CN107525698A - Standard sample and its application for individual particle aerosol mass spectrometer performance adjustment - Google Patents
Standard sample and its application for individual particle aerosol mass spectrometer performance adjustment Download PDFInfo
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- CN107525698A CN107525698A CN201610464288.7A CN201610464288A CN107525698A CN 107525698 A CN107525698 A CN 107525698A CN 201610464288 A CN201610464288 A CN 201610464288A CN 107525698 A CN107525698 A CN 107525698A
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- standard sample
- mass spectrometer
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- aerosol mass
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N2001/2893—Preparing calibration standards
Abstract
The present invention relates to a kind of standard sample for individual particle aerosol mass spectrometer performance adjustment and its application.The standard sample includes following components:LiNO3、NaNO3、KNO3、Cu(NO3)2、AgNO3、Pb(NO3)2With N (phosphoric acid methyl) glycine.The standard sample coordinates aerosol generator to use, and solves the ununified debugging standard samples of current SPAMS, the problem of so as to cause different SPAMS instrument performance inconsistent.And there is ion abundant information, the advantages that mass number wide coverage can reflect organic and inorganic two parts ionization property simultaneously, and ionic strength is high, easy to use, and stability is good.
Description
Technical field
The present invention relates to analysis technical field, is applied to individual particle aerosol mass spectrometer more particularly to one kind
The standard sample that can be debugged and its application.
Background technology
Individual particle aerosol mass spectrometer (SPAMS) is that one kind being capable of the single aerosol particle of real time on-line monitoring
The sophisticated analytical instruments of particle diameter and chemical composition.The general principle of its work is:Aerosol particle is differential true
Under empty condition, by sample introduction micro pore sheet air inlet dynamics lens, and standard is accumulated into the case where the latter acts on
Straight particle beam.Particle beam then passes through two difference 6cm 532nm lasers, and caused scattering light is successively
Detected after the focusing of ellipsoid mirror-reflection by photomultiplier, detection signal is transferred to sequence circuit and calculated
Go out the flying speed of particle, and then converse the particle diameter of particle.Particle after calibrating goes successively to ionized region,
And by 266nm Nd:The melting ionization of YAG ultraviolet pulse lasers produces negative ions, in a series of electric field actions
Under, ion reaches microchannel plate detector, and its detection signal is finally collected card and collects and be converted to mass spectrum letter
Number.
Compared to conventional aerosol detection method, SPAMS have can detect particle size, without sample before
Processing, individual particle level analysis, real time on-line monitoring, chemical constituent while many advantages such as detection.
Therefore, the technology relatively broadly be applied to atmospheric environment analysis and research field, and material science,
Also there is certain application in the fields such as biology, national defence, further with individual particle aerosol mass spectrometry technical research
Deeply, its application will further extend.But present problems faced is that SPAMS debugging is basic
It is using atmospheric aerosol as standard, and atmospheric aerosol changes with the change in space over time, therefore
The uniformity of different instrument performances is difficult to ensure that as debugging standard.The leading indicator of SPAMS performance characterizations
For source resolution result, embodiments method referenced patent CN 102601059A.Briefly, one group is given
Data, according to the algorithm of setting, the particle with similar mass spectral characteristic is classified as same type by instrument, no
Particle with mass spectral characteristic can be divided into several different types, and each type accounts for the ratio of total particle number i.e.
To reorganize the source resolution of data.Source resolution result and instrument performance are closely related.So far, we are not yet
Find the standard sample for being specifically applied to SPAMS debugging.
The content of the invention
Based on this, present invention aim to address current SPAMS not to unify debugging standard sample, so as to
The problem of causing different SPAMS instrument performance inconsistent.Therefore, the invention provides one kind to be used for single
The standard sample of grain aerosol mass spectrometer performance adjustment.
