CN104568940A - Method for detecting hydrogen sulfide gas based on nanocrystalline celluloses - Google Patents
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Abstract
The invention relates to a method for detecting hydrogen sulfide gas based on nanocrystalline celluloses. The method comprises the following steps: preparing a nanocrystalline cellulose solution, adding a lead ion solution, feeding a to-be-detected gas, observing the color change of the solution, and detecting at 300 nm wavelength by using an ultraviolet-visible spectrophotometer. The method disclosed by the invention has good selectivity, and the method can specifically detect hydrogen sulfide; the method is quicl to detect, and the color of the solution is changed from colourless to light yellow or brown in a few seconds, and can be kept stable in a certain period of time; the method is high in sensitivity, and the detectable lowest concentration of hydrogen sulfide gas is 1 mg/m<3>; and the method is less in required reagents, simple in operation, and convenient for popularization and application.
Description
Technical field
The present invention relates to toxic gas detection field, particularly relate to a kind of method detecting hydrogen sulfide gas based on nanocrystalline cellulose.
Background technology
Sulfuretted hydrogen is a kind of colourless gas having rotten egg smell, has pungency and asphyxiating.People contacts sulfuretted hydrogen mainly through respiratory system, when concentration of hydrogen sulfide is lower, has spread effect to the local of respiratory tract and eye; When concentration is higher, can impacts the central nervous system of whole body, even cause suffocating; When very high concentrations, olfactory fatigue and unconsciously its taste can be caused.Have the generation of sulfuretted hydrogen in the industry such as organophosphorus pesticide, leather, sulfur dye, pigment and animal glue, a large amount of sulfuretted hydrogen all can be had to overflow during place's operations such as swampland, cloaca, septic tank and deposition of dirt pond, operating worker is poisoning unrare.
Along with the continuous quickening of China's process of industrialization, the background concentration of Air Hydrogen Sulfide also improves constantly, and therefore, just seems significant to the detection of Air Hydrogen Sulfide, can detect that low concentration hydrogen sulphide just seems particularly important for health.The detection method of existing hydrogen sulfide gas mainly contains: 1) iodimetric titration; 2) methylene blue method; 3) lead acetate reaction rate method; 4) painted length detection tube method; 5) Laser absorption spectroscopy; 6) fluorometry; 7) metal oxide sensor; 8) electrochemical sensor; 9) vapor-phase chromatography.Wherein, iodimetric titration is longer for the low content gas sample time, and manual operation is loaded down with trivial details, is unfavorable for datumization sample and transform; Methylene blue method is only applicable to measure the more stable purified natural gas of concentration of hydrogen sulfide; The accuracy of painted length detection tube method is not high; Fluorescence molecule detects lead ion to be needed to use expensive luminaire, and electrochemical sensor design is complicated, complex operation; Although vapor-phase chromatography is highly sensitive, but gas chromatograph is to the pre-service of gas producing device, the configuration of gas chromatograph sampling system and deactivation process, and all requiring high to the preparation level of calibrating gas, often test result poor reproducibility, test result is inaccurate.All there is certain limitation in said method technology.Therefore be necessary to set up a kind of can the method for sulfuretted hydrogen in Accurate Determining indoor-outdoor air environment.
Summary of the invention
The object of the invention is to the detection method setting up a kind of sulfuretted hydrogen, detection can be made simpler, cheap, efficient.
For reaching this object, the present invention by the following technical solutions:
On the one hand, the invention provides a kind of method detecting hydrogen sulfide gas based on nanocrystalline cellulose (NCC), described method comprises the steps: first preparation of nano crystalline cellulose (NCC) solution, then in this solution, lead ion solution is added, pass into hydrogen sulfide gas to be measured, observe solution colour change and detect with ultraviolet-visible spectrophotometer.
The present invention utilizes sulphion and lead ion to generate the reaction detection sulfuretted hydrogen of vulcanized lead, and nanocrystalline cellulose (NCC) plays the effect of dispersed sulfur lead.First NCC solution is prepared, after adding lead acetate, lead ion is dispersed in NCC surface by electrostatic interaction, now solution is colourless, after passing into hydrogen sulfide gas, generate the composite particles of micron-sized vulcanized lead and NCC in solution, NCC is dispersed in the middle of particle, and solution colour is rendered as faint yellow or brown.NCC can play the effect of stable vulcanized lead, and solution colour is stablized.
