CN101408505A - Method for evaluating 'double-way linearity and balance' performance of electric detection system of spectrometer - Google Patents
Method for evaluating 'double-way linearity and balance' performance of electric detection system of spectrometer Download PDFInfo
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- CN101408505A CN101408505A CNA2007100469457A CN200710046945A CN101408505A CN 101408505 A CN101408505 A CN 101408505A CN A2007100469457 A CNA2007100469457 A CN A2007100469457A CN 200710046945 A CN200710046945 A CN 200710046945A CN 101408505 A CN101408505 A CN 101408505A
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Abstract
The invention discloses a method which is applied to an atomic absorption spectrometer and is used for evaluating the performance of dual-channel linearity and balance of an electric detection system. The invention is characterized in that the performance of the dual-channel linearity and balance of the electric detection system for the atomic absorption spectrometer is evaluated by using a mercury lamp-potassium dichromate non-standard gradient measurement method and a mathematical model thereof. By using the characteristics of the stray light of the mercury lamp and the gradient measurement method, the standard substance is not required, therefore, the operation is simple and rapid, the mathematical reasoning is strict, the result is correct, and meanwhile, the sample channel linearity, the reference channel linearity and the dual-channel balancing performance index can be enhanced. The invention leads the quantitative and rapid evaluation on the electric detection system for the atomic absorption spectrometer to be possible, meanwhile, provides the rapid, correct and economical method and the mathematical model for the self-checking and the measurement of the detection system for the spectrometer and also provides a direction for enhancing the detection performance of the spectrometer.
Description
Technical field
The invention belongs to the spectrometric instrument field, be specifically related to the detection evaluation method of Atomic Absorption Spectrometer device electro-detection system, the method for the no normal gradients measurement for Evaluation of particularly a kind of use " mercury lamp-potassium dichromate " Atomic Absorption Spectrometer device electro-detection system " two pass linearity and balance " performance.
Background technology
At first proposed atomic absorption spectrography (AAS) is applied to chemical analysis by Australian physicist Walsh from 1950's, now become one of most important instrument of quantitative elementary analysis and be widely used in each analysis field.Need accurate background correction to absorb owing to often running into serious background interference in the sample analysis, background correction method commonly used has deuterium lamp background correction, Zeeman effect background correction, self-priming background correction.Deuterium lamp background correction, Zeeman effect background correction, self-priming background correction are all measured simultaneously with two pass and are realized background deduction, are the sample road together wherein, and in order to the total absorption of measuring samples, another road is a library track, in order to measure the absorption of sample background.Influence three aspects of limitation, optical system factor, Circuits System factor that the background correction effect mainly comprises analytical approach itself.In the Circuits System factor emphasis be circuit zero partially, drift, noise, that two pass is linear is signal-balanced etc. with two pass, wherein two pass linear with the signal-balanced background correction ability that directly influenced of two pass, therefore, correctly estimate two pass linear with the signal-balanced performance of two pass in the research and development of instrument be a key and important techniques in making.
At present, still there is not the standard method of measurement of instrument electro-detection system linear and the signal-balanced performance of two pass in the country of Atomic Absorption Spectrometer and the industry technology standard.The user is if the measurement that will carry out electro-detection system linear and the signal-balanced performance of two pass to the commodity Atomic Absorption Spectrometer is impossible basically.
Traditional, there is dual mode in instrument producer to the evaluation method of Atomic Absorption Spectrometer electro-detection system linear and the signal-balanced performance of two pass:
1, use a light source of demarcating through authoritative institution, the luminous energy that output is linear detects the output signal from instrument; Maximum difficult point is to be difficult to make standard sources and want the modulation of source pattern of detecting instrument consistent in this method, another shortcoming is to need standard sources, and this method is actually and can't operates.
2, utilize the standard solution of a series to measure estimation.Use the overall linear scope that this method can detecting instrument, can not directly characterize electro-detection system linear and the signal-balanced performance of two pass, at most estimation at last.
Therefore, how to estimate linear the correction in the exploitation at instrumental background of two pass quickly and accurately and become a technical bottleneck with the signal-balanced performance of two pass.
So far still there is not the method that report uses " mercury lamp-potassium dichromate " no normal gradients measurement for Evaluation Atomic Absorption Spectrometer device electro-detection system " two pass linearity and balance " performance both at home and abroad.
Summary of the invention
Technical matters to be solved by this invention is based on and estimates the linear method that the no normal gradients measurement for Evaluation of a kind of use " mercury lamp-potassium dichromate " Atomic Absorption Spectrometer device electro-detection system " two pass linearity and balance " performance is provided with the signal-balanced performance of two pass of Atomic Absorption Spectrometer electro-detection system two pass quickly and accurately.Method of the present invention need not standard substance, and simple to operate fast mathematical reasoning is tight, and the result is accurate, and the road of sampling simultaneously linearity, library track linearity, two pass balance quality index.