Concrete technical scheme is as follows:
A kind of standard sample for individual particle aerosol mass spectrometer performance adjustment, include the component of following proportioning:
In wherein some embodiments, the standard sample includes the component of following proportioning:
In wherein some embodiments, the standard sample includes the component of following proportioning:
In wherein some embodiments, the standard sample is the aqueous solution being prepared by said components and water,
The concentration of each component in aqueous is:
In wherein some embodiments, the concentration of each component in aqueous is:
In wherein some embodiments, the concentration of each component in aqueous is:
Present invention also offers a kind of preparation of the standard sample for individual particle aerosol mass spectrometer performance adjustment
Method.
Concrete technical scheme is as follows:
A kind of preparation method of standard sample for individual particle aerosol mass spectrometer performance adjustment, including it is following
Step:
(1) preparation of Standard Stock solutions:LiNO is weighed respectively3、NaNO3、KNO3、Cu(NO3)2、
AgNO3With Pb (NO3)2Into respective sample bottle, then 50mL deionized water dissolvings are used respectively, obtain each gold
Belong to the Standard Stock solutions of salt component;N- (phosphoric acid methyl) glycine is weighed, it is water-soluble with 30mL deionizations
Solution, obtains the Standard Stock solutions of N- (phosphoric acid methyl) glycine;Weigh LiNO3、NaNO3、KNO3、
Cu(NO3)2、AgNO3、Pb(NO3)2Quality with N- (phosphoric acid methyl) glycine be respectively 0.01~0.1g,
0.01~0.1g, 0.01~0.1g, 0.1~0.5g, 0.1~0.5g, 1~5g, 0.1~0.5g;
(2) preparation of the aqueous solution of standard sample:LiNO is pipetted respectively3、NaNO3、KNO3、Cu(NO3)2、
AgNO3With Pb (NO3)2Standard Stock solutions into same sample bottle, its volume be respectively 0.2~0.3mL,
0.3~0.4mL, 0.3~0.4mL, 0.6~0.9mL, 0.6~0.9mL and 0.6~0.9mL, Ran Houjia
Enter deionized water dissolving mixing, be settled to 50mL with deionized water, add 1~2mL N- (phosphoric acid methyl)
The Standard Stock solutions of glycine, mix, produce.
In wherein some embodiments, step (1) weighs LiNO3、NaNO3、KNO3、Cu(NO3)2、
AgNO3、Pb(NO3)2Quality with N- (phosphoric acid methyl) glycine be respectively 0.01-0.05g, 0.01-0.05g,
0.01-0.05g、0.5-1g、0.1-0.3g、1-3g、0.1-0.3g。
Present invention also offers a kind of application of above-mentioned standard sample.
Concrete technical scheme is as follows:
Application of the above-mentioned standard sample in the method for performance adjustment is carried out to individual particle aerosol mass spectrometer.
In wherein some embodiments, the method bag that performance adjustment is carried out to individual particle aerosol mass spectrometer
Include following steps:Above-mentioned standard sample is put into the aerosol generator of individual particle aerosol mass spectrometer, controlled
It is 0.5~0.6LPM that aerosol processed, which produces flow, gathers aerosol particle, counts the average peak of each characteristic ion
Area, then conditioning instrumentation parameter make the performance of each individual particle aerosol mass spectrometer reach unanimity.
Present invention also offers a kind of method that performance adjustment is carried out to individual particle aerosol mass spectrometer.
Concrete technical scheme is as follows:
A kind of method that performance adjustment is carried out to individual particle aerosol mass spectrometer, comprises the following steps:Will be above-mentioned
Standard sample is put into the aerosol generator of individual particle aerosol mass spectrometer, is controlled aerosol to produce flow and is
0.5~0.6LPM, aerosol particle is gathered, count the average peak area of each characteristic ion, then conditioning instrumentation ginseng
Number makes the performance of each individual particle aerosol mass spectrometer reach unanimity.
