CN104568940B - 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 hydrogen sulfide gas are detected based on nanocrystalline cellulose in toxic gas detection field, more particularly, to one kind
Method.
Background technology
Hydrogen sulfide is a kind of colourless gas having rotten egg abnormal smells from the patient, has zest and asphyxiating.People mainly passes through breathing
System contacts hydrogen sulfide, when concentration of hydrogen sulfide is relatively low, has stimulation to the local of respiratory tract and eye；When concentration is higher,
The central nervous system of whole body can be impacted, even result in and suffocate；When very high concentrations, olfactory fatigue can be caused to can not help
Its taste.There are the generation of hydrogen sulfide, marshland, the moon in the industry such as organophosphorus pesticide, leather, sulfur dye, pigment and animal glue
A large amount of hydrogen sulfide all can be had during ditch, anaerobic tank and deposition of dirt pond etc. operation to overflow, operating worker poisoning is not uncommon for.
With the continuous quickening of China's process of industrialization, the background concn of Air Hydrogen Sulfide also improves constantly, therefore, right
The detection of Air Hydrogen Sulfide just seems significant, can detect that low concentration hydrogen sulphide just seems particularly heavy for health
Will.The detection method of existing hydrogen sulfide gas mainly has：1) iodimetric titration；2) methylene blue method；3) lead acetate reaction rate method；4)
Coloring length detection tube method；5) Laser absorption spectroscopy；6) fluorimetry；7) metal oxide sensor；8) electrochemistry passes
Sensor；9) gas chromatography.Wherein, iodimetric titration is longer for the low content gas sample time, and artificial complex operation, is unfavorable for
Digitization collection and transmission；Methylene blue method is only applicable to measure the more stable purified natural gas of concentration of hydrogen sulfide；Coloring length inspection
Test tube method accuracy is not high；Fluorescence molecule detection lead ion needs using expensive luminaire, and electrochemical sensor sets
Meter is complicated, complex operation；Although gas chromatography sensitivity is high, gas chromatograph is to the pretreatment of gas producing device, gas phase color
The configuration of spectrometer sampling system and deactivation are processed, and require high, often test knot to the preparation level of calibrating gas
Fruit poor reproducibility, test result is inaccurate.All there is certain limitation in said method technology.It is therefore desirable to setting up a kind of permissible
The method of hydrogen sulfide in Accurate Determining indoor and outdoor air environment.
Content of the invention
It is an object of the invention to setting up a kind of detection method of hydrogen sulfide, enable to detect simpler, cheap, high
Effect.
For reaching this purpose, the present invention employs the following technical solutions：
On the one hand, the invention provides a kind of method that hydrogen sulfide gas are detected based on nanocrystalline cellulose (NCC), described
Method comprises the steps：Preparation of nano crystalline cellulose (NCC) solution first, then adds lead ion solution in this solution,
It is passed through hydrogen sulfide gas to be measured, observe solution colour change and detected with ultraviolet-visible spectrophotometer.
The present invention utilizes sulphion and lead ion to generate the reaction detection hydrogen sulfide of vulcanized lead, nanocrystalline cellulose (NCC)
Play the effect of dispersed sulfur lead.Prepare NCC solution first, after adding lead acetate, lead ion is dispersed in by electrostatic interaction
NCC surface, now solution is colourless, after being passed through hydrogen sulfide gas, generates the compound of micron-sized vulcanized lead and NCC in solution
Granule, NCC is dispersed in the middle of granule, and solution colour is rendered as faint yellow or brown.NCC can play the work of stable vulcanized lead
With so that solution colour is stable.
As optimal technical scheme, the final concentration of 0.2-5mg/mL of heretofore described nanocrystalline cellulose solution, example
As being 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, preferably 1mg/mL.
Preferably, the final concentration of 0.2-5mM of described lead ion solution, can be for example 0.2mM, 0.4mM, 0.5mM,
0.8mM, 1.0mM, 1.2mM, 1.5mM, 1.8mM, 2.0mM, 2.5mM, 3.0mM, preferably 1mg/mL.
Preferably, described lead ion solution is lead acetate or lead nitrate solution.
The Detection wavelength of heretofore described ultraviolet-visible spectrophotometer is 300-500nm, and such as Detection wavelength is permissible
It is 300nm, 310nm, 320nm, 330nm, 340nm, 350nm, 360nm, 370nm, 380nm, 390nm or 400nm, preferably
300-350nm, more preferably 300nm.
