CN1161451A - Karl Fischer moisture determination instrument - Google Patents
Karl Fischer moisture determination instrument Download PDFInfo
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- CN1161451A CN1161451A CN 97100943 CN97100943A CN1161451A CN 1161451 A CN1161451 A CN 1161451A CN 97100943 CN97100943 CN 97100943 CN 97100943 A CN97100943 A CN 97100943A CN 1161451 A CN1161451 A CN 1161451A
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Abstract
The invented instrument is composed of a metering tube on the main frame connecting to the metering pump, plane valve and reaction cup connecting to the stirring machine. Through ducts they are connected to the reagent bottle, solvent bottle and waste liquid bottle separately. In the main frame the control circuit is installed. through the operation of keys, the liquid suction, liquid return, continuous-rapid-slow-terminal of point of titration, stirring, pouring solvent in and draining waste liquid etc. whole process can be accomplished automatically. The whole system features good property of airtight, capable of preventing water-infiltration and poison gas escaping, wide range (from 10 PPM-100%) of measurement, high accuracy and convenient for operation.
Description
The present invention relates to a kind of volumetric method karl Fischer moisture determination instrument that material moisture content is measured.
Needing certain water gaging to participate in the principle of reaction when the karl Fischer moisture determination method is based on iodine oxidation sulphuric dioxide, is the most single-minded to water in all kinds of chemical analysis, the most accurately assay method.It is widely used in medicine, oil, and chemical industry, industry such as food become international and domestic general standard method, and the key that the karl Fischer method is applied is to be equipped with suitable cheap and good-quality instrument.
In the background technology field, traditional manual instrument is in manual mode karl Fischer reagent to be added buret and carries out titration, and titration end-point judges that by the deflection of observing the ammeter pointer of swinging visual titration pipe scale is read reagent titration volume; Semi-automatic instrument also is that manual mode adds buret with karl Fischer reagent, clamps proofed sleeve with solenoid valve and controls titration, and terminal point can judge automatically that reagent titration volume is still read with visual titration pipe scale.The instrumentation inconvenience of above-mentioned two kinds of assay methods, human factor is more, and resolution and measuring accuracy are lower, and reappearance is relatively poor, and whole device sealing is poor, and the effusion of toxic gas has certain harmfulness to operating personnel's health.
The objective of the invention is: a kind of full-automatic totally-enclosed volumetric method karl Fischer moisture determination instrument is provided, and reagent sucks, and automatically performing of gauge line titration and endpoint improves the moisture determination precision reliability.
For reaching above-mentioned goal of the invention, the technical solution used in the present invention is: the gauge line that is connected with volume pump is housed on main frame, two-position three way plane valve (hereinafter to be referred as the plane valve), the reaction cup that is connected with stirring motor, insert the electrode in the reaction cup, drying tube is housed on the reaction cup, one end of titration conduit is communicated with the titration mouth of plane valve, the other end of titration conduit is communicated with titrating head in the reaction cup, one end of conduit is communicated with a mouth of plane valve, and the other end of conduit is communicated with gauge line.Main frame one side master places the reagent bottle that karl Fischer reagent is housed, the conduit that drying tube is arranged respectively on the bottle graft head web member and be communicated with another mouthful of plane valve.Place electric diaphragm pump in the solvent bottle seat of main frame opposite side, place solvent bottle on the solvent bottle seat, the conduit that drying tube is housed respectively and is communicated with on the bottle graft head web member with reaction cup, another root conduit is communicated with electric diaphragm pump and drying tube.Place another electric diaphragm pump in the waste liquid bottle seat of main frame opposite side, place waste liquid bottle on the waste liquid bottle seat, the drawing liquid conduit that drying tube is housed respectively and is communicated with on the bottle graft head web member with reaction cup, conduit is communicated with another electric diaphragm pump and drying tube.The alterating and direct current source circuit is housed, control circuit, motor-drive circuit that control volume pump motor, plane valve motor and stirring motor rotate and the control circuit that solvent injects and waste liquid is discharged in the main frame.Volume pump sucks karl Fischer reagent by the plane valve of button automatic switchover direction, return liquid and get rid of bubble and the moisture content titration and the endpoint of carrying out in solvent or the sample, inject solvent and effluent discharge by the key control electric diaphragm pump, improve moisture determination precision and reliability.
