuit through a solenoid valve 82 to allow the sample to leak into the ionization chamber of the analyzer tube where it is ionized; Momentary depression of switch 19 will energize relays II and III to simultaneously start timing motors M2 and M4 and, at the same time, supply power to one side of the open switch 42 so that when switch 42 is closed, it will terminate the C through C position. Further rotation of the drum driven by timing motor M4 will close switch 44 to energize relay XII to initiate the sample evacuation step by energizing timing motor M5. The circuit involved in the energizing of relay II includes one of the power mains 12, the switch 11, conductor A, switch 14C, conductor 20, switch 19, conductor 21, switch 183, conductor E, conductor 96, the winding of relay II, conductor 83 and conductor B, contacts on switch 11 and the other power main conductor 12. Actuation of relay II closes points 69 thereof to complete a holding power circuit for this relay so that it will not be knocked out when switch 19 is released. Relay III is supplied actuating power by means of one of the power mains 12, switch 11, conductor A, switch 14C, conductor 20, switch 19, conductor 49, conductor 50, switch 18C, conductor F, the winding of relay III, conductor 89, conductor B, switch 11 and the other power main 12. Actuation of relay III opens contacts thereof and, in so doing, the armature or movable Contact completes a holding power circuit for this relay. Since the scanning pilot light 16 is now connected in parallel with the coil of relay III, it will be lighted when the coil of this relay is energized. At the same time that relay II is energized, power is supplied through conductor 76, the relay points 65 of relay X, conductor 77, to the timing motor M2, whose power circuit is completed through conductor B. Simultaneously, the actuation of relay III will break the points and cause the moving point or armature thereof to complete a new circuit which will start timing motor M4. This circuit involves one of the powcr mains 12, switch 11, conductor A, conductor 75, conductor 99, the points of relay III, conductor 117, the timing motor M4 and conductor B, which returns to the switch 11 and the other side of the power mains 12. The initial rotational movement of timing motors M2 and M4 will complete auxiliary power circuits for these motors by closing switches 28 and 40. Substantially simultaneously with the closing of switch 40, switch 41 is opened to break the circuit through the standby pilot light 17. Timing motor M2, being a one revolution per minute motor, will complete its entire cycle in one minute. However, timing motor M4, being a /5 revolution per minute motor, will complete its cycle in five minutes. Therefore, timing motor M2 will complete its cycle, thereby performing all of its functions before timing motor M4 has rotated its switch actuating drum sufliciently far to close switch 42 to thereby energize relay XI to knockout all previously energized relays. Switch 42 will not be closed by the drum rotated by timing motor M until the time required for the scan to progress through C mass has elapsed. Further rotation of timing motor M4 will cause its switch actuating drum to close switch 43. However, since no power is supplied to this circuit, the closing of this switch is ineffective. Continued rotation of the switch actuating drum, driven by timing motor M4, in its cycle will next close switch 44 to actuate relay XII and thereby start the pump-out cycle by initiating the operation of timing motor M5. Timing motor M5 is a /6 revolution per minute motor and will, in its cycle of operation, perform the same functions attributed to it in the description of previously described analyses. It is to be understood that at the ends of the cycles of motors M2, M4 and M5 that all previously operated switches, which have been actuated directly by the switch actuating drums or by the relays which have been energized by switches controlled by the switch 9'. actuating drums, have all been returned to their normal position, the scanning pilot light 16 turned out and the standby pilot light 17 turned. on toindicate that the mass spectrometer now stands ready to receive a new sample for analysis.

When it is desired to analyze a sample for hydrocarbons C through C switch 18 is rotated clockwise to its fifth position. Changing switch 18 from its fourth position, which was used for the C through C scan, to its fifth position for the C through C scan, produces only one change in circuitry. In the new position, position five, power is supplied to switch 43 instead of switch 42 so that the knock-out relay XI will not be energized until switch 43 is closed. Although switch 42, operated by the switch actuating drum, driven by timing motor M4,.

will close prior to the closing of switch 43, it will not produce any effect since it is not in a power circuit. Therefore, the scan will continue through masses, at which time switch 43 will be closed to energize knock-out relay XI. Further rotation of the drum driven by timing motor M4 will close switch 44 to energize relay XII to initiate the pump-out cycle by starting timing motor M5.

