CN102706996A - Analysis of Ar and O2, N2, CO2 and N2O in atmospheric air through one-time sampling with gas phase chromatography - Google Patents
Analysis of Ar and O2, N2, CO2 and N2O in atmospheric air through one-time sampling with gas phase chromatography Download PDFInfo
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- CN102706996A CN102706996A CN2012102127900A CN201210212790A CN102706996A CN 102706996 A CN102706996 A CN 102706996A CN 2012102127900 A CN2012102127900 A CN 2012102127900A CN 201210212790 A CN201210212790 A CN 201210212790A CN 102706996 A CN102706996 A CN 102706996A
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Abstract
The invention relates to analysis of Ar and O2, N2, CO2 and N2O in atmospheric air through one-time sampling with gas phase chromatography. The method comprises the following steps of: making carrier gas of which the purity is over 99.999 percent flow through a purifier under the output pressure of 0.20-0.60MPa till the purity of the purified carrier gas is over 99.9999 percent or over 99.99999 percent; introducing the purified carrier gas into a chromatographic column in which a sample to be tested is placed in a gas chromatograph, performing adsorption and desorption, feeding into an electron capture detector for detecting, and inputting detected data into a chromatographic work station in the gas chromatograph by using the electron capture detector; and meanwhile, feeding carrier gas and Ar and O2, N2, CO2 and N2O in the sample to be detected into the chromatographic column in the gas chromatograph, performing adsorption and desorption, feeding into a thermal conductivity cell detector for detecting, and inputting detected data into the chromatographic work station in the gas chromatograph by using the thermal conductivity cell detector to obtain an analysis result chromatogram. According to the invention, easiness in operating is realized, the data accuracy error can be lowered effectively, and the sample measuring period is shortened.
Description
Technical field
The present invention relates to technical fields such as mine safety, environmental protection, the preparation of empty branch, relate in particular to Ar+O in the vapor-phase chromatography single injected sampling analyse atmos
2, N
2, CO
2, N
2O.
Background technology
At present, adopt Ar+O in the gc analysis atmosphere
2, N
2, CO
2, N
2The O component needs the above sample introduction of secondary just can obtain net result, and this mode not only causes the data precision error bigger, and has prolonged the sample measurement cycle.
Summary of the invention
Technical matters to be solved by this invention provides Ar+O in a kind of effective reduction data precision error, the vapor-phase chromatography single injected sampling analyse atmos in shortening sample measurement cycle
2, N
2, CO
2, N
2O.
For addressing the above problem Ar+O in the vapor-phase chromatography single injected sampling analyse atmos of the present invention
2, N
2, CO
2, N
2O is characterized in that: at first with purity greater than 99.999% carrier gas with the output pressure of 0.20 ~ 0.60MPa through clarifier, make carrier gas purity after the purification greater than 99.9999% or greater than 99.99999%; Then the carrier gas after the said purification is fed the chromatographic column of having placed testing sample in the gas chromatograph with the flow of 15 ~ 75ml/min, under 25 ~ 50 ℃ temperature
In, under 25 ~ 250 ℃ the temperature after the adsorption/desorption effect, the Ar+O in the said testing sample
2, N
2, CO
2, N
2O gets into electron capture detector (ECD) (ECD) and under 90 ~ 350 ℃ temperature, detects CO
2, N
2O, and detected data are inputed to the chromatographic work station in the said gas chromatograph by said electron capture detector (ECD) (ECD); Ar+O in said carrier gas simultaneously and the said testing sample
2, N
2, CO
2, N
2O gets into the chromatographic column in the gas chromatograph jointly
, under 25 ~ 250 ℃ the temperature after the adsorption/desorption effect, the Ar+O in the said testing sample
2, N
2, CO
2, N
2O gets into thermal conductivity cell detector (TCD) and under 90 ~ 350 ℃ temperature, detects Ar+O
2, N
2, and detected data are inputed to the chromatographic work station in the said gas chromatograph by said thermal conductivity cell detector (TCD), can obtain the analysis result chromatogram.
Said carrier gas is He, Ne, Ar, H
2In any one.
