CN105136698B - A kind of assay method and device of volatilizable compound - Google Patents
A kind of assay method and device of volatilizable compound Download PDFInfo
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- CN105136698B CN105136698B CN201510518539.0A CN201510518539A CN105136698B CN 105136698 B CN105136698 B CN 105136698B CN 201510518539 A CN201510518539 A CN 201510518539A CN 105136698 B CN105136698 B CN 105136698B
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Abstract
The present invention is a kind of assay method and device of volatilizable compound, disclose a kind of assay method and device of inorganic gas, it is by making inorganic gas to be measured and derivatization reagent that redox reaction occur, then the compound of generation is measured using light scattering/fluorescence/absorption process, and then measures the content of inorganic gas.Its detection device includes：Redox reaction unit, the purification separation device for the reaction product to be measured, sample cell, excitation light source and detection device occur for inorganic gas to be measured and derivatization reagent.Compared with current detection method and device, the analysis that the present invention is suitable for inorganic gas measures, and also is adapted for doing the detection terminal of gas-chromatography, has detection limit low, the advantages that finding speed is fast, and apparatus is simple.
Description
Technical field
The invention belongs to technical field of analytical chemistry, in particular to the method for nonmetallic compound quantitative determination and
Detection device.
Background technology
The measurement of the inorganic gas such as carbon monoxide, carbon dioxide, nitrogen, nitrogen oxides, hydrogen, oxygen, ammonia, chlorine dioxide
It is widely present in the sample of the fields such as food, environment, material, chemical industry.The presence of these compounds generates human health very big
Harm.For example, the ammonia nitrogen in surface water body and body of groundwater can cause water eutrophication phenomenon to generate, it is main in water body
Oxygen consumption pollutant, it is toxic to fish and certain aquatiles.Itrogenous organic substance is not very in animality organic matter and human and animal excreta
Stablize, is readily decomposed to ammonia and also the mankind are damaged.Ammonia nitrogen in water can be converted to nitrite under certain condition, such as
Fruit long-term drinking, the nitrite in water will be combined with protein form nitrosamine, this is a kind of strong carcinogen, strong to human body
Health is totally unfavorable.Equally, the nitrogen oxides in the fields such as food and environment, nitrite anions, fluoride, sulfide, sulphite
Very big harm also is caused to the mankind with bromide etc..Therefore, it is above-mentioned it is total it is multi-field in, these nonmetallic compounds need frequent
It measures.This has great importance to environmental protection, human health.
Currently, these compound test methods are substantially spectrophotometry and gas chromatography, this not only needs complicated
Sample pre-treatments program influences detection speed, while also having serious interference, and the detection limit of measurement is also undesirable.For example, surveying
When determining total nitrogen, the Kjeldahl's method generally used at present not only needs the reagents such as a large amount of concentrated sulfuric acid, simultaneously in Specimen eliminating
Also to pass through the programs such as the absorption titration of ammonia.Cause the analysis cost of this method high, analysis time is long, and detection limit is bad.In addition
Reagent colorimetric method measures ammonia, then needs the mercuric iodixde complex ion using severe toxicity to develop the color, environmental pollution is bigger, separately
Outer method blank is also not easily controlled, and keeps detection limit bad.And to food and environment Nitrite and air nitrogen oxides
It measures, the colorimetric analysis used, it is also desirable to which sample pre-treatments have the deficiencies of interference is big, and analysis cost is low, detection limit is poor.
