CN105548075A - Device and method for detecting oxygen content in glass medicine bottle - Google Patents
Device and method for detecting oxygen content in glass medicine bottle Download PDFInfo
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- CN105548075A CN105548075A CN201610042058.1A CN201610042058A CN105548075A CN 105548075 A CN105548075 A CN 105548075A CN 201610042058 A CN201610042058 A CN 201610042058A CN 105548075 A CN105548075 A CN 105548075A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/39—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using tunable lasers
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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Abstract
The invention discloses a device and a method for detecting the oxygen content in a glass medicine bottle. According to technical scheme, a DFB laser device is subjected to current tuning, so that the light efficiency of laser comprehensively scans places near to the absorption line of oxygen; the laser device is matched with a TO5 encapsulation part and outputs laser beams with high energy density through a collimating lens assembly; a single light path is opened to penetrate through the glass medicine bottle to be detected within a short light path length; the laser beams are converted into an electric signal through a photoelectric diode by a focusing lens assembly. A weak signal detection part takes a high-precision phase lock amplifier as a core and outputs digital information of second harmonic; the digital information is transmitted to an industrial control computer for smooth data filtration and background deduction of an open space through a communication module; characteristic values are extracted and transmitted to a built concentration inversion model for processing to accurately measure the oxygen content in the glass medicine bottle. The single-light-path gas absorption system can detect oxygen residues in the colorless glass medicine bottle with the diameter greater than 16 mm.
Description
Technical field
The present invention relates to gas detection technology field, particularly the pick-up unit of oxygen content and method in a kind of glass medicine bottle.
Background technology
In medicine bottle, oxygen is the principal element affecting the quality guarantee period of medicament phase, and medicine bottle be evacuated or blanketing gas process in unavoidably to have a small amount of air remaining, oxygen proportion in bottle is caused to increase further if medicine bottle seals bad meeting, once exceed industry standard, medicine will be very possible in shelf-life endomorphism, bring very serious impact to the health of patient.
Mainly through sampling Detection, the pharmacy corporation of current more than 98% judges that whether this batch of product oxygen level be qualified, for the physical method of the medicine bottle available coarse of sampling or by relevant oxygen analyser detection.And the oxygen analyser on market mainly relies on the classic methods such as chemical colorimetry, vapor-phase chromatography, electrochemical process, magnet and oxide analysing method, these traditional analytic systems need complicated pre-service, non-damaged data cannot be realized, and measuring error is large, analysis time is long, and system maintenance work amount is large.
Summary of the invention
In order to overcome the technical matters of current medicine bottle oxygen level monitoring inconvenience, the invention provides pick-up unit and the method for oxygen content in a kind of glass medicine bottle that can detect oxygen level in medicine bottle accurately and conveniently.
In order to realize above-mentioned technical purpose, technical scheme of the present invention is,
The pick-up unit of oxygen content in a kind of glass medicine bottle.Comprise generating device of laser and laser receiver.Described generating device of laser is arranged at the side of medicine bottle to be measured.Described laser receiver is arranged at the opposite side of medicine bottle to be measured and receives the laser that generating device of laser launches.Described host computer communication connection laser receiver.
Generating device of laser comprises:
For providing the Saw-tooth Signal Waveform Generator of the sawtooth signal through adjusting the humorous signal amplitude of too low frequency modulation and frequency parameter.
For the totalizer of cumulative sawtooth signal and sine wave signal.
For adjusting laser diode modulation and the temperature controller of the working temperature parameter of laser instrument.
For generation of the laser instrument of laser.
The modulation of described Saw-tooth Signal Waveform Generator, totalizer, laser diode and temperature controller are connected successively with laser instrument.
Laser receiver comprises:
For assembling the focus lens assembly of the laser through medicine bottle to be measured.
For receiving the laser after convergence and light signal being converted to the photodetector assembly of electric signal.
For receiving and carrying out phase sensitive detection to electric signal.Select the lock-in amplifier that the numerical information of second harmonic exports.
For receiving numerical information and exporting the communication module of host computer to.
Described photodetector assembly, lock-in amplifier are connected successively with communication module.
The high-frequency tuning sine wave signal that lock-in amplifier produces after adjusting time constant, high-frequency modulation signal amplitude and frequency simultaneously delivers to totalizer.
