CN103487481B - A kind of expiration ammonia analyser - Google Patents
A kind of expiration ammonia analyser Download PDFInfo
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- CN103487481B CN103487481B CN201310482977.7A CN201310482977A CN103487481B CN 103487481 B CN103487481 B CN 103487481B CN 201310482977 A CN201310482977 A CN 201310482977A CN 103487481 B CN103487481 B CN 103487481B
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Abstract
A kind of expiration ammonia analyser, carry out Measurement and analysis by analysis module to gathered breath, described analysis module is made up of sample chamber, T-valve, ammonia filtrator, ammonia gas sensor and pump; By control module, described analysis module is controlled, and carry out the collection of information, process, storage and communication etc.This analyser counterpart expiration ammonia concentration is utilized to carry out analytical calculation.
Description
Technical field
The present invention relates to expiration gas detection field.
Background technology
In blood, the change of ammonia level is relevant with multiple physiological maladies (as liver, stomach, pulmonary dysfunction etc.), and when the ammonia in blood is too high, can discharge by exhaling, this means that expiratory air ammonia as the biomarker of various diseases and metabolic process, can provide a kind of non-invasive diagnosis means for clinical.
In recent years, the research detected about expiration ammonia is a lot, and that delivers on " DigestiveDiseasesandSciences " in 2002 as D.J.Kearney measures research for helicobacter pylori Infect And Diagnose about exhalation ammonia; P.Gouma reported in 2010 and adopts the microsensor based on metal oxide to carry out the detection sensitivity that exhalation ammonia detect delay can reach ppb magnitude on " IeeeSensorsJournal "; GiovanniNeri has delivered employing IMS and CRDS technology real-time analysis hemodialysis patients exhalation ammonia level in 2012 at " NephrologyDialysisTransplantation ", have studied in dialysis procedure the relation between the situation of change of ammonia concentration of breathing out and BUN and Kt/V.
Also a kind of ammonia gas sensor and a kind of by measuring expiration ammonia with the method for diagnosing helicobacter pylori infection with this ammonia gas sensor is disclosed in US2004/0077965A1, ammonia gas sensor in this invention is directly exhaled with mouth and is connected, the surfacing of this ammonia gas sensor is teflon, is an anhydrous soda acid sensor; In use, the changing value of the substrate ammonia concentration level that record experimenter mouth is exhaled and ammonia gas level, compares the Infection Status of the helicobacter pylori determining this experimenter with the numerical value of feminine gender/positive infected with Helicobacter pylori in this invention.
But the reference value scope of the mouth expiration ammonia mentioned in above-mentioned research is very wide, even if test value also not to have from 0.1-3ppm not etc. under the condition of Control release (as fasting), this is unfavorable for the specific diagnosis of disease.The reason of this phenomenon is caused to be:
1) ammonia is very easily water-soluble, and amino molecule becomes a hydration ammonia (NH with hydrone by Hydrogenbond
3h
2o), a hydration ammonia energy fraction is ionized into ammonium ion (NH
4 +) and hydroxide ion (OH
-), NH in solution
3and NH
4 +relative quantity depend on the pH of solution, in an acidic solution, H
+can by whole NH
3change into NH
4 +, by basified, NH
4 +lose H
+be converted into NH again
3, during pH value of solution=9.3, NH
3and NH
4 +relative quantity half-and-half.So in the whole process of exhaling, ammonia participates in passage gas and exchanges, and ammonia concentration, by lung, can constantly change in the process in air flue and oral cavity;
2) mouth expiration humidity nearly 100%, once breathe out be condensed into saturation water gas very soon, a large amount of ammonia gas dissolves, in water, causes the on the low side of result;
3) chemical property of ammonia molecule is very active, the surface of channel wall and analytical instrument inside is easy to provide binding site for vapor phase ammonia molecule, adsorption-desorption is caused to balance: if gas phase ammonia concentration increases above gas wall equilibrium concentration, will adsorb, if and phase concentrations declines, amino molecule will desorption.The existence of polar molecule water, can compete identical binding site, thus the response time causing ammonia concentration to change is more long with amino molecule.The service condition of surfacing, area, flow velocity, Sample moisture and equipment, the response time even can in hour.
