CN105954228A - Method for measuring content of sodium metal in oil sand based on near infrared spectrum - Google Patents
Method for measuring content of sodium metal in oil sand based on near infrared spectrum Download PDFInfo
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- CN105954228A CN105954228A CN201610521997.4A CN201610521997A CN105954228A CN 105954228 A CN105954228 A CN 105954228A CN 201610521997 A CN201610521997 A CN 201610521997A CN 105954228 A CN105954228 A CN 105954228A
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- near infrared
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- 238000000034 method Methods 0.000 title claims abstract description 48
- 239000003027 oil sand Substances 0.000 title claims abstract description 44
- 238000002329 infrared spectrum Methods 0.000 title claims abstract description 26
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 title abstract description 7
- 239000000523 sample Substances 0.000 claims abstract description 65
- 238000001228 spectrum Methods 0.000 claims abstract description 24
- 230000008569 process Effects 0.000 claims abstract description 7
- 238000012545 processing Methods 0.000 claims abstract description 7
- 229910052751 metal Inorganic materials 0.000 claims abstract description 5
- 239000002184 metal Substances 0.000 claims abstract description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 46
- 239000011734 sodium Substances 0.000 claims description 46
- 229910052708 sodium Inorganic materials 0.000 claims description 46
- 238000004458 analytical method Methods 0.000 claims description 15
- 238000004611 spectroscopical analysis Methods 0.000 claims description 11
- 238000012937 correction Methods 0.000 claims description 6
- 238000012360 testing method Methods 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 239000010931 gold Substances 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 230000001066 destructive effect Effects 0.000 abstract 1
- 238000000691 measurement method Methods 0.000 abstract 1
- 238000005457 optimization Methods 0.000 abstract 1
- 238000000513 principal component analysis Methods 0.000 abstract 1
- 238000004445 quantitative analysis Methods 0.000 abstract 1
- 238000011084 recovery Methods 0.000 abstract 1
- 238000010561 standard procedure Methods 0.000 abstract 1
- 238000001514 detection method Methods 0.000 description 11
- 230000008878 coupling Effects 0.000 description 4
- 238000010168 coupling process Methods 0.000 description 4
- 238000005859 coupling reaction Methods 0.000 description 4
- 230000001939 inductive effect Effects 0.000 description 4
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- WURBVZBTWMNKQT-UHFFFAOYSA-N 1-(4-chlorophenoxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)butan-2-one Chemical compound C1=NC=NN1C(C(=O)C(C)(C)C)OC1=CC=C(Cl)C=C1 WURBVZBTWMNKQT-UHFFFAOYSA-N 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- 238000003321 atomic absorption spectrophotometry Methods 0.000 description 2
- 238000004166 bioassay Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000005504 petroleum refining Methods 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
Abstract
The invention relates to a method for nondestructively measuring content of sodium metal in oil sand based on a near infrared spectrum. The method comprises the following steps of: (1) collecting oil sand samples and measuring the content of sodium metal in all the samples according to a standard method; (2) collecting sample spectrums by use of a reflection-type near-infrared analyser probe; (3) performing spectrum pretreatment, reducing dimensionality by use of principal component analysis, and selecting modeling wave bands; (4) establishing a sodium metal content quantitative calibration model by use of partial least squares; and (5) measuring the spectrums of the to-be-measured samples, and verifying the content of sodium metal by use of the established model. Compared with a traditional measurement method, the method provided by the invention is free from complicated sample pretreatment, and has the characteristics of simplicity in operation, rapidness, non-destructive property, no sample pollution and no environmental pollution, and the like, so that a new method is provided for analyzing the metal content; Furthermore, the method can be used for real-time online quantitative analysis, and has direct practical significance in performing real-time control and optimization on an oil sand processing process, improving the recovery rate and the like.
Description
Technical field
The present invention relates to oil-sand quickly analyze and spectroscopic data process field, be specifically related to a kind of oil-sand based near infrared spectrum
The measuring method of middle metallic sodium content.
Background technology
Sodium in oil-sand, potassium, calcium, magnesium, the metallic element such as ferrum in the oil-sand course of processing to the oil product response rate, equipment
Corrosion, efficiency of energy utilization and environmental pollution index etc. all have a significant impact.In the waste water and dregs of processing factory's discharge, high
The sodium metal of concentration, pollutes the environment, is detrimental to health.Additionally, in oil-sand sodium content can act also as oil plant differentiate with
Hide the important parameter in oil engineering.Therefore, sodium content in oil-sand is accurately quickly measured to the analysis of petroleum refining process and control
System, reduces environmental pollution etc. significant.
The method measuring at present both at home and abroad sodium metal broadly falls into chemical analysis, mainly have atomic absorption spectrophotometry (ASS),
Inductive coupling plasma emlssion spectrometry (ICP-AES), inductive coupling ICP-MS (ICP-MS), gas chromatogram
One mass spectrography (GC-MS), enzyme sensor detection method and bioassay method etc..Wherein atomic absorption spectrophotometry (ASS) is right
Sample pre-treatments is loaded down with trivial details and time-consuming；Inductive coupling plasma emlssion spectrometry (ICP-AES) apparatus expensive, plant maintenance expense
By height, operation complexity；Sample is easily carried out multiple by inductive coupling ICP-MS (ICP-MS) by environmental disturbances and needing
Miscellaneous pretreatment, the detection time is long；Gas chromatography and mass spectromentry method (GC-MS) the detection time is long, and workload is big, and cost is high,
Sample pretreatment is required harsher；Enzyme sensor and bioassay method are the most affected by environment, and accuracy of detection is difficult to ensure that,
And it is long to detect the cycle.
