CN105203497A - Method for predicting content of hydrogen sulfide in desulfurization amine liquid through near-infrared light - Google Patents
Method for predicting content of hydrogen sulfide in desulfurization amine liquid through near-infrared light Download PDFInfo
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- CN105203497A CN105203497A CN201410307163.4A CN201410307163A CN105203497A CN 105203497 A CN105203497 A CN 105203497A CN 201410307163 A CN201410307163 A CN 201410307163A CN 105203497 A CN105203497 A CN 105203497A
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Abstract
A method for predicting the content of hydrogen sulfide in desulfurization amine liquid through near-infrared light comprises the following steps; (1), collecting representative desulfurization amine liquid samples of different concentrations and determining the hydrogen sulfide content of the samples by using a standard method; (2), determining near infrared spectrums of the samples collected in the step (1), taking a 4000-6000 cm<-1> spectral range as a characteristic spectral region, carrying out second-order differential treatment on spectrograms in the characteristic spectral region, carrying out regression analysis by associating the absorbancy of the characteristic spectral region with the hydrogen sulfide content measured using the standard method, and building a correction model; (3), determining the near infrared spectrums of samples to be determined, carrying out second-order differential treatment on spectrograms, taking the 4000-6000 cm<-1> spectral range as the characteristic spectral region, and substituting absorbancy of the characteristic spectral region into the correction model so as to obtain the hydrogen sulfide content of the samples to be determined. The operation is simple, the analysis speed is high, the prediction is accurate and the analysis operation environment is improved effectively.
Description
Technical field
The present invention is a kind of method by Forecast of Spectra hydrogen sulfide content in desulfurized amine, specifically, is a kind of method being predicted hydrogen sulfide content in desulfurized amine by near infrared spectrum.
Background technology
Along with the development of oil Refining Technologies, the desulfurization of refinery gas and petroleum products has become one of the emphasis and key of Petrochemical Enterprises.Due to the continuous increase of residual oil mixed refining ratio, the sulfur content of refinery gas raises rapidly, and most refinery all adopts the good amine desulfurization hydrogen of desulfurized effect (H
2s) technique.Amine liquid for desulphurization in this technique is divided into lean solution and rich solution, and hydrogen sulfide content is wherein the key factor determining desulfurized effect, therefore needs strict control and calibrating.
Containing the component such as desulfurizing agent (as methyldiethanolamine), water, sulfuretted hydrogen, oily substance in amine liquid for desulphurization, color sample is comparatively dark, has certain viscosity and with stench.The analytical approach of hydrogen sulfide content in desulfurized amine general is at present iodimetric titration, the method complex steps, and disturbing factor is more, needs to carry out twice titration, very easily causes personal error, reduces and analyzes repeatability and accuracy; And because analysis time is longer, analyst needs to be in bad smell for a long time, poison also larger to health.
The feature that near-infrared spectral analytical method has fast, efficient, automaticity is high, be widely used in various concentration analysis occasion, wherein just there is the application utilizing hydrogen sulfide content in near-infrared spectrum analysis gas, but also directly do not use the method to carry out the analytical applications of hydrogen sulfide content in doctor solution at present.
Summary of the invention
The object of this invention is to provide a kind of method being predicted hydrogen sulfide content in desulfurized amine by near infrared spectrum, this method can be predicted the hydrogen sulfide content in amine liquid for desulphurization by near infrared spectrum, simple to operate, analysis speed is fast, prediction accurately, and effectively can improve the environment of analysis operation.