What the chemistry in detecting that current ammonia detects was relatively ripe mainly contains reagent colorimetric method, indophenol blue colorimetry etc., and wherein reagent colorimetric method is because of easy and simple to handle, and colour developing fast, is generally used more; Indophenol blue colorimetry is highly sensitive, develop the color more stable, interference is few, but operating conditions requires strict, developing time length is the main cause affecting Fast Measurement, and GB GB/T18204.25 " public place Ammonia in Air assay method " regulation is measure the ammonia in air with indophenol blue colorimetry.Sample mode is: the in-built 10ml absorbing liquid of absorption tube, with 0.5ml/min flow, and gas production 5L.This method developing time is longer, and sample size is comparatively large, is not suitable for human body and exhales.
The method of the ammonia concentration in accurate measurement ppb concentration range and instrument are still the target that researcher explores.Be directly used in the instrument detecting expiration ammonia concentration in the market little, be mostly in the laboratory study stage, sensor selectivity is difficult to meet the demands, the many components in expiration, and especially humidity is larger to the interference of measuring.The selectivity how improving measurement is the gordian technique that expiration ammonia is measured.The nephrolux type expiration ammonia analyser of Pranalytica company of the current U.S. adopts gas photoacoustic sensors, daily output OralAmmoniaAnalyzer is optical sensor, but due to its expensive equipment, and analytical cycle is longer, use trouble, and be unsuitable for the use of expiration detection field.
And ammonia concentration of exhaling detects and is applied to clinical diagnosis disease and there is no clear and definite point of contact value, the expiration ammonia density of hepatic renal dysfunction patient is generally at about 2ppm, Healthy People is at about 300ppb, exhale the change of ammonia density at about 500ppb before and after the oral urea of patient of helicobacter pylori infections, consider situation, expiration ammonia analytical instrument needs to reach following performance index and requires:
Summary of the invention
The present invention is directed to above problem and the one that proposes is improved one's methods and device, improve the convenience of repeatability that expiration ammonia measures and application.
Because ammonia is very easily water-soluble, NH in solution
3and NH
4 +relative quantity depend on the pH of solution and be in the problem of mobile equilibrium, fasting 8-12h, and can not carry out diet in test process, can ensure intraoral acid base equilibrium, slowly exhale the NH that can allow in oral cavity
4 +more change into NH
3.
Due to mouth expiration humidity nearly 100%, be condensed into the problem of saturation water gas very soon once breathe out, in sample chamber, increase thermostat module, maintain sample chamber temperature and be not less than expiratory air temperature, expiratory air condensation can be prevented.
Because the chemical property of ammonia molecule is very active, the surface of channel wall and analytical instrument inside is easy to provide binding site for vapor phase ammonia molecule, cause the problem that adsorption-desorption balances, sample chamber inwall, pipeline and sensor inwall should be noted that on Material selec-tion, the present invention selects polytetrafluoroethylmaterial material, ammonia its surface absorption less.
Because the ammonia gas sensor of high sensitivity high selectivity is measured very important to expiration ammonia, for the trace measurement of ppb concentration range, improve the selectivity measured more crucial.As when ammonia is tested, the interference of humidity on sensor response is comparatively large, and the relative humidity of breath is close to 100%, and under this humidity, the impact of ammonia gas sensor response signal is close to 1000ppb, and the test of this counterpart expiration ammonia causes serious interference.In addition, the micro constitutent of other complexity in expiration, as sulfide, CO
2deng all likely causing interference to measurement.
Improving selectivity to realize by catalyst formulation selection and technology for preparing electrode improvement, also improve by sensor construction design, can also achieve the goal by selecting the filtrator that can filter interference gas.
