The mensuration part of carbon and sulfur automatic analyzer
Technical field
The utility model relates to a kind of chemical composition analysis instrument, particularly a kind of carbon and sulfur automatic analyzer that is used for measuring the massfraction (percentage composition) of metals such as steel, iron, alloy and ore, coke or two kinds of elements of nonmetal carbon sulphur.
Background technology
At present, departments such as industries such as domestic metallurgy, mineral products, iron and steel, casting, machinery, building and quality technical supervision, colleges and universities institutes, use the infrared carbon sulfur analyzer of import except some national large enterprises, primary study laboratory, most enterprises and institutions all adopt quasi-instrument hand-manipulated to measure the percentage composition of carbon, sulphur two elements.This carbon and sulfur analytical instrument comprises measures part (comprise and survey sulphur part, carbon determination part) and control section, and control section is a prior art, no longer describes.The described survey sulphur part of measuring in the part, comprise welding bottle, by pipeline and welding bottle be docile and obedient preface polyphone purification pipe, combustion furnace, dust removing tube, flowmeter, iodine, the sulfur-absorbing cup of starch mixed liquor, buret, iodine liquid bottle are housed, iodine liquid bottle is connected with welding bottle again, and relevant position is provided with solenoid valve in pipeline.The described survey sulphur of measuring in the part partly comprises eudiometer, the leveling bottle of being docile and obedient the preface polyphone by pipeline and described sulfur-absorbing cup, and leveling bottle is connected with described welding bottle again; Eudiometer is connected with the carbon absorption bottle that potassium hydroxide solution is housed by pipeline.
When measuring the content of sulphur, operating personnel will lean on the situation of visual titration intraluminal fluid position variation and the situation of the mixed liquor change color in the sulfur-absorbing cup to judge titration end-point, and randomness is very big, and the result often causes personal error bigger.When measuring the content of carbon, operating personnel will estimate the situation of liquid level change in eudiometer; Thereby calculate the content of carbon.Because be range estimation, personal error is bigger.
Though some instrument adopts the amplification of electronic circuit signal or singlechip technology and has increased functions such as gauge outfit demonstration on the basis of manual titrator, but fundamentally do not change the method for " range estimation ", so its systematic error is big, these deficiencies that wait slowly complicated, measuring speed of manually-operated still can not make users really satisfied.
Summary of the invention
The technical problems to be solved in the utility model is exactly that existing carbon and sulfur analytical instrument is because of need range estimation liquid level change and mixed liquor change color, the problem that cause that the test result error is big, test process is complicated, operation is loaded down with trivial details provides that a kind of analysis speed is quick, test result is accurate, the mensuration part of easy and simple to handle, stable performance, carbon and sulfur automatic analyzer that maintenance cost is cheap.
The mensuration part of carbon and sulfur automatic analyzer described in the utility model comprises at least surveys the sulphur part, this survey sulphur partly comprises welding bottle, by pipeline and welding bottle be docile and obedient preface polyphone purification pipe, combustion furnace, dust removing tube, flowmeter, iodine, the sulfur-absorbing cup of starch mixed liquor, buret, iodine liquid bottle are housed, iodine liquid bottle is connected with welding bottle again, and relevant position is provided with solenoid valve in pipeline; Buret is provided with the pressure transducer of liquid level change in contact pilotage and the reaction buret, the photoelectric sensor of the mixed liquor change color that responds in the mixed liquor in sulfur-absorbing cup.
Because the pressure transducer of liquid level change in the reaction buret is set on buret, the photoelectric sensor of reaction mixture change color is set in the mixed liquor in sulfur-absorbing cup, so when measuring the content of sulphur, do not need the situation of operating personnel's visual titration intraluminal fluid position variation and the situation of the mixed liquor change color in the sulfur-absorbing cup, and by the situation of liquid level change in the pressure transducer induction buret, by the situation that photoelectric sensor induction mixed liquor change color changes, eliminated personal error.