Methods described comprises the steps：
(1) prepare 0.4-10mg/mL nanocrystalline cellulose solution and 0.4-10mM lead ion solution, and two kinds of solution are mixed
Close uniformly, the final concentration of 0.2-5mg/mL of nanocrystalline cellulose solution, the final concentration of 0.2- of lead ion solution after mixing
5mM；
(2) hydrogen sulfide gas are passed through in the mixed solution that step (1) obtains, observe solution colour change, and with ultraviolet-
Visible spectrophotometer detects, qualitatively detects hydrogen sulfide.
The method of the invention can also be according to the sulfuration standard curve that done of na concn Lai quantitative detection stink damp
The content of body.
As optimal technical scheme, method of the present invention comprises the steps：
(1) 0.4-10mg/mL nanocrystalline cellulose solution and 0.4-10mg/mL lead ion solution are prepared, and molten by two kinds
Liquid mix homogeneously；
(2) formulating vulcanization sodium solution, concentration is respectively 10 μM, 20 μM, 40 μM, 80 μM, 120 μM, 160 μM and 200 μM, existing
Join existing use；
(3) take the mixed solution that step (1) obtains, add volume ratio 1：The sulfuration of the variable concentrations that 1 step (2) obtains
Sodium solution, mix, the final concentration of 0.2-5mg/mL of nanocrystalline cellulose solution after mixing, lead ion solution final concentration of
0.2-5mM, final concentration of 5 μM of sodium sulfide, 10 μM, 20 μM, 40 μM, 60 μM, 80 μM, 100 μM；
(4) in observation of steps (3) solution color change, and with ultraviolet-visible spectrophotometer detection, standard of making is bent
Line；
(5) take the mixed solution that 1-100mL step (1) obtains, add volume ratio 1：1 deionized water, is passed through sulfur to be measured
Change hydrogen, observe the color change of solution, and with ultraviolet-visible spectrophotometer detection, according to the standard curve of step (4)
Calculate the concentration of hydrogen sulfide.
The response time being passed through under test gas described in step (5) is 0.01-3 hour, and preferably 0.02-1 hour, such as when
Between can be 0.02 hour, 0.5 hour, 1 hour, 1.5 hours, 2 hours, 2.5 hours or 3 hours.
Under test gas are passed through in detection solution, observe solution colour and change over, find system in a long time
It is stable.
As optimal technical scheme, method of the present invention comprises the steps：
(1) 4mg/mL nanocrystalline cellulose solution and 4mg/mL lead ion solution are prepared, and by volume 1:1 is molten by two kinds
Liquid mix homogeneously；
(2) formulating vulcanization sodium solution, concentration is respectively 10 μM, 20 μM, 40 μM, 80 μM, 120 μM, 160 μM and 200 μM；
(3) take the mixed solution that step (1) obtains, add volume ratio 1:The sulfuration of the variable concentrations that 1 step (2) obtains
Sodium solution, mixes, the now final concentration of 1mg/mL of nanocrystalline cellulose solution, the final concentration of 1mM of lead ion solution, sulfuration
Final concentration of 5 μM of sodium, 10 μM, 20 μM, 40 μM, 60 μM, 80 μM, 100 μM；
(4) in observation of steps (3) solution color change, and with ultraviolet-visible spectrophotometer detection, standard of making is bent
Line；
(5) take the mixed solution that step (1) obtains, add volume ratio 1:1 deionized water, is passed through stink damp to be measured
Body, reacts 0.01-1 hour, observes solution colour change, and with ultraviolet-visible spectrophotometer detection, according to step (4)
Standard curve calculates the concentration of hydrogen sulfide.
To those skilled in the art, even if not understanding the Cleaning Principle of the present invention, equally can implement, reproducing this
Invention, that is, whether the Cleaning Principle of the present invention is cheer and bright, does not affect enforcement and the reproduction of the present invention.A kind of base of the present invention
In lead ion detection and the minimizing technology of nanocrystalline cellulose, the Cleaning Principle of the present invention is：
The present invention utilizes sulphion and lead ion to generate the reaction detection hydrogen sulfide of vulcanized lead, nanocrystalline cellulose (NCC)
Play the effect of dispersed sulfur lead.Prepare NCC solution first, after adding lead acetate, lead ion is dispersed in by electrostatic interaction
NCC surface, now solution is colourless, after being passed through hydrogen sulfide gas, generates micron-sized vulcanized lead granule in solution, NCC divides
It is dispersed in the middle of granule, solution colour is rendered as faint yellow or brown.NCC can play the effect of stable vulcanized lead so that solution
Colour stable.