The present invention compares with background technology, and the useful effect that is had is:
1. adopt hermetic bottle graft head web member and piping system, guaranteed the good leakproofness of system, prevent that the intrusion of moisture content in the atmosphere and toxic gas from overflowing to the infringement of human body;
2. the electrode output signal is judged through circuit control system, realizes continuously-fast-at a slow speed-titration process of terminal point, and the result can be shown or printed by charactron;
3. moisture determination wide ranges can be from the high-load of the low content to 100% of 10PPM;
4. the resolution of reagent titration reaches 0.01ML, and the moisture determination precision is better than soil 1%;
5. carry out reagent by button and suck, return liquid, pre-titration and measurement function, easy to operate.
The analyzer of this structure can be used in various titrators and the solution dispenser equally.
Description of drawings:
Fig. 1, perspective view of the present invention;
Fig. 2, main frame lateral plan;
Fig. 3, volume pump structural representation;
Fig. 4, two-position three way plane valve arrangement synoptic diagram;
Fig. 5, two-position three way plane valve valve gap vertical view;
Fig. 6, valve position switch and valve motor shaft sleeve connection diagram;
Fig. 7, bottle graft head web member structural representation;
Fig. 8, control system circuit structure schematic diagram.
Below in conjunction with accompanying drawing, provide details of the present invention by description to embodiment.
As shown in Figure 1, the alterating and direct current source circuit is housed in the main frame, main control circuit, control volume pump motor, motor-drive circuit that plane valve motor and stirring motor rotate and solvent inject and waste liquid is discharged control circuit.Power switch 3 is housed on the host panel, and reset key 4 is prepared key 5, and pre-titration key 6 is measured key 7, returns liquid key 8, solvent bond 9, discharge opeing key 10, digital display tube 11 and terminal point 12, excessive 13 and stir 14 light emitting diode.As shown in Figure 2, plate is equipped with supply socket 15 behind the main frame, and fuse holder 16 and electric diaphragm pump supply socket 17 are equipped with on the right panel and are stirred power switch 18 and stirring rate regulator potentiometer 19.The gauge line 43 that is connected with volume pump 1 is housed on the main frame, plane valve 2, the reaction cup 20 that is connected with stirring motor 94, the column 21 of fixation reaction cup, insert the electrode 41 in the reaction cup 20, drying tube 38 is housed on the reaction cup 20,2.3 mouthfuls of one end of titration conduit 30 and plane valve 2 are communicated with, the other end of titration conduit 30 is communicated with titrating head 31 in the reaction cup 20, one end of conduit 42 is communicated with the 2-2 mouth of plane valve 2, one end of conduit 42 is communicated with the 2-2 mouth of plane valve 2, and the other end of conduit 42 is communicated with gauge line 43.Main frame left side reagent bottle seat 22 is placed the reagent bottle 23 that karl Fischer reagent is housed, be equipped with respectively on the bottle graft head web member 28 drying tube 37 and with 2.1 mouthfuls of conduits that are communicated with 29 of plane valve 2.Place electric diaphragm pump 27.1 in the solvent bottle seat 24.1 on main frame right side, place solvent bottle 25 on the solvent bottle seat 24.1, the conduit 34 that drying tube 39 is housed respectively on the bottle graft head web member and is communicated with reaction cup 20, another root conduit 33 is communicated with electric diaphragm pump 27.1 and drying tube 39.Place electric diaphragm pump 27.2 in the waste liquid bottle seat 24.2 on main frame right side, place waste liquid bottle 26 on the waste liquid bottle seat 24.2, the drawing liquid conduit 35 that drying tube 40 is housed respectively on the bottle graft head web member and is communicated with reaction cup 20, conduit 36 is communicated with electric diaphragm pump 27.2 and drying tube 40.
As shown in Figure 3, volume pump 1 it comprise the volume pump body component, drive disk assembly and piston limiting component.The volume pump body component, comprise that the upper end has the gauge line 43 of liquid outlet, one end of the piston rod 47 in the gauge line 43 is equipped with piston head 46, the piston cap 44 that matches with piston head 46, for making piston cap 44 good with the leakproofness of gauge line 43, can between piston head 46 and piston cap 44, add O type circle 45, gauge line 43 end faces add O type circle 65, whole parts are fixed on the little assembled plate 66 with gland 64, and little assembled plate 66 is fixed on the assembled plate 50 by column 63; Drive disk assembly, comprise the volume pump motor 48 that is contained on the assembled plate 50, on 48 in the motor driving gear 52, worm screw 49 are housed successively, driving gear 52 is through transmission gear 56, driven gear 57, driving screw mandrel 58 rotates, the other end of piston rod 47 and screw mandrel cover 59 is connected, and screw mandrel 58 drives screw mandrels cover 59 moves up and down piston in gauge line 43, and worm screw 49 is meshed with worm gear 53 on the variable resistance position sensor 55 that is contained in the fixed mount 54; The piston limiting component comprises the bent plate 61 that is contained on the screw mandrel cover 59, and set screw 62 up and down is equipped with in bent plate 61 ends, and bent plate 61 can move up and down along backstay 60, on the little assembled plate 66 upper limit position switch 67 is housed, and lower position switch 68 is housed on the assembled plate 50.Whole metering pump part is fixed on the instrument base plate through post 51.