The pick-up unit of oxygen content in described a kind of glass medicine bottle.The light frequency that described laser instrument produces covers the absorption line of oxygen.
The pick-up unit of oxygen content in described a kind of glass medicine bottle.Also comprise for making laser alignment launch to pass the collimator lens assembly of medicine bottle to be measured and the focus lens assembly for assembling the laser through medicine bottle to be measured.Described collimation lens is arranged between laser instrument and medicine bottle to be measured.Described focus lens assembly is arranged between medicine bottle to be measured and photodetector assembly.
The pick-up unit of oxygen content in described a kind of glass medicine bottle.The surface of collimation lens and condenser lens is coated with the logical plated film of 700-800nm band.
The pick-up unit of oxygen content in described a kind of glass medicine bottle.Also comprise and in glass medicine bottle, reflecting the first diaphragm of the optical noise too much caused for reducing laser and entering the second diaphragm of the optical noise that photodetector causes for eliminating parasitic light.The first described diaphragm is arranged between collimator lens assembly and tested seal glass medicine bottle.The second described diaphragm is arranged between focus lens assembly and photodetector assembly.
Oxygen content detection method in a kind of glass medicine bottle.Comprise the following steps:
Step one: gather the glass medicine bottle standard items of known oxygen content as initial modeling sample.
Step 2: every bottle of standard items are detected and obtains taking second harmonic as the testing result of expression-form.And data prediction is carried out to testing result.To obtain the high spectrum peak area of second harmonic half as eigenwert.
Step 3: linear least square fitting is carried out to the high spectrum peak area of pretreated each second harmonic half and corresponding concentration.Obtain oxygen concentration inverse model.
Step 4: Site Detection is carried out to tested glass medicine bottle and vacuum medicine bottle.Data are average, filtering, after characteristics extraction and deduction background scene process in real time.Detection data are sent to the oxygen concentration inverse model set up in step 3.Acquisition oxygen content predicts the outcome.
Oxygen content detection method in described a kind of glass medicine bottle.Before execution step one.First laser operating parameters is set.Change working temperature and the working current of laser instrument respectively.With the transmitted beam wavelength of wavemeter writing laser.Observe the absorption signal waveform after opto-electronic conversion simultaneously.Absorption peak is finally made to be in absorption signal center.
Oxygen content detection method in described a kind of glass medicine bottle.Before execution step one.First optimization system parameter.Change the delay time of the sweep amplitude of low frequency sawtooth signal and sweep frequency, the modulation amplitude of high_frequency sine wave signal and modulating frequency, phase locking unit successively.Repeatedly test.Extract secondary harmonic amplitude and obtain respective standard difference.Determine corresponding parameter value.
Oxygen content detection method in described a kind of glass medicine bottle.In described step one.Standard items at least comprise the glass medicine bottle that oxygen content is the two or more known oxygen content of 0%.
Oxygen content detection method in described a kind of glass medicine bottle.Data prediction in described step 2 comprises the following steps:
Step 1: all second harmonic signals are obtained to each modeling sample sampling and is averaged.Obtain row second harmonic data.
Step 2: gliding smoothing filtering fast processing.Gather the multiple data points about current data point.These points are carried out least square fitting with 3 order polynomials.The value of this measurement point is gone out by the polynomial computation that matching obtains.As sharpening result.
Step 3: extract half high spectrum peak area.Obtain with the sample area corresponding to the half-peak breadth of second harmonic as wavelength coverage by trapezoidal integration.The spectrum peak area of second harmonic within the scope of this.As second harmonic signal eigenwert.
Step 4: background deduction.The eigenwert obtained in step 3 is deducted the eigenwert corresponding to 0% sample in initial modeling sample.
Technique effect of the present invention is, for optical system noise, adopts collimator lens assembly and focus lens assembly, leads to plated film at its surface band, all arrange diaphragm simultaneously, eliminate optical noise to greatest extent after collimator lens assembly and before photodetector.For the high strong noise background of open space, by systematic parameter Optimal Experimental, determine corresponding parameter value, adopt high precision phase locking unit simultaneously, directly export numerical information by gpib interface, make system under the short out light path of open monochromatic light, also can accurately obtain second harmonic information.In Quantitative Prediction Model of the present invention, second harmonic eigenwert of getting is its partly high spectrum peak area, is conducive to suppressing spectral drift impact, the impact that minimizing residual amplitude modulation and other disturbance fluctuation are brought, discrimination is larger, is more suitable for the accurate quantification process of short light path, trace gas concentration.