Invention content
Insufficient existing for existing method above in order to overcome, the present inventor discloses a kind of measurement side of new inorganic gas
Method and device, content are as follows：
A kind of assay method of inorganic gas, it is characterised in that carried out by following step：
（1）In a reactor, a certain amount of redox reagent is filled, inorganic gas to be measured is made to pass through the oxidation
Go back original reagent area carries out redox reaction, and generating new has volatile substance；
（2）So that the new volatile materials that above-mentioned reaction generates is passed through a separating purifying device, makes volatility product
It is purified；
（3）So that purified product is loaded into non-dispersive photometer by carrier gas, carries out light scattering/fluorescence/absorption and survey
Amount, and then measure the content of inorganic gas to be measured.The volatility to be surveyed is generated after determinand is reacted with redox reagent
When product does not interfere with, the separate purification steps of volatility product（2）Cancel.Wherein light scattering/fluorescence/absorptiometry
Wave-length coverage is in 100nm-850nm.Wherein the wave-length coverage of light scattering/fluorescence/absorptiometry is in 160nm-320nm.Exciting light
Source can choose continuous light source, can also choose monochromatic source.In the present invention, wavelength that preferably excitation light source and detector receive
It is preferred that in 160nm -320nm.
The several preferred assay method summaries of the present invention are as follows：
（1）A length of 20-25 cm, internal diameter 1-1.5mm, outer diameter 2-3 mm U type stainless steel tubes in, by filling
The requirement of chromatographic column is filled, the different reagents of length 15-18 cm；The different reagents refer to：
（2）It is for determination of carbon monoxide：60-80 mesh Raney nickels, at 375 DEG C and hydrogen progress redox is anti-
It answers, measures the methane of generation；
（3）For the measurement of micro chlorine：To contain 30%（w /w）The clay particle transforming agent of ammonium sulfate, at room temperature chlorine
Gas and ammonium ion carry out redox reaction, measure the chlorination nitrogen of generation;
（4）For the measurement of ammonia：For 60-80 mesh carbon granules catalyst, ammonia is carried out at 700 DEG C and carbon carries out redox
Reaction, measures the hydride hydrogen of generation；
（5）For the measurement of chlorine dioxide：The 60-80 mesh kaolin particles of solid thiocarbamide are loaded with for surface, at room temperature
The chlorine dioxide and thiocarbamide of progress carry out redox reaction, measure the ammonium chloride of generation；
Currently preferred sampling device is the six-way valve sampling device using gas-chromatography, is connected to reaction unit
Before.
Determinand of the present invention is inorganic gas.These inorganic gas not will produce on given determining instrument device
Fluorescence/light scattering/absorption signal, or the fluorescence/light scattering/absorption signal intensity generated are very low, and Accurate Determining of arriving is wanted
It asks.In this case, it by being reacted with redox reagent, generates new with very high sensitivity on given instrument
Gaseous volatile.These inorganic gas include inorganic gaseous compound, the phosphorus of gaseous state inorganic compound, oxygen and the oxygen of nitrogen and nitrogen
And the inorganic gaseous state of inorganic gaseous compound, carbon and its inorganic gaseous compound of phosphorus, hydrogen and its inorganic gaseous compound, boron is waved
Send out object, sulphur and its inorganic compound, halogen simple substance and its inorganic gaseous compound.Typically these inorganic gas include（But no
It is limited to）For：Carbon monoxide, carbon dioxide, nitrogen, nitrogen oxides, hydrogen, oxygen, ozone, ammonia, hydrogen sulfide, halogen simple substance, gas
State halide etc..
Redox reagent in the present invention can be gas, liquid, solid.It is carried out with inorganic gas to be measured
Redox reaction form can be gas-solid/liquid/gas reactions, gas liquid reaction and gas-solid reaction.In addition, when inorganic gas to be measured dissolves
Can also be liquid-liquid reactions or liquid-solid reaction when in the solution.To the redox reagent of liquid and solid, can select to apply
Solid particles surface mode is overlayed on, inorganic gas to be measured can also be passed into liquid redox reagent solution in the form of being bubbled
In.
It requires at least to generate a kind of new gaseous state when redox reaction occurs for redox reagent in the present invention to wave
Object is sent out, which has very strong fluorescence/light scattering or gas molecule in space absorption signal on selected instrument.Work as selective oxidation
Go back original reagent and inorganic gas to be measured react generation two or more have fluorescence/light scattering signal on instrument
When volatility, you can with select a variety of products signal value and for quantitative, one such generation can also be selected
Volatile matter is quantitative, should remove another kind at this time and be not used in quantitative volatile matter.