As Fig. 4, Fig. 5, shown in Figure 6, it comprises plane valve part and valve driver part plane valve 2.The plane valve part, comprise the valve body 69 that has three runner 2-1,2-2,2-3, have deep-slotted chip breaker 73 (arc does not draw among the figure) on one end face, and the valve gap 70 that can be connected with three runner 2-1,2-2,2-3, pass the valve rod 71 of valve gap 70 and valve body 69, through spring compression valve body 69 and valve gap 70, whole valve is supported on the casing top panel 76 with valve fixed mount 74 valve rod 71 1 ends with bonnet 72, and is fixing with valve retainer plate 75; The valve driver part, comprise the valve motor 77 that is contained on the plate 81, valve rod 71 inserts in the valve motor shaft sleeve 78, when valve motor 77 rotates through valve motor shaft sleeve 78, valve rod 71 drives valve gap 70 and rotates, make the deep-slotted chip breaker 73 of valve gap 70 upper surfaces connect three runners in turn, valve position switch 79,80 is equipped with in valve motor shaft sleeve 78 sides, and plate 81 is fixed on the instrument top panel 76 through screw nut 82.
As shown in Figure 7, bottle graft head web member, be included on the circular bead surface of bottle stopper head 83 and be with bottle cap 85, the bottle stopper head 83 small end faces of cylinder and bottle graft head 84 closely cooperate, have two stepped bore a, b in the bottle graft head 84, and be interconnected, one of them stepped bore a directly is communicated with bottle stopper head 83 central through hole c.In order to increase sealing, on the roundlet cylinder on bottle stopper head 83 circular bead surfaces, be with O RunddichtringO 86, keep certain clearance between O RunddichtringO 86 and bottle cap hole, formation is rotatably assorted.
As shown in Figure 8, be control system circuit structure schematic diagram, it comprises the power of alterating and direct current circuit I, main control circuit II, motor-drive circuit III that control volume pump motor, plane valve motor and stirring motor rotate and solvent injection and waste liquid are discharged control circuit IV.Wherein:
Power of alterating and direct current circuit I, AC power circuit be by power switch 3, and fuse 16 and transformer 95 are formed, output～15V ,～110V or～the 220V alternating voltage; DC power supply circuit, by diode D1～D4, capacitor C 1 is formed the bridge rectifier wave filter, through three-terminal voltage-stabilizing integrated package 7806 and capacitor C 2, output+6V DC voltage, by diode D5～D8, capacitor C 3, C5 form the bridge rectifier wave filter, through three-terminal voltage-stabilizing integrated package 7805 and capacitor C 4, output+5V DC voltage, through three-terminal voltage-stabilizing integrated package 7905 and capacitor C 6, output-5V DC voltage.
Main control circuit II: the end that it comprises reset key 4 connect power supply respectively and behind relay J 6-1 normally opened contact, J9 ground connection, the other end connect respectively limit switch 67 c end, lower position switch 68 the d end and after the J9-3 normally opened contact meets J9 ground connection; An end of preparing key 5 connects a end of limit switch 67 and connects pre-titration key 6 and mensuration key 7, ground connection behind the common port of another termination J1-2 normally opened contact and J1-1 normally closed contact through J1-2 normally opened contact, J1-1 normally closed contact through J2 through J1, J2-1 normally closed contact respectively; Pre-titration key 6 and an end of measuring key 7 be ground connection and connect J2-4 normally opened contact, J2-3 normally closed contact common port through J9-1 normally closed contact, J9-2 normally opened contact, mono-stable timing circuit 87, buzzer 88 after respectively, and the f of J9-1 normally closed contact and the public termination lower position switch 68 of J9-2 normally opened contact holds; Return a termination J2-3 normally closed contact of liquid key 8, ground connection behind another termination J3; One termination power of reference power supply 89, the other end connect potentiometer RW1, variable resistance position sensor 55 respectively, equal ground connection behind potentiometer RW2 and resistance in series R4, R3, R2, the R1, potentiometer RW2 one termination electrode 41; Digital display tube 11 and print system 96 connect variable resistance position sensor 55 through A/D converter 90; Comparer A1 one input end is through the common port of resistance R 6 connecting resistance R1 and R2, another input end is distinguished receiving electrode 41 and ground connection after resistance R 5, output terminal is through resistance R 9, capacitor C 7 couplings connect the base stage of triode GB1, the E utmost point ground connection of GB1, the C utmost point of GB1 meets J4, the other end of J4 connects pre-titration key 6 and measures key 7 through the J5-1 normally closed contact respectively, through the J5-2 normally opened contact, timing oscillator 92, triode GB5, ground connection behind the J8, through the J4-1 normally opened