CN105044042A - Concentration detection method of manganese in trace amount in drinking water and waveguide used therein - Google Patents
Concentration detection method of manganese in trace amount in drinking water and waveguide used therein Download PDFInfo
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- CN105044042A CN105044042A CN201510235554.4A CN201510235554A CN105044042A CN 105044042 A CN105044042 A CN 105044042A CN 201510235554 A CN201510235554 A CN 201510235554A CN 105044042 A CN105044042 A CN 105044042A
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- manganese
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Abstract
The invention relates to a concentration detection method of manganese in trace amount in drinking water and a waveguide used therein. The concentration detection method includes the following steps: 1) with a strong oxidant, oxidizing manganese ions in the drinking water to form MnO4<-> ion to obtain a sample for later use; 2) through a peristaltic pump, outputting the sample into a sample chamber of the waveguide; and 3) irradiating the surface of the waveguide by laser, receiving a reflected light through CCD and detecting the gray level of the center of a black line through the CCD and calculating the concentration of manganese in trace amount. The waveguide is formed by assembling flat sheet glass, a glass gasket and a glass substrate from top to bottom, wherein an upper metal film layer is deposited on the upper surface of the flat sheet glass and a lower metal film layer is deposited on the upper surface of the glass substrate. The glass gasket is provided with a sample inlet and a sample outlet, and the space in the glass gasket is the sample chamber.
Description
Technical field
The present invention relates to and a kind ofly drink Trace Manganese in Water concentration detection method and the waveguide for the method.
Background technology
Manganese is one of necessary trace element of human body and animals and plants, but the manganese of excess intake then can produce ill-effect to body.Manganese enters human body by water and food, in organ-tissue enrichments such as liver, kidney, brains, and produces infringement in various degree to the breathing of people, nerve and reproductive system.
Therefore, to the detection of Fe content in water, for ensureing that health has great importance.
In current detection water, the common method of Fe content has following several: atomic absorption method, the mensuration of manganese in water can be directly used in, because the method has the features such as anti-interference, sensitivity is higher, accuracy is good, widespread use in the industries such as environmental protection, edge gold medicine, but it measures process technology and requires higher, instrument needs the atomising device of the sample solution of manganese, and testing cost is higher.By Formaldehyde Oxime Method application is comparatively wide, in the world one of analytical approach becoming standard.But By Formaldehyde Oxime Method reagent used is not easy to preserve.Potassium metaperiodate oxidizing process selectivity is better, be often used, but sensitivity is lower, cannot be used in the detection of drinking Trace Manganese in Water concentration.
Summary of the invention
Goal of the invention of the present invention is that providing a kind of drinks Trace Manganese in Water concentration detection method and the waveguide for the method, and to drinking, Trace Manganese in Water Concentration Testing is effective, and testing cost is low, easy to operate.
The present invention is based on same inventive concept, there are two independent technique schemes:
1, one drinks Trace Manganese in Water concentration detection method, it is characterized in that:
Utilize strong oxidizer that the manganese ion in potable water is oxidized to mauve ion
ion, for subsequent use as sample;
Utilize peristaltic pump by the sample chamber of above-mentioned sample output waveguide;
Irradiate the surface of waveguide with laser, receive reflected light with CCD, by the gray scale of CCD detection black line center, calculate and obtain Trace Amount Manganese concentration.
Irradiate the surface of waveguide with the laser that wavelength is 532nm, the angle of divergence of laser is less than 0.3mrad.
Utilize strong oxidizer that the manganese ion in potable water is oxidized to mauve ion
during ion, the reducing substances in potable water and chlorion need be removed, utilize H
3pO
4the red Fe sheltered in potable water
3+.
Strong oxidizer is potassium metaperiodate or ammonium persulfate.
2, an above-mentioned waveguide of drinking Trace Manganese in Water concentration detection method, is characterized in that: sheet glass, glass seal, glass substrate from top to bottom fit together; The upper surface of sheet glass deposits upper strata metal film, and the upper surface of glass substrate deposits lower metal film; Glass seal has sample inlet and sample export, and the space in glass seal is sample chamber.
The material of upper strata metal film is silver, and the thickness of upper strata metal film is 35nm.
The material of sheet glass is optical glass, and its thickness is 300 μm.
The material of glass seal is optical glass, and its thickness is about 500 μm.
The material of lower metal film is silver, and its thickness is about 200nm.
The material of glass substrate is optical glass, and its thickness is 1000 μm.
