CN109613168A - The method for monitoring sulfur dioxide concentration in gas attack chamber on-line - Google Patents
The method for monitoring sulfur dioxide concentration in gas attack chamber on-line Download PDFInfo
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- CN109613168A CN109613168A CN201811230147.4A CN201811230147A CN109613168A CN 109613168 A CN109613168 A CN 109613168A CN 201811230147 A CN201811230147 A CN 201811230147A CN 109613168 A CN109613168 A CN 109613168A
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- gas attack
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- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 41
- 238000012544 monitoring process Methods 0.000 title claims abstract description 17
- 238000010521 absorption reaction Methods 0.000 claims abstract description 36
- 239000012488 sample solution Substances 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 21
- 239000012490 blank solution Substances 0.000 claims abstract description 20
- 239000000243 solution Substances 0.000 claims abstract description 15
- 239000012086 standard solution Substances 0.000 claims abstract description 13
- 238000004255 ion exchange chromatography Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 239000012982 microporous membrane Substances 0.000 claims abstract description 6
- 238000011088 calibration curve Methods 0.000 claims abstract description 3
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 11
- 150000002500 ions Chemical class 0.000 claims description 9
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- 238000004587 chromatography analysis Methods 0.000 claims description 6
- 238000004458 analytical method Methods 0.000 claims description 5
- 238000005070 sampling Methods 0.000 claims description 5
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- 238000005259 measurement Methods 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000005337 ground glass Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 238000005374 membrane filtration Methods 0.000 claims 1
- 239000007789 gas Substances 0.000 description 56
- 238000012360 testing method Methods 0.000 description 19
- 238000005260 corrosion Methods 0.000 description 10
- 230000007797 corrosion Effects 0.000 description 10
- 239000000523 sample Substances 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 239000000809 air pollutant Substances 0.000 description 1
- 231100001243 air pollutant Toxicity 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 230000005226 mechanical processes and functions Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/96—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation using ion-exchange
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
- G01N17/002—Test chambers
Abstract
The invention discloses the methods of sulfur dioxide concentration in on-line monitoring gas attack chamber, connect absorption bottle in the gas outlet of gas attack chamber including (1)；(2) absorbing liquid is packed into absorption bottle；The absorption bottle of replacement in every 0.5~1 hour；(3) absorbing liquid in replaced absorption bottle is sample solution；Sample solution and blank solution are passed through into 0.45 μm of filtering with microporous membrane, ion chromatograph is implanted sequentially and is analyzed；(4) by the SO of 6 groups of various concentrations3 2‑And SO4 2‑Mixed standard solution passes through 0.45 μm of filtering with microporous membrane, carries out ion chromatography, measures SO3 2‑And SO4 2‑Retention time and peak area, draw standard curve；(5) SO in sample solution and blank solution is calculated with calibration curve method3 2‑And SO4 2‑Content, the two merges into SO2Content, (6) SO2With the SO absorbed in every liter of solution2Mass number indicates.
Description
Technical field
Sulfur dioxide gas corrosion test chamber internal corrosion gas is monitored on-line using solution absorption method the present invention relates to a kind of
The method of sulfur dioxide concentration in the method, in particular to on-line monitoring gas attack chamber of concentration.
Background technique
Gas attack test, especially SO2、H2The test of S gas attack is the materials corrosion resistances such as assessment metal, clad plate
The important tests method of energy.The concentration of etchant gas is mainly pressure according to gas cylinder, flow in gas attack chamber at present
Meter reading and volume of the chamber converse next.This conversion is based on " storage pressure is a known constant " or " gas cylinder
Pressure is a known linear change at any time " and " the etchant gas purity in gas cylinder is constant during the whole test process "
What hypotheses were set up.But due to the pressure of gas cylinder as the loss of gas in bottle is a variable, and gas pressure
Variation be not at any time a linear change, and do not ensure that the purity of etchant gas during test in gas cylinder not
Variation, so the actual concentrations of etchant gas exist partially in the concentration and chamber of the etchant gas in the chamber that conversion obtains
Difference.This deviation just seems especially prominent when low concentration (ppm rank) gas attack is tested, and will have a direct impact on technical staff
Judgement to gas attack test result.Because being difficult to obtain the corrosion gas density in accurate chamber, it is difficult standard
True Control experiment time and test process.This problem has constrained gas attack test method in automobile, building materials, coating etc.