As optimal technical scheme, the final concentration of the solution of nanocrystalline cellulose described in the present invention is 0.2-5mg/mL, can be such as 0.2mg/mL, 0.4mg/mL, 0.5mg/mL, 0.8mg/mL, 1.0mg/mL, 1.2mg/mL, 1.5mg/mL, 1.8mg/mL, 2.0mg/mL, 2.5mg/mL, 3mg/mL, be preferably 1mg/mL.
Preferably, the final concentration of described lead ion solution is 0.2-5mM, such as, can be 0.2mM, 0.4mM, 0.5mM, 0.8mM, 1.0mM, 1.2mM, 1.5mM, 1.8mM, 2.0mM, 2.5mM, 3.0mM, is preferably 1mg/mL.
Preferably, described lead ion solution is lead acetate or lead nitrate solution.
The determined wavelength of ultraviolet-visible spectrophotometer described in the present invention is 300-500nm, such as determined wavelength can be 300nm, 310nm, 320nm, 330nm, 340nm, 350nm, 360nm, 370nm, 380nm, 390nm or 400nm, be preferably 300-350nm, more preferably 300nm.
Described method comprises the steps:
(1) prepare 0.4-10mg/mL nanocrystalline cellulose solution and 0.4-10mM lead ion solution, and mixed by two kinds of solution, after mixing, the final concentration of nanocrystalline cellulose solution is 0.2-5mg/mL, and the final concentration of lead ion solution is 0.2-5mM;
(2) hydrogen sulfide gas is passed in the mixed solution that step (1) obtains, observe solution colour change, and detect with ultraviolet-visible spectrophotometer, detect sulfuretted hydrogen qualitatively.
The typical curve that the method for the invention can also be done according to sodium sulphide concentration carrys out the content of quantitative detection hydrogen sulfide gas.
As optimal technical scheme, method of the present invention comprises the steps:
(1) prepare 0.4-10mg/mL nanocrystalline cellulose solution and 0.4-10mg/mL lead ion solution, and two kinds of solution are mixed;
(2) formulating vulcanization sodium solution, concentration is respectively 10 μMs, 20 μMs, 40 μMs, 80 μMs, 120 μMs, 160 μMs and 200 μMs, now with the current;
(3) mixed solution that step (1) obtains is got, the sodium sulfide solution of the variable concentrations that the step (2) adding volume ratio 1:1 obtains, mixing, after mixing, the final concentration of nanocrystalline cellulose solution is 0.2-5mg/mL, the final concentration of lead ion solution is 0.2-5mM, the final concentration of sodium sulphide is 5 μMs, 10 μMs, 20 μMs, 40 μMs, 60 μMs, 80 μMs, 100 μMs;
(4) observe the color change of solution in step (3), and detect with ultraviolet-visible spectrophotometer, make typical curve;
(5) mixed solution that 1-100mL step (1) obtains is got, add the deionized water of volume ratio 1:1, pass into hydrogen sulfide gas to be measured, observe the color change of solution, and detect with ultraviolet-visible spectrophotometer, the concentration of sulfuretted hydrogen is calculated according to the typical curve of step (4).
The reaction time passing into gas to be measured described in step (5) is 0.01-3 hour, and be preferably 0.02-1 hour, the such as time can be 0.02 hour, 0.5 hour, 1 hour, 1.5 hours, 2 hours, 2.5 hours or 3 hours.
Passed into by gas to be measured and detect in solution, observe solution colour and change in time, discovery system is stable in a long time.
As optimal technical scheme, method of the present invention comprises the steps:
(1) prepare 4mg/mL nanocrystalline cellulose solution and 4mg/mL lead ion solution, and two kinds of solution are mixed by 1:1 by volume;
(2) formulating vulcanization sodium solution, concentration is respectively 10 μMs, 20 μMs, 40 μMs, 80 μMs, 120 μMs, 160 μMs and 200 μMs;
(3) mixed solution that step (1) obtains is got, the sodium sulfide solution of the variable concentrations that the step (2) adding volume ratio 1:1 obtains, mixing, now the final concentration of nanocrystalline cellulose solution is 1mg/mL, the final concentration of lead ion solution is 1mM, the final concentration of sodium sulphide is 5 μMs, 10 μMs, 20 μMs, 40 μMs, 60 μMs, 80 μMs, 100 μMs;
(4) observe the color change of solution in step (3), and detect with ultraviolet-visible spectrophotometer, make typical curve;
(5) mixed solution that step (1) obtains is got, add the deionized water of volume ratio 1:1, pass into hydrogen sulfide gas to be measured, reaction 0.01-1 hour, observation solution colour changes, and detect with ultraviolet-visible spectrophotometer, the concentration of sulfuretted hydrogen is calculated according to the typical curve of step (4).