Below in conjunction with accompanying drawing, the invention will be further described.
Accompanying drawing explanation
Fig. 1 is the one-piece construction schematic diagram of apparatus of the present invention;
Fig. 2 is the light channel structure schematic diagram of apparatus of the present invention.
Embodiment
See Fig. 1, the present embodiment is made up of Saw-tooth Signal Waveform Generator 1, totalizer 2, laser diode modulation and temperature controller 3, laser instrument 4, collimator lens assembly 5, tested seal glass medicine bottle 6, focus lens assembly 7, photodetector assembly 8, lock-in amplifier 9, gpib interface card 10, computing machine 11, first diaphragm 12 and the second diaphragm 13.Laser diode modulation and temperature controller 3 keep the working temperature constant of laser instrument 4, Saw-tooth Signal Waveform Generator 1 produces low frequency sawtooth working current, the high-frequency tuning signal that superposition lock-in amplifier 9 produces, be sent to laser diode modulation and temperature controller 3, the light output wavelength of laser instrument 4 is covered near the absorption line 760nm of oxygen.Laser instrument 4 is equipped with TO5 and encapsulates accessory, through the laser beam of the exportable high-energy-density of collimator lens assembly 5.Monochromatic light road is through after detected glass medicine bottle 6, line focus lens subassembly 7, convert light signal to electric signal by photodetector assembly 8 and export lock-in amplifier 9 to, second harmonic numerical information is selected to export, be sent to computing machine 11 by gpib interface card 10 and carry out data processing, fast and accurate measurement oxygen level.
The present embodiment have employed and makes laser alignment launch with the collimator lens assembly 5 through medicine bottle to be measured in generating device of laser, and reduce the first diaphragm 12 that laser reflects the optical noise too much caused in glass medicine bottle, the focus lens assembly 7 for assembling through the laser of medicine bottle to be measured is have employed in laser receiver, and the second diaphragm 13 of the optical noise that photodetector causes is entered for eliminating parasitic light, the introducing of these devices effectively can improve measuring accuracy during actual use, contributes to commercial Application.
The communication module of the present embodiment have employed gpib interface card as the device communicated with host computer, can select corresponding communication module according to actual needs in practice, comprises and is not limited to various communication interface, or realizes with wired and wireless.
The laser instrument that the present embodiment adopts is the Distributed Feedback Laser of continuation mode work, and centre wavelength is the absorption line 760.885nm of oxygen, TO5 encapsulation, and the spot diameter at 5cm place is 2.5mm, and Output optical power reaches 1 milliwatt.Optimal Parameters after experiment process has: laser. operating temperature is 28.25 DEG C, and working direct current is 36.1mA, and low frequency sawtooth signal frequency is 5Hz, and amplitude is 14mV, and high-frequency tuning signal frequency is 10KHz, and amplitude is 12mV.
The light frequency that LASER Light Source sends and light intensity control by its Injection Current, to be subject to DC bias current, low frequency sawtooth electric current and High Frequency Sine-wave Current joint effect in WMS system, the output wavelength of laser instrument and light intensity are approximated to linear change with Injection Current intensity.Ignore phase-modulation, if v
0for the centre frequency at oxygen absorption peak, caused by the DC bias of Injection Current, K
vfor low frequency sawtooth electric current-light frequency relation, A is sawtooth current amplitude, and high_frequency sine wave frequency modulating signal is f, and modulation amplitude is v
m, be also referred to as depth of modulation, then output frequency v (t) of laser instrument is:
v(t)＝v
0+AK
vt+v
msin(wt)(1)
Make v
c=v
0+ AK
vt, then (1) formula becomes:
v(t)＝v
c+v
msin(wt)(2)
The output intensity I of laser instrument
0t () is: I
0(t)=I'
0(t) [1+ α sin (wt)] (3)
I'
0t () represents the mean change of the output intensity caused by low-frequency current, α represents the intensity modulation coefficient that high_frequency sine wave causes.
According to Beer-Lambert law, frequency is v, and intensity is I
0t the transmitted light intensity of incident light after gas absorption of () is:
I(v,t)＝I
0(t)exp[-S(T)NLPg(v)](4)
S (T) for Absorption Line line strong, be only the function of temperature T, unit is (cm-1/ (molecule*cm-2)), N is the volumetric concentration absorbing gas, and unit is that 1, L is for absorbing optical length, unit is cm, P is the static total pressure of gas, and unit is atm, g (v) is Absorption Line linear function.