The automatic control system forming the subject matter of the instant application is also adapted for use when it is desired to use the mass spectrometer to make a type analysis of a sample. By type analysis is meant analysis of samples of gasoline, fuel oils, kerosine, gas oils, or anything C or heavier which is, at normal temperature and pressure, in liquid form. Such samples must be heated to convert them into vapor form before they are introduced into the ionization chamber for ionization and analysis. Therefore, further reference to the type analysis will include expressions which refer to the hot bottle operation, meaning an operation conducted for the purpose of analyzing samples containing hydrocarbons of mass C or heavier. When conducting a type analysis, the sweep voltages, one of which is to be selected, remain the same as for previously described analyses. The magnetic field, however, through which the ions are accelerated to cause them to scan the collector target in the analyzer tube, is increased manually to a predetermined value which, when used with the selected accelerating voltage, will cause the target to be first scanned with C ions, followed by increasingly heavier ions.

When it is desired to analyze the sample for hydrocarbon ions having masses C and heavier, switch 18 is advanced clockwise to its sixth position. In this position switch 18A supplies power through conductor M to the winding of relay XIII to actuate it to thereby set up hot bottle pump-out circuits which will be actuated when timing-motor M runs through its cycle. Switch 18B is ineffective since the contact point in the sixth position thereof is not connected to any circuit. Switch 18C will complete a circuit for relay II since it is connected by conductor 113 to points 2 to 5 inclusive of switch 188.

With switch 18 turned to its sixth position, relay II will be actuated and, since the scanning pilot light 16 is in parallel with the actuating coil of relay II, it will be lighted; timing motor M2'will be supplied with power to start it; relay XIII will be actuated; and power supplied to switch 36, which, when closed, will end the type scan.

Power is supplied to relay II by the circuit which includes one of the power mains 12, switch 11, conductor A, conductor 20, switch 19, conductor 49, conductor 50, switch 180, conductor 113, conductor E, the winding of relay II, conductor 88, conductor B, switch 11 and the other power supply main 12. Actuation of relay II will close the points 69 to complete a holding circuit for this relay so that the release of switch 19 will not knock-out the relay. Closing of the points 70 by relay II completes a power circuit for timing motor M3. The power circuit for timing motor M3, thus completed, includes one side of the power mains 12, switch 11, conductor A, conductor 75, points 68 of relay XI, conductor 84, the points 80 of I control selection switch which in a first position permitsv relay III, the closed points7tl of relay II, conductor 81',

timing motor M3, conductor B, switch 11 and the other power supply main 12, The initial rotational movement of timing motors M2 and M3 will close switches 28and 34 to complete auxiliary power circuits for these motors so that the release of switch 19 will'not cut off the power to them. Switch 35 is opened substantially simultaneous-' 1y with the closing of switches 28 and 34 to break the standby pilot light power supply circuit to turn off the standby pilot light. Timing motor M2 will follow its usual cycle and in so doing will simultaneously close switches 29 and 30 to select a scanning voltage; Although these two switches will condition two scanning voltage selection circuits, only one scanning voltage will be selected. The closing of switches 29 and 30 will re spectively energize relays IV and V. The armature 71 and 72 of relays IV and V will be moved to their up position to complete voltage selection circuits. However, since the circuit completed by the armature 72 is opened by the operation of the armature 71 to its up position,-

this circuit will be ineffective and the circuit completed by the armature 71 of relay IV in its up position will select the highest available negative voltage for the charg ing voltage for the sweep condenser. The circuit, thus completed, includes the conductor CC-1, the switch 14A,

conductor CC, points 67 of relay IX, conductor 118, the

points of relay IV and conductor BB. Timing motor M2, in completing its cycle, performs the same functions attributed to it in the description of other analyses. Timing motor M3, being a V revolution per minute motor, will continue to run, after timing motor M2 has completed its cycle, until the time required to complete the type scan has elapsed, at which time switch 36 will be closed to energize relay XI, which, in turn, knocks out relays II and IV to X inclusive. In completing its cycle, timing motor M3 will close switches 37 and 38. However, since they are in dead circuits, closing them will produce no.