Technical matters to be solved by this invention can be achieved through the following technical solutions:
The method of the no normal gradients measurement for Evaluation of a kind of use " mercury lamp-potassium dichromate " Atomic Absorption Spectrometer device electro-detection system " two pass linearity and balance " performance is characterized in that, may further comprise the steps:
1, with the mercury lamp be light source, its spectrum line selects potassium bichromate solution to measure it in the absorbance of measuring under the spectral line as measuring spectral line;
2, utilize the method for adjusting photodetector photomultiplier negative high voltage, change the testing circuit gain, simulate the basic background values of absorbance of the different sizes of series, measures the two pass molecule absorption data of same potassium bichromate solution under the different big or small absorbance basic value conditions of series;
3, use following mathematics computing model to obtain sample road linear correlation coefficient r _ s, library track linearly dependent coefficient r_r, two pass balance related coefficient r_sr, two pass balanced line property coefficient p desired value:
(1) potassium bichromate solution molecule absorption mathematics computing model
ΔS(i)＝S1(i)-S0(i)；
ΔR(i)＝R1(i)-R0(i)；
Wherein, S1 is actual measurement sample road potassium bichromate solution absorbance, and S0 is the actual measurement sample road simulation absorbance of n.s., and R1 is actual measurement library track potassium bichromate solution absorbance, and R0 is a n.s. actual measurement library track simulation absorbance;
(2) the linear dependency number in road is learned computation model
i＝0..7；
Linear model: X (i)=k*I; K=0.3
Linear data: the S ' in sample road (i)=X (i)+Δ S (i)-Δ S (0);
Library track linear data: R ' (i)=X (i)+Δ R (i)-Δ R (0);
(3) linear fit computational mathematics model
Calculate through linear fit, can obtain the corresponding linear equation coefficient, and obtain linearly dependent coefficient r above-mentioned data rows, as follows respectively:
A. linear equation: the S ' in sample road (i)=k X (i);
Linear correlation coefficient r _ the s in sample road
B. library track linear equation: R ' (i)=k X (i);
Library track linearly dependent coefficient r_r
C. two pass balance linear equation: S ' (i)=p X (i);
Two pass balance related coefficient r_sr
Wherein: p is a two pass balanced line property coefficient
4, estimate electro-detection system " two pass linearity and balance " performance
R_s is 0.999 to 1: the sample road is better linear;
R_r is 0.999 to 1: library track is better linear;
R_sr is 0.999 to 1: the two pass balance is better;
P: two pass balanced line property coefficient is good more near 1 background correction ability more.
Spectrum line wavelength of the present invention is 253.7nm, and this is because Hg lamp 253.7nm heat input is strong, and other spectral line energy is very little, can get rid of stray light, therefore selects the linearity of Hg lamp surveying instrument just can directly reflect instrument electro-detection system linearity.
The two pass molecule absorption data that the present invention measures same potassium bichromate solution under the absorbance basic value condition of the different sizes of series are to place the cuvette model molecule to absorb and then change negative high voltage by the 25ng/mL potassium bichromate solution to obtain different background and deduct.
Good effect of the present invention is: need not use standard substance, utilize the spectral characteristic of Hg lamp and the absorption characteristic of potassium bichromate solution, relative measurement method under the simulation absorbance, got rid of the influence to measurement result of instrument parasitic light, can be quick, directly provide the quantizating index of electro-detection system " two pass linearity and balance " performance: the linear related coefficient in sample road, the library track linearly dependent coefficient, two pass balance related coefficient, make quantitative and quick evaluation appts electro-detection system become possibility, self check and test and appraisal for the instrument detecting system simultaneously provide one fast, correctly, economical method and mathematical model have also been pointed out a direction for the detection performance that improves instrument.
Description of drawings
Fig. 1 is a Hg lamp all band spectral scan figure spectrogram.
Fig. 2 for the present invention according to table 1 " Hg lamp-K
2Cr
2O
7" S ' in method electro-detection system " linearity and balance " the Performance Detection data analysis table is the linear synoptic diagram in S road of data drafting (i).
Fig. 3 for the present invention according to table 1 " Hg lamp-K
2Cr
2O
7" R ' in method electro-detection system " linearity and balance " the Performance Detection data analysis table is the linear synoptic diagram in R road of data drafting (i).
Fig. 4 for the present invention according to table 1 " Hg lamp-K
2Cr
2O
7" S ' in method electro-detection system " linearity and balance " the Performance Detection data analysis table (i), (i) the S-R two pass balance synoptic diagram drawn of data of R '.