To those skilled in the art, even if do not understand Cleaning Principle of the present invention, can implement equally, reproduce the present invention, namely whether Cleaning Principle of the present invention is cheer and bright, do not affect enforcement of the present invention and reproduction.A kind of lead ion based on nanocrystalline cellulose of the present invention detects and minimizing technology, and Cleaning Principle of the present invention is:
The present invention utilizes sulphion and lead ion to generate the reaction detection sulfuretted hydrogen of vulcanized lead, and nanocrystalline cellulose (NCC) plays the effect of dispersed sulfur lead.First prepare NCC solution, after adding lead acetate, lead ion is dispersed in NCC surface by electrostatic interaction, now solution is colourless, after passing into hydrogen sulfide gas, generates micron-sized vulcanized lead particle in solution, NCC is dispersed in the middle of particle, and solution colour is rendered as faint yellow or brown.NCC can play the effect of stable vulcanized lead, and solution colour is stablized.
Compared with prior art, the present invention has following beneficial effect:
1) detection method of the present invention has good selectivity, because the present invention cannot detect the gases such as sulphuric dioxide, ammonia, air, carbon dioxide, methane and ethene, only can detect sulphuric dioxide;
2) detection method of the present invention detects fast, and the color of solution just can change faint yellow or brown into by colourless several seconds kinds, and keeps stable within a certain period of time;
3) detection method of the present invention is highly sensitive, and the least concentration of the hydrogen sulfide gas that can detect is 1mg/m
3;
4) needed for detection method of the present invention, reagent is few, simple to operate, easy to utilize.
Accompanying drawing explanation
Fig. 1 is hydrogen sulfide gas Cleaning Principle figure of the present invention.
Fig. 2 is the color diagram that the inventive method and variable concentrations sodium sulphide react.
Fig. 3 is that the present invention is to variable concentrations sodium sulphide UV spectrophotometer measuring result.
Fig. 4 is 300nm absorbance of the present invention and sodium sulphide concentration linear relationship.
Fig. 5 is the color diagram that the inventive method and gas with various react.
Fig. 6 is that under the inventive method and gas with various react 300nm dulling luminosity ratio is comparatively.
Fig. 7 is that sodium sulphide reaction system of the present invention changes detection figure in time.
Fig. 8 be NCC pattern of the present invention and exist with or without NCC time vulcanized lead TEM figure.
Embodiment
For further setting forth the technological means and effect thereof that the present invention takes, further illustrate technical scheme of the present invention below in conjunction with accompanying drawing by embodiment, but the present invention is not confined in scope of embodiments.
Embodiment 1:
The concrete detection method of the present embodiment is as follows:
(1) prepare the nanocrystalline cellulose solution of 0.4mg/mL and the lead acetate solution of 0.4mM, and by they by volume number 1:1 mix;
(2) hydrogen sulfide gas is passed into the solution in step (1).
(3) observe solution colour change, and under 300nm, detect the light absorption value of solution with ultraviolet-visible spectrophotometer.
Embodiment 2:
The concrete detection method of the present embodiment is as follows:
(1) prepare the nanocrystalline cellulose solution of 10mg/mL and the lead acetate solution of 10mM, and by they by volume number 1:1 mix;
(2) hydrogen sulfide gas is passed into the solution in step (1).
(3) observe solution colour change, and under 300nm, detect the light absorption value of solution with ultraviolet-visible spectrophotometer.
Embodiment 3:
The concrete detection method of the present embodiment is as follows:
(1) prepare the nanocrystalline cellulose solution of 4mg/mL and the lead acetate solution of 4mM, and by they by volume number 1:1 mix;
(2) hydrogen sulfide gas is passed into the solution in step (1).
(3) observe solution colour change, and under 300nm, detect the light absorption value of solution with ultraviolet-visible spectrophotometer.
Embodiment 4:
The concrete detection method of the present embodiment is as follows:
(1) prepare the nanocrystalline cellulose solution of 4mg/mL and the lead nitrate solution of 8mM, and by they by volume number 1:2 mix;
(2) hydrogen sulfide gas is passed into the solution in step (1).
(3) observe solution colour change, and under 300nm, detect the light absorption value of solution with ultraviolet-visible spectrophotometer.