The method being predicted hydrogen sulfide content in desulfurized amine by near infrared spectrum provided by the invention, comprises the steps:
(1) the representational amine liquid for desulphurization sample of variable concentrations is collected, with the hydrogen sulfide content of standard method working sample,
(2) measure the near infrared spectrum that (1) step collects sample, get 4000 ~ 6000cm
-1spectrum range be characteristic spectrum area, carry out second-order differential process to the spectrogram of characteristic spectrum area, the hydrogen sulfide content of the sample its absorbance measured with standard method is associated, and carries out regretional analysis, sets up calibration model,
(3) measure the near infrared spectrum of testing sample, get 4000 ~ 6000cm
-1spectrum range be characteristic spectrum area, second-order differential process is carried out to the spectrogram of characteristic spectrum area, by the absorbance of characteristic spectrum area substitute into calibration model, obtain the hydrogen sulfide content of testing sample.
The hydrogen sulfide content of the absorbance of sample near infrared spectrum characteristic spectrum area with the sample measured with standard method is associated by the inventive method, calibration model is set up by multiple regression analysis, again by calibration model, predicted the hydrogen sulfide content of testing sample in the absorbance of characteristic spectrum area by testing sample.The method is simple to operate, analysis speed is fast, can greatly improve analysis operation environment, improves analysis efficiency.
Accompanying drawing explanation
Fig. 1 is the near infrared spectrum of typical desulphurization amine liquid.
Fig. 2 is the near infrared spectrum predicted value of hydrogen sulfide content and the correlogram of standard method measured value of the inventive method checking collection sample.
Embodiment
The inventive method collects the representational amine liquid for desulphurization sample of variable concentrations, measures its hydrogen sulfide content, then measure its near infrared spectrum with standard method.Getting amine liquid for desulphurization sample near infrared spectrum wave number is 4000 ~ 6000cm
-1interval be characteristic spectrum area, the spectrogram in this spectrum district is carried out second-order differential process, again the hydrogen sulfide content that the absorbance of characteristic spectrum area and sample standard method measure is associated, set up calibration model, the near infrared spectrum of testing sample is measured again by the condition identical with setting up calibration model, carry out identical spectrogram process, by the absorbance of characteristic spectrum area, by the sulfur content of calibration model prediction testing sample.
The inventive method (1) step is collect the representational amine liquid for desulphurization sample of variable concentrations, measures its hydrogen sulfide content, for setting up calibration model with standard method.
(1) quantity of the amine liquid for desulphurization sample of step collection is no less than 30, and in preferred sample, sulfuretted hydrogen is evenly distributed in the scope that may occur.Preferred sample size is 50 ~ 600, more preferably 100 ~ 500.
(1) amine liquid for desulphurization that step is collected comprises the lean solution before desulfurization and the rich solution after desulfurization, and rich solution is the amine liquid for desulphurization of gained after lean solution absorbing hydrogen sulphide.The hydrogen sulfide content distribution range of the sample collected is preferably 0.1 ~ 45g/L.
The inventive method (2) step is be associated with the hydrogen sulfide content that standard assay records by the absorbance of the near infrared spectrum characteristic spectrum area of the representational amine liquid for desulphurization sample collected, and sets up calibration model.
(2) during the near infrared spectrum of step working sample, preferably will the cuvette sealing of dress sample, preferably make sample injection rate IR reach 2/3rds of cuvette volume, and ensure that the temperature of each working sample is identical.
(2) temperature of step working sample near infrared spectrum preferably 20 ~ 38 DEG C.
(2), after step carries out second-order differential to the spectrogram of characteristic spectrum area, for reducing or eliminating and the impact of the information that has nothing to do of spectroscopic data and noise, preferably vector normalization and average centralization process are carried out again to the absorbance after second-order differential process.
(2) step adopts regression analysis will collect the near infrared spectrum characteristic spectrum area of sample through second-order differential process, to be preferably associated with the sulfur content that standard method measures through the absorbance of vector normalization and average centralization process again and to set up calibration model.
The multiple regression analysis setting up calibration model employing can be partial least square method (PLS), least square method (CLS), inverse least square method (ILS), principal component regression (PCR) or robust partial least-squares method (RPLS).Preferred partial least square method (PLS).