Said clarifier is meant that being the container that 30 ~ 45 ㎜, length are interior dress molecular sieve, discolour silica gel and deoxidation-Tuo hydrocarbon-decarburization oxide filler of 250 ~ 450 ㎜ by three series connection and internal diameter forms; An end of the container of dress discolour silica gel links to each other with the container of said interior dress molecular sieve in said, and its other end then links to each other with the container of said interior dress deoxidation-Tuo hydrocarbon filler-decarburization oxide; The container of dress molecular sieve communicates with said carrier gas in said; Deoxidation in the container of dress deoxidation-Tuo hydrocarbon-decarburization oxide filler in said, the volumetric ratio of taking off hydrocarbon, decarburization oxide are 1:1:1, and communicate with said chromatographic column
.
Filling 4A molecular sieve and 5A molecular sieve in the container of dress molecular sieve in said, and the volumetric ratio of 4A molecular sieve, 5A molecular sieve is 1:1.
Said deoxidation filler is meant dehydrogenation catalyst.
The said hydrocarbon filler that takes off is meant and takes off hydrocarbon catalyst.
Said decarburization oxide is meant the purifying carbon dioxide catalyzer.
Said chromatographic column
be meant internal diameter be 1 ~ 5mm, column length be 2 ~ 8m and in fill out Porapak, Chromosorb, GDX porous polymer bead stainless-steel tube, or internal diameter is that 0.25 ~ 0.53mm, column length are the PLOT Q quartz capillary of 30 ~ 90m.
Said chromatographic column
be meant internal diameter be 1 ~ 5mm, column length be 2 ~ 8m and in fill out the stainless-steel tube of molecular sieve, or internal diameter is that 0.25 ~ 0.53mm, column length are the PLOT MS quartz capillary of 30 ~ 90m; Wherein molecular sieve is a kind of in 4A, 5A, 13X, the carbonaceous molecular sieve.
The present invention compared with prior art has the following advantages:
1, owing to the present invention two root chromatogram columns and electron capture detector (ECD) (ECD), thermal conductivity cell detector (TCD) are cascaded; Therefore; Can realize the purpose that single injected sampling is analyzed, thereby reduce the data precision error effectively, also shorten the sample measurement cycle simultaneously.
2, owing to need the above sample introduction of secondary in the prior art, the double above time, therefore will obtain two chromatograms respectively at electron capture detector (ECD) (ECD) and thermal conductivity cell detector (TCD); And the present invention only needs single injected sampling, just can obtain a complete analysis result chromatogram, is merely 1/2nd (referring to Fig. 2 ~ 7) of prior art its analysis time.Simultaneously, data precision has also obtained effective raising (referring to table 1).
Table 1: adopt the standard gas of the inventive method mensuration and the Ar+O of steel cylinder air
2, N
2, CO
2, N
2O component data
Annotate: national chromatographic data precision relative standard deviation RSD (%)<5%.
3, the present invention is simple, easy to operate.
Description of drawings
Do further detailed explanation below in conjunction with the accompanying drawing specific embodiments of the invention.
Fig. 1 is a gas phase chromatographic device synoptic diagram of the present invention.
Fig. 2 is single injected sampling ECD of the present invention, TCD analytical standard gas (N
2O=3.2ppm, CO
2=307ppm, N
2=99.96%) normalizing chromatogram.
Fig. 3 is single injected sampling ECD of the present invention, TCD analytical standard gas (N
2O=3.2ppm, CO
2=307ppm, N
2=99.96%) expansive color spectrogram.
Fig. 4 is single injected sampling ECD of the present invention, TCD analyse atmos normalizing chromatogram.
Fig. 5 is single injected sampling ECD of the present invention, TCD analyse atmos expansive color spectrogram.
Fig. 6 is single injected sampling ECD of the present invention, TCD analytical standard gas (N
2O=3.2ppm, CO
2=307ppm, N
2=99.96%) atmosphere stack contrast normalizing chromatogram.
Fig. 7 is single injected sampling ECD of the present invention, TCD analytical standard gas (N
2O=3.2ppm, CO
2=307ppm, N
2=99.96%) atmosphere stack contrast expansive color spectrogram.