The purification method of the new volatility object generated after heretofore described redox reaction, is mainly used for
To being generated in redox reaction technique to the new noisy substance of determination of volatile matter.These substances are primarily referred to as reaction examination
The solid subparticle that agent and reagent carrier generate, as after fine grained carbon, a large amount of water mists, catalyst base dusting fine grained,
The fine grained of dusting etc. that solid reagent generates when reacting.In general these chaff interferents are not that reaction itself generates, and
It is reaction environment condition（The fine particulate of reagent and catalyst when carrying, heating reaction are blown in such as carrier gas）It is caused.Separately
Outside, the new substance generated during redox reaction, these substances belong to non-volatile, but due to thin of its generation
Grain is downloaded to detector by carrier gas, also will generate interference to detection, these substances also need away.In short, to new volatilization to be measured
Other than object, and it can be loaded into the substance that sample cell generates interference to measuring by carrier gas, belong to the chaff interferent model described in the present invention
Farmland.For above-mentioned chaff interferent, purification method is usually used condensation, silica wool filtering and the methods of absorption or specific reaction and goes
Except these chaff interferents.
When the product to be surveyed of generation does not interfere with after determinand is reacted with redox reagent, the separation of determinand is net
Change unit to cancel.
The present invention further discloses the device of inorganic gas assay method, the device includes being gone back for determinand oxidation
Former reaction member 1, determinand isolation of purified unit 2, excitation light source 3, sample cell 4 and detector 5；Test substance is aerobic by containing
The region for changing reduction reaction reagent makes determinand pass through redox reaction and is generated as another kind with light scattering/fluorescence/absorption
Gaseous volatile, and then pass through the measurement that light scattering/fluorescence/absorption process carries out determinand.In addition to improving the spirit measured
Sensitivity has lens 6 between excitation light source 3 and sample cell 4, sample cell and detector 5.
Gas separation unit in apparatus of the present invention refers to containing other interference in the under test gas component generated after reacting
Adsorptive hindrance object may be used, by chemically reacting removing interference in the device for the removal interfering component that group timesharing uses, the device
The methods of object removes chaff interferent, while not influencing the measurement of determinand.It is generated after determinand is reacted with redox reagent
When the product to be surveyed does not interfere with, which cancels.
Redox reaction unit in the present invention refers to being gone back on the detector by oxidation without signal inorganic gas
Original reaction is converted into the derivative for the determinand for having reaction on the detector.Redox reaction reagent in unit can be grain
Shape, filiform, netted and liquid or gas etc..When redox reagent is gas, then because this using gas source feed mode and is waited for
Inorganic gas is surveyed to be reacted into reaction member together.To solid redox reagent, it is preferably loaded in a cylinder
Glass or metal tube in.Specifically, when redox reaction needs catalysis, it is also contemplated that the reaction member is heated,
Or it is reacted under a certain pressure to ensure having higher derivatization efficiency.It is specifically recommended that can be with when being catalyzed
It is catalyzed using induction heating method, microwave heating catalysis process, ultraviolet radiation.These the relevant technologies principles at present can be very
It is found on more documents.The selection of specific method and condition depends on specifically reacting required condition.
In the present invention, the form that inorganic gas component to be measured is entered reaction member can be that interval enters, can also
It is to continuously enter.This depend primarily on specific determinand sample size number and operation feasibility.If it is batch sampling, one
As be six-way valve injection port sample introduction using gas-chromatography.When inorganic gas sample introduction to be measured, can by its in a gaseous form by
It is injected into carrier gas stream, can also first dissolve under test gas in a liquid, be injected into carrier gas stream in the form of a solution or reaction is single
In element apparatus.
The line source of the more preferable 160-320nm of light source in the present invention（For example the high intensity pulses of atomic fluorescence are empty
Heart cathode modulation）, the valuable laser light source of price can not had in this way.And it can be examined using existing atomic fluorescence of zero dispersion
Instrument is surveyed, new instrument production is saved.The benefit that detecting instrument is made using existing atomic fluorescence of zero dispersion is also resided in, due to
Detector is made using solar blind photomultiplier, thus the interference of visible light can be reduced, improves selectivity, the noise obtained
Than.Lamp current setting at this time can refer to the pertinent instruments determination condition in the following examples, generally 20-60mA.