Because the main function of SPAMS instruments is that Atmospheric particulates composition is analyzed, therefore it is required that standard
Properties of samples is as close possible to Atmospheric particulates property, Atmospheric particulates property main standard:(1) cation
Main matter composition and division in a proportion coverage is m/z1~208, and the main matter composition and division in a proportion coverage of anion is m/z-98~-1;
(2) inorganic ions and organic ion are included;(3) total ion current intensity (TIC) > 300;(4) toggle rate > 7;
(5) slugging average > 20%.
According to above-mentioned requirements, and as standard sample performance must stablize and convenient use requirement, invent
People finally gives the standard sample of the present invention for SPAMS performance adjustments by substantial amounts of experimental study
Product.Solve the ununified debugging standard samples of current SPAMS, so as to cause different SPAMS instrument
The problem of device performance is inconsistent, after according to standard sample configured information conditioning instrumentation, SPAMS source resolution spectrograms
Reach unanimity, i.e., different SPAMS instrument performance reaches unanimity.
The standard sample for SPAMS performance adjustments of the present invention has further the advantage that:
(1) ion abundant information, mass number wide coverage:The prevailing quality number that its cation includes has
M/z7,23,30,39,42,47,63,65,107,109,206,207,208, anion includes
Prevailing quality number have m/z-16, -17, -26, -46, -62, -63, -79, -122, -169, can cover
Normal atmospheric aerosol ion mass range.
(2) organic and inorganic two parts ionization property can be reflected simultaneously:In standard sample containing six kinds of metals from
Sub and a kind of organic component, is reflected on mass spectrogram, inorganic component has Li in cation+、Na+、K+、Cu+、
Ag+、Pb+Deng organic debris has C2H2O+、PO+Deng;In anion inorganic component have O-, OH-, NO2-,
NO3 -Deng organic debris has PO3 -、C3H7NO5P-Deng.
(3) ionic strength is high:The ionic strength of standard sample is totally better than atmospheric aerosol sample, especially
Anion.
(4) toggle rate and slugging average are close actual:The toggle rate of standard sample is more than 7/second, and slugging average is big
In 17%, and different according to air quality in practical application, atmospheric aerosol toggle rate 2~18/second it
Between change, slugging average is generally higher than 20%.
(5) it is easy to use:In the aqueous solution of the standard sample, its solvent only has deionized water, prepares it
After can be used directly, and can reuse.
(6) stability is good, retention cycle length:The Standard Stock solutions holding time is more than 90 days, standard sample
The aqueous solution retention cycle of product is more than 30 days.
Brief description of the drawings
Fig. 1 is the feature spectrogram of the standard sample in embodiment 2;
Fig. 2 is the feature spectrogram of atmospheric aerosol;
Fig. 3 be embodiment 4 in SPAMS instrument parameter is adjusted with standard sample before air-source
Parse pie chart;
Fig. 4 be embodiment 4 in SPAMS instrument parameter is adjusted with standard sample after air-source
Parse pie chart.
Embodiment
The standard for individual particle aerosol mass spectrometer performance adjustment below in conjunction with specific embodiment to the present invention
Sample and its application are further elaborated.
Embodiment 1
A kind of standard sample for individual particle aerosol mass spectrometer performance adjustment of the present embodiment is by six kinds of gold
The aqueous solution that category salt and a kind of water soluble organic substance mix by a certain percentage.Its preparation method includes following
Step:
(1) preparation of Standard Stock solutions
The each component of quality shown in table 1 is weighed using assay balance, is put into corresponding sample bottle, Ran Hou
50mL deionized water dissolvings are separately added into each component of metal salt, 30mL deionized waters are added in organic matter
Dissolving, produce the Standard Stock solutions of each component.