Embodiment
Embodiment 1As shown in Figure 1, Ar+O in the vapor-phase chromatography single injected sampling analyse atmos
2, N
2, CO
2, N
2O, at first with purity greater than 99.999% carrier gas with the output pressure of 0.20MPa through clarifier, make carrier gas purity after the purification greater than 99.9999% or greater than 99.99999%; Carrier gas after will purifying then feeds the chromatographic column of having placed testing sample in the gas chromatograph with the flow of 15ml/min, under 25 ℃ temperature
In, under 25 ℃ the temperature after the adsorption/desorption effect, the Ar+O in the testing sample
2, N
2, CO
2, N
2O gets into electron capture detector (ECD) (ECD) and under 90 ℃ temperature, detects CO
2, N
2O, and detected data are inputed to the chromatographic work station in the gas chromatograph by electron capture detector (ECD) (ECD); Ar+O in carrier gas simultaneously and the testing sample
2, N
2, CO
2, N
2O gets into the chromatographic column in the gas chromatograph jointly
, under 25 ℃ the temperature after the adsorption/desorption effect, the Ar+O in the testing sample
2, N
2, CO
2, N
2O gets into thermal conductivity cell detector (TCD) and under 90 ℃ temperature, detects Ar+O
2, N
2, and detected data are inputed to the chromatographic work station in the gas chromatograph by thermal conductivity cell detector (TCD), can obtain the analysis result chromatogram.
Wherein: carrier gas is He.
Chromatographic column
be meant internal diameter be 1mm, column length be 8m and in fill out Porapak, Chromosorb, GDX porous polymer bead stainless-steel tube.
Chromatographic column
be meant internal diameter be 1mm, column length be 8m and in fill out the stainless-steel tube of molecular sieve; Wherein molecular sieve is a kind of in 4A, 5A, 13X, the carbonaceous molecular sieve.
Embodiment 2As shown in Figure 1, Ar+O in the vapor-phase chromatography single injected sampling analyse atmos
2, N
2, CO
2, N
2O, at first with purity greater than 99.999% carrier gas with the output pressure of 0.60MPa through clarifier, make carrier gas purity after the purification greater than 99.9999% or greater than 99.99999%; Carrier gas after will purifying then feeds the chromatographic column of having placed testing sample in the gas chromatograph with the flow of 75ml/min, under 50 ℃ temperature
In, under 250 ℃ the temperature after the adsorption/desorption effect, the Ar+O in the testing sample
2, N
2, CO
2, N
2O gets into electron capture detector (ECD) (ECD) and under 350 ℃ temperature, detects CO
2, N
2O, and detected data are inputed to the chromatographic work station in the gas chromatograph by electron capture detector (ECD) (ECD); Ar+O in carrier gas simultaneously and the testing sample
2, N
2, CO
2, N
2O gets into the chromatographic column in the gas chromatograph jointly
, under 250 ℃ the temperature after the adsorption/desorption effect, the Ar+O in the testing sample
2, N
2, CO
2, N
2O gets into thermal conductivity cell detector (TCD) and under 350 ℃ temperature, detects Ar+O
2, N
2, and detected data are inputed to the chromatographic work station in the gas chromatograph by thermal conductivity cell detector (TCD), can obtain the analysis result chromatogram.
Wherein: carrier gas is Ne.
Chromatographic column
be meant internal diameter be 5mm, column length be 2m and in fill out Porapak, Chromosorb, GDX porous polymer bead stainless-steel tube.
Chromatographic column
be meant internal diameter be 5mm, column length be 2m and in fill out the stainless-steel tube of molecular sieve; Wherein molecular sieve is a kind of in 4A, 5A, 13X, the carbonaceous molecular sieve.