As to improvement of the present utility model, it is measured part and comprises also that carbon determination part, this carbon determination partly comprise by pipeline and described sulfur-absorbing cup and be docile and obedient eudiometer, the leveling bottle that preface is contacted that leveling bottle is connected with described welding bottle again; Eudiometer is connected with the carbon absorption bottle that KOH solution is housed by pipeline, and eudiometer is provided with the pressure transducer of liquid level change in the reacting dose inflator; Leveling bottle is provided with contact pilotage.
Because eudiometer is provided with the pressure transducer of liquid level change in the reacting dose inflator, so when measuring the content of carbon, do not need operating personnel to estimate the situation of liquid level change in the eudiometer, and, eliminated personal error by the situation of liquid level change in the pressure transducer induction eudiometer.
Further improve as the mensuration part to above-mentioned carbon and sulfur automatic analyzer, it comprises that also one is equipped with the carbon absorption bottle of soda lime its carbon determination part, and it is connected on the carbon absorption bottle and the pipeline between the eudiometer that KOH solution is housed; Be connected with solenoid valve on the pipeline between described two carbon absorption bottles; On the pipeline between welding bottle and iodine liquid bottle, the leveling bottle, be respectively arranged with solenoid valve; On the pipeline between sulfur-absorbing cup and buret, the eudiometer, be respectively arranged with solenoid valve.
Mensuration part for any carbon and sulfur automatic analyzer recited above is provided with constant volume tube in sulfur-absorbing cup, this constant volume tube is connected with a waste liquid bottle by pipeline again, also is connected with solenoid valve on this pipeline.
For the mensuration part of any carbon and sulfur automatic analyzer recited above, described combustion furnace is the arc burning stove.
The beneficial effects of the utility model.Mensuration part described in the utility model and existing control section combine, and can form a carbon and sulfur automatic analyzer.Control section comprises A/D conversion, programmed control and result's demonstration, printing etc., because of it is a prior art, no longer describes.This carbon and sulfur automatic analyzer analysis speed is quick, test result is accurate, easy and simple to handle, stable performance, maintenance cost are cheap.
One, energy consumption is little
When the utility model adopts the arc burning stove, be to reach the purpose of sample perfect combustion, its little power consumption, 4000 samples of electric energy analysis once with under excess oxygen, ignite heat that sample produces by specimen reaction of electric arc firing method; Sample burning rate fast (about 6 seconds); Master Cost is few, and a copper earthenware snail can be analyzed more than 3600 times, only 15 yuan.And existing analyser Chang Peiyong's is tubular furnace, this equipment before starting working, must heat up 1-2 hour can operate as normal, and burning sample speed slow (about 60 seconds/time), power consumption simultaneously big (per hour about 4 degree of power consumption), sample of every test needs porcelain boat of loss (0.5 yuan /): also need often to change porcelain tube, ferrosilicon rod simultaneously, consume greatly the cost height.
Two, measure high speed, accurate
1, for the analysis of carbon
Existing analyser is manually to lift bottle to cause liquid level official post carbon dioxide to enter the carbon absorption bottle, reads the convert percentage composition of carbon of scale (range estimation) according to the volume differences that absorbs front and back.This measure not only labour intensity greatly and is only read scale with the human eye range estimation and is caused artificial reading error easily.Adopting the carbon and sulfur analytical instrument of this mensuration part is that the solenoid valve conduction gas circuit makes carbon dioxide enter the carbon absorption bottle by hydraulic method, the pressure reduction that produces according to liquid level change in the eudiometer produces the percentage composition that different magnitudes of voltage and standard substance reference entr screen directly show mensuration by pressure transducer, eliminates artificial reading error.