contact, timing oscillator 91, triode GB4, ground connection behind the J7, the C utmost point of GB1 is ground connection behind J4-2 normally opened contact and resistance 12 also; Comparer A2 one input end is through the common port of resistance R 7 connecting resistance R2 and R3, another input end receiving electrode 41, output terminal connects the base stage of triode GB2 through resistance R 10, capacitor C 8 couplings, the E utmost point ground connection of GB2, the C utmost point of GB2 is ground connection and meet J5 behind the normally opened contact of J5-3, resistance 13 respectively, and the other end of J5 connects pre-titration key 6 respectively and measures key 7 and connect the J5-2 normally opened contact; Comparer A3 one input end is through resistance R 8 connecting resistance R3 and R4 and common port, another input end receiving electrode 41, output terminal connects the base stage of triode GB3 through resistance R 11, capacitor C 9 couplings, the E utmost point ground connection of GB3, the C utmost point of GB3 meets J6, and the other end of J6 connects pre-titration key 6 respectively and measures key 7 and connect the J5-2 normally opened contact.
Motor-drive circuit III: it comprises behind the end series connection J2-5 normally opened contact that exchanges the 15V power supply, J7-1, the J8-1 normally closed contact and the J3-1 normally opened contact, with in parallel after the J1-7 normally opened contact connects a winding of volume pump motor 48, behind another winding of one termination volume pump motor 48 of interchange 110V power supply, connect 1 end of valve position switch 80 through capacitor C 10; One end of alternating current 220V power supply J3-3 in parallel, J1-5 normally opened contact, the g end of the public termination valve position switch 79 of one, h end back are connected with k end, the j end of valve position switch 80, and its another common port connects the j end of valve position switch 80 behind the J2-7 normally opened contact; The i end of valve position switch 79 is connected with the k end of valve position switch 80: direct current+5V power supply is through stirring switch 18, stirring motor 94 triode GB6 connect Sheffer stroke gate 93, stirring rate regulator potentiometer 19 1 ends directly all connect Sheffer stroke gate 93 through diode D9, capacitor C 11 and an end through the common port and an end of diode D10, diode D9 and capacitor C 11;
Solvent injects and waste liquid is discharged control circuit IV: it comprises that an end of alternating current 220V power supply is through solvent bond 9, discharge opeing key 10 connects electric diaphragm pump 27.1 and electric diaphragm pump 27.2 one ends, the other end of electronic barrier film 27.1 of another termination of alternating current 220V power supply and electric diaphragm pump 27.2 respectively.
The course of work is as follows: after the opening power, and during by the 5 moments connection of preparation key, the J1 energising, the J1-2 closure makes J1 keep energising, and the J1-5 closure makes valve motor 77 turn to valve 2 and connects directions with reagent bottle 23, threshold switch 79 make volume pump motor 48～the 110V power connection, the J1-7 closure is connected volume pump motor 48～15V reversal of power, and the gauge line descent of piston sucks reagent, stop to lower position switch 68,, connect reset key 4 if require the Halfway Stopping operation, the J1 outage, the stall of volume pump motor is if the gas in gauge line 42 and the conduit 29 need be got rid of, can carry out back the liquid operation, when pressing back liquid key 8, the J3 energising, the J3-3 closure makes valve motor 77 also turn to valve 2 and connects direction with reagent bottle 22, threshold switch 79 is switched on volume pump motor 48～110V power supply, the J3-1 closure is connected volume pump motor 48～15V power supply forward, and the gauge line upstroke is discharged gas, when pressing back liquid key 8 again, key 8 disconnects, and is out of service, before carrying out pre-titration or measuring, need by solvent bond 9, start electronic barrier film inflator pump 27-1 solvent is injected reaction cup 20, and open and stir switch 18, it is bright to stir pilot lamp 14, governing speed adjusting knob 19, the stirrer 32 that is contained in the reaction cup 20 is rotated with suitable speed, stirring solvent is even, by pre-titration key 6 or mensuration key 7, the J2 energising, J2-1 cuts off J1 is disconnected, and the closed J2 of maintenance of J1-1 switches on, and the J2-7 closure makes valve motor 77 turn to valve 2 and connects direction with reaction cup 20, threshold switch 80 makes volume pump motor 48～110V power connection, the J2-5 closure is connected volume pump motor～15V power supply forward, and gauge line upstroke, karl Fischer reagent begin to carry out the moisture content titration, in titration process, to two platinum electrode 41 detection signals samplings, relatively carry out titration control through comparer and setting value, process is divided into three phases, phase one is a