The preparation of the Standard Stock solutions of each component of table 1
(2) preparation of the aqueous solution of standard sample
The Standard Stock solutions of step (1) configuration are taken out, LiNO is pipetted respectively using liquid-transfering gun3、NaNO3、
KNO3、Cu(NO3)2、AgNO3With Pb (NO3)2Standard Stock solutions in same sample bottle, its volume
Respectively 0.2mL, 0.3mL, 0.3mL, 0.6mL, 0.6mL, 0.9mL, it is water-soluble then to add deionization
Solution, mix, be settled to 50mL with deionized water, add 2mL N- (phosphoric acid methyl) glycine
(C3H8NO5P Standard Stock solutions), mix, produce.
Embodiment 2
The aqueous solution for the standard sample that embodiment 1 is prepared is poured into SPAMS aerosol generator, is adjusted
Solar term colloidal sol flow is 0.57LPM, and service condition is:Laser energy is 0.5mJ, the μ s of Time delay 0.8,
Balance 1V, sampling length 25 μ s, input range 5V, signal skew 2.5V, background threshold values 3V are triggered,
PMT threshold values -0.17V, PKL are arranged to peak height more than 5 and peak area is more than 30 and effectively peak number is more than 3.
Strike counts, and gathers 1000 particles, records the average peak area of toggle rate, slugging average and relevant ions.
As a result show:The toggle rate and slugging average of standard sample are more than 7 close to reality, the toggle rate of standard sample
Individual/second, slugging average are more than 17%, and according to air quality difference, atmospheric aerosol toggle rate in practical application
Change between 2~18/second, slugging average is generally higher than 20%.
The feature spectrogram of standard sample is as shown in figure 1, from Fig. 1 results:
(1) ion abundant information:The prevailing quality number that the cation of standard sample includes have m/z7,23,30,
39th, 42,47,63,65,107,109,206,207,208, the prevailing quality number that anion includes has
M/z-16, -17, -26, -46, -62, -63, -79, -122, -168, can cover normal atmospheric aerosol
Mass range of ions (as shown in Figure 2).
(2) organic and inorganic two parts ionization property can be reflected simultaneously:Standard sample solution contains six kinds of metals
Ion and a kind of organic component, are reflected on mass spectrogram, inorganic component has Li in cation+、Na+、K+、
Cu+、Ag+、Pb+Deng organic debris has C2H2O+、PO+Deng;Inorganic component has O in anion-、OH-、
NO2 -、NO3 -Deng organic debris has PO3 -、C3H7NO5P-Deng.
(3) ionic strength is high:From Fig. 1 and Fig. 2 contrast as can be seen that the ionic strength of standard sample is total
Body is better than the ionic strength of atmospheric aerosol sample, especially anion.
The checking of the standard sample property of embodiment 3
(1) checking of standard sample stability
The aqueous solution for the standard sample that embodiment 1 is configured, add in SPAMS aerosol generator, adjust
Solar term colloidal sol flow is 0.57LPM, and continuous operation, service condition are under prescribed conditions:Laser energy is
0.5mJ, the μ s of Time delay 0.8, trigger balance 1V, sampling length 25 μ s, input range 5V, and signal is inclined
2.5V is moved, background threshold values 3V, PMT threshold values -0.17V, PKL is arranged to peak height more than 5 and peak area is big
It is more than 3 in 30 and effective peak number, per 1000 particles of collection every other hour, continuous acquisition 10 times,
Count the average peak area of the toggle rate of sample, slugging average and relevant ions.As a result as shown in table 2, it is each
Thus the RSD values of index illustrate that properties of samples is stable in continuous operation 10% or so.