Introduction partial least square method below sets up the process of calibration model:
When adopting PLS method establishment calibration model, its modeling is according to for than Er-Lang Bai law:
Y＝XB+E，
In formula,
Y-by m sample, (m × n) absorbance matrix that n wavelength points array becomes;
X-by m sample, (m × 1) concentration vector of 1 component composition;
B-1 component, (1 × n) sensitivity vectors that n wavelength points array becomes;
The residual matrix of E-m × n absorbance.
Described wavelength is counted as spectrometer information number of recording in setting spectrum range.
The general algorithm setting up calibration model is as follows:
1, carry out average centralization process to each element of absorbance matrix Y (characteristic spectrum area absorbance is gained after second-order differential process) and concentration vector X, namely all data deduct the mean value of its corresponding data group (column vector); Then carry out vector normalized, namely each vector component is divided by the important summation of vector.
2, the absorbance matrix Y after normalizing and concentration vector X carries out principal component decomposition:
Wherein:
T
k(m × 1)-be the factor score of absorbance matrix, y-score;
V
k(1 × n)-be the factor loading of absorbance matrix, y-loading;
R
k(m × 1)-be the factor score of concentration vector, x-score;
Q
kthe factor loading of (1 × 1)-a be number, concentration vector, x-loading;
P-main cause subnumber.
E
y-absorbance matrix residual error
E
x-concentration vector residual error
In order to ensure the T that drawn by Y can and the R that draws of X between have good linear dependence, can introduce the information about R when Y is decomposed into T, or introduce the information of T when X is decomposed into R, this reaches by exchanging iteration variable when iteration, unite two into one by above-mentioned two decomposable processes, namely have:
r
k＝b
kt
k(3)
B
k(1 × 1)-r
kand t
kregression coefficient
3, eigenvector and main cause subnumber p is solved
Ignore residual error battle array E, according to formula (1) and (2), have during p=1:
Y＝tv
t
Premultiplication t
t: v
t=t
ty/t
tt
The right side takes advantage of v to obtain: t=Yv/v
tv
X＝rq
Premultiplication r
t: q=r
tx/r
tr, both sides obtain with except q: r=X/q
[1] the weight vectors w of absorbance matrix is asked,
The a certain row getting concentration array X make the initial iteration value of r, replace t with r, calculate w equation: Y=rw
tsolution be: t=Yw/w
tw
[2] normalization w:
[3] ask the factor score t of absorbance matrix, calculate t by w after normalization
Equation: Y=tw
tsolution be: t=Yw/w
tw
[4] ask the weight u value of concentration vector, replace r to calculate u with t
The solution of equation: X=tu is: u=t
tx/t
tt
Ask the factor score r of concentration vector, x-score, calculates r by u
The solution of equation: X=ru is: r=X/u
Replace t to return [1] step with this r again and calculate w, by w
tcalculate t
newly, so iterate, as t restrains (‖ t
newly-t
old‖≤10
-6‖ t
newly‖), under continuation, walk computing, otherwise return step [1].
The load vectors v of absorbance matrix is asked, y-loading by the t after restraining
Equation: Y=tv
tsolution be: v
t=t
ty/t
tt
The load q value of concentration vector is asked, x-loading by r
The solution of equation: X=rq is: q=r
tx/r
tr
Obtain the r corresponding to first main gene thus
1, q
1, t
1,
Substitute into formula (3) and obtain b
1:
Residual error battle array E is calculated by formula (1) and (2)
E
X,1＝X-r
1q
1＝X-b
1t
1q
1(4)
E
Y,1＝Y-t
1v(5)
With E
x, 1replace X, E
y, 1replace Y, return step [1] and calculate next component
r
2，q
2，t
2，
b
2
E is calculated by formula (4) and (5)
x, 2, E
y, 2, by that analogy, obtain all main genes of X, Y.
[11] with cross-verification method determination main cause subnumber.
The inventive method (3) step is the hydrogen sulfide content of the absorbance prediction testing sample with the nearly red spectral characteristic spectrum area of testing sample.