Due to the physicochemical characteristics of ammonia, find and can filter interference gas composition and the material of adsorb ammonia is very not difficult, so improve ammonia to measure the method that selectivity can utilize difference, as in patent CN101571506, the measurement of PARA FORMALDEHYDE PRILLS(91,95) concentration is just calculated by the difference of twice measurement: what first time measured is the response signal of sensor to sample gas, sample gas is passed through sensor by a filtrator by after formaldehyde selective adsorption wherein by second time again, now the response signal of sensor has just deducted the impact of formaldehyde separately, the two difference reflection be exactly the contribution that concentration of formaldehyde responds sensor.The key of this method is taked to be find the filtering material gas of institute's analysis to measure to selective adsorption.
Nafion pipe is a kind of H that can be displaced through wherein
20, NH
3, alcohol, DMSO and THF equimolecular, and other major parts are inorganic, organic molecule all will be retained in sample gas.When utilizing method of difference to carry out the analysis of expiration ammonia, as expiration sample is directly managed by Nafion, then H
20 and NH
3capital is removed, and does not reach the object of difference measurement.Consider that Nafion pipe removes the partial pressure difference of power resources water in the inside and outside gas of pipe of water, as manage inside and outside humidity or water partial pressure consistent, the humidity of sample gas can not change, so Nafion pipe is placed on in the enclosed environment of gas same humidity to be measured, keep the inside and outside humidity of Nafion pipe consistent, then, when sample gas is by Nafion pipe, wherein moisture can not be removed, and ammonia is wherein removed, thus reach the object optionally removing ammonia.Switch three-way valve switching gas circuit can be passed through during analysis, allow gas to be measured when testing, first time is responded except entering sensor after ammonia composition wherein by Nafion pipe thread, second time is not directly responded sample gas by Nafion pipe, and the difference calculating twice response current is the response current of wherein ammonia.
According to above-mentioned principle thinking, the present invention devises a kind of expiration ammonia analyser, be made up of analysis module and control module, respectively Measurement and analysis is carried out to gathered expiration gas, described analysis module is controlled, and carry out the collection of information, process, storage and communication etc., it is characterized in that: described analysis module (100) is composed in series by pipeline (106) by sample chamber (101), T-valve (102), ammonia gas sensor (104) and pump (105); One at described T-valve (102) exports and is connected an ammonia filtrator (103) between ammonia gas sensor (104); Described ammonia filtrator (103) is placed in a closed sleeve pipe by Nafion pipe and forms, and the sponge of filling liquid water, water suction in the space between Nafion pipe with sleeve pipe or other materials are to maintain the relative humidity of this enclosure space for 100%.
Described ammonia filtrator (103) is loaded on humidity by Nafion pipe and forms in the enclosed environment of 100%.Described sample chamber (101) and the selected material of pipeline (106) are the material to ammonia gas absorption inertia, such as teflon etc.The volume of described sample chamber (101) is 200 ~ 2000ml, and thermostat module is equipped with in sample chamber, ensures that the temperature of sample chamber is not less than 38 DEG C.
The above-mentioned expiration ammonia analyser of use carry out mouth expiration ammonia detect before should fasting 8-12h, and can not diet be carried out in test process, to ensure intraoral acid base equilibrium, improve the repeatability of test.
Utilize above-mentioned expiration ammonia analyser carry out mouth expiration ammonia detect process as follows:
A) sample: mouth expiration/nose is exhaled in described sample chamber (101); Or with pump (105), gas to be measured is evacuated in sample chamber (101);
B) analyze: the first step: control T-valve (102), bled by pump (105), by the gas in air chamber (101) through T-valve (102), ammonia filtrator (103), ammonia gas sensor (104), pump (105) is emptying afterwards, records its steady-state response electric current (I
1); Second step: I
1after stable, switch described T-valve (102) and make gas in sample chamber (101) through T-valve (102), pipeline (106), ammonia gas sensor (104), pump (105) is emptying afterwards, records its steady-state response electric current (I
2);
C) calculate: by electric current (I
1), electric current (I
2) and transducer sensitivity (k) calculation sample room in gas concentration: C=(I
2-I
1)/k.