The sample stability test result of table 2
(2) checking of the standard sample term of validity
The Standard Stock solutions for each component that embodiment 1 is configured are tested once every two weeks, the water of standard sample
Solution is tested weekly once.Keep each parameter setting of instrument consistent (with (1)), collection 1000 every time
Grain, it is each to gather seven times, count the peak area of the toggle rate of sample, slugging average and relevant ions.Each component
Standard Stock solutions test result is as shown in table 3, the peak area of its toggle rate, slugging average and relevant ions
RSD values substantially all below 10%;The aqueous solution test result of standard sample is as shown in table 4, and it is triggered
The RSD values of rate, slugging average and related anion have part flat substantially all below 10% in cation
Regular change, wherein Na is presented with the testing time in equal peak area+Relative peak area increases with the time and becomes big,
And increasing degree is larger, and Cu+、Ag+Diminish Deng increasing with the time, and amplitude of variation will compared with the former
It is small.Although this part ion is not complete stability, because its change has regularity, therefore and without prejudice to it
Use.
The stability test result of the Standard Stock solutions of table 3
The aqueous stability test result of the standard sample of table 4
The application example of the standard sample of embodiment 4
(1) three SPAMS are linked together, instrument parameter is set unanimously, and design parameter is:Low rule
3 readings are 2.1-2.3torr, laser energy 0.5mJ, the μ s of Time delay 0.8, trigger balance 1V, sampling
Length 25 μ s, input range 5V, signal skew 2.5V, background threshold values 3V, PMT threshold values -0.17V,
PKL is arranged to peak height more than 5 and peak area is more than 30 and effectively peak number is more than 3.Gather 1h air simultaneously
Aerosol particle, source resolution pie chart as shown in figure 3, wherein accounting it is larger fire coal and biomass RSD
Respectively 20.3% and 31.3%, the tail gas and the RSD of industrial technology that accounting is taken second place are above 40%, explanation
Source resolution difference is larger between three instruments.
(2) three SPAMS are linked together, instrument parameter is set with (1), and embodiment 1 is configured
Standard sample the aqueous solution respectively collection 1000 aerosol particles, its experimental data is as shown in table 5, except
Toggle rate and slugging average substantially close to outer, the RSD of the average peak area of most of ions more than 30%,
Illustrate that three SPAMS instrument performance difference is larger.
The ion average peak area of standard sample before table 5 is adjusted
(3) on the basis of (2), three SPAMS instrument relevant parameter (laser energy) is adjusted,
The RSD values of the average peak area of most of ions are made to diminish as far as possible, as shown in table 6, after regulation, mostly
The RSD values of the average peak area of number ion are substantially below 30%, and now, 9# laser energies are reduced to 0.3mJ,
48# laser energies increase to 0.7mJ, and remaining parameter keeps constant.
The ion average peak area of standard sample after table 6 is adjusted
(4) under conditions of the instrument parameter regulated in (3), three SPAMS are gathered simultaneously again
The aerosol particle of 1h air samples, source resolution pie chart is as shown in figure 4, wherein combustion of the accounting up to more than 30%
The RSD of coal component drops to 8.4% from 20.3%, the biomass components of accounting 20% and the RSD of airborne dust component
8.6%, 1.2% is dropped to from 31.3%, 10.3% respectively, the vehicle exhaust and industrial technology that accounting is 10%
RSD drops to 29.1% and 18.9% from 41.3%, 44.8% respectively, it can be seen that when the standard with the present invention
Sample is debugged to each SPAMS instrument parameter, makes the average spectrogram of most of ions of standard sample tend to
When consistent, each SPAMS instrument performance also tends to unanimously.
Each technical characteristic of embodiment described above can be combined arbitrarily, not right to make description succinct
The all possible combination of each technical characteristic in above-described embodiment is all described, as long as however, these skills
Contradiction is not present in the combination of art feature, is all considered to be the scope of this specification record.
Embodiment described above only expresses the several embodiments of the present invention, and its description is more specific and detailed,
But can not therefore it be construed as limiting the scope of the patent.It should be pointed out that for this area
For those of ordinary skill, without departing from the inventive concept of the premise, some deformations can also be made and changed
Enter, these belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be with appended power
Profit requires to be defined.