Embodiment 5:
The concrete detection method of the present embodiment is as follows:
(1) prepare the nanocrystalline cellulose solution of 4mg/mL and the lead acetate solution of 4mM, and by they by volume number 1:1 mix;
(2) formulating vulcanization sodium solution, concentration is respectively 10 μMs, 20 μMs, 40 μMs, 80 μMs, 120 μMs, 160 μMs and 200 μMs, now with the current;
(3) get the mixed solution of 100 μ L nanocrystalline cellulose and lead acetate, add the sodium sulfide solution of the above-mentioned variable concentrations of 100 μ L, mixing, the final concentration of sodium sulphide is 5 μMs, 10 μMs, 20 μMs, 40 μMs, 60 μMs, 80 μMs and 100 μMs;
(4) observe solution colour change, and detect the change of solution absorbance with ultraviolet-visible spectrophotometer;
(5) get the absorbance mapping at solution 300nm place, find there is good linear relationship between absorbance and sodium sulphide concentration.
The rising along with sodium sulphide concentration can be found out from Fig. 2, the color burn of solution, equally along with sodium sulphide concentration raises in Fig. 3, spectrophotometer detected value also increases, Fig. 4 sodium sulphide typical curve linear dependence is good, and the sodium sulphide typical curve of gained is Y=0.25394+0.01126X (R
2=0.99871).
Embodiment 6:
The concrete detection method of the present embodiment is as follows:
(1) prepare the NCC solution of 2mg/mL and the lead acetate solution of 2mM, and their equal-volumes are mixed;
(2) pass into hydrogen sulfide gas, sulphuric dioxide, ammonia, methane, ethene, carbon dioxide, nitrogen, argon gas and air to the solution in step (1), and prepare a blank.
(3) observe solution colour change, and detect the change of solution absorbance with ultraviolet-visible spectrophotometer.
Only produce color change to hydrogen sulfide gas as apparent from Fig. 5, Fig. 6 detection system, and only have very low absorptivity to sulphuric dioxide, other gases can not react substantially, the detection hydrogen sulfide gas that institute in this way can be stable and be not subject to other gases affect.
Embodiment 7:
The concrete detection method of the present embodiment is as follows:
(1) prepare the NCC solution of 4mg/mL and the lead acetate solution of 4mM, and their equal-volumes are mixed;
(2) get the mixed solution of 100 μ L NCC and lead acetate, add the sodium sulfide solution of 100 μ L 100 μMs;
(3) observe 0 minute, 3 minutes, 6 minutes, 15 minutes, 30 minutes and solution colour change in 60 minutes, and under 300nm, detect each time period solution light absorption value with ultraviolet-visible spectrophotometer.
As can be seen from Figure 7, detection method of the present invention is highly stable, and within an hour, detected value does not change.
Embodiment 8:
The concrete detection method of the present embodiment is as follows:
(1) prepare the NCC solution of 4mg/mL and the lead acetate solution of 4mM, and by they with water by volume 1:1:2 mix;
(2) 5mg/m is passed into the solution in step (1)
3hydrogen sulfide gas.
(3) observe solution colour change, and detect the change of solution absorbance with ultraviolet-visible spectrophotometer.
(4) measure the absorbance of absorbing liquid at 300nm place, and read corresponding concentration value from typical curve.
Embodiment 9:
The concrete detection method of the present embodiment is as follows:
(1) prepare the NCC solution of 4mg/mL and the lead acetate solution of 4mM, and by they with water by volume 1:1:2 mix;
(2) 1mg/m is passed into the solution in step (1)
3hydrogen sulfide gas.
(3) observe solution colour change, and detect the change of solution absorbance with ultraviolet-visible spectrophotometer.
(4) measure the absorbance of absorbing liquid at 300nm place, and read corresponding concentration value from typical curve.
The TEM figure of vulcanized lead when Fig. 8 illustrates NCC pattern of the present invention and exists with or without NCC, lead ion is dispersed in NCC surface by electrostatic interaction, and after passing into hydrogen sulfide gas, generate micron-sized vulcanized lead particle in solution, NCC is dispersed in the middle of particle.
In sum, method of the present invention can the detection hydrogen sulfide gas of quantitative and qualitative analysis, and quick and precisely, keeps stablizing in long-time.Meanwhile, detection method selectivity of the present invention is strong, can specific detection hydrogen sulfide gas.By the detection of the hydrogen sulfide gas of variable concentrations, method of the present invention can detect the concentration of hydrogen sulfide gas accurately, and most low energy detects 1mg/m
3hydrogen sulfide gas.
Applicant states, the present invention illustrates method detailed of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned method detailed, does not namely mean that the present invention must rely on above-mentioned method detailed and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of auxiliary element, the concrete way choice etc. of each raw material of product of the present invention, all drops within protection scope of the present invention and open scope.