Fourier progression expanding method is pressed by by the light intensity after gas absorption:
Each harmonic component H
ncan be obtained by phase locking unit phase sensitive detection:
Because-S (T) NLPg (v) is much smaller than 1, so each harmonic component H
nfor:
Above formula shows, each harmonic component amplitude of detection signal is directly proportional to gas concentration, also be system correlation parameter as the amplitude of the centre wavelength of gas, the amplitude of low frequency sweep electric current and frequency, high-frequency modulation signal and frequency etc., generally select second harmonic signal to export.And for each selected harmonic signal, all positions in absorption region, its amplitude all with concentration proportional.So with the sample area corresponding to the half-peak breadth of second harmonic for wavelength coverage, within the scope of this, half of second harmonic high spectrum peak area S is:
Wherein,
the wavelength coverage of the sample area of Δ v corresponding to the half-peak breadth of second harmonic, h is each point height in half high spectrum peak area, and k is the concentration ratio factor that each point is corresponding.
Above formula shows, half high spectrum peak area of second harmonic is also linear with corresponding gas concentration.So, after experiment condition is determined, the amplification level of representation signal entirety is carried out with half high spectrum peak area of second harmonic component, be conducive to suppressing spectral drift impact, the impact that minimizing residual amplitude modulation and other disturbance fluctuation are brought, discrimination is larger, is more suitable for the accurate quantification process of short light path trace gas concentration.
In the present embodiment, the second harmonic sampling number getting a complete cycle is 500point, and each measuring object (comprising tested glass medicine bottle and vacuum medicine bottle) samples 10 subharmonic and carries out the data pre-service such as on average, and treatment step is specific as follows:
Step one: 10 times second harmonic signal is averaged, reduces random noise.Be averaging processing by 10 row sampled datas, obtain row second harmonic data.
Step 2: gliding smoothing filtering fast processing, suppresses system PERIODIC INTERFERENCE.I.e. image data point x
ithese points are carried out least square fitting with 3 order polynomials, go out the value of this measurement point, as sharpening result by the polynomial computation that matching obtains by left and right totally 15 points.
Step 3: the extraction of half high spectrum peak area.Obtain with the sample area corresponding to the half-peak breadth of second harmonic for wavelength coverage by trapezoidal integration, the spectrum peak area of second harmonic within the scope of this, as second harmonic signal eigenwert.
Step 4: background deduction, eliminates the oxygen impact in open path in air and reduces system spectrum drift.The eigenwert corresponding to on-the-spot vacuum medicine bottle sample is deducted by the eigenwert in step 3.
Finally, data in step 4 are sent to oxygen concentration inverse model, obtain oxygen content predict the outcome and show on computers in real time, oxygen concentration inverse model obtained by carrying out linear least square fitting to the high spectrum peak area of pretreated each second harmonic half and corresponding concentration.
Claims (10)
1. the pick-up unit of oxygen content in a glass medicine bottle, it is characterized in that, comprise generating device of laser and laser receiver, described generating device of laser is arranged at the side of medicine bottle to be measured, described laser receiver is arranged at the opposite side of medicine bottle to be measured and receives the laser that generating device of laser launches
Generating device of laser comprises:
For providing the Saw-tooth Signal Waveform Generator (1) of the sawtooth signal through adjusting the humorous signal amplitude of too low frequency modulation and frequency parameter,
For the totalizer (2) of cumulative sawtooth signal and sine wave signal,
For adjusting laser diode modulation and the temperature controller (3) of the working temperature parameter of laser instrument,
For generation of the laser instrument (4) of laser,
The modulation of described Saw-tooth Signal Waveform Generator (1), totalizer (2), laser diode and temperature controller (3) are connected successively with laser instrument (4),
Laser receiver comprises:
For assembling the focus lens assembly (7) of the laser through medicine bottle to be measured,
For receiving the laser after convergence and light signal being converted to the photodetector assembly (8) of electric signal,
For receiving and carrying out phase sensitive detection to electric signal, select the lock-in amplifier (9) that the numerical information of second harmonic exports,
For receiving numerical information and exporting the communication module (10) of host computer to,
Described photodetector assembly (8), lock-in amplifier (9) are connected successively with communication module,
Lock-in amplifier (9) the high-frequency tuning sine wave signal simultaneously produced after adjusting time constant, high-frequency modulation signal amplitude and frequency delivers to totalizer (2).