The popularization and application of multiple industries.
Solution absorption method is to make a large amount of air by absorbing liquid by way of pumping, in such atmosphere original concentration compared with
Small SO2、H2The etchant gas such as S are concentrated in absorbing liquid, convenient to carry out analysis measurement to its concentration.Solution absorption method is
It is widely used in the air pollutants monitoring of environment protection field, the company of low concentration pollutant (ppm grades) suitable for space
Continuous monitoring.The considerations of solution absorption method is for absorbing liquid stability and absorbing liquid assimilation effect, the sampling time generally 0.5~
Or so 1 hour.Thus, what solution absorption method embodied is the content of the etchant gas in the short period in air.And it is general rotten
The time for losing gas test is several hundred hours to thousands of hours, and the corrosion gas density in gas attack chamber is small 0.5~1
When in concentration can be considered as it is constant.Therefore, SO during available test is analyzed by continuous sampling, repeatedly2、H2The corruption such as S
Lose the situation of change of gas content.
Air enters in case in order to prevent during corrosion test for gas attack chamber, and interference test is as a result, can be right
Chamber uses Seal Design.In addition, in order to during guarantee test gas pressure it is constant, avoid the consumption in corrosion process from drawing
Gas concentration changes in lift, and etchant gas is continuously to be passed through by air inlet, continuously exported by gas outlet during test.
Derived corrosive gas is to avoid pollution atmosphere, needs matched purification device to absorb, is discharged into atmosphere after purification.
Summary of the invention
The purpose of the present invention is to provide the methods of sulfur dioxide concentration in on-line monitoring gas attack chamber, convenient for setting
Count test period, Control experiment process.
The purpose of the present invention is achieved by the following technical programs: sulfur dioxide in on-line monitoring gas attack chamber
The method of concentration, which is characterized in that this method comprises the following steps:
(1) a sealable absorption bottle is connected in the gas outlet of gas attack chamber；
(2) 300~1000 milliliters of absorbing liquids are packed into absorption bottle；The absorption bottle of replacement in every 0.5~1 hour, every time more
Absorption bottle is changed, the absorbing liquid for the equivalent newly prepared is added in bottle；
(3) absorbing liquid in replaced absorption bottle is sample solution；Sample solution and blank solution are passed through into 0.45 μ
M filtering with microporous membrane is implanted sequentially ion chromatograph and is analyzed, and obtains the chromatography of ions figure of sample solution and blank solution；
(4) by the SO of 6 groups of various concentrations3 2-And SO4 2-Mixed standard solution pass through 0.45 μm of filtering with microporous membrane, with
(3) ion chromatography is carried out under identical chromatographic condition, measures SO3 2-And SO4 2-Retention time and peak area, with peak area
SO is drawn to concentration3 2-And SO4 2-Standard curve；
(5) SO in sample solution and blank solution is calculated with calibration curve method3 2-And SO4 2-Content, unit be μ g, the two
Merge into SO2Content, unit be μ g；
(6)SO2Final measurement result is relative value, is the SO to absorb in every liter of solution2Mass number indicates.
Further, the air inlet rubber tube of salable absorption bottle and gas attack chamber in the step (1)
Gas outlet is connected, and the gas outlet rubber tube of salable absorption bottle is connected with the gas cleaning plant of gas attack chamber.
Further, ground glass sealing joint can be selected in salable absorption bottle in the step (1), and rubber can also be used
Plug sealing.
