CN1034269A - Multi-beam atom-absorbing spectrograph - Google Patents
Multi-beam atom-absorbing spectrograph Download PDFInfo
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- CN1034269A CN1034269A CN 88105002 CN88105002A CN1034269A CN 1034269 A CN1034269 A CN 1034269A CN 88105002 CN88105002 CN 88105002 CN 88105002 A CN88105002 A CN 88105002A CN 1034269 A CN1034269 A CN 1034269A
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Abstract
This invention belongs to instrument field for a kind of Atomic Absorption Spectrometer.It is used to the various trace elements content in the automatic analysis of liquid sample on the commercial production flow process.The principal character of this invention is that radiation source has also adopted the light made from the multiple-limb fibre-optic bundle to converge device except that adopting many hollow cathode lamps, the characteristic spectral line of many elements to be measured that many hollow cathode lamps are sent pools a branch of light, makes light beam carry out multielement by atomizer then and analyzes simultaneously.Adopt this technology can avoid the mechanical wear that the lamp method causes of changing of passing through, can improve the reliability and stability of instrument.
Description
This invention belongs to instrument field, particularly relevant a kind of Atomic Absorption Spectrometer.
Atomic Absorption Spectrometer (or claiming atomic absorption spectrophotometer (AAS)) is an analytical instrument commonly used in the present laboratory.This kind instrument is used to analyze the trace element that contains in the liquor sample.General Atomic Absorption Spectrometer mainly is made up of radiation source, atomizer, optical splitter, detector, electric wiring and computing machine six parts.The ultimate principle of atomic absorption spectroscopy is that the characteristic spectral line that radiation source sends element to be measured is absorbed by the ground state atom of element to be measured in the atomizer, will disturb the spectral line discharge through optical splitter.Receive characteristic spectral line after being absorbed by detector.Characteristic spectral line according to element to be measured is absorbed the degree that weakens, and is obtained by the content of element to be measured in the sample by lambert beer law.The commercial apparatus of current atom absorption spectrometer all is being used to chamber, is used for the Atomic Absorption Spectrometer that the industrial manufacture process flow process analyzes automatically and does not also have
The radiation source of modern general Atomic Absorption Spectrometer all is to adopt many hollow cathode lamps, for example 6, be installed on the revolvable lamp bracket, and lamp bracket is by direct motor drive.Per minute is analysed the element a kind of to be measured in the sample.The lamp bracket rotation once inserts light path with corresponding lamp, if analyze 6 kinds of elements, needs rotation 6 times, and to being used for the instrument in laboratory, this radiation source can meet the demands.But when this instrument was used for the industrial manufacture process flow process and analyzes automatically, there were two problems in this radiation source, the one, and long-term rotary lamp frame can cause mechanical wear, makes optical system for alignment produce difficulty; The 2nd, long-term rotary lamp frame, the reliability of instrument is difficult to guarantee.
The purpose of this invention provides a kind of Atomic Absorption Spectrometer that the industrial manufacture process flow process is carried out on-line automatic analysis that is used for.
The complete machine structure of this invention shown in Fig. 1 (Fig. 1 is a multi-beam atom-absorbing spectrograph complete machine structure synoptic diagram), it by radiation source, automatically the sampling and sample pretreatment device (18) atomizer, optical splitter, detector, electric wiring and computer system seven parts form.
The radiation source of this invention is the multielement radiation source, and it is by many fixing hollow cathode lamps of arranging (1 to 6), and hollow cathode lamp power supply (15) and light converge device and forms.Light converges device and is made up of the lens (7 to 12,14) at multiple-limb fibre-optic bundle (13) on the fixed support that is installed between hollow cathode lamp (1 to 6) and the flame atomizer (16) and two ends thereof, the multiple-limb end of multiple-limb fibre-optic bundle (13) scatter, and passes through the centrally aligned of lens (7 to 12) and corresponding hollow cathode lamp (1 to 6) respectively; And flame atomizer (16) is aimed at through lens (14) in the pool side of multiple-limb fibre-optic bundle (13).Requiring this kind multiple-limb fibre-optic bundle (13) to see through wavelength smoothly is black light and the visible lights of 200 nanometers to 750 nanometers.The function that light converges device is that the characteristic spectral line of many elements to be measured that many hollow cathode lamps (1 to 6) are sent pools a branch of light, and light beam is analyzed so that carry out multielement simultaneously by atomizer.