Compared with prior art, the present invention has the advantages that：
1) detection method of the present invention has good selectivity, due to the present invention all cannot detect sulfur dioxide, ammonia,
The gases such as air, carbon dioxide, methane and ethylene, can detect sulfur dioxide only；
2) the detection method detection of the present invention is quick, the color of solution several seconds kinds just can by colourless be changed into faint yellow or
Brown, and keep stable within a certain period of time；
3) the detection method sensitivity of the present invention is high, and the least concentration of the hydrogen sulfide gas that can detect is 1mg/m3；
4) reagent needed for the detection method of the present invention is few, simple to operate, easy to utilize.
Brief description
Fig. 1 is hydrogen sulfide gas detection principle diagram of the present invention.
Fig. 2 is the color diagram that the inventive method is reacted with variable concentrations sodium sulfide.
Fig. 3 is the present invention to variable concentrations sodium sulfide UV spectrophotometer measuring result.
Fig. 4 is 300nm absorbance of the present invention and sodium sulfide concentration linear relationship.
Fig. 5 is the color diagram that the inventive method is reacted with gas with various.
Fig. 6 is the inventive method and gas with various reacts under 300nm dulling luminosity ratio relatively.
Fig. 7 is that sodium sulfide reaction system of the present invention changes over detection figure.
Fig. 8 be NCC pattern of the present invention and in the presence of having or not NCC vulcanized lead TEM figure.
Specific embodiment
For further illustrating the technological means and its effect that the present invention taken, below in conjunction with accompanying drawing and by specifically real
Apply mode to further illustrate technical scheme, but the present invention is not limited 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 acetic acid lead solution of 0.4mM, and they are pressed parts by volume
Number 1:1 mixing；
(2) it is passed through hydrogen sulfide gas to the solution in step (1).
(3) observe solution colour change, and detect the light absorption value of solution with ultraviolet-visible spectrophotometer under 300nm.
Embodiment 2：
The concrete detection method of the present embodiment is as follows：
(1) prepare the nanocrystalline cellulose solution of 10mg/mL and the acetic acid lead solution of 10mM, and they are pressed volume parts
1:1 mixing；
(2) it is passed through hydrogen sulfide gas to the solution in step (1).
(3) observe solution colour change, and detect the light absorption value of solution with ultraviolet-visible spectrophotometer under 300nm.
Embodiment 3：
The concrete detection method of the present embodiment is as follows：
(1) prepare the nanocrystalline cellulose solution of 4mg/mL and the acetic acid lead solution of 4mM, and they are pressed volume parts 1:
1 mixing；
(2) it is passed through hydrogen sulfide gas to the solution in step (1).
(3) observe solution colour change, and detect the light absorption value of solution with ultraviolet-visible spectrophotometer under 300nm.
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 they are pressed volume parts 1:
2 mixing；
(2) it is passed through hydrogen sulfide gas to the solution in step (1).
(3) observe solution colour change, and detect the light absorption value of solution with ultraviolet-visible spectrophotometer under 300nm.
Embodiment 5：
The concrete detection method of the present embodiment is as follows：
(1) prepare the nanocrystalline cellulose solution of 4mg/mL and the acetic acid lead solution of 4mM, and they are pressed volume parts 1:
1 mixing；
(2) formulating vulcanization sodium solution, concentration is respectively 10 μM, 20 μM, 40 μM, 80 μM, 120 μM, 160 μM and 200 μM, existing
Join existing use；
(3) take the mixed solution of 100 μ L nanocrystalline cellulose and lead acetate, add the sulfuration of the above-mentioned variable concentrations of 100 μ L
Sodium solution, mixes, final concentration of 5 μM of sodium sulfide, 10 μM, 20 μM, 40 μM, 60 μM, 80 μM and 100 μM；
(4) observe solution colour change, and detect the change of solution absorbance with ultraviolet-visible spectrophotometer；
(5) take the absorbance at solution 300nm to map, find to have between absorbance and sulfuration na concn and linearly close well
System.
From Fig. 2 can find out with sulfuration na concn rising, the color burn of solution, dense likewise as sodium sulfide in Fig. 3
Degree raises, and spectrophotometer detected value also increases, and Fig. 4 sodium sulfide standard curve linear dependence is good, the sodium sulfide of gained
Standard curve is Y=0.25394+0.01126X (R2=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 acetic acid lead solution of 2mM, and their equal-volumes are mixed；
(2) to the solution in step (1) be passed through hydrogen sulfide gas, sulfur dioxide, ammonia, methane, ethylene, carbon dioxide,
Nitrogen, argon and air, and prepare a blank.
(3) observe solution colour change, and detect the change of solution absorbance with ultraviolet-visible spectrophotometer.