Continuous Titration, when moisture content drop reaction in the reaction cup 20 when finishing, electrode current increases sharply, and produces voltage drop V through resistance R 5, by the setting voltage on comparer A1 and the R1 V1 falls relatively, when V 〉=V1, trigger comparator A1 counter-rotating makes triode GB1 conducting, the J4 energising, the J4-1 closure makes timing oscillator 91 work, the switch-on and-off of pilot relay J7 electric current, and J7-1 disconnects or is closed, make volume pump motor 48～15V power supply forward is disconnected or logical, the gauge line piston is interrupted up, enters the quick titration of subordinate phase, when electrode current continues to raise, voltage drop V falls V2 relatively by comparer A2 with setting voltage (R1+R2), when V 〉=V2, trigger comparator A2 counter-rotating makes triode GB2 conducting, the J5 energising, J5-1 disconnects fast titration is stopped, the J7-1 closure, and the J5-2 closure makes timing oscillator 92 work simultaneously, the switch-on and-off of pilot relay J8 electric current, J8-1 disconnects or is closed, make volume pump motor 48～15V power supply forward is disconnected or logical, the gauge line piston is interrupted up, enter the titration at a slow speed of phase III, when electrode current raises again, voltage drop V falls V3 relatively by comparer A3 with setting voltage (R1+R2+R3), when V 〉=V3, trigger comparator A3 counter-rotating, make triode GB3 conducting, the J6 energising, the J6-1 closure makes the 12 bright and J9 energisings of terminal point pilot lamp, J9-1 is disconnected, J2-4 disconnects, the J2 outage, and J2-5 and J2-7 all disconnect, 48 stop motions of volume pump motor, titration stops, and the J9-2 closure makes buzzer 88 send the sound of " toot " through mono-stable timing circuit 87 simultaneously, realize the dual prompting of acousto-optic of terminal point, when carrying out pre-titration or measuring, if need stop running, by reset key 4, the J2 outage, volume pump motor 48 is out of service, is preparing back liquid, in pre-titration and the mensuration all processes, the gauge line piston position by the analog electrical signal of variable resistance position sensor 55 output through A/D converter 90, to digital display tube 11 demonstrations or print system 96 printings, after repeatedly measuring, when waste liquid need be got rid of in the reaction cup 20, by discharge opeing key 10, start electronic membrane suction pump 27-2 waste liquid is discharged.
Below the process of using moisture content in this Instrument measuring sample is described.
Turn on the power switch, power light and LED charactron are bright, by preparing key, plane valve switching direction, connect the karl Fischer reagent bottle, the gauge line descent of piston, karl Fischer reagent is sucked in the gauge line, when descent of piston stops during to lower limit automatically, charactron is shown as zero, if underfill reagent and have gas still in the gauge line, then press back the liquid key, upstroke, gas pushed back in the reagent bottle overflow, repeat above process two to three times, can be with air scavenge in the pipeline, be full of karl Fischer reagent in the gauge line, at this moment, by solvent bond solvent is injected reaction cup, open the stirring switch, adjusting knob reaches suitable stirring rate, press pre-titration key, the plane valve automatically switches to the titrator direction, the gauge line piston begins up, karl Fischer reagent splashes in the reaction cup through conduit and titrating head continuously, react rapidly with the moisture content in the solvent, when moisture content reaction finished, the electric current that passes through on two platinum electrodes increased sharply, and instrument is judged when reaching fast titration value of setting, the gauge line piston begins to be interrupted up, carry out fast titration, electric current continue to increase, when reaching slow titration value of setting, change slow titration over to, when electric current reached the terminal point value of setting, titration stopped, and the terminal point pilot lamp is bright, if water cut is too much in the buzzer prompting solvent, upstroke does not reach terminal point yet to upper limit, repeats to press again and prepares key and pre-titration key, until reaching terminal point, do not exist moisture content in the reaction cup solvent this moment, can carry out the demarcation of karl Fischer reagent water equivalent, the water quality standard sample of accurate weighing is added rapidly in the reaction cup, carry out strong stirring, write down beginning digital display value, press pre-titration key again and begin titration, write down terminal point digital display value, calculate the water equivalent T of karl Fischer reagent then according to following formula up to terminal point:
T=M
Mark/ (V
Eventually-V
Just) MG/ML
M
Mark---add the pure water quality of standard specimen, V
Eventually---the displayed value (volume) that titration stops,
V
Just---the displayed value (volume) that titration begins.