Embodiment 3As shown in Figure 1, Ar+O in the vapor-phase chromatography single injected sampling analyse atmos
2, N
2, CO
2, N
2O, at first with purity greater than 99.999% carrier gas with the output pressure of 0.40MPa through clarifier, make carrier gas purity after the purification greater than 99.9999% or greater than 99.99999%; Carrier gas after will purifying then feeds the chromatographic column of having placed testing sample in the gas chromatograph with the flow of 45ml/min, under 35 ℃ temperature
In, under 100 ℃ the temperature after the adsorption/desorption effect, the Ar+O in the testing sample
2, N
2, CO
2, N
2O gets into electron capture detector (ECD) (ECD) and under 220 ℃ temperature, detects CO
2, N
2O, and detected data are inputed to the chromatographic work station in the gas chromatograph by electron capture detector (ECD) (ECD); Ar+O in carrier gas simultaneously and the testing sample
2, N
2, CO
2, N
2O gets into the chromatographic column in the gas chromatograph jointly
, under 100 ℃ the temperature after the adsorption/desorption effect, the Ar+O in the testing sample
2, N
2, CO
2, N
2O gets into thermal conductivity cell detector (TCD) and under 220 ℃ temperature, detects Ar+O
2, N
2, and detected data are inputed to the chromatographic work station in the gas chromatograph by thermal conductivity cell detector (TCD), can obtain the analysis result chromatogram.
Wherein: carrier gas is Ar.
Chromatographic column
be meant internal diameter be 3mm, column length be 5m and in fill out Porapak, Chromosorb, GDX porous polymer bead stainless-steel tube.
Chromatographic column
be meant internal diameter be 3mm, column length be 5m and in fill out the stainless-steel tube of molecular sieve; Wherein molecular sieve is a kind of in 4A, 5A, 13X, the carbonaceous molecular sieve.
Embodiment 4As shown in Figure 1, Ar+O in the vapor-phase chromatography single injected sampling analyse atmos
2, N
2, CO
2, N
2O, at first with purity greater than 99.999% carrier gas with the output pressure of 0.50MPa through clarifier, make carrier gas purity after the purification greater than 99.9999% or greater than 99.99999%; Carrier gas after will purifying then feeds the chromatographic column of having placed testing sample in the gas chromatograph with the flow of 30ml/min, under 40 ℃ temperature
In, under 200 ℃ the temperature after the adsorption/desorption effect, the Ar+O in the testing sample
2, N
2, CO
2, N
2O gets into electron capture detector (ECD) (ECD) and under 200 ℃ temperature, detects CO
2, N
2O, and detected data are inputed to the chromatographic work station in the gas chromatograph by electron capture detector (ECD) (ECD); Ar+O in carrier gas simultaneously and the testing sample
2, N
2, CO
2, N
2O gets into the chromatographic column in the gas chromatograph jointly
, under 200 ℃ the temperature after the adsorption/desorption effect, the Ar+O in the testing sample
2, N
2, CO
2, N
2O gets into thermal conductivity cell detector (TCD) and under 200 ℃ temperature, detects Ar+O
2, N
2, and detected data are inputed to the chromatographic work station in the gas chromatograph by thermal conductivity cell detector (TCD), can obtain the analysis result chromatogram.
Wherein: carrier gas is H
2
Chromatographic column
is meant that internal diameter is that 0.25mm, column length are the PLOT Q quartz capillary of 90m.
Chromatographic column
is meant that internal diameter is that 0.25mm, column length are the PLOT MS quartz capillary of 90m.
Embodiment 5As shown in Figure 1, Ar+O in the vapor-phase chromatography single injected sampling analyse atmos
2, N
2, CO
2, N
2O, at first with purity greater than 99.999% carrier gas with the output pressure of 0.55MPa through clarifier, make carrier gas purity after the purification greater than 99.9999% or greater than 99.99999%; Carrier gas after will purifying then feeds the chromatographic column of having placed testing sample in the gas chromatograph with the flow of 65ml/min, under 45 ℃ temperature
In, under 225 ℃ the temperature after the adsorption/desorption effect, the Ar+O in the testing sample
2, N
2, CO
2, N
2O gets into electron capture detector (ECD) (ECD) and under 300 ℃ temperature, detects CO
2, N
2O, and detected data are inputed to the chromatographic work station in the gas chromatograph by electron capture detector (ECD) (ECD); Ar+O in carrier gas simultaneously and the testing sample
2, N
2, CO
2, N
2O gets into the chromatographic column in the gas chromatograph jointly
, under 225 ℃ the temperature after the adsorption/desorption effect, the Ar+O in the testing sample
2, N
2, CO
2, N
2O gets into thermal conductivity cell detector (TCD) and under 300 ℃ temperature, detects Ar+O
2, N
2, and detected data are inputed to the chromatographic work station in the gas chromatograph by thermal conductivity cell detector (TCD), can obtain the analysis result chromatogram.