Wherein the demarcating by following method of transducer sensitivity k: the ammonia being first C by the zero gas of drying and concentration known passes in sample chamber (101) respectively, then controlling T-valve (102) makes gas in sample chamber (101) through T-valve (102), pipeline (106), ammonia gas sensor (104), pump (105) is emptying afterwards, records its steady-state response electric current (zero current I
0, calibrating gas electric current I
c), the sensitivity of described sensor is calculated by following formula: k=(I
c-I
0)/C.
Accompanying drawing explanation
Fig. 1. apparatus of the present invention gas circuit structure schematic diagram.
Fig. 2. be the response curve of this analytical equipment to ammonia analytical test.
Fig. 3. be the linear relationship between result and distribution concentration utilizing this analytical equipment to test 0 ~ 4000ppb ammonia gas.
Specific embodiment
Fig. 1 gives the concrete structure schematic diagram of expiration ammonia analyser: be made up of analysis module 100 and control module 200, respectively Measurement and analysis is carried out to gathered expiration gas, described analysis module is controlled, and carries out the collection of information, process, storage and communication etc.
Analysis module (100) is composed in series by pipeline (106) by sample chamber (101), T-valve (102), ammonia gas sensor (104) and pump (105); An ammonia filtrator (103) is had between an outlet and ammonia gas sensor (104) of described T-valve (102).
Sample chamber (101) wherein and the selected material of pipeline (106) are teflon.Described sample chamber (101) volume is 500ml, and in sample chamber, thermostat module is housed, and to ensure that the temperature of Quality control room is not less than 38 DEG C, preferably constant is at 40-60 DEG C.
Ammonia filtrator (103) is managed by Nafion, outer sleeve and the filler between the two in space form, and wherein Nafion pipe is rich pure ME110 type, and outer sleeve is the PP pipe of 12mm*36.5cm.Different according to the humidity of gas to be measured, Nafion pipe and different filler selectable in the space between sleeve pipe: when carrying out mouthful breath tester, the sponge of filling liquid water, water suction or other materials are to maintain the relative humidity of this enclosure space for 100%; When dry gas is tested, desiccant-filled, comprise molecular sieve, silica gel, activated alumina etc.; When the gas that humidity is known is tested, also can fill the saturated brine solution of corresponding humidity.
This is to keep the dividing potential drop of the water vapor in Nafion pipe internal and external environment consistent, when such sample gas is by Nafion pipe, only the ammonia in sample gas can be removed Nafion pipe, and the concentration of other gases is constant, thus reaches the object optionally removing ammonia.Switch three-way valve switching gas circuit can be passed through during analysis, allow gas to be measured when testing, first time is responded except entering sensor after ammonia composition wherein by Nafion pipe thread, second time is not directly responded sample gas by Nafion pipe, and the difference calculating twice response current is the response current of wherein ammonia.
Control module 300 is made up of correlation function electricity modules such as realization control, measurement, storage, communication and printings.
The whole process of this expiration ammonia analyser to ammonia concentration analysis is:
A) sample: mouth expiration/nose is exhaled in described sample chamber (101); Or with pump (105), gas to be measured is evacuated in sample chamber (101);
B) analyze: the first step: control T-valve (102), bled by pump (105), by the gas in air chamber (101) through T-valve (102), ammonia filtrator (103), ammonia gas sensor (104), pump (105) is emptying afterwards, records its steady-state response electric current (I
1); Second step: I
1after stable, switch described T-valve (102) and make gas in sample chamber (101) through T-valve (102), pipeline (106), ammonia gas sensor (104), pump (105) is emptying afterwards, records its steady-state response electric current (I
2);
C) calculate: by electric current (I
1), electric current (I
2) and transducer sensitivity (k) calculation sample room in gas concentration: C=(I
2-I
1)/k.