Will become apparent from detection system from Fig. 5, Fig. 6 and only color change is produced to hydrogen sulfide gas, and sulfur dioxide is only had
Very low absorbance, other gases will not react substantially, in this way can be stable detection hydrogen sulfide gas 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 acetic acid lead solution of 4mM, and their equal-volumes are mixed；
(2) take the mixed solution of 100 μ L NCC and lead acetate, add the sodium sulfide solution of 100 μM of 100 μ L；
(3) observe 0 minute, 3 minutes, 6 minutes, 15 minutes, 30 minutes and the change of 60 minutes solution colours, and with ultraviolet-
Visible spectrophotometer detects each time period solution light absorption value under 300nm.
From figure 7 it can be seen that the detection method of the present invention is highly stable, within an hour, detected value does not occur
Change.
Embodiment 8：
The concrete detection method of the present embodiment is as follows：
(1) prepare the acetic acid lead solution of NCC solution and the 4mM of 4mg/mL, and by them by volume 1 with water：1：2 mix
Close；
(2) it is passed through 5mg/m to 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 absorbance at 300nm for the absorbing liquid, and corresponding concentration value is read from standard curve.
Embodiment 9：
The concrete detection method of the present embodiment is as follows：
(1) prepare the acetic acid lead solution of NCC solution and the 4mM of 4mg/mL, and by them by volume 1 with water：1：2 mix
Close；
(2) it is passed through 1mg/m to 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 absorbance at 300nm for the absorbing liquid, and corresponding concentration value is read from standard curve.
Fig. 8 illustrate NCC pattern of the present invention and have or not NCC in the presence of vulcanized lead TEM figure, lead ion pass through electrostatic interaction
It is dispersed in NCC surface, after being passed through hydrogen sulfide gas, in solution, generates micron-sized vulcanized lead granule, NCC is dispersed in granule and works as
In.
In sum, the detection hydrogen sulfide gas that the method for the present invention can be qualitative and quantitative, and quick and precisely, when long
Interior holding is stable.Meanwhile, the detection method specificity of the present invention is strong, can specific detection hydrogen sulfide gas.By difference
The detection of the hydrogen sulfide gas of concentration, the method for the present invention can accurately detect the concentration of hydrogen sulfide gas, and mental retardation detects
To 1mg/m3Hydrogen sulfide gas.
Applicant states, the present invention illustrates the method detailed of the present invention by above-described embodiment, but the present invention not office
It is limited to above-mentioned method detailed, that is, do not mean that the present invention has to rely on above-mentioned method detailed and could implement.Art
Technical staff is it will be clearly understood that any improvement in the present invention, the equivalence replacement to each raw material of product of the present invention and auxiliary element
Interpolation, selection of concrete mode etc., within the scope of all falling within protection scope of the present invention and disclosure.
Claims (12)
1. a kind of method based on nanocrystalline cellulose detection hydrogen sulfide gas is it is characterised in that methods described includes walking as follows
Suddenly：Preparation of nano crystalline cellulose solution first, then adds lead ion solution in this solution, is passed through hydrogen sulfide gas to be measured,
Observe solution colour change and detected with ultraviolet-visible spectrophotometer；
Methods described specifically includes following steps：(1) prepare 0.4-10mg/mL nanocrystalline cellulose solution and 0.4-10mM lead from
Sub- solution, and by two kinds of solution mix homogeneously, the final concentration of 0.2-5mg/mL of nanocrystalline cellulose solution, lead ion after mixing
The final concentration of 0.2-5mM of solution；
(2) hydrogen sulfide gas are passed through in the mixed solution that step (1) obtains, observe solution colour change, and use ultraviolet-visible
Spectrophotometer detects, qualitatively detects hydrogen sulfide.
2. method according to claim 1 is it is characterised in that the final concentration of 1mg/ of described nanocrystalline cellulose solution
mL.
3. method according to claim 1 is it is characterised in that the final concentration of 1mM of described lead ion solution.
4. method according to claim 1 is it is characterised in that described lead ion solution is lead acetate or lead nitrate solution.
5. method according to claim 1 is it is characterised in that the Detection wavelength of described ultraviolet-visible spectrophotometer is
300-500nm.
6. method according to claim 5 is it is characterised in that the Detection wavelength of described ultraviolet-visible spectrophotometer is
300-350nm.
7. method according to claim 6 is it is characterised in that the Detection wavelength of described ultraviolet-visible spectrophotometer is
300nm.
8. the method according to any one of claim 1-7 is it is characterised in that methods described is used for determining of hydrogen sulfide gas
Amount detection.