Wherein: carrier gas is H
2
Chromatographic column
is meant that internal diameter is that 0.53mm, column length are the PLOT Q quartz capillary of 30m.
Chromatographic column
is meant that internal diameter is that 0.53mm, column length are the PLOT MS quartz capillary of 30m.
Embodiment 6As shown in Figure 1, Ar+O in the vapor-phase chromatography single injected sampling analyse atmos
2, N
2, CO
2, N
2O, at first with purity greater than 99.999% carrier gas with the output pressure of 0.25MPa through clarifier, make carrier gas purity after the purification greater than 99.9999% or greater than 99.99999%; Carrier gas after will purifying then feeds the chromatographic column of having placed testing sample in the gas chromatograph with the flow of 20ml/min, under 35 ℃ temperature
In, under 150 ℃ the temperature after the adsorption/desorption effect, the Ar+O in the testing sample
2, N
2, CO
2, N
2O gets into electron capture detector (ECD) (ECD) and under 150 ℃ temperature, detects CO
2, N
2O, and detected data are inputed to the chromatographic work station in the gas chromatograph by electron capture detector (ECD) (ECD); Ar+O in carrier gas simultaneously and the testing sample
2, N
2, CO
2, N
2O gets into the chromatographic column in the gas chromatograph jointly
, under 150 ℃ the temperature after the adsorption/desorption effect, the Ar+O in the testing sample
2, N
2, CO
2, N
2O gets into thermal conductivity cell detector (TCD) and under 150 ℃ temperature, detects Ar+O
2, N
2, and detected data are inputed to the chromatographic work station in the gas chromatograph by thermal conductivity cell detector (TCD), can obtain the analysis result chromatogram.
Wherein: carrier gas is H
2
Chromatographic column
is meant that internal diameter is that 40mm, column length are the PLOT Q quartz capillary of 60m.
Chromatographic column
is meant that internal diameter is that 40mm, column length are the PLOT MS quartz capillary of 60m.
Above-mentioned
Embodiment 1 ~ 6In, clarifier is meant that being the container that 30 ~ 45 ㎜, length are interior dress molecular sieve, discolour silica gel and deoxidation-Tuo hydrocarbon-decarburization oxide filler of 250 ~ 450 ㎜ by three series connection and internal diameter forms.One end of the container of interior dress discolour silica gel links to each other with the container of interior dress molecular sieve, and its other end then links to each other with the container of interior dress deoxidation-Tuo hydrocarbon filler-decarburization oxide; The container of interior dress molecular sieve communicates with carrier gas; In deoxidation in the container of dress deoxidation-Tuo hydrocarbon-decarburization oxide filler, the volumetric ratio of taking off hydrocarbon, decarburization oxide be 1:1:1, and communicate with chromatographic column
.
In filling 4A molecular sieve and 5A molecular sieve in the container of dress molecular sieve, and the volumetric ratio of 4A molecular sieve, 5A molecular sieve is 1:1.
The deoxidation filler is meant dehydrogenation catalyst.Taking off the hydrocarbon filler is meant and takes off hydrocarbon catalyst.The decarburization oxide is meant the purifying carbon dioxide catalyzer.
Gas chromatograph is the commercially available prod, and its sampling ring is 0.5 ~ 5ml, and the sampling period is 0.01 ~ 2s.
Claims (9)
1. Ar+O in the vapor-phase chromatography single injected sampling analyse atmos
2, N
2, CO
2, N
2O is characterized in that: at first with purity greater than 99.999% carrier gas with the output pressure of 0.20 ~ 0.60MPa through clarifier, make carrier gas purity after the purification greater than 99.9999% or greater than 99.99999%; Then the carrier gas after the said purification is fed the chromatographic column of having placed testing sample in the gas chromatograph with the flow of 15 ~ 75ml/min, under 25 ~ 50 ℃ temperature
In, under 25 ~ 250 ℃ the temperature after the adsorption/desorption effect, the Ar+O in the said testing sample
2, N
2, CO
2, N
2O gets into electron capture detector (ECD) and under 90 ~ 350 ℃ temperature, detects CO
2, N
2O, and detected data are inputed to the chromatographic work station in the said gas chromatograph by said electron capture detector (ECD); Ar+O in said carrier gas simultaneously and the said testing sample
2, N
2, CO
2, N
2O gets into the chromatographic column in the gas chromatograph jointly
, under 25 ~ 250 ℃ the temperature after the adsorption/desorption effect, the Ar+O in the said testing sample
2, N
2, CO
2, N
2O gets into thermal conductivity cell detector and under 90 ~ 350 ℃ temperature, detects Ar+O
2, N
2, and detected data are inputed to the chromatographic work station in the said gas chromatograph by said thermal conductivity cell detector, can obtain the analysis result chromatogram.