2. the pick-up unit of oxygen content in a kind of glass medicine bottle according to claim 1, is characterized in that, the light frequency that described laser instrument (4) produces covers the absorption line of oxygen.
3. the pick-up unit of oxygen content in a kind of glass medicine bottle according to claim 1, it is characterized in that, also comprise for making laser alignment launch to pass the collimator lens assembly (5) of medicine bottle to be measured and the focus lens assembly (7) for assembling the laser through medicine bottle to be measured, described collimation lens is arranged between laser instrument (4) and medicine bottle to be measured, and described focus lens assembly (7) is arranged between medicine bottle to be measured and photodetector assembly (8).
4. the pick-up unit of oxygen content in a kind of glass medicine bottle according to claim 3, is characterized in that, the surface of collimation lens (5) and condenser lens (7) is coated with the logical plated film of 700-800nm band.
5. the pick-up unit of oxygen content in a kind of glass medicine bottle according to claim 4, it is characterized in that, also comprise and in glass medicine bottle, reflecting first diaphragm (12) of the optical noise too much caused for reducing laser and entering second diaphragm (13) of the optical noise that photodetector causes for eliminating parasitic light, described the first diaphragm (12) is arranged between collimator lens assembly (5) and tested seal glass medicine bottle (6), described the second diaphragm (13) is arranged between focus lens assembly (7) and photodetector assembly (8).
6. an oxygen content detection method in glass medicine bottle, is characterized in that, comprise the following steps:
Step one: gather the glass medicine bottle standard items of known oxygen content as initial modeling sample;
Step 2: detect every bottle of standard items and obtain taking second harmonic as the testing result of expression-form, and carry out data prediction to testing result, to obtain the high spectrum peak area of second harmonic half as eigenwert;
Step 3: linear least square fitting is carried out to the high spectrum peak area of pretreated each second harmonic half and corresponding concentration, obtains oxygen concentration inverse model;
Step 4: Site Detection is carried out to tested glass medicine bottle and vacuum medicine bottle, data are average, filtering, after characteristics extraction and deduction background scene process in real time, detection data are sent to the oxygen concentration inverse model set up in step 3, obtain oxygen content and predict the outcome.
7. oxygen content detection method in a kind of glass medicine bottle according to claim 6, it is characterized in that, before execution step one, first laser operating parameters is set, change working temperature and the working current of laser instrument respectively, with the transmitted beam wavelength of wavemeter writing laser, observe the absorption signal waveform after opto-electronic conversion simultaneously, finally make absorption peak be in absorption signal center.
8. oxygen content detection method in a kind of glass medicine bottle according to claim 7, it is characterized in that, before execution step one, first optimization system parameter, change the delay time of the sweep amplitude of low frequency sawtooth signal and sweep frequency, the modulation amplitude of high_frequency sine wave signal and modulating frequency, phase locking unit successively, repeatedly test, extract secondary harmonic amplitude and obtain respective standard difference, determining corresponding parameter value.
9. oxygen content detection method in a kind of glass medicine bottle according to claim 7, is characterized in that, in described step one, standard items at least comprise the glass medicine bottle that oxygen content is the two or more known oxygen content of 0%.
10. oxygen content detection method in a kind of glass medicine bottle according to claim 9, it is characterized in that, the data prediction in described step 2 comprises the following steps:
Step 1: all second harmonic signals are obtained to each modeling sample sampling and is averaged, obtain row second harmonic data;
Step 2: gliding smoothing filtering fast processing, gathers the multiple data points about current data point, these points is carried out least square fitting with 3 order polynomials, goes out the value of this measurement point, as sharpening result by the polynomial computation that matching obtains;
Step 3: extract half high spectrum peak area, obtain with the sample area corresponding to the half-peak breadth of second harmonic for wavelength coverage by trapezoidal integration, the spectrum peak area of second harmonic within the scope of this, as second harmonic signal eigenwert;
Step 4: background deduction, deducts the eigenwert corresponding to 0% sample in initial modeling sample by the eigenwert obtained in step 3.
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