By the method for (2) step, the near infrared spectrum of testing sample is measured under condition identical with it, second-order differential process is carried out to the spectrogram of its characteristic spectrum area, then carries out the average centralization identical with modeling and vector normalized, obtain the absorbance y of testing sample
to be measured, predict its hydrogen sulfide content x by correction mode
to be measured, step is as follows:
[1] by y
to be measuredand the v stored in trimming process
kcalculate t
k (to be measured)
[2] by the t obtained
k (to be measured)and the b stored in trimming process
kcalculate r
k (to be measured)
R
k (to be measured)=b
kt
k (to be measured)
[3] by the r obtained
k (to be measured)and the q stored in trimming process
k, utilize formula (2) to calculate x
to be measured.
Further describe the present invention below by example, but the present invention is not limited to this.
Example 1
(1) collect the representational amine liquid for desulphurization sample of variable concentrations, measure its hydrogen sulfide content with standard method
Collect 445 amine liquid for desulphurization samples, adopt its hydrogen sulfide content of iodometric determination.Get wherein that 377 samples are as calibration set, its hydrogen sulfide content distribution range is: 0.34 ~ 40.32g/L; 68 remaining samples are as checking collection, and its hydrogen sulfide content distribution range is: 1.46-35.33g/L.
(2) near infrared spectrum of working sample,
The instrument of working sample near infrared spectrum is AntarisII near infrared spectrometer (ThermoFisher company), wears temperature control modules.
Amine liquid for desulphurization sample is filled cuvette about 2/3rds position, seal with sealed membrane.Cuvette after sealing is put into controllable temperature sample cell shelf and carries out transmitted spectrum collection, spectra collection temperature is 25 DEG C, is 3500 ~ 10000cm between acquisition zone
-1, multiple scanning 128 times, resolution is 4cm
-1, gather the spectrum of 445 samples altogether.Typical amine liquid for desulphurization near infrared spectrum as shown in Figure 1, because solution comprises water amount is comparatively large, therefore has obvious water peak.
(3) calibration model is set up with PLS
By above-mentioned calibration set 377 samples at characteristic interval 4000 ~ 6000cm
-1near infrared spectrum carry out second-order differential process, then carry out vector normalization and average centralization process, obtain absorbance matrix Y.By the hydrogen sulfide content of iodometric determination corresponding for sample spectra each in Y matrix composition concentration vector X.Be associated with concentration vector X PLS by absorbance matrix Y and set up calibration model, main cause subnumber is 12, and the root-mean-square error of validation-cross is 1.96g/L, and measured value and predicted value related coefficient are 0.966.
(4) model evaluation
Hydrogen sulfide content prediction is carried out to checking collection 68 samples, concentrates 68 samples at characteristic interval 4000 ~ 6000cm checking
-1near infrared spectrum carry out second-order differential process, then carry out average centralization and vector normalized, obtain the absorbance y of each sample
to be measured, absorbance is substituted into calibration model, obtains the predicted value of sample hydrogen sulfide content.The measured value of checking collection sample hydrogen sulfide content predicted value and standard method is in table 1, and all checking collection predicted values of sample and the correlativity of measured value are shown in Fig. 2.
As shown in Table 1, predicting the outcome of the inventive method coincide better with the measured value of standard method, and predicted root mean square error (RMSEP) is 1.24g/L, and related coefficient is 0.968.Comparatively large to the relative error that predicts the outcome of lean solution, and rich solution predicts the outcome generally, and comparatively lean solution is good.
Example 2
Get poor, a rich amine liquid for desulphurization sample respectively, by method replication four near infrared spectrums of example 1 (2) step, by measure at every turn at characteristic interval 4000 ~ 6000cm
-1near infrared spectrum carry out second-order differential process, then carry out average centralization and vector normalized, obtain the absorbance of sample, then substitute into calibration model, obtain the predicted value of sample hydrogen sulfide content.Four replications the results are shown in Table 2.