The automatic sampling of this invention and sample pretreatment device are shown in Fig. 2 (Fig. 2 takes a sample and sample pretreatment device synoptic diagram automatically).This device is to the automatic sampling part of different technological process of productions difference slightly.Fig. 2 is applicable to the situation that fluid to be measured circulates in transporting chute.P1 and P2 are the liquid pump among Fig. 2, and GV1 is the solenoid valve of 15 millimeters of diameters, and EV1 is the solenoid valve of 6 millimeters of diameters to EV17, (47) be the fluid to be measured transporting chute, (48) are coarse filter, and (49) are sampling jar, (50) be distilled water container, (51) be water constant volume bottle, (52) are sample constant volume bottle, and (53) are reaction cup, (54) be magnetic stirrer, (55) be filtrator, (56) are the sample cup, and (57) are distilled water bottle.The function of this device is to fetch sample apace from the technological process of production, and filter, sample pretreatment operations such as constant volume and dilution, give atomizer with the sample of cleaning.The running program of this device is as follows: open valve GV1 and EV1 and pump P1, fluid to be measured is flowed out by chute (47) bottom, returns chute (47) after filtering through coarse filter (48).Shut-off valve EV1 when sampling, open valve EV2 and EV3, the sample stream after then being filtered by coarse filter (48) is crossed sampling jar.Through after several seconds, shut-off valve EV2 and EV3, open valve EV1, then sample is taken in the sampling jar (49).Open valve EV4 and EV5, sample flow in the sample constant volume bottle (52), and unnecessary sample flows out from the overflow vent on bottle top, makes sample obtain constant volume.Open valve EV8, sample flows into reaction cup (53), remaining sample in the water flushing sample constant volume bottle (52) in the open valve EV7 water constant volume bottle (51), the sample in the diluting reaction cup (53) simultaneously.Generally need tens of times of dilutions.Starting magnetic stirrer (54) stirs sample.Open valve EV9, EV10 and EV12 open pump P2 then, and sample stream is crossed filtrator (55), discharges from valve EV12.This part sample is not wanted, because the sample of incipient stage may be diluted by water remaining in valve, pump and the pipeline.Through after several seconds, open valve EV11 and shut-off valve EV12, then the sample of cleaning flows in the sample cup (56), and when needs were analyzed, open valve EV16, sample just were inhaled in the flame atomizer (16). alliance garden is from Ρ 3 after each sampling finishes), filtrator (55), sample cup (56) etc. clean, its operation is as follows: open valve EV6 is to EV10 and EV14 and pump P2, then reaction cup (53) is rinsed.Secondly, open valve EV13, shut-off valve EV10, then filtrator (55) is reversed flushing.Then, open valve EV11, EV12 and EV15, then sample pipeline and sample cup (56) are cleaned.
The atomizer of this invention is (Fig. 3 is the atomizer synoptic diagram) as shown in Figure 3, and it is made up of flame atomizer (16) and combustion controller 17.Flame atomizer is that its function of general-purpose device is to make the liquor sample solution atomization, makes fuel (for example acetylene) burning that enters in the flame atomizer simultaneously.Utilize the high temperature of combustion flame to make the sample after the atomizing remove moisture and make the element in the sample become ground state atom.The building block that all belongs to combustion controller among Fig. 3 except that (16), (18) has air compressor (58), acetylene steel alkynes (59), pneumatic setter (60 and 61), tensimeter (62 and 63), flow controller (64,65 and 66), flowmeter (67,68 and 69), nozzle (70), igniting resistance silk (71), flame eye (72), fire monitor (73) and solenoid valve (EV18 is to EV22).The function of combustion controller is the correct igniting of control flame atomizer and flame-out, and its running program is as follows: start air compressor (58), open valve EV18.When air manometer (62) is indicated at 2.3kg/cm
2More than reach the acetylene pressure gauge indication at 0.6kg/cm
2Allow to carry out next step program when above.Above-mentioned pressure just often, open valve EV19 and EV20, igniting resistance silk (71) energising, secondly open valve EV21 and EV22, flame atomizer (16) igniting.Shut-off valve EV22, igniting resistance silk (71) outage.When lighting a fire just often, flame eye sends signal and allows to carry out analysis operation.If undesired, then shut-off valve EV18 and EV21 at once, and send alerting signal.After analysis operation finishes, stop working shut-off valve EV18 and EV21.When flame-out normal, flame eye sends signal and allows to carry out next step program.If undesired, then send alerting signal.Close EV19 and EV20 at last, stop air compressor (58).At the whole run durations of instrument, if the fire monitor sends warning, then shut-off valve EV18 and EV21 at once.
The optical splitter of this invention as shown in Figure 1, it is made up of lens (19), entrance slit (20), plane mirror (21), concave grating (22) and exit slit (23 to 28).Its function is the light that a branch of light of many characteristic spectral lines that contain different elements that will be injected by entrance slit (20) is dispersed into the characteristic spectral line of many different elements, penetrates from exit slit (23 to 28) respectively.
The detector of this invention is that (29 to 34) its function among many general photomultipliers such as Fig. 1 is the light that receives respectively by the characteristic spectral line of the different elements of optical splitter outgoing, and converts thereof into electric signal.The electric wiring of this invention is made up of (35 to 40) among amplifier such as Fig. 1 and power supply (41), and its function is that the electric signal that photomultiplier is sent here is amplified, and gives computer system then.The computer system of this invention is made up of analog to digital converter (42), meter computing machine (43), keyboard (44), printer (45) and display (46), the function of computer system is the electric signal that reception amplifier (35 to 40) is sent here, through showing and print the content of various tested elements in the sample after the data processing, also to control the action that spectrometer complete machine each several part is coordinated simultaneously, to finish analysis task automatically.