2, for the analysis of sulphur
It is that sulphuric dioxide enters sulfur-absorbing cup by manual titration iodine titer that existing analyser is decided sulphur, and the range estimation terminal point is with the standard substance reference, according to the convert percentage composition of sulphur of the milliliter number that consumes iodine liquid.This measure easily causes manual titration's speed to be difficult to grasp, range estimation terminal colour disunity, and difficult the grasp causes the test result personal error big, and precision is not high.Adopting the carbon and sulfur analytical instrument of this mensuration part is to enter sulfur-absorbing cup by sulphuric dioxide, produce different strong and weak electric currents by photoelectric sensor according to change in color, by control section control fast, middling speed, the rate of titration of iodine liquid at a slow speed, make reference with standard substance, according to the liquid level difference of iodine liquid in the buret, produce different voltage then, through the A/D conversion by pressure transducer, calculate the percentage composition of sulphur, and output screen shows.Thoroughly like this effect a radical cure the personal error that manual titration causes with human eye visualization of color terminal point, thereby both guaranteed precision, improved speed again.
3, the change of calibrating method
Adopt the carbon and sulfur analytical instrument of this mensuration part to set up standard regression equation, working curve, carried out the multiple spot calibration, overcome and a bit calibrated defective, thereby further widened test specification, more guaranteed the precision of test.
The foundation of regression equation, working curve: the standard specimen of 3-5 different carbon content of test, sulfur content, each value (being carbon content, sulfur content) of the standard specimen that provided is imported in computer, according to the different electrical signals that produces by each sensor, simulate the working curve and the storage of surveying sulphur, carbon determination respectively, for the use of measuring unknown sample.
Adopt the carbon and sulfur analytical instrument of this mensuration part, its sensor produces different magnitudes of voltage and changes through A/D, by carbon content, the sulfur content of control section according to standard substance, and the carbon content of conversion measured object, sulfur content, output screen shows, and print result as required.
Description of drawings
Fig. 1 is the structural representation of a kind of embodiment.
Embodiment
The utility model is described in further detail below in conjunction with accompanying drawing.
Embodiment shown in Fig. 1 is the structural representation of carbon and sulfur automatic analyzer, and it comprises measures part and control section.Control section comprises A/D conversion, programmed control and result's demonstration, printing etc., because of it is a prior art, no longer describes.
One, preoperative preliminary work
Open arc burning stove power supply and carry out preheating, open again and subtract air valve 2 and connect oxygen.The start-up control part enters duty.The copper crucible that is loaded with sample is placed in the arc burning body of heater rising lower furnace body 6 and upper furnace body 5 sealings.
16,26,39,31 energisings of control section control electromagnetic valve are opened, oxygen pressure in one road pipeline makes that acid solution is pressed in the eudiometer 24 in the leveling bottle 17, when wherein liquid rises to when running into electrode 23, the electric action of liquid, electrode 23 and electrode 18 are short-circuited, solenoid valve 16,26 outages are closed.At this moment measure in the gas letter and be full of acid solution.
Another road oxygen enters in the iodine liquid bottle 38 through solenoid valve 39, and the iodine liquid in this bottle is flowed in the waste liquid bottle through constant volume tube 30.Be short-circuited when running into electrode 36,37 when the iodine liquid in the buret 34 rises to, solenoid valve 39,31 outages are closed, excessive iodine liquid then is back in the iodine liquid bottle.
Two, survey sulphur principle of work and process
After the preliminary work before the complete operation, control section is opened solenoid valve 3,11 energisings, and oxygen then purifies by the interior purification pipe 4 that lime chloride and soda lime are housed, and the oxygen after purifying is in quartz ampoule enters body of heater.At interval after several seconds, copper electrode 14 arc automatic starting make sample 8 in the copper crucible 7 when reaching certain temperature (about 1375 ℃), burning rapidly under excess oxygen, and the Main Ingredients and Appearance that the burning back generates is O
2, CO
2, SO
2Mixed gas, enter in the sulfur-absorbing cup 28 through the spinner-type flowmeter of dust removing tube 9 and flow control 80-120l/h and solenoid valve 11, the condenser pipe 32 that energising is being opened.Iodine, starch mixed liquor are housed, H wherein in sulfur-absorbing cup
2O and SO
2Gas generation chemical reaction generates H
2SO
3, and H
2SO
3Discoloration iodine, starch solution are faded, promptly become colorless by blue look.Be contained in two photoelectric sensors 19 on the sulfur-absorbing cup and can be at any time produce different electric signal according to the change color of iodine, starch solution, this electric signal imports in the control section again immediately, by control section come again control electromagnetic valve 33 carry out soon, in, the titration of slow three kinds of modes, when wherein iodine makes H
2SO
3All be oxidized to H
2SO
4The time, be that titration finishes when returning to original blue look when initial again, solenoid valve 33 outages are at this moment closed, and stop titration.Mail to control section and be installed at the electric signal that the pressure transducer 35 on the buret 34 produces the liquid level difference before and after the titration that receives, calculate the percentage composition of trying to achieve sulphur according to this signal and relevant criterion regression equation by control section.