Embodiment
For technological means, creation characteristic that the present invention is realized, reach purpose and effect is easy to understand, below in conjunction with concrete diagram, further set forth the present invention.
As can be seen from Figure 1,253.8nm is the peak wavelength that detects behind the Hg lamp full wavelength scanner; This figure can see that other spectral line energy outside the Hg lamp 253.8nm is relatively very weak, and stray light can be ignored when this wavelength measurement.Utilize the parasitic light standard substance to detect parasitic light simultaneously and show, the Hg lamp at the stray light ratio of the spectrum line of 253.7nm less than 0.1%; Therefore select the linear of Hg lamp surveying instrument just can directly reflect instrument electro-detection system linearity.
Use the method concrete operations step of " mercury lamp-potassium dichromate " no normal gradients measurement for Evaluation Atomic Absorption Spectrometer device electro-detection system " two pass linearity and balance " performance as follows:
1, instrument and reagent are prepared: prepare 1 of Hg hollow cathode lamp; Potassium bichromate solution 5ml (concentration is generally 25ng/mL); 1 of quartz colorimetric utensil, 1 of single groove cell rack.
2, do not have normal gradients in the Atomic Absorption Spectrometer device and measure, step is as follows:
1) open Atomic Absorption Spectrometer, and instrument condition is set, wherein element lamp is chosen as the Hg lamp, and wavelength is 253.7nm, and enters measurement pattern;
2) the single groove cell rack that will insert cuvette is placed on the flame combustion head in the sample chamber, and regulate the flame combustion head height, cuvette about and front and back position, make hot spot pass the cuvette center, this position is the colorimetric measurement position, and use fixedly cell rack of adhesive tape or glue, to be convenient for measuring.
3) potassium bichromate solution is poured in the quartz colorimetric utensil;
4) instrument is transferred 0A;
5) measure and write down current sample road absorbance, library track absorbance;
6) quartz colorimetric utensil of potassium bichromate solution will be housed, insert single groove cell rack, measure and write down current sample road absorbance, library track absorbance;
7) take out the quartz colorimetric utensil that potassium bichromate solution is housed;
8) change the instrument negative high voltage, making sample road absorbance, library track absorbance is about 0.3A;
9) repeat the 6th) to 8) step, (" sky " expression is not put potassium chromate solution in light path to measure and write down two kinds of sample states; " solution " expression is placed potassium chromate solution in light path) under sample road absorbance, library track absorbance;
10) repeat the 7th several times) to 9) step, change the instrument negative high voltage, make one by one that absorbance is 0.6,0.9,1.2,1.5,1.8, about 2.1A, measure and write down two kinds of sample road absorbance, library track absorbances under the sample state;
3, test result is inserted form, sees Table S in 1 (i), R (i).
Utilize the mathematical model among the present invention that the actual measurement test result is calculated, obtain:
S (i): potassium chromate solution sample road absorbance; Δ R (i): potassium chromate solution library track absorbance
S ' is (i): the linear data in sample road; R ' is (i): the library track linear data.
4, to the linear data S ' of linear model data X (i), sample road (i), library track linear data R ' (i) carries out linear fit (trend analysis) and make Fig. 2, Fig. 3 and Fig. 4 each other, obtain:
A. linear equation: the S ' in sample road (i)=k X (i);
Linear correlation coefficient r _ the s in sample road
B. library track linear equation: R ' (i)=k X (i);
Library track linearly dependent coefficient r_r
C. two pass balance linear equation: S ' (i)=p X (i);
Two pass balance related coefficient r_sr
Wherein: p is a two pass balanced line property coefficient
5, estimate electro-detection system " two pass linearity and balance " performance according to linearly dependent coefficient.
From Fig. 2, Fig. 3, Fig. 4, can see electro-detection system " two pass linearity and balance " performance; R_s=√ 0.9999=0.9999: the sample road is better linear;
R_r=√ 0.9977=0.9988: the library track linearity is poor than the sample road;
R_sr=√ 0.9971=0.9985: the two pass balance is bad;
P=0.9392: the background correction ability is poor than sample.
From Fig. 2, Fig. 3, Fig. 4, also can see:
R_s is 0.999 to 1: the sample road is better linear;
R_r is 0.999 to 1: library track is better linear;
R_sr is 0.999 to 1: the two pass balance is better;
P: two pass balanced line property coefficient is good more near 1 background correction ability more.