In addition light source can also be done using pulse laser, the excitation wavelength of laser preferably between 180-700nm, preferably protect by intensity at this time
It holds in 10mJ/s or more.The detector of the present invention is particularly suitable for cooperation gas-chromatography and uses.
The carrier gas of the present invention can be inert gas, can also be also to be used as redox anti-while making carrier gas
The gas answered.It is recommended that using the relatively high inert gas of purity.If with air, it should there is purifier to carry out air pure
Filtering.In general, the flow of carrier gas can be adjusted according to detecting instrument and parameter request, and carrier gas flux is generally in 30-500
Ml/min；If using atomic fluorescence of zero dispersion photometer, carrier gas flux is preferably in 250-400 ml/mins.
Sample cell in the present invention, effect are the gaseous volatiles to be measured generated after reacting（After purification）Herein by
The light of excitation light source excites to form light scattering/fluorescence/absorption, and then light scattering/fluorescence/absorption is detected by detector.Sample
Product pond can make closed form using quartz material, can also use the original of existing atomic fluorescence of zero dispersion photometer
Sonization device, belongs to open type at this time.The volume for being used for conveying sample gas in sample cell cannot be too big, otherwise can influence to measure
Effective volume concentration reduces sensitivity.Preferably refer to atomic fluorescence of zero dispersion atomizer center sample feeding pipe internal diameter into
In general row design is used between 5 millimeters to 20 millimeters of the quartz ampoule inside diameter ranges of flowing carrier gas.There are two sample cell both ends
Mouthful, the air inlet pipe of a connection gaseous volatile to be measured, another connection evacuated tube.
Possessed good effect exists the assay method of inorganic gas disclosed by the invention compared with prior art with device
In：
（1）The detection device of the present invention does not have grating, and this reduces the losses of light, while using light scattering/fluorescence/suction
Receipts method measures, and has and its high sensitivity and low detection limit (several ppb).In addition, with high choosing when due to gaseous state sample introduction
Selecting property does not interfere with object appearance.Therefore measure with high sensitivity simultaneously, it may have well selectivity.
（2）The detector of the present invention, usually used photomultiplier.If excitation light source wavelength closely in ultra-violet (UV) band, this
When use solar blind photomultiplier because its visible light not in by environment is influenced, there is very high anti-interference ability and steady
It is qualitative.
（3）The method of the present invention is used for the direct injection analysis of inorganic gas, and measurable inorganic gas type is more, range
Extensively.Conventional method measures inorganic gas, generally to select the instrument of several types, equipment investment is bigger, and detection efficiency compares
It is low.Method can be carried out detecting using a kind of instrument, improve detection efficiency, save equipment investment.（4）The method of the present invention
There is no offline sample pre-treatments, but converted by redox reaction using inorganic gas direct-on-line to be measured, therefore
Loss when the offline pre-treatment of sample is eliminated the need for, the rate of recovery is improved, there is very high accuracy of measurement.Also make measurement simultaneously
Speed is greatly improved.In addition, since this method carries out micro-reaction online, minimal amount of reagent, analysis cost are used
It significantly reduces.From the above mentioned, this method has novelty and creativeness.This method and device be simple, high sensitivity, using wide
The features such as general, strong applicability.
Description of the drawings：
Fig. 1 is the structural schematic diagram of volatilizable compound device；Wherein
1- is determinand redox reaction unit；2- determinand isolation of purified units；3- excitation light sources；
4- sample cells；5- detectors；6- lens；Unit is added in 7- reaction reagents；8- carrier gas inlets；
9- carrier gas exports.