As shown in Table 2, the predicted value of the inventive method to poor, rich amine liquid for desulphurization hydrogen sulfide content all has good repeatability.
Table 1
Table 2
| Analysis times | Lean solution hydrogen sulfide content, g/L | Rich solution hydrogen sulfide content, g/L |
| 1 | 0.85 | 37.42 |
| 2 | 0.83 | 36.91 |
| 3 | 0.80 | 37.01 |
| 4 | 0.85 | 38.44 |
| Mean value | 0.833 | 37.445 |
| Relative standard deviation | 2.80％ | 1.90％ |
Claims (6)
1. predicted a method for hydrogen sulfide content in desulfurized amine by near infrared spectrum, comprise the steps:
(1) the representational amine liquid for desulphurization sample of variable concentrations is collected, with the hydrogen sulfide content of standard method working sample,
(2) measure the near infrared spectrum that (1) step collects sample, get 4000 ~ 6000cm
-1spectrum range be characteristic spectrum area, carry out second-order differential process to the spectrogram of characteristic spectrum area, the hydrogen sulfide content of the sample its absorbance measured with standard method is associated, and carries out regretional analysis, sets up calibration model,
(3) measure the near infrared spectrum of testing sample, get 4000 ~ 6000cm
-1spectrum range be characteristic spectrum area, second-order differential process is carried out to the spectrogram of characteristic spectrum area, by the absorbance of characteristic spectrum area substitute into calibration model, obtain the hydrogen sulfide content of testing sample.
2. in accordance with the method for claim 1, it is characterized in that the amine liquid for desulphurization sample size that (1) step is collected is no less than 30, and in sample, hydrogen sulfide content is evenly distributed in the scope that may occur.
3., in accordance with the method for claim 1, when it is characterized in that the near infrared spectrum of working sample, by the cuvette sealing of dress sample, and ensure that the temperature of each working sample is identical.
4. in accordance with the method for claim 1, after it is characterized in that (2) step carries out second-order differential to the spectrogram of characteristic spectrum area, then carry out vector normalization and average centralization process.
5. in accordance with the method for claim 1, it is characterized in that the standard method measuring hydrogen sulfide content in amine liquid for desulphurization sample is iodimetric titration.
6. the regretional analysis that in accordance with the method for claim 1, it is characterized in that setting up calibration model employing is partial least square method (PLS), least square method (CLS), inverse least square method (ILS), principal component regression (PCR) or robust partial least-squares method (RPLS).
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| CN110927328A (en) * | 2019-12-13 | 2020-03-27 | 中国石油化工股份有限公司 | Method for measuring content of soluble hydrogen sulfide in desulfurization solution |
| CN111504938A (en) * | 2019-01-30 | 2020-08-07 | 中国石油天然气股份有限公司 | Method for measuring total hydrogen sulfide content in liquid sulfur |
| CN113324945A (en) * | 2021-05-28 | 2021-08-31 | 中国石油化工股份有限公司 | Method for predicting aromatic hydrocarbon content in industrial white oil by near infrared spectrum |
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| CN110470628A (en) * | 2018-12-28 | 2019-11-19 | 山东益丰生化环保股份有限公司 | A kind of method that near infrared detection industry thiocarbamide produces sulphur hydrogen radical content in feed liquid |
| CN111504938A (en) * | 2019-01-30 | 2020-08-07 | 中国石油天然气股份有限公司 | Method for measuring total hydrogen sulfide content in liquid sulfur |
| CN110927328A (en) * | 2019-12-13 | 2020-03-27 | 中国石油化工股份有限公司 | Method for measuring content of soluble hydrogen sulfide in desulfurization solution |
| CN114486805A (en) * | 2020-10-23 | 2022-05-13 | 中国石油化工股份有限公司 | Method for determining process parameters of hydrogen peroxide production process |
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