After demarcating the karl Fischer reagent water equivalent, can carry out the mensuration of moisture content in the sample, after any titration process is finished, as soon as possible in the sample adding sample cell solvent with accurate weighing, evenly stir certain hour and write down initial displayed value, press pre-titration key then and begin titration process, when reaching terminal point, write down terminal point digital display value, be calculated as follows the percentage composition of water in the sample:
X=((V
Eventually-V
Just) * T/M
Sample) * 100%
M
Sample---the quality of sample.
If any a plurality of samples, the moisture determination step is measured continuously in the repeat samples.
Claims (2)
1. karl Fischer moisture determination instrument, it comprises reaction cup, stirrer, reagent bottle, solvent bottle and waste liquid bottle is characterized in that:
1) be equipped with on the main frame with volume pump [1 ］ gauge line [43] that is connected, two-position three way plane valve [2] (hereinafter to be referred as the plane valve), the reaction cup [20] that is connected with stirring motor [94], insert the electrode [41] in the reaction cup [20], drying tube [38] is housed on the reaction cup [20], one end of titration conduit [30] is communicated with [2-3] mouth of plane valve [2], the other end of titration conduit [30] is communicated with titrating head [31] in the reaction cup [20], one end of conduit [42] is communicated with [2-2] mouth of plane valve [2], and the other end of conduit [42] is communicated with gauge line [43];
2) main frame one is sidelong and is put the reagent bottle [23] that karl Fischer reagent is housed, the conduit [29] that drying tube [37] is housed respectively on the bottle graft head web member [28] and is communicated with [2-1] mouth of plane valve [2];
3) place electric diaphragm pump [27.1] in the solvent bottle seat [24.1] of main frame opposite side, solvent bottle seat [24.1] is gone up and is placed solvent bottle [25], the conduit [34] that drying tube [39] is housed respectively on the bottle graft head web member and is communicated with reaction cup [20], another root conduit [33] is communicated with electric diaphragm pump [27.1] and drying tube [39];
4) place electric diaphragm pump [27.2] in the waste liquid bottle seat [24.2] of main frame opposite side, waste liquid bottle seat [24.2] is gone up and is placed waste liquid bottle [26], the drawing liquid conduit [35] that drying tube [40] is housed respectively on the bottle graft head web member and is communicated with reaction cup [20], conduit [36] is communicated with electric diaphragm pump [27.2] and drying tube [40];
5) the power of alterating and direct current circuit I is housed in the main frame, main control circuit II, motor-drive circuit III that control volume pump motor, plane valve motor and stirring motor rotate and solvent injection and waste liquid are discharged control circuit IV.
2. karl Fischer moisture determination instrument according to claim 1, described volume pump [1], plane valve [2], bottle graft head web member, main control circuit II, motor-drive circuit III and solvent inject and waste liquid is discharged control circuit IV, it is characterized in that:
1) volume pump [1], it comprises:
A. volume pump body component: comprise that the upper end has the gauge line [43] of liquid outlet, one end of the piston rod [47] in the gauge line [43] is equipped with piston head [46], the piston cap [44] that matches with piston head [46], whole parts are fixed on the little assembled plate [66] with gland [64];
B. drive disk assembly: comprise the volume pump motor [48] that is contained on the assembled plate [50], driving gear [52] is through transmission gear [56], driven gear [57], driving screw mandrel [58] rotates, the other end of piston rod [47] is connected with screw mandrel cover [59], and screw mandrel [58] drives screw mandrel cover [59] moves up and down piston in gauge line [43]; Worm screw [49] is meshed with the worm gear [53] that is connected with sensor [55];
C. piston limiting component: comprise the bent plate [61] that is contained on the screw mandrel cover [59], set screw [62] up and down is equipped with in bent plate [61] end, and upper limit position switch [67] is housed on the little assembled plate [66], and lower position switch [68] is housed on the assembled plate [50];
2) plane valve [2], it comprises:
A. plane valve part: comprise have three runners [2-1 ］, the valve body [69] of [2-2], [2-3], have deep-slotted chip breaker on one end face, and the valve gap [70] that can be connected with three runners [2-1], [2-2], [2-3], pass valve gap [70] and valve body [69] valve rod [71 ］, an end of valve rod [71] with bonnet [72] through spring compression valve body [69] and valve gap [70];
B. valve driver part: comprise the valve motor [77] that is contained on the plate [81], valve rod [71] inserts in the valve motor shaft sleeve [78], and valve position switch [79], [80] are equipped with in valve motor shaft sleeve [78] side;
3) bottle graft head web member: be included on the circular bead surface of bottle stopper head [83] and be with bottle cap [85], bottle stopper head [83] the small end face of cylinder and bottle graft head [84] closely cooperate, have two stepped bore [a], [b] in the bottle graft head [84], and be interconnected, one of them stepped bore [a] directly is communicated with bottle stopper head [83] central through hole [c].