Embodiment 1
Following most preferred embodiment illustrates in details, elaborates the features and advantages of the present invention.Although the present invention is only by several
Kind form has been disclosed, but those of ordinary skill in the art are clear that：With the shape of the part in the present invention, big
The relevant modification of small and arrangement, increase and decrease and deletion, belong to central inventive range described in the claims in the present invention.Therefore,
When attempting to fall into this scope of the appended claims by other changes under teachings suggestion in this or implementation
Within when, belong to right scope of the present invention.Reagent used in the present invention is by commercially available.
Embodiment 1
Determination of carbon monoxide：In the U type stainless steel tubes of a length of 25 cm, internal diameter 1.5mm, 2 mm of outer diameter, by filling out
Fill the requirement filling about 15 cm Raney nickels of length of chromatographic column（60-80 mesh, can market buy）, Raney nickel pipe is sandwiched in
It is heated to ensure in pedestal in one heating furnace（375 degrees Celsius of constant temperature）Uniformly.Gas phase color is connected in U-shaped stainless steel tube one end
The outlet of the six-way valve sampling device of spectrum, six-way valve sample feeding pipe are connected with two gas of nitrogen and hydrogen gas cylinder of needle valve pressure regulation
Body is high-purity, and is purified through over-molecular sieve after bottle outlet.U-tube outlet be connected to one atomic fluorescence of zero dispersion light
On degree meter, excitation light source is done using the hollow cathode lamp of the cadmium of the instrument.In the flow for adjusting nitrogen and hydrogen（It is per minute）
Than for 122ml:Behind 78ml=1.5, by air sample to be measured（It is gone out carbon dioxide with alkali asbestos in advance）50ul is injected with sample introduction needle
The measurement of methane content after under test gas six-way valve is converted, and then determine the content of carbon monoxide in air sample.It measures
As a result have with gas-chromatography FID detection methods and coincide well.
Embodiment 2
The measurement of micro chlorine：In the U type glass tubes of a length of 25 cm, internal diameter 1.5mm, 2 mm of outer diameter, by filling out
Fill requirement filling about 15 cm of length of chromatographic column, the clay particle transforming agent containing ammonium sulfate（Liquid containing ammonium sulfate 30%）U-tube
One end connects the escape pipe of the six-way valve sampling device of gas-chromatography, and six-way valve sample feeding pipe is connected with the argon gas of needle valve pressure regulation
Cyclinder gas.To remove clay and ammonium sulfate fine grained, then U-tube outlet is connected to a screen pipe equipped with silica wool
Again with one atomic fluorescence of zero dispersion photometer on, do excitation light source using the hollow cathode lamp of the arsenic of the instrument.
After adjusting argon gas and being 200ml/min, the sample to be measured containing chlorine is injected into tri-chlorination after six-way valve is converted with sample introduction needle
The measurement of nitrogen content, and then obtain the content of chlorine in sample to be tested.Measurement result has good kiss with gas-chromatography ECD detection methods
It closes.
Embodiment 3
The measurement of ammonia：In the U type stainless steel tubes of a length of 25 cm, internal diameter 1.5mm, 2 mm of outer diameter, by fill color
Compose the carbon granules catalyst of about 15 cm of requirement filling length of column（60-80 mesh, can market buy）, catalyst tube is sandwiched in one
It is heated to ensure in pedestal in a heating furnace（700 degrees Celsius of constant temperature）Uniformly.Gas-chromatography is connected in U-shaped stainless steel tube one end
The escape pipe of six-way valve sampling device, six-way valve sample feeding pipe are connected with two gas of argon gas and hydrogen gas cylinder of needle valve pressure regulation
It is high-purity, and by passing through molecular sieve purification after bottle outlet.U-tube outlet be connected to a screen pipe equipped with silica wool with
Remove the fine grained carbon that is carried by carrier gas, then again with one atomic fluorescence of zero dispersion photometer on, use the instrument
The hollow cathode lamp of cadmium does excitation light source.In the flow for adjusting argon gas and hydrogen（It is per minute）Than for 122ml:78ml=1.5
Afterwards, ammonia sample 50ul to be measured is injected to the measurement of micro HCN contents after under test gas six-way valve is converted with sample introduction needle.
Measurement result has with gas-chromatography FID detection methods coincide well.