Table 1. " Hg lamp-K
2Cr
2O
7" method electro-detection system " linearity and balance " Performance Detection data analysis table
This table is an Atomic Absorption Spectrometer electro-detection system " linearity and balance " Performance Detection measured data;
Project is explained in the table
N: period
Negative high voltage: photodetector cathode voltage
Sample state: " sky " expression is not put potassium chromate solution in light path; " solution " expression is placed potassium chromate solution in light path
S (i): actual measurement sample road absorbance
R (i): actual measurement library track absorbance
Δ S (i): potassium chromate solution sample road absorbance
Δ R (i): potassium chromate solution library track absorbance
X (i): linear model, X (i)=k*I; (k=0.3 here)
S ' is (i): the linear data in sample road
R ' is (i): the library track linear data
More than show and described ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that describes in the foregoing description and the instructions just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (3)
1, the method for the no normal gradients measurement for Evaluation of a kind of use " mercury lamp-potassium dichromate " Atomic Absorption Spectrometer device electro-detection system " two pass linearity and balance " performance is characterized in that, may further comprise the steps:
1), be light source with the mercury lamp, its spectrum line selects potassium bichromate solution to measure it in the absorbance of measuring under the spectral line as measuring spectral line;
2), utilize the method for adjusting photodetector photomultiplier negative high voltage, change the testing circuit gain, simulate the basic background values of absorbance of the different sizes of series, measures the two pass molecule absorption data of same potassium bichromate solution under the different big or small absorbance basic value conditions of series;
3), use following mathematics computing model to obtain sample road linear correlation coefficient r _ s, library track linearly dependent coefficient r_r, two pass balance related coefficient r_sr, two pass balanced line property coefficient p desired value:
(1) potassium bichromate solution molecule absorption mathematics computing model
ΔS(i)＝S1(i)-S0(i)；
ΔR(i)＝R1(i)-R0(i)；
Wherein, S1 is actual measurement sample road potassium bichromate solution absorbance, and S0 is the actual measurement sample road simulation absorbance of n.s., and R1 is actual measurement library track potassium bichromate solution absorbance, and R0 is a n.s. actual measurement library track simulation absorbance;
(2) the linear dependency number in road is learned computation model
i＝0..7；
Linear model: X (i)=k*I; K=0.3
Linear data: the S ' in sample road (i)=X (i)+Δ S (i)-Δ S (0);
Library track linear data: R ' (i)=X (i)+Δ R (i)-Δ R (0);
(3) linear fit computational mathematics model
Calculate through linear fit, can obtain the corresponding linear equation coefficient, and obtain linearly dependent coefficient r above-mentioned data rows, as follows respectively:
A. linear equation: the S ' in sample road (i)=k X (i);
Linear correlation coefficient r _ the s in sample road
B. library track linear equation: R ' (i)=k X (i);
Library track linearly dependent coefficient r_r
C. two pass balance linear equation: S ' (i)=p X (i);
Two pass balance related coefficient r_sr
Wherein: p is a two pass balanced line property coefficient
4), estimate electro-detection system " two pass linearity and balance " performance
R_s is 0.999 to 1: the sample road is better linear;
R_r is 0.999 to 1: library track is better linear;
R_sr is 0.999 to 1: the two pass balance is better;
P: two pass balanced line property coefficient is good more near 1 background correction ability more.
2, method according to claim 1 is characterized in that, described spectrum line wavelength is 253.7nm.
3, method according to claim 1, it is characterized in that the two pass molecule absorption data of same potassium bichromate solution are to place absorption of cuvette model molecule and then change negative high voltage to obtain different background by the 25ng/mL potassium bichromate solution to deduct under the absorbance basic value condition of the different sizes of series of described measurement.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105223185A (en) * | 2015-11-10 | 2016-01-06 | 福建省计量科学研究院 | A kind of evaluation method of Raman spectrum fast detector |
| CN107014785A (en) * | 2017-05-15 | 2017-08-04 | 浙江全世科技有限公司 | A kind of improved method of emission spectrum background correction |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US3778162A (en) * | 1972-03-24 | 1973-12-11 | Continental Oil Co | Apparatus for the collection and measurement of the amount of mercury vapors present in a volume of air or other gases |
| CN1034269A (en) * | 1988-01-12 | 1989-07-26 | 东北工学院 | Multi-beam atom-absorbing spectrograph |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105223185A (en) * | 2015-11-10 | 2016-01-06 | 福建省计量科学研究院 | A kind of evaluation method of Raman spectrum fast detector |
| CN105223185B (en) * | 2015-11-10 | 2018-03-23 | 福建省计量科学研究院 | A kind of evaluation method of Raman spectrum fast detector |
| CN107014785A (en) * | 2017-05-15 | 2017-08-04 | 浙江全世科技有限公司 | A kind of improved method of emission spectrum background correction |
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