9. method according to claim 1 is it is characterised in that methods described comprises the steps：
(1) 0.4-10mg/mL nanocrystalline cellulose solution and 0.4-10mM lead ion solution are prepared, and by two kinds of solution mixing all
Even；
(2) formulating vulcanization sodium solution, concentration is respectively 10 μM, 20 μM, 40 μM, 80 μM, 120 μM, 160 μM and 200 μM；
(3) take the mixed solution that step (1) obtains, add volume ratio 1：The sodium sulfide of the variable concentrations that 1 step (2) obtains is molten
Liquid, mixes, the final concentration of 0.2-5mg/mL of nanocrystalline cellulose solution, the final concentration of 0.2- of lead ion solution after mixing
5mM, final concentration of 5 μM of sodium sulfide, 10 μM, 20 μM, 40 μM, 60 μM, 80 μM, 100 μM；
(4) in observation of steps (3) solution color change, and with ultraviolet-visible spectrophotometer detection, make standard curve；
(5) take the mixed solution that 1-100mL step (1) obtains, add volume ratio 1：1 deionized water, is passed through hydrogen sulfide to be measured
Gas, observes the color change of solution, and with ultraviolet-visible spectrophotometer detection, is calculated according to the standard curve of step (4)
The concentration of hydrogen sulfide.
10. method according to claim 9 it is characterised in that the response time being passed through under test gas described in step (5) be
0.01-3 hour.
11. methods according to claim 10 are it is characterised in that be passed through the response time of under test gas described in step (5)
For 0.01-1 hour.
12. methods according to claim 9 are it is characterised in that methods described comprises the steps：
(1) 4mg/mL nanocrystalline cellulose solution and 4mM lead ion solution are prepared, and by volume 1:Two kinds of solution are mixed by 1
Uniformly；
(2) formulating vulcanization sodium solution, concentration is respectively 10 μM, 20 μM, 40 μM, 80 μM, 120 μM, 160 μM and 200 μM；
(3) take the mixed solution that step (1) obtains, add volume ratio 1:The sodium sulfide of the variable concentrations that 1 step (2) obtains is molten
Liquid, mixes, the now final concentration of 1mg/mL of nanocrystalline cellulose solution, the final concentration of 1mM of lead ion solution, sodium sulfide
Final concentration of 5 μM, 10 μM, 20 μM, 40 μM, 60 μM, 80 μM, 100 μM；
(4) in observation of steps (3) solution color change, and with ultraviolet-visible spectrophotometer detection, make standard curve；
(5) take the mixed solution that step (1) obtains, add volume ratio 1:1 deionized water, is passed through hydrogen sulfide gas to be measured, instead
Answer 0.01-1 hour, observe solution colour change, and with ultraviolet-visible spectrophotometer detection, bent according to the standard of step (4)
Line calculates the concentration of hydrogen sulfide.
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| CN101672790A (en) * | 2009-10-13 | 2010-03-17 | 北京化工大学 | Quick detecting tube for micro-hydrogen sulfide gas |
| CN101799418A (en) * | 2010-01-26 | 2010-08-11 | 四川大学 | Material sensitive to sulfide and hydrogen peroxide as well as preparation method and application thereof |
| US7955504B1 (en) * | 2004-10-06 | 2011-06-07 | State Of Oregon Acting By And Through The State Board Of Higher Education On Behalf Of Oregon State University | Microfluidic devices, particularly filtration devices comprising polymeric membranes, and method for their manufacture and use |
| CN102313733A (en) * | 2010-07-05 | 2012-01-11 | 中国石油集团川庆钻探工程有限公司川东钻探公司 | Method for rapid testing hydrogen sulfide content in drilling fluid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US7955504B1 (en) * | 2004-10-06 | 2011-06-07 | State Of Oregon Acting By And Through The State Board Of Higher Education On Behalf Of Oregon State University | Microfluidic devices, particularly filtration devices comprising polymeric membranes, and method for their manufacture and use |
| CN101672790A (en) * | 2009-10-13 | 2010-03-17 | 北京化工大学 | Quick detecting tube for micro-hydrogen sulfide gas |
| CN101799418A (en) * | 2010-01-26 | 2010-08-11 | 四川大学 | Material sensitive to sulfide and hydrogen peroxide as well as preparation method and application thereof |
| CN102313733A (en) * | 2010-07-05 | 2012-01-11 | 中国石油集团川庆钻探工程有限公司川东钻探公司 | Method for rapid testing hydrogen sulfide content in drilling fluid |
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