Embodiment 4
The measurement of chlorine dioxide：In the U type glass tubes of a length of 20 cm, internal diameter 1.5mm, 2 mm of outer diameter, by filling out
The surface for filling about 15 cm of requirement filling length of chromatographic column is loaded with the kaolin particle of solid thiocarbamide（60-80 mesh, surface carry sulphur
Urea 10%）.U-shaped stainless steel tube one end connects pure chlorine dioxide（By purification）The escape pipe of gas generating unit, U-tube are another
One end outlet is connected to a screen pipe equipped with silica wool to remove clay and thiocarbamide fine grained, then again with one with
Atomic fluorescence of zero dispersion photometer on, do excitation light source using the hollow cathode lamp of the cadmium of the instrument.It is sent out in chlorine dioxide
The carrier gas of raw device（Argon gas）Flow is to measure the sulfide content generated after Chlorine Dioxide Oxidation thiocarbamide under 300ml/min.It surveys
The result for determining the chlorine dioxide of result and iodometric determination has good coincide.
Embodiment 5
Titanium dioxide Carbon analysis：One atomic fluorescence of zero dispersion photometer on, use the cadmium of the instrument
Hollow cathode lamp does excitation light source, and 20 milliliter 10% of potassium bisulfide solution is then added in 50 milliliters of test tubes.It is passed through
The carrier gas argon of 300 ml/mins seals up test tube immediately with test tube lid, and reference explanation book attached drawing and patent Shen are arranged in detail
Please number be 2014103809342 applications for a patent for invention.With syringe by CO to be measured2In gas injection to solution, reaction is made to generate
The water mist that generates when being carried through a condenser by carrier gas to remove bubbling of hydrogen sulfide, be then connected to arriving for instrument again
Sample cell passes through the content of light scattering/fluorescence/absorptiometry carbon dioxide.
Claims (3)
1. a kind of assay method of inorganic gas, it is characterised in that carried out by following step：
（1）In a reactor, a certain amount of redox reagent is filled, inorganic gas to be measured is made to be tried by redox
Agent carries out redox reaction, and generating new has volatile substance；The inorganic gas to be measured refers to an oxidation
Carbon, oxygen, ozone, hydrogen sulfide, ammonia, nitrogen oxides, chlorine and chlorine dioxide；
（2）So that the new volatile materials that above-mentioned reaction generates is passed through a separating purifying device, volatility product is made to obtain
Purification；
（3）The purified product with light scatter properties or with photoluminescent property is set by carrier gas to be loaded into non-dispersive atom glimmering
In light photometer, light scattering or fluorescence measurement are carried out, and then measure the content of inorganic gas to be measured.
2. inorganic gas assay method according to claim 1, it is characterised in that when inorganic gas to be measured and redox try
New volatile materials is generated after agent reaction when measurement does not interfere on instrument, the separate purification steps of volatility product
（2）Cancel.
3. the device of inorganic gas assay method described in a kind of claim 1, it is characterised in that the device includes nothing to be measured
Machine gas redox reaction member（1）, reaction product isolation of purified unit（2）, excitation light source（3）, sample cell（4）, inspection
Survey device（5）；Wherein excitation light source（3）It is the high-strength hollow cathode fluorescent lamp on atomic fluorescence of zero dispersion photometer, sample cell（4）It is
Quartz ampoule atomizer on atomic fluorescence of zero dispersion photometer, detector（5）It is the day on atomic fluorescence of zero dispersion photometer
Blind photomultiplier；Inorganic gas to be measured keeps it anti-with redox reagent by the region containing redox reaction reagent
It should be generated as another volatile matter with light scattering or photoluminescent property, and then inorganic gas is carried out by light scattering or fluorescence method
Measurement.
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| CN108132327A (en) * | 2016-12-01 | 2018-06-08 | 中国科学院大连化学物理研究所 | A kind of hydrazine gas-detecting device and its method |
| CN108132328A (en) * | 2016-12-01 | 2018-06-08 | 中国科学院大连化学物理研究所 | A kind of hydrazine gas detection method |
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