The general volumetric flask for selecting capacity as 500 or 1000ml is used as absorption bottle as needed in actual mechanical process
Rubber stopper sealing, is then accordingly added the absorbing liquid of corrresponding quality.
Further, in the step (2), SO is being carried out2When gas attack is tested, the absorbing liquid is K2CO3It is water-soluble
Liquid, concentration is 1 × 10-2Within the scope of~1mmol/L.With the pure potassium carbonate reagent of analysis and deionized water accurate formulation.
Further, the step (3), (4) intermediate ion chromatographiccondition are as follows: leacheate is 1.8mmol/L Na2CO3+
1.7mmol/L NaHCO3, elute flow velocity are as follows: 0.7~1.0mL/min；Sampling volume: 50 μ L；
Further, the preparation of mixed standard solution is to take 12 100mL volumetric flasks in the step (4), is matched by table 1
SO processed3 2-And SO4 2-Mixed standard solution.
Table 1:SO3 2-And SO4 2-Mixed standard solution
| Bottle number | 1 | 2 | 3 | 4 | 5 | 6 |
| SO3 2-Concentration (mg/L) | 0 | 5.0 | 10.0 | 15.0 | 20.0 | 25.0 |
| SO4 2-Concentration (mg/L) | 0 | 5.0 | 10.0 | 15.0 | 20.0 | 25.0 |
Further, SO in sample solution and blank solution in the step (5)3 2-And SO4 2-Content be respectively as follows:
Wherein,
W1、W2SO in sample solution3 2-And SO4 2-Content, unit be μ g；
W01、W02SO in blank solution3 2-And SO4 2-Content, unit be μ g；
K1、K2SO in standard solution3 2-And SO4 2-Concentration and peak area ratio；
A1、A2SO in sample solution3 2-And SO4 2-Peak area；
A01、A02SO in blank solution3 2-And SO4 2-Peak area；
V --- overall solution volume.
Then, SO2Content are as follows:
Wherein,
W(SO2SO in)-chamber2Content, unit are μ g；
-SO2Molal weight, g/mol；
-SO3 2-Molal weight, g/mol；
-SO4 2-Molal weight, g/mol；
Foreign countries have using probe is installed additional in chamber at present, monitor the side of corrosion gas density in gas attack chamber
Method.But monitoring probe also will receive the corrosion of corrosive gas in chamber, long-time service will affect monitoring result, use one
New probe is needed replacing after the section time, it is expensive.
Compared with prior art, the invention has the following beneficial effects:
(1) it can know the corrosion gas density in chamber, accurately so that more accurately design experiment time, control try
Test process.
(2) what absorbing liquid was selected is the good solution of potassium carbonate of chemical stability, ensure that the reproducibility of test result.
(3) in SO2In analytic process, the chromatography of ions analyzes SO simultaneously3 2-And SO4 2-, can avoid SO3 2-Incomplete oxygen
Change leads to SO2Lower result.
(4) compared to the method for probe monitors, the method for the present invention is more preferable using stability, the lower solution absorption method of cost
(chemical method) is simpler, easily operated.
(5) the method for the present invention uses nontoxic carbonate absorption agent, more safe and environment-friendly.
(6) ion chromatography method is easy to operate, and step is simple, since the error that analytic process is brought into is small, improves point
Analyse the accuracy of result.
Detailed description of the invention
The present invention is described in further details in the following with reference to the drawings and specific embodiments.
Fig. 1 is sample solution A in the embodiment of the present invention1Chromatography of ions figure；
Fig. 2 is SO in the embodiment of the present invention3 2-And SO4 2-Mixed standard solution chromatography of ions figure, mixed standard solution are
5mg/L SO3 2-+5mg/L SO4 2-。
Specific embodiment
The method that the present invention monitors sulfur dioxide concentration in gas attack chamber on-line, includes the following steps:
1, it will seal with rubber stopper and absorption is made equipped with 300mL, the volumetric flask that concentration is 0.1mmol/L potassium carbonate absorbing liquid
Bottle, volumetric flask volume are 500mL, are connected between the gas outlet and gas cleaning plant of gas attack chamber with rubber tube.