Claims (10)
1. a kind of standard sample for individual particle aerosol mass spectrometer performance adjustment, it is characterised in that described
Standard sample includes the component of following proportioning:
2. the standard sample according to claim 1 for individual particle aerosol mass spectrometer performance adjustment,
Characterized in that, the standard sample includes the component of following proportioning:
3. the standard sample according to claim 2 for individual particle aerosol mass spectrometer performance adjustment,
Characterized in that, the standard sample includes the component of following proportioning:
4. the standard sample according to claim 1 for individual particle aerosol mass spectrometer performance adjustment,
Characterized in that, the standard sample is the aqueous solution being prepared by the component described in claim 1 and water,
The concentration of each component in aqueous is:
5. the standard sample according to claim 4 for individual particle aerosol mass spectrometer performance adjustment,
Characterized in that, the concentration of each component in aqueous is:
6. a kind of preparation method of standard sample for individual particle aerosol mass spectrometer performance adjustment, its feature
It is, comprises the following steps:
(1) preparation of Standard Stock solutions:LiNO is weighed respectively3、NaNO3、KNO3、Cu(NO3)2、
AgNO3With Pb (NO3)2Into respective sample bottle, then 50mL deionized water dissolvings are used respectively, obtain each gold
Belong to the Standard Stock solutions of salt component;N- (phosphoric acid methyl) glycine is weighed, it is water-soluble with 30mL deionizations
Solution, obtains the Standard Stock solutions of N- (phosphoric acid methyl) glycine;Weigh LiNO3、NaNO3、KNO3、
Cu(NO3)2、AgNO3、Pb(NO3)2Quality with N- (phosphoric acid methyl) glycine be respectively 0.01~0.1g,
0.01~0.1g, 0.01~0.1g, 0.1~1.0g, 0.1~0.5g, 1~5g, 0.1~0.5g;
(2) preparation of the aqueous solution of standard sample:LiNO is pipetted respectively3、NaNO3、KNO3、Cu(NO3)2、
AgNO3With Pb (NO3)2Standard Stock solutions into same sample bottle, its volume be respectively 0.2~0.3mL,
0.3~0.4mL, 0.3~0.4mL, 0.6~0.9mL, 0.6~0.9mL and 0.6~0.9mL, Ran Houjia
Enter deionized water dissolving mixing, be settled to 50mL with deionized water, add 1~2mL N- (phosphoric acid methyl)
The Standard Stock solutions of glycine, mix, produce.
7. the standard sample according to claim 6 for individual particle aerosol mass spectrometer performance adjustment
Preparation method, it is characterised in that step weighs LiNO in (1)3、NaNO3、KNO3、Cu(NO3)2、
AgNO3、Pb(NO3)2Quality with N- (phosphoric acid methyl) glycine be respectively 0.01-0.05g, 0.01-0.05g,
0.01-0.05g、0.5-1g、0.1-0.3g、1-3g、0.1-0.3g。
8. the standard sample described in claim any one of 1-5 is carrying out performance to individual particle aerosol mass spectrometer
Application in the method for debugging.
9. application according to claim 8, it is characterised in that described to individual particle aerosol mass spectrometer
The method for carrying out performance adjustment comprises the following steps:The standard sample is put into individual particle aerosol mass spectrometer
Aerosol generator in, control aerosol produce flow be 0.5~0.6LPM, gather aerosol particle, unite
The average peak area of each characteristic ion is counted, then conditioning instrumentation parameter makes the performance of each individual particle aerosol mass spectrometer
Reach unanimity.
A kind of 10. method that performance adjustment is carried out to individual particle aerosol mass spectrometer, it is characterised in that including
Following steps:Standard sample described in claim any one of 1-5 is put into the gas of individual particle aerosol mass spectrometer
In colloidal sol generator, it is 0.5~0.6LPM to control aerosol to produce flow, gathers aerosol particle, and statistics is each
The average peak area of characteristic ion, then conditioning instrumentation parameter tend to the performance of each individual particle aerosol mass spectrometer
Unanimously.
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