effect. Near the end of the cycle of timing motor M3, switch 39 will be closed to energize relay XII to start the pump-out operation. Since relay XIII has been energized, the pump-out operation will be applied to the hot bottle. Actuation of relay XII will start the timing motor V, whose initial rotational movement will complete an auxiliary power circuit for it and it will follow its usual cycle, as described above. Since relay XIII has been actuated, the closing of switch 47 by the drum actuated by timing motor M5 will produce no effect since the contacts 108 have been opened to break that circuit. The moving contact of points 108 in opening will complete a new circuit which involves the switch 48. This new circuit will supply power to the solenoid operated valve 215 to open it so that the hot bottle 216 and the constant volume and constant pressure chamber 212 can be pumped out. This circuit comprises the power bus 83, conductor QQ, points on switch 14C, conductor PP, the points on relay XIII, conductor 224, switch 48, conductor 225,

conductor 226, conductors 227 and the power bus 218.

At the time timing motor M5 is started, the evacuating" pilot light 15 will be turned on. At the end of the cycle of timing motor M5, the evacuating pilot light 15 will be turned off and the standby pilot light 17 will be turned automatic selection switch having means associated therewith, including solenoid operated valves, acting, when it is placed in the second position, to introduce a sample to r I the sample cell of the spectrometer; said program initiating switch having means associated therewith to act, when it is momentarily depressed, to set up and maintain circuits selected by presetting of the program selection switch, said preselected circuits including: a first timing motor and a series of switches driven thereby and relays associated therewith comprising sequentially operated means acting firstly to establish a holding circuit to keep said first motor in operation and to start a second timing motor, means acting secondly to set up a circuit including a resistance to permit reduction of the magnetic field of the mass spectrometer to permit scanning of a preselected range of masses, means acting thirdly to turn on galvanometer circuits and mass marker circuits in the mass spectrometer, means acting fourthly to activate mass marker reset, means acting fifthly to actuate the recording element of the mass spectrometer and to initiate scanning; the second timing motor and a series of switches driven thereby and relays associated therewith comprising sequentially operated means acting firstly to provide a holding circuit to keep said second motor in operation, means acting secondly, after time lapse sufiicient to complete scanning, to open relays and permit return of all switches controlling the spectrometer to their normal standby position, means acting thirdly to actuate a third timing motor; said third timing motor and a series of switches driven thereby and relays associated therewith comprising sequentially operated means acting firstly to provide a holding circuit to keep said third motor in operation, means acting secondly to actuate a solenoid to open the sample cell of the spectrometer to pump-out, means acting thirdly to actuate a solenoid to open the sample manifold to pump-out and means acting fourthly to complete the opening of all operating circuits and place the whole of the equipment and circuitry associated with the spectrometer in standby condition.