Claims (9)
1. one kind is detected the method for hydrogen sulfide gas based on nanocrystalline cellulose, it is characterized in that, described method comprises the steps: first preparation of nano crystalline cellulose solution, then in this solution, lead ion solution is added, pass into hydrogen sulfide gas to be measured, observe solution colour change and detect with ultraviolet-visible spectrophotometer.
2. method according to claim 1, is characterized in that, the final concentration of described nanocrystalline cellulose solution is 0.2-5mg/mL, is preferably 1mg/mL.
3. method according to claim 1 and 2, is characterized in that, the final concentration of described lead ion solution is 0.2-5mM, is preferably 1mM;
Preferably, described lead ion solution is lead acetate or lead nitrate solution.
4. the method according to any one of claim 1-3, is characterized in that, the determined wavelength of described ultraviolet-visible spectrophotometer is 300-500nm, is preferably 300-350nm, more preferably 300nm.
5. the method according to any one of claim 1-4, is characterized in that, described method comprises the steps:
(1) prepare 0.4-10mg/mL nanocrystalline cellulose solution and 0.4-10mM lead ion solution, and mixed by two kinds of solution, after mixing, the final concentration of nanocrystalline cellulose solution is 0.2-5mg/mL, and the final concentration of lead ion solution is 0.2-5mM;
(2) hydrogen sulfide gas is passed in the mixed solution that step (1) obtains, observe solution colour change, and detect with ultraviolet-visible spectrophotometer, detect sulfuretted hydrogen qualitatively.
6. the method according to any one of claim 1-4, is characterized in that, described method is used for the quantitative detection of hydrogen sulfide gas.
7. method according to claim 6, is characterized in that, described method comprises the steps:
(1) prepare 0.4-10mg/mL nanocrystalline cellulose solution and 0.4-10mg/mL lead ion solution, and two kinds of solution are mixed;
(2) formulating vulcanization sodium solution, concentration is respectively 10 μMs, 20 μMs, 40 μMs, 80 μMs, 120 μMs, 160 μMs and 200 μMs;
(3) mixed solution that step (1) obtains is got, the sodium sulfide solution of the variable concentrations that the step (2) adding volume ratio 1:1 obtains, mixing, after mixing, the final concentration of nanocrystalline cellulose solution is 0.2-5mg/mL, the final concentration of lead ion solution is 0.2-5mM, the final concentration of sodium sulphide is 5 μMs, 10 μMs, 20 μMs, 40 μMs, 60 μMs, 80 μMs, 100 μMs;
(4) observe the color change of solution in step (3), and detect with ultraviolet-visible spectrophotometer, make typical curve;
(5) mixed solution that 1-100mL step (1) obtains is got, add the deionized water of volume ratio 1:1, pass into hydrogen sulfide gas to be measured, observe the color change of solution, and detect with ultraviolet-visible spectrophotometer, the concentration of sulfuretted hydrogen is calculated according to the typical curve of step (4).
8. the method according to any one of claim 1-7, is characterized in that, the reaction time passing into gas to be measured described in step (5) is 0.01-3 hour, is preferably 0.01-1 hour.
9. the method according to any one of claim 6-8, is characterized in that, described method comprises the steps:
(1) prepare 4mg/mL nanocrystalline cellulose solution and 4mM lead ion solution, and two kinds of solution are mixed by 1:1 by volume;
(2) formulating vulcanization sodium solution, concentration is respectively 10 μMs, 20 μMs, 40 μMs, 80 μMs, 120 μMs, 160 μMs and 200 μMs;
(3) mixed solution that step (1) obtains is got, the sodium sulfide solution of the variable concentrations that the step (2) adding volume ratio 1:1 obtains, mixing, now the final concentration of nanocrystalline cellulose solution is 1mg/mL, the final concentration of lead ion solution is 1mM, the final concentration of sodium sulphide is 5 μMs, 10 μMs, 20 μMs, 40 μMs, 60 μMs, 80 μMs, 100 μMs;
(4) observe the color change of solution in step (3), and detect with ultraviolet-visible spectrophotometer, make typical curve;
(5) mixed solution that step (1) obtains is got, add the deionized water of volume ratio 1:1, pass into hydrogen sulfide gas to be measured, reaction 0.01-1 hour, observation solution colour changes, and detect with ultraviolet-visible spectrophotometer, the concentration of sulfuretted hydrogen is calculated according to the typical curve of step (4).
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| CN113267461A (en) * | 2021-06-25 | 2021-08-17 | 山东益丰生化环保股份有限公司 | Method for detecting sulfide content in electronic-grade thiourea |
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