The ammonia gas sensor that the present embodiment expiration ammonia analyser is selected is self-control electrochemical ammonia sensor, its sensitivity k is demarcated by the carrying out of following method: the dry ammonia being first 1000ppb by the zero gas of drying and concentration known passes in sample chamber (101) respectively, then controlling T-valve (102) makes gas in sample chamber (101) through T-valve (102), pipeline (106), ammonia gas sensor (104), pump (105) is emptying afterwards, records its steady-state response electric current (zero gas steady-state response electric current I
0, calibrating gas steady-state response electric current I
c), the sensitivity calculating described sensor by lower be that formula calculates: k=(I
c-I
0)/C=0.145nA/ppb.
Utilize this analyser carry out ammonia concentration measure time current-responsive curve as shown in Figure 2, wherein I
1for deducting the steady-state response electric current of the gas response that ammonia is left in sample gas, I
2for the steady-state response electric current of sample gas all components.
Test 0 ~ 4000ppb dry ammonia Standard Gases with described ammonia analyser, as shown in Figure 3, result shows that within the scope of this, measurement result and distribution concentration are substantially identical to result, and linearly dependent coefficient is 0.995.
Test drying nitrogen with described ammonia analyser, meet with a response electric current I
1for 5251.1nA, I
2for 5253.3nA, end product is 15.2ppb, tests the nitrogen of humidity 100%, and meet with a response electric current I
1' be 5502.4nA, I
2' be 5504.8nA, end product is 16.5ppb.Relatively drying nitrogen response current I
1with humidity 100% nitrogen response current I
1', can find that response current fruit is very large by the impact of humidity, the response when humidity of same gas increases by 100% increases 1733ppb, and the end product calculated by method of difference is consistent.This illustrates that method of difference effectively can overcome the interference of humidity to measurement result.
Measure the ammonia calibrating gas (2000ppb and 4000ppb) that relative humidity is 100% with described ammonia analyser, result is as shown in table 2, shows that the impact of humidity on measurement result is less than 10%.
Bibliographical information affects the various factors of expiration ammonia density, wherein fasting, feed, drink water and drink cola and have impact to measurement result, inventor is according to this has been preliminary test, table 3 gives to the result data of experimenter's (healthy 20 years old women) repeated test mouth expiration ammonia gas level that (test condition is: fasting 12h, and can not diet be carried out in test process, to ensure intraoral acid base equilibrium), table 4 gives this experimenter and (comprise fasting under different test condition, feed, drink water and drink cola) mouth expiration ammonia concentration, it is 279ppb that experimental result shows that this experimenter tests the mouth expiration ammonia concentration obtained after fasting 12h, the repeated deviation of testing 5 times is 16%, feed deutostoma expiration ammonia concentration increases to 724ppb, the deutostoma expiration ammonia concentration that drinks water is reduced to 405ppb, 201ppb is reduced to after drinking cola.With document (Ammoniainbreathandemittedfromskin), the test result of the mouth expiration ammonia of fasting, feed reports that result is consistent, drink water, with document (Factorsin uencingbreathammoniadetermination), the impact of laughable counterpart expiration ammonia concentration reports that result is consistent.
The exhale technical indicator of ammonia analyser of the present invention is as follows, can meet the requirement that mouth expiration ammonia concentration detects:
Claims (6)
1. an expiration ammonia analyser, be made up of analysis module and control module, analysis module carries out Measurement and analysis to gathered breath, control module controls described analysis module, and carry out the collection of information, process, storage and communication, it is characterized in that: described analysis module (100) is composed in series by pipeline (106) by sample chamber (101), T-valve (102), ammonia gas sensor (104) and pump (105); One at described T-valve (102) exports and is connected an ammonia filtrator (103) between ammonia gas sensor (104); Described ammonia filtrator (103) is placed in a closed sleeve pipe by Nafion pipe and forms, and the sponge of filling liquid water, water suction in the space between Nafion pipe with sleeve pipe or other materials are to maintain the relative humidity of this enclosure space for 100%.