2. Apparatus for automatic operation of a mass spectrometer comprising a source of alternating current supply; an on-otf switch associated therewith, an automatic control selection switch which, in a first position, permits manual operation of the spectrometer and which, in a second position, permits automatic operation, a program selection switch, and a program initiation switch; said automatic switch having means associated therewith including solenoid-operated valves acting, when it is placed in the second position, to introduce a sample into the mass spectrometer; said program initiating switch having means associated therewith to act, whenit is momentarily depressed, to set up and maintain circuits selected by presetting of the program selection switch, said preselected circuits including: a first timing motor and a series of switches driven thereby and relays associatcd therewith comprising sequentially operated means acting firstly to provide a holding circuit to keep said first motor in operation, means acting secondly to permit reduction of the magnetic field of the mass spectrometer to permit scanning of a first selected range of masses, means acting thirdly to actuate the galvanometer of the mass spectrometer and also to complete mass marker circuits within the spectrometer, means acting fourthly to actuate the recording element of the spectrometer and to bring about a decaying scanning voltage, means acting fifthly after a time lapse sufiicient to complete a first scanning to open relays and permit return of all switches controlling the mass spectrometer to their normal standby position, and means acting sixthly to start a second timing motor and a third timing motor; said second timing motor and a series of switches driven thereby and relays associated therewith comprising sequentially operatcd means acting firstly to provide a holding circuit for keeping said second motor in operation, means acting secondly to select the highest voltage for a second scanning operation of the spectrometer, means acting thirdly to complete galvanometer circuits and mass marker circuits within the spectrometer, means acting fourthly to reset the mass marker, means acting fifthly to actuate the recorder of the mass spectrometer and to initiate the second scanning; said third timing motor and a series of switches driven thereby and relays associated therewith comprising sequentially operated means acting firstly to set up a holding circuit to keep said third motor in operation, means acting secondly, after time lapse sufficient for completion of said second scanning to open relays and permit return of all switches controlling the mass spectrometer to their normal standby position, means acting thirdly to start a fourth timing motor; said fourth timing motor and a series of switches driven thereby and relays associated therewith comprising sequentially operated means acting firstly to provide a holding circuit for keeping said fourth motor in operation, means acting secondly to actuate a solenoid to open the sample cell of the spectrometer to pump-out, means acting thirdly to actuate a solenoid to open the sample manifold of the spectrometer to pump-out and means acting fourthly to complete the opening of all operating circuits and place the whole of the equipment and circuitry associated with the spectrometer in standby condition.

3. Apparatus for automatic operation of a mass spectrometer comprising: a source of alternating current supply, a first switch to connect and disconnect the alternating current supply to the operating circuitry, a second switch to permit selection of manual program control or auto' matic program control, a third switch whereby connection may be made to any one of a plurality of program circuits each arranged to operate according to a preselected program, and a fourth switch for program initiation; circuit elements to conduct alternating current from said first switch in closed position to said second switch, circuit elements whereby said current passing through said second switch when it is set in the automatic position is conducted to said third or program selection switch, sald fourth switch being so placed in the circuitry between the second switch and the third switch that operation of the program selected by the third switch cannot begin until the circuits of the program selected by the third switch are actuated by momentary depression of the fourth switch; solenoid valves actuated by current flowing through said second switch when in automatic setting to introduce a sample to the sample cell of the spectrometer; said program circuits associated with said third switch each including a plurality of constant speed timing motors, a switch actuating drum driven by each motor, a plurality of switches so positioned on each of said drums as to be actuated sequentially, circuits and relays associated with each of said switches and also so associated with the circuitry of the mass spectrometer that sequential operation of the switches causes sequential progression through preselected operating steps of the mass spectrometer.

References Cited in the file of this patent UNITED STATES PATENTS Hoskins Apr. 24, 1945 Riggle et al July 26, 1955 Burney et al Aug. 2, 1955

Patent Citations
Cited PatentFiling datePublication dateApplicantTitle
US2374205 *Jul 3, 1943Apr 24, 1945Cons Eng CorpMass spectrometry
US2714164 *Feb 23, 1954Jul 26, 1955John W RiggieMass spectrometer sampling system
US2714667 *Jun 18, 1946Aug 2, 1955Appleton William HCalutron operation
Referenced by
Citing PatentFiling datePublication dateApplicantTitle
US3943363 *Sep 17, 1974Mar 9, 1976Entreprise De Recherches Et D'activities Petrolieres ElfDevice for automatic analysis mass spectrometry
Classifications
U.S. Classification250/288, 315/315, 250/430, 315/323, 315/110
International ClassificationH01J49/02, H01J49/04
Cooperative ClassificationH01J49/04, H01J49/022
European ClassificationH01J49/04, H01J49/02A