4) main control circuit I, it comprises:
A. an end of reset key [4] connect power supply respectively and behind relay J 6-1 normally opened contact, J9 ground connection, the other end connect respectively limit switch [67] c end, lower position switch [68] the d end and after the J9-3 normally opened contact meets J9 ground connection;
B. an end of preparing key [5] connects a end of limit switch [67] and connects pre-titration key [6] and mensuration key [7], ground connection behind the common port of another termination J1-2 normally opened contact and J1-1 normally closed contact through J1-2 normally opened contact, J1-1 normally closed contact through J2 through J1, J2-1 normally closed contact respectively;
C. pre-titration key [6] and an end of measuring key [7] respectively through J9-1 normally closed contact, J9-2 normally opened contact, mono-stable timing circuit [87], buzzer [88] after ground connection with connect J2-4 normally opened contact, J2-3 normally closed contact common port, the f of the public termination lower position switch of J9-1 normally closed contact and J9-2 normally opened contact [68] holds;
D. return a termination J2-3 normally closed contact of liquid key [8], ground connection behind another termination J3;
E. a termination power of reference power supply [89], the other end meet potentiometer RW1, RW1 respectively and connect variable resistance position sensor [55], equal ground connection behind potentiometer RW2 and resistance in series R4, R3, R2, the R1, potentiometer RW2 one termination electrode [41];
F. digital display tube [11] and print system [96] connect variable resistance position sensor [55] through A/D converter [90];
G. comparer A1 one input end is through the common port of resistance R 6 connecting resistance R1 and R2, another input end is distinguished receiving electrode [41] and ground connection after resistance R 5, output terminal is through resistance R 9, capacitor C 7 couplings connect the base stage of triode GB1, the E utmost point ground connection of GB1, the C utmost point of GB1 meets J4, the other end of J4 connects titration key [6] and measures key [7] through the J5-1 normally closed contact respectively, through the J5-2 normally opened contact, timing oscillator [92], triode GB5, ground connection behind the J8, through the J4-1 normally opened contact, timing oscillator [91], triode GB4, ground connection behind the J7, the C utmost point of GB1 is ground connection behind J4-2 normally opened contact and resistance [12] also;
H. comparer A2 one input end is through the common port of resistance R 7 connecting resistance R2 and R3, another input end receiving electrode [41], output terminal connects the base stage of triode GB2 through resistance R 10, capacitor C 8 couplings, the E utmost point ground connection of GB2, the C utmost point of GB2 is ground connection and meet J5 behind the normally opened contact of J5-3, resistance 13 respectively, and the other end of J5 connects pre-titration key [6] respectively and measures key [7] and connect the J5-2 normally opened contact;
I. comparer A3 one input end is through resistance R 8 connecting resistance R3 and R4 and common port, another input end receiving electrode [41], output terminal connects the base stage of triode GB3 through resistance R 11, capacitor C 9 couplings, the E utmost point ground connection of GB3, the C utmost point of GB3 meets J6, and the other end of J6 connects pre-titration key [6] respectively and measures key [7] and connect the J5-2 normally opened contact;
5) motor-drive circuit III, it comprises:
A. exchange behind the end series connection J2-5 normally opened contact, J7-1, J8-1 normally closed contact of 15V power supply and the J3-1 normally opened contact, with in parallel after the J1-7 normally opened contact connects a winding of volume pump motor [48], behind another winding of one termination volume pump motor [48] of interchange 110V power supply, connect 1 end of valve position switch [80] through capacitor C 10;
B. an end of alternating current 220V power supply J3-3 in parallel, J1-5 normally opened contact, the g end of the public termination valve position switch of one [79], h end back are connected with k end, the j end of valve position switch [80], and its another common port connects the j end of valve position switch [80] behind the J2-7 normally opened contact; The i end of valve position switch [79] is connected with the k end of valve position switch [80];
C. direct current+5V power supply is through stirring switch [18], stirring motor [94] triode GB6 connects Sheffer stroke gate [93], stirring rate regulator potentiometer [19] one ends directly all connect Sheffer stroke gate [93] through diode D9, capacitor C 11 and an end through the common port and an end of diode D10, diode D9 and capacitor C 11;
6) solvent injects and waste liquid discharge control circuit IV, it comprises: an end of alternating current 220V power supply is through solvent bond [9], discharge opeing key [10] connects electric diaphragm pump [27.1] and electric diaphragm pump [27.2] one ends respectively, the electronic barrier film of another termination [27.1] of alternating current 220V power supply and the other end of electric diaphragm pump [27.2].