After absorbing 30min, removes absorption bottle and change new absorption bottle.Absorbing liquid in absorption bottle can also be in 300~1000 milliliters of models
Interior value is enclosed, the absorption bottle of replacement in every 0.5~1 hour replaces absorption bottle every time, the absorption for the equivalent newly prepared is added in bottle
Liquid.K2CO3The concentration of aqueous solution can also be 1 × 10-2It is accurate with analytical reagents and deionized water within the scope of~1mmol/L
It prepares.
2, by absorbing liquid in absorption bottle with pipette pipette 100mL into beaker with blank solution sample 100mL pass through
Sample solution A is made in 0.45 μm of filtering with microporous membrane respectively1With blank solution A0。
3,12 100mL volumetric flasks are taken, the SO of 6 groups of various concentrations is prepared by table 13 2-And SO4 2-Hybrid standard series.
4, by sample solution A1), blank solution A0) and standard serial solution carry out ion chromatography point under the same conditions
Analysis, ion chromatography condition are as follows: leacheate is 1.8mmol/L Na2CO3+1.7mmol/LNaHCO3, elution flow velocity is 0.7mL/
Min, sampling volume are 50 μ L.Elute flow velocity can also within the scope of 0.7~1.0mL/min value.
5, sample solution ion chromatography SO3 2-And SO4 2-, as shown in Fig. 2, specific test result is shown in Table 2.
Table 2: ion chromatography test result
| A1 | |
| SO3 2-Concentration (mg/L) | 1.08 |
| SO4 2-Concentration (mg/L) | 3.87 |
SO in sample solution and blank solution3 2-And SO4 2-Content be respectively as follows:
Wherein,
W1、W2SO in sample solution3 2-And SO4 2-Content, unit be μ g；
W01、W02SO in blank solution3 2-And SO4 2-Content, unit be μ g；
K1、K2SO in standard solution3 2-And SO4 2-Concentration and peak area ratio；
A1、A2SO in sample solution3 2-And SO4 2-Peak area；
A01、A02SO in-blank solution3 2-And SO4 2-Peak area；
V --- overall solution volume.
Then, SO2Content are as follows:
Wherein,
W(SO2SO in)-chamber2Content, unit are μ g；
—SO2Molal weight, g/mol；
—SO3 2-Molal weight, g/mol；
—SO4 2-Molal weight, g/mol；
Then it obtains,
SO2Measurement result: 3.44 μ g.
The present invention collects the SO flowed out in gas attack chamber using solution absorption method2Etchant gas, and by from
Sub- chromatography SO4 2-And SO3 2-, obtain etchant gas SO2Content.It is supervised compared to existing probe of being placed in cabinet
It surveys, it is simpler, accurate, cheap.
The above embodiment of the present invention is not limiting the scope of the present invention, and embodiments of the present invention are not limited to
This, all this kind above content according to the present invention is not departing from this according to the ordinary technical knowledge and customary means of this field
Modification, replacement or change under the premise of inventing above-mentioned basic fundamental thought, to other diversified forms that above structure of the present invention is made
More, it should belong within protection scope of the present invention.