2. a kind of expiration ammonia analyser as claimed in claim 1, it is characterized in that: for different controlled humidity requirements, fill gaps drying agent between the Nafion pipe of described ammonia filtrator (103) and sleeve pipe, comprise molecular sieve, silica gel, activated alumina, or fill the saturated brine solution of corresponding humidity.
3. a kind of expiration ammonia analyser as claimed in claim 1, is characterized in that: the selected material of described sample chamber (101) and pipeline (106) is the inert material of not adsorb ammonia, comprises teflon or it is material modified.
4. a kind of expiration ammonia analyser as claimed in claim 1, is characterized in that: described sample chamber (101) are equipped with thermostat module, ensures that the temperature of sample chamber is not less than 38 DEG C.
5. an expiration ammonia measuring method, the method uses analyser described in claim 1, and its process comprises sampling, analyzes and calculates three steps, it is characterized in that described analytic process is carried out as follows:
Sampling: mouth expiration/nose is exhaled in described sample chamber (101); Or with pump (105), gas to be measured is evacuated in sample chamber (101);
Analyze: the first step: control T-valve (102), bled by pump (105), by the gas in air chamber (101) through T-valve (102), ammonia filtrator (103), ammonia gas sensor (104), pump (105) is emptying afterwards, records its first steady-state response electric current I
1; Second step: I
1after stable, switch described T-valve (102) and make gas in sample chamber (101) through T-valve (102), pipeline (106), ammonia gas sensor (104), pump (105) is emptying afterwards, records its second steady-state response electric current I
2;
Calculate: by the first steady-state response electric current I
1, the second steady-state response electric current I
2and gas concentration in transducer sensitivity k calculation sample room: C=(I
2-I
1)/k.
6. a kind of expiration ammonia measuring method as claimed in claim 5, it is characterized in that: the sensitivity k of wherein said sensor (104) demarcates by following method: first the ammonia of the zero gas of drying and concentration known is passed in sample chamber (101) respectively, then controlling T-valve (102) makes gas in sample chamber (101) through T-valve (102), pipeline (106), ammonia gas sensor (104), pump (105) is emptying afterwards, records its steady-state response electric current: zero gas steady-state response electric current I
0, calibrating gas steady-state response electric current I
c, the sensitivity of described sensor is calculated by following formula: k=(I
c-I
0)/C.
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| AU2015217215A1 (en) | 2014-02-11 | 2016-08-11 | The Board Of Trustees Of The Leland Stanford Junior University | Rapid small volume detection of blood ammonia |
| CN104181228B (en) * | 2014-09-18 | 2017-02-22 | 电子科技大学 | Method capable of accelerating response of trace gas integrated detector |
| CN104391107B (en) * | 2014-11-28 | 2016-03-02 | 无锡市尚沃医疗电子股份有限公司 | A kind of Exhaled nitric oxide measuring method not needing control expiratory gas flow |
| CN105891405A (en) * | 2016-03-30 | 2016-08-24 | 深圳三相生物传感科技有限公司 | Device for diagnosing human body helicobacter pylori (Hp) infection and method for detecting content of ammonia in breath of human body |
| CN105866224A (en) * | 2016-03-30 | 2016-08-17 | 深圳三相生物传感科技有限公司 | Kit for diagnosing human body Helicobacter pylori infection, and method for detecting content of ammonia gas in human body breath |
| CN105891301B (en) * | 2016-04-21 | 2019-04-16 | 长沙三相医疗器械有限公司 | The method of ammonia level in the system for diagnosing human body helicobacter pylori infections and detection people's expiratory air established based on fuel cell |
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| CN110780063A (en) * | 2019-12-10 | 2020-02-11 | 无锡市尚沃医疗电子股份有限公司 | Expiratory ammonia detection method and device |
| CN111505217A (en) * | 2020-05-19 | 2020-08-07 | 东南大学 | Human body exhaled gas detection system |
| CN113296122A (en) * | 2021-05-20 | 2021-08-24 | 安徽大学 | Laser radar quality control device |
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