The beneficial effect that the present invention has:
The present invention utilizes strong oxidizer to be oxidized to mauve by the manganese ion in potable water
ion, as sample, utilizes peristaltic pump by the sample chamber of above-mentioned sample output waveguide; Irradiate the surface of waveguide with laser, receive reflected light with CCD, by the gray scale of CCD detection black line center, calculate and obtain Trace Amount Manganese concentration.The present invention's wavelength is the surface of the laser irradiation waveguide of 532nm, due to exciting of ultrahigh-order mode, will occur the absorption black line occurred because of attenuated total reflection (ATR) in reflected light.Due to the minimal value R of ATR absorption peak
minclosely related with the extinction coefficient κ of sample, and the size of κ is proportional to the concentration of sample, therefore, by the gray scale (R of CCD detection black line center
min), can be calculated Trace Amount Manganese concentration.The present invention's waveguide, as sample chamber and resonant cavity, has high power density and high-quality-factor (Q value), and detect and have high sensitivity, Detection results is good, and apparatus structure is simple, testing cost is low, be easy to carry, easy to operate, just with popularization.
Waveguide of the present invention is from top to bottom fitted together by sheet glass, glass seal, glass substrate; The upper surface of sheet glass deposits upper strata metal film, and the upper surface of glass substrate deposits lower metal film; Glass seal has sample inlet and sample export, and the space in glass seal is sample chamber.The material of upper strata metal film is silver, and the thickness of upper strata metal film is 35nm.The material of sheet glass is optical glass, and its thickness is 300 μm.The material of glass seal is optical glass, and its thickness is about 500 μm.The material of lower metal film is silver, and its thickness is about 200nm.The material of glass substrate is optical glass, and its thickness is 1000 μm.The design of waveguiding structure of the present invention, the selection of parameter, can ensure to have best Detection results.
Accompanying drawing explanation
Fig. 1 is the assembling schematic diagram of waveguide of the present invention;
Fig. 2 is that Trace Manganese in Water concentration C CD detects schematic diagram.
Embodiment
As shown in Figure 1, sheet glass 1, glass seal 2, glass substrate 3 from top to bottom fit together; The upper surface of sheet glass 1 deposits upper strata metal film, and the upper surface of glass substrate 3 deposits lower metal film 4; Glass seal 2 has sample inlet 5 and sample export 6, and the space in glass seal 2 is sample chamber.The material of upper strata metal film is silver, and the thickness of upper strata metal film is 35nm.The material of sheet glass 1 is optical glass, and its thickness is 300 μm.The material of glass seal 2 is optical glass, and its thickness is about 500 μm.The material of lower metal film 4 is silver, and its thickness is about 200nm.The material of glass substrate 3 is optical glass, and its thickness is 1000 μm.
During detection, first, the cuvette in colour developing box is utilized to add the potable water closing manganese, in phosphoric acid solution (concentration is 2.3mol/L), add potassium metaperiodate and sensitive chromogenic reaction occurs manganese, generate aubergine permanganate, be oxidized to mauve by the manganese ion in potable water
ion, for subsequent use as sample; In process color, reducing substances and chlorion can disturb colour developing, must remove in advance, Fe
3+solution can be made to be yellow, to utilize H
3pO
4the red Fe sheltered in potable water
3+.
Utilize peristaltic pump by the sample chamber of above-mentioned sample output waveguide;
Irradiate the surface of waveguide with the laser that wavelength is 532nm, the angle of divergence of laser is less than 0.3mrad.Reflected light is received by CCD detection element, because laser has live width and the angle of divergence of nanometer scale, by designing in advance, can guarantee to excite a ultrahigh-order mode near incident angle, due to exciting of ultrahigh-order mode, the absorption black line occurred because of attenuated total reflection (ATR) in reflected light, will be there is.
The minimal value R of ATR absorption peak
minprovided by following formula:
Wherein, Im (β °) represents intrinsic loss, and the extinction coefficient κ of intrinsic loss and sample is closely related, Im (Δ β
l) represent radiation loss.β °=k
0n
0sin θ is guided mode propagation constant, and k
0=2 π/λ are the propagation constant in air, n
0for air refraction, θ is incident angle.When intrinsic loss equals radiation loss Im (β °)=Im (Δ β
l) time, there is R
min=0.R
min=0 is also the starting condition (sample is aqueous solution, and the concentration of manganese is zero) of testing.When in solution, the concentration of manganese increases, the size due to extinction coefficient κ is proportional to the concentration of sample, causes the increase of intrinsic loss Im (β °), thus makes R
minbecome large.Therefore, by the gray scale R of CCD detection black line center
min, can be calculated Trace Amount Manganese concentration, R
minthe scale of change is determined by the measurement of standard solution.