Claims (7)
1. the method for monitoring sulfur dioxide concentration in gas attack chamber on-line, which is characterized in that this method includes following step
It is rapid:
(1) a sealable absorption bottle is connected in the gas outlet of gas attack chamber；
(2) 300~1000 milliliters of absorbing liquids are packed into absorption bottle；The absorption bottle of replacement in every 0.5~1 hour, replacement is inhaled every time
Bottle is received, the absorbing liquid for the equivalent newly prepared is added in bottle；
(3) absorbing liquid in replaced absorption bottle is sample solution；Sample solution and blank solution is micro- by 0.45 μm
Hole membrane filtration is implanted sequentially ion chromatograph and is analyzed, and obtains the chromatography of ions figure of sample solution and blank solution；
(4) by the SO of 6 groups of various concentrations3 2-And SO4 2-Mixed standard solution pass through 0.45 μm of filtering with microporous membrane, with (3) phase
Ion chromatography is carried out under same chromatographic condition, measures SO3 2-And SO4 2-Retention time and peak area, with peak area to dense
Degree draws SO3 2-And SO4 2-Standard curve；
(5) SO in sample solution and blank solution is calculated with calibration curve method3 2-And SO4 2-Content, unit be μ g, the two merge
For SO2Content, unit be μ g；
(6)SO2Final measurement result is relative value, is the SO to absorb in every liter of solution2Mass number indicates.
2. the method for sulfur dioxide concentration, feature exist in on-line monitoring gas attack chamber according to claim 1
In: the air inlet rubber tube of absorption bottle is connected with the gas outlet of gas attack chamber in the step (1), and absorption bottle goes out
Port rubber tube is connected with the gas cleaning plant of gas attack chamber.
3. the method for sulfur dioxide concentration, feature exist in on-line monitoring gas attack chamber according to claim 1
In: absorption bottle is selected ground glass sealing joint or is adopted and seals with rubber stopper in the step (1).
4. the method for sulfur dioxide concentration, feature exist in on-line monitoring gas attack chamber according to claim 1
In: in the step (2), carrying out SO2When gas attack is tested, the absorbing liquid is K2CO3Aqueous solution, concentration is 1 × 10-2
Within the scope of~1mmol/L, prepared with the pure potassium carbonate reagent of analysis and deionized water.
5. the method for sulfur dioxide concentration, feature exist in on-line monitoring gas attack chamber according to claim 1
In: the step (3), (4) intermediate ion chromatographiccondition are as follows: leacheate is 1.8mmol/L Na2CO3+1.7mmol/L
NaHCO3, elute flow velocity are as follows: 0.7~1.0mL/min；Sampling volume: 50 μ L.
6. the method for sulfur dioxide concentration, feature exist in on-line monitoring gas attack chamber according to claim 1
In: the preparation of mixed standard solution is to take 12 100mL volumetric flasks in the step (4), prepares SO by following proportion3 2-With
SO4 2-Mixed standard solution, wherein 1# bottles of SO3 2-Concentration be 0,1# bottles of SO4 2-Concentration be 0；2# bottles of SO3 2-Concentration be
5.0,2# bottles of SO4 2-Concentration be 5.0；3# bottles of SO3 2-Concentration be 10.0,3# bottles of SO4 2-Concentration be 10.0；4# bottles of SO3 2-'s
Concentration is 15.0,4# bottles of SO4 2-Concentration be 15.0；5# bottles of SO3 2-Concentration be 20.0,5# bottles of SO4 2-Concentration be 20.0；6#
Bottle SO3 2-Concentration be 25.0,6# bottles of SO4 2-Concentration be 25.0；The unit of concentration is mg/L.
7. the method for sulfur dioxide concentration, feature exist in on-line monitoring gas attack chamber according to claim 1
In: SO in sample solution and blank solution in the step (5)3 2-And SO4 2-Content be respectively as follows:
Wherein,
W1、W2SO in sample solution3 2-And SO4 2-Content, unit be μ g；
W01、W02SO in-blank solution3 2-And SO4 2-Content, unit be μ g；
K1、K2SO in-standard solution3 2-And SO4 2-Concentration and peak area ratio；
A1、A2SO in-sample solution3 2-And SO4 2-Peak area；
A01、A02SO in-blank solution3 2-And SO4 2-Peak area；
V --- overall solution volume.
Then, SO2Content are as follows:
Wherein,
W(SO2SO in)-chamber2Content, unit are μ g；
—SO2Molal weight, g/mol；
-SO3 2-Molal weight, g/mol；
—SO4 2-Molal weight, g/mol.
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Application publication date: 20190412 |
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