The spectrometer complete machine of this invention is analyzed on the industrial manufacture process flow process automatically by computer system control, and its running program is as follows.
1. complete machine energising: connect computer power supply, carry out preheating.Except not lighting the hollow cathode lamp, connect each circuit power of instrument, carry out preheating.
2. measure and select: divide one-shot measurement and circulation to measure two kinds.When selecting one-shot measurement, stop automatically after the measurement once measuring.When selecting circulation to measure, at regular intervals every measuring once.Need give stop signal when stopping as need.Measure and select signal to send into through keyboard, also can send by the computing machine of upper level by the operator.
3. process of measurement:
(1) checks and write down each road value at electric zero point, will report to the police when exceeding certain limit.
(2) light hollow cathode lamp, preheating 10 minutes.
(3) light flame atomizer, preheating 3 minutes; Spray blank water sample, clean the slit of atomizer.
(4) spray blank water sample, check and write down each road transmittance values.To report to the police when surpassing certain limit.Start sampling and sample pretreatment device automatically simultaneously, to the fluid to be measured on the technological process of production take a sample, pretreatment operation such as filtration, constant volume and dilution.
(5) the spray sample solution writes down each road transmittance values, through after the Computer Processing, shows and prints the tested component concentrations value in each road.
(6) clean sampling and sample pretreatment device automatically.
When (7) selecting one-shot measurement, after aforesaid operations finished, flame atomizer was flame-out, and the hollow cathode lamp outage when selecting circulation to measure, through certain hour at interval, repeats above-mentioned 4,5 and 6 three step programs.
4. circulation is measured and stopped: this signal is sent by the computing machine of operator or upper level.After signal sent, flame atomizer was flame-out, the hollow cathode lamp outage.
Multi-beam atom-absorbing spectrograph of the present invention is when carrying out multielement analysis, can avoid changing the caused mechanical wear of lamp method, when whole optical systems of instrument are analyzed on the industrial manufacture process flow process automatically without any the mechanical activity part, thereby improve the reliability and stability of instrument.
The present invention can be applicable to departments such as metallurgy, chemical industry, oil, electric power, light industry and environmental protection, and it can be used to the various trace elements content in the on-line measurement liquor sample on the technological process of production.All elements at laboratory Atomic Absorption Spectrometer energy measurement, the present invention all can measure.
Claims (3)
1, a kind of Atomic Absorption Spectrometer that includes radiation source, atomizer, optical splitter, detector, electric wiring and computer system is characterized in that:
(1) this Atomic Absorption Spectrometer also contains automatic sampling and sample pretreatment device;
(2) radiation source of this Atomic Absorption Spectrometer is that hollow cathode lamp power supply and light converge device and forms by many fixing hollow cathode lamps of arranging.
2, it is with the lens composition of the multiple-limb fibre-optic bundle that can see through black light that wavelength be the 200-750 nanometer and visible light smoothly with its two ends that Atomic Absorption Spectrometer as claimed in claim 1, the light that it is characterized in that constituting this Atomic Absorption Spectrometer radiation source part converge device.
3,, it is characterized in that the multiple-limb fibre-optic bundle that said light converges device is fixed on the fixed support as claim 1,2 described Atomic Absorption Spectrometers; The multiple-limb end of multiple-limb fibre-optic bundle scatter, and passes through the centrally aligned of lens and corresponding hollow cathode lamp respectively, and the pool side of multiple-limb fibre-optic bundle is through the lens alignment flame atomizer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88105002 CN1034269A (en) | 1988-01-12 | 1988-01-12 | Multi-beam atom-absorbing spectrograph |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88105002 CN1034269A (en) | 1988-01-12 | 1988-01-12 | Multi-beam atom-absorbing spectrograph |
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| Publication Number | Publication Date |
|---|---|
| CN1034269A true CN1034269A (en) | 1989-07-26 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 88105002 Pending CN1034269A (en) | 1988-01-12 | 1988-01-12 | Multi-beam atom-absorbing spectrograph |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101408505B (en) * | 2007-10-11 | 2011-01-05 | 上海光谱仪器有限公司 | Method for evaluating 'double-way linearity and balance' performance of electric detection system of spectrometer |
| CN104865206A (en) * | 2015-04-24 | 2015-08-26 | 上海伯顿医疗设备有限公司 | Single photoelectric tube five-channel atomic absorption spectrometer |
-
1988
- 1988-01-12 CN CN 88105002 patent/CN1034269A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101408505B (en) * | 2007-10-11 | 2011-01-05 | 上海光谱仪器有限公司 | Method for evaluating 'double-way linearity and balance' performance of electric detection system of spectrometer |
| CN104865206A (en) * | 2015-04-24 | 2015-08-26 | 上海伯顿医疗设备有限公司 | Single photoelectric tube five-channel atomic absorption spectrometer |
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