Suppose the wavelength X=532nm of incident laser, the dielectric coefficient ε of upper strata metal film
1=-10.5+i0.8, thickness h
1=35nm, the refractive index n of sheet glass
2=1.50, thickness is h
2=300 μm, the thickness h of glass seal and sample chamber
4=h
3=500 μm, the dielectric coefficient ε of lower metal film
5=ε
1=-10.5+i0.8, thickness h
5=200nm.The refractive index n of initial sample
3=1.3342, do not conforming in manganese situation, the imaginary part of sample refractive index is 0, is water white liquid.If laser is decided to be θ at the center incident angle of waveguide surface
in=4.56 °, then by the attenuated total reflection that can be calculated as shown in Figure 2 (ATR) curve, the reflectivity R of ATR peak base
min≈ 0.If experiment, then manifest the maximum black line of a gray scale in reflected light.Along with the increase of manganese concentration, due to the effect with developer, color from light to dark, shows that the imaginary part (extinction coefficient κ) of sample refractive index becomes large gradually by 0, the gray scale of the black line that CCD detection arrives also (R from large to small
minchange from small to big).If the reflectivity change using 1% as the resolution of ccd detector, then may detect extinction coefficient changes delta κ=10
-6.In the detection of reality, realize the detection resolution of 0.1 μ g/L.
Claims (10)
1. drink a Trace Manganese in Water concentration detection method, it is characterized in that:
Strong oxidizer is utilized to be oxidized to mauve by the manganese ion in potable water
ion, for subsequent use as sample;
Utilize peristaltic pump by the sample chamber of above-mentioned sample output waveguide;
Irradiate the surface of waveguide with laser, receive reflected light with CCD, by the gray scale of CCD detection black line center, calculate and obtain Trace Amount Manganese concentration.
2. according to claim 1ly drink Trace Manganese in Water concentration detection method, it is characterized in that: the surface irradiating waveguide with the laser that wavelength is 532nm, the angle of divergence of laser is less than 0.3mrad.
3. according to claim 2ly drink Trace Manganese in Water concentration detection method, it is characterized in that: utilize strong oxidizer that the manganese ion in potable water is oxidized to mauve ion
during ion, the reducing substances in potable water and chlorion need be removed, utilize H
3Po
4the red Fe sheltered in potable water
3+.
4. drink Trace Manganese in Water concentration detection method according to claim 1-3 described in any one, it is characterized in that: strong oxidizer is potassium metaperiodate or ammonium persulfate.
5. for a waveguide for method described in claim 1, it is characterized in that: sheet glass, glass seal, glass substrate from top to bottom fit together; The upper surface of sheet glass deposits upper strata metal film, and the upper surface of glass substrate deposits lower metal film; Glass seal has sample inlet and sample export, and the space in glass seal is sample chamber.
6. waveguide according to claim 5, is characterized in that: the material of upper strata metal film is silver, and the thickness of upper strata metal film is 35nm.
7. waveguide according to claim 7, is characterized in that: the material of glass seal is optical glass, and its thickness is about 500 μm.
8. waveguide according to claim 6, is characterized in that: the material of glass seal is optical glass, and its thickness is about 500 μm.
9. waveguide according to claim 7, is characterized in that: the material of lower metal film is silver, and its thickness is about 200nm.
10. waveguide according to claim 8, is characterized in that: the material of glass substrate is optical glass, and its thickness is 1000 μm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105548093A (en) * | 2016-01-23 | 2016-05-04 | 宜春学院 | High-sensitivity oscillating field optical waveguide sensor |
| CN107167452A (en) * | 2017-06-08 | 2017-09-15 | 复拓科学仪器（苏州）有限公司 | The stink damp body detecting method and detection means of waveguide are coated based on double-sided metal |
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Patent Citations (4)
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| JPH10170427A (en) * | 1996-12-06 | 1998-06-26 | Shimadzu Corp | Detector cell and optical measurement device |
| US7330263B2 (en) * | 2004-02-04 | 2008-02-12 | Fujifilm Corporation | Measurement method and apparatus |
| CN1595121A (en) * | 2004-06-24 | 2005-03-16 | 上海交通大学 | Optical waveguide biochemical sensor and measurement system based on free space coupling |
| WO2009091039A1 (en) * | 2008-01-16 | 2009-07-23 | Nippon Telegraph And Telephone Corporation | Surface plasmon resonance measuring device, sample cell, and measuring method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105548093A (en) * | 2016-01-23 | 2016-05-04 | 宜春学院 | High-sensitivity oscillating field optical waveguide sensor |
| CN107167452A (en) * | 2017-06-08 | 2017-09-15 | 复拓科学仪器（苏州）有限公司 | The stink damp body detecting method and detection means of waveguide are coated based on double-sided metal |
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