2. Ar+O in the vapor-phase chromatography single injected sampling analyse atmos as claimed in claim 1
2, N
2, CO
2, N
2O is characterized in that: said carrier gas is He, Ne, Ar, H
2In any one.
3. Ar+O in the vapor-phase chromatography single injected sampling analyse atmos as claimed in claim 1
2, N
2, CO
2, N
2O is characterized in that: said clarifier is meant that being the container that 30 ~ 45 ㎜, length are interior dress molecular sieve, discolour silica gel and deoxidation-Tuo hydrocarbon-decarburization oxide filler of 250 ~ 450 ㎜ by three series connection and internal diameter forms; An end of the container of dress discolour silica gel links to each other with the container of said interior dress molecular sieve in said, and its other end then links to each other with the container of said interior dress deoxidation-Tuo hydrocarbon filler-decarburization oxide; The container of dress molecular sieve communicates with said carrier gas in said; Deoxidation in the container of dress deoxidation-Tuo hydrocarbon-decarburization oxide filler in said, the volumetric ratio of taking off hydrocarbon, decarburization oxide are 1:1:1, and with said chromatographic column
Communicate.
4. Ar+O in the vapor-phase chromatography single injected sampling analyse atmos as claimed in claim 3
2, N
2, CO
2, N
2O is characterized in that: filling 4A molecular sieve and 5A molecular sieve in the container of dress molecular sieve in said, and the volumetric ratio of 4A molecular sieve, 5A molecular sieve is 1:1.
5. Ar+O in the vapor-phase chromatography single injected sampling analyse atmos as claimed in claim 3
2, N
2, CO
2, N
2O is characterized in that: said deoxidation filler is meant dehydrogenation catalyst.
6. Ar+O in the vapor-phase chromatography single injected sampling analyse atmos as claimed in claim 3
2, N
2, CO
2, N
2O is characterized in that: the said hydrocarbon filler that takes off is meant and takes off hydrocarbon catalyst.
7. Ar+O in the vapor-phase chromatography single injected sampling analyse atmos as claimed in claim 3
2, N
2, CO
2, N
2O is characterized in that: said decarburization oxide is meant the purifying carbon dioxide catalyzer.
8. Ar+O in the vapor-phase chromatography single injected sampling analyse atmos as claimed in claim 1
2, N
2, CO
2, N
2O is characterized in that: said chromatographic column
Be meant internal diameter be 1 ~ 5mm, column length be 2 ~ 8m and in fill out Porapak, Chromosorb, GDX porous polymer bead stainless-steel tube, or internal diameter is that 0.25 ~ 0.53mm, column length are the PLOT Q quartz capillary of 30 ~ 90m.
9. Ar+O in the vapor-phase chromatography single injected sampling analyse atmos as claimed in claim 1
2, N
2, CO
2, N
2O is characterized in that: said chromatographic column
Be meant internal diameter be 1 ~ 5mm, column length be 2 ~ 8m and in fill out the stainless-steel tube of molecular sieve, or internal diameter is that 0.25 ~ 0.53mm, column length are the PLOT MS quartz capillary of 30 ~ 90m; Wherein molecular sieve is a kind of in 4A, 5A, 13X, the carbonaceous molecular sieve.
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CN114935610A (en) * | 2022-04-05 | 2022-08-23 | 陕西长青能源化工有限公司 | Method and system for simultaneously measuring contents of sulfur-containing and alcohol-containing components in acid gas by gas chromatography |
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