Three, carbon determination principle of work and process
After survey sulphur was finished, control section was opened solenoid valve 27 energisings, and under the pressure of oxygen transmitted, (Main Ingredients and Appearance was O to the mixed gas after absorbing in the sulfur-absorbing cup 28 like this
2, CO
2) again in the inlet inflator 24, the acid solution force feed that is full of in the amount gas cylinder in leveling bottle 17; When the acid solution in the leveling bottle 17 rises to when running into electrode 19, electric action by this solution is short-circuited electrode 18 and 19 at electrode, solenoid valve 27 outages are closed, the circuit of connecting solenoid valve 26 is simultaneously opened it, make gaseous tension and atmospheric pressure balance in the eudiometer 24 like this, finish zero process.After several seconds, 26 outages of control section control electromagnetic valve are closed at interval, and solenoid valve 16,21 energisings are opened, and under the pressure of oxygen, again the acidic aqueous solution in the leveling bottle 17 are pushed back in the eudiometer 24 mixed gas (the O in the eudiometer 24
2, CO
2) then be pressed towards in the carbon absorption bottle 20, the soda lime that is equipped with in the carbon absorption bottle 20 12 is just and CO
2Gas reacts, and sponges a part of CO
2Remaining mixed gas is pressed into behind solenoid valve 21 in another carbon absorption bottle 22,13 of KOH solution that is equipped with in the carbon absorption bottle 22 and CO
2Gas generation chemical reaction carries out absorbing the second time, and oxygen is pressed into the KOH solution 13 of internal layer the skin of carbon absorption bottle 22.When the acidic aqueous solution in the eudiometer 24 is run into electrode 23, electrode 23 and electrode 18 are short-circuited, solenoid valve 16 outages are closed and logical atmosphere, KOH solution 13 under this state in the carbon absorption bottle 22 is flowed in the internal layer by skin again, when KOH solution is gone up 43 tops of the float in the internal layer, acidic aqueous solution in the eudiometer stops to descend, like this because CO
2Being absorbed of gas just produced liquid level difference in the eudiometer 24.At interval after several seconds, 3,11,21 outages of control section control electromagnetic valve are closed, and be installed at the liquid level difference of the acidic aqueous solution before and after twice absorption that the pressure transducer 25 on the eudiometer 24 will receive and the electric signal that produces mails to control section, calculate the percentage composition of trying to achieve carbon by control section according to this signal and relevant criterion regression equation.
Present embodiment is used for the mensuration of material carbon such as iron and steel, alloy, ore, coke, sulphur percentage composition, being specially carbon is 0.01-6.00%, change sample weighting amount and can be extended to about 8.00%, sulphur is 0.001-2.00%, and changing sample weighting amount and vs concentration can be extended to about 3%.Analytical error all meets or is better than GB standard GB/T223.69-1997 and CB/T123.68-1997; Minute is as if not containing sampling, claiming the sample time then to have only about 60 seconds; Working environment there is not specific (special) requirements, room temperature 5-40 ℃, atmospheric pressure 680-780mmHg.The present embodiment trinity, both carbon determination or sulphur separately, but carbon sulphur translocation again.
Present embodiment makes sample burning, light-operated titration, data acquisition, data computation, result show, print and finish automatically by means of Computer Control Technology and sensing technology, so automaticity is very high, simple to operate, measure fast, accurately, consumptive material is few, maintenance cost is extremely low.