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 97100943 CN1076476C (en) | 1997-01-29 | 1997-01-29 | Karl Fischer Moisture determination instrument |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 97100943 CN1076476C (en) | 1997-01-29 | 1997-01-29 | Karl Fischer Moisture determination instrument |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1161451A true CN1161451A (en) | 1997-10-08 |
| CN1076476C CN1076476C (en) | 2001-12-19 |
Family
ID=5165418
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 97100943 Expired - Fee Related CN1076476C (en) | 1997-01-29 | 1997-01-29 | Karl Fischer Moisture determination instrument |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1076476C (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100335898C (en) * | 2005-03-08 | 2007-09-05 | 张家港市国泰华荣化工新材料有限公司 | Method for measuring water content in C1-C8 low level primary amine |
| CN100368808C (en) * | 2004-04-07 | 2008-02-13 | 董慧茹 | Method and device for improving Karl Fischer water content determination |
| CN102043010A (en) * | 2010-12-10 | 2011-05-04 | 毛骏尼 | Semi-automatic moisture meter |
| CN102269767A (en) * | 2011-05-09 | 2011-12-07 | 中国海洋大学 | Liquid quantitative sample injection device |
| CN102937618A (en) * | 2012-10-26 | 2013-02-20 | 河北省电力公司电力科学研究院 | Post-desulphurization flue gas moisture content determination method and apparatus |
| CN103674756A (en) * | 2013-12-13 | 2014-03-26 | 神华集团有限责任公司 | Method for measuring content of moisture in high pressure liquid phase hydrocarbon substance |
| CN103698187A (en) * | 2013-12-27 | 2014-04-02 | 天津口岸检测分析开发服务有限公司 | Automatic preparation instrument and automatic distribution method of standard solution |
| CN111024887A (en) * | 2019-12-11 | 2020-04-17 | 上海仪电科学仪器股份有限公司 | Moisture determination method |
-
1997
- 1997-01-29 CN CN 97100943 patent/CN1076476C/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100368808C (en) * | 2004-04-07 | 2008-02-13 | 董慧茹 | Method and device for improving Karl Fischer water content determination |
| CN100335898C (en) * | 2005-03-08 | 2007-09-05 | 张家港市国泰华荣化工新材料有限公司 | Method for measuring water content in C1-C8 low level primary amine |
| CN102043010A (en) * | 2010-12-10 | 2011-05-04 | 毛骏尼 | Semi-automatic moisture meter |
| CN102269767A (en) * | 2011-05-09 | 2011-12-07 | 中国海洋大学 | Liquid quantitative sample injection device |
| CN102937618A (en) * | 2012-10-26 | 2013-02-20 | 河北省电力公司电力科学研究院 | Post-desulphurization flue gas moisture content determination method and apparatus |
| CN102937618B (en) * | 2012-10-26 | 2016-02-03 | 河北省电力公司电力科学研究院 | A kind of flue gas after desulfurization water capacity assay method and device |
| CN103674756A (en) * | 2013-12-13 | 2014-03-26 | 神华集团有限责任公司 | Method for measuring content of moisture in high pressure liquid phase hydrocarbon substance |
| CN103674756B (en) * | 2013-12-13 | 2016-06-08 | 神华集团有限责任公司 | Measure the method for moisture content in high pressure liquid phase hydrocarbon substance |
| CN103698187A (en) * | 2013-12-27 | 2014-04-02 | 天津口岸检测分析开发服务有限公司 | Automatic preparation instrument and automatic distribution method of standard solution |
| CN103698187B (en) * | 2013-12-27 | 2016-03-30 | 天津口岸检测分析开发服务有限公司 | A kind of standard solution configures instrument and auto-allocation method automatically |
| CN111024887A (en) * | 2019-12-11 | 2020-04-17 | 上海仪电科学仪器股份有限公司 | Moisture determination method |
| CN111024887B (en) * | 2019-12-11 | 2022-04-01 | 上海仪电科学仪器股份有限公司 | Moisture determination method |
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|---|---|
| CN1076476C (en) | 2001-12-19 |
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