Near-infrared spectral analysis technology with its detection speed soon, do not destroy sample, without or minimum sample carried out pretreatment,
Environmentally safe, be easily achieved the advantages such as on-line analysis, be applied successfully to petrochemical industry, agricultural, food,
Many fields such as macromolecule, medical science pharmacy.But about the research of the near infrared ray of tenor in oil-sand the most not
Appear in the newspapers.
Summary of the invention
For solving the problems referred to above, the present invention proposes the measurement side of metallic sodium content in a kind of oil-sand based near infrared spectrum
Method.
For achieving the above object, the present invention adopts the following technical scheme that
(1) oil sands sample is gathered: gather the oil sands sample under different geological conditions, and be classified as calibration set and checking collection；
(2) measure Gold Samples and belong to sodium content: the content of metallic sodium during method measures all oil sands sample according to the traditional standard, note
Record data；
(3) collection of spectrum: be positioned under specified temp by calibration set sample, waits that sample temperature reaches steady statue.With
Reflective near infrared probe contacts with sample surfaces, gathers the near infrared spectrum data of sample.The placement temperature of change sample,
Gather the spectrum under different temperatures.
(4) pretreatment of spectrum and singular point are rejected: to the near infrared spectrum gathered in above-mentioned (3), carry out baseline correction and
First differential processes, and the spectrum after processing is carried out pivot analysis (PCA), rejects unusual sample spot, eventually form modeling
Spectroscopic data collection.
(5) quantitative calibration models is set up: contain the oil-sand metallic sodium of calibration set in pretreated modeling spectroscopic data collection and (2)
Measure definite value, choose specific spectrum frequency range, set up metallic sodium content and near infrared light by partial least square method (PLS)
The calibration model being associated between spectrum.
(6) checking of calibration model: pop one's head in identical reflective near infrared, collects the near infrared spectrum of checking collection sample, according to
The quantitative calibration models set up in step (5) predicts its metallic sodium content, compares the measured value of this sample metal sodium content with pre-
Measured value, and according to actual error requirement, chooses the wave band of calibration model and is optimized.
(7) testing sample analysis: gather the spectrum of oil-sand to be measured, utilizes the calibration model that step (5) and step (6) are set up,
Dope the content of oil-sand metallic sodium to be measured.
The present invention has techniques below benefit
(1) simple to operate: reflective near infrared probe, without sample pretreatment, is directly placed in sample surfaces by sample.
(2) sample nondestructive: without using any reagent, do not damage sample, pollution-free.
(3) detection is rapidly: the measurement time of spectrum only, need to be greatly shortened less than one minute compared with traditional measuring method
Detection time.
(4) may be implemented in line detection: its detection rapidly, in the oil-sand course of processing sodium content can be detected in real time thus and
Time process conditions and Fed-batch are adjusted, reduce infringement to equipment, improve energy efficiency.
(5) favorable reproducibility: spectral measurement good stability is little by external interference.
(6) accuracy of detection is high: result shows that the absolute error between model predication value and conventional determining value is less than, and both
Between there is preferable dependency, its correlation coefficient is, it was predicted that root-mean-square error is, illustrates that the precision of the method is higher,
Sodium tenor detection offer method in the qualification and Tibetan oil engineering of oil kind, has the using value of reality.
Accompanying drawing explanation
Fig. 1 is the flow chart of the measuring method of metallic sodium content in a kind of oil-sand based near infrared spectrum of present example.
Fig. 2 is different oil sands sample former in the measuring method of metallic sodium content in a kind of oil-sand based near infrared spectrum of present example
The beginning curve of spectrum.
Fig. 3 is pretreated oil-sand light in the measuring method of metallic sodium content in a kind of oil-sand based near infrared spectrum of present example
Spectral curve.
Fig. 4 is strange in pivot analysis figure in the measuring method of metallic sodium content in a kind of oil-sand based near infrared spectrum of present example
Dissimilarity
Fig. 5 is the modeling of oil-sand metallic sodium in the measuring method of metallic sodium content in a kind of oil-sand based near infrared spectrum of present example
Frequency range.
Fig. 6 is a young waiter in a wineshop or an inn for calibration model in the measuring method of metallic sodium content in a kind of oil-sand based near infrared spectrum of present example
Multiplying factor.
Fig. 7 is that in a kind of oil-sand based near infrared spectrum of present example, in the measuring method of metallic sodium content, checking collects sample analysis value
Comparison diagram with this method model predication value.
Fig. 8 is oil-sand metallic sodium the reddest in the measuring method of metallic sodium content in a kind of oil-sand based near infrared spectrum of present example
External pelivimetry and the comparison diagram of actual analysis value.
Detailed description of the invention
In order to make objects and advantages of the present invention clearer, below in conjunction with example, the present invention is implemented step and carry out in detail
Describe in detail bright.
Step 1: gathering the oil sands sample under different geological conditions, this example sample number is 200, wherein 100 samples are made
For calibration set, other 65 samples, as checking collection, are tested as unknown sample for remaining 35；
Step 2: method measures the content of metallic sodium in all samples and records data according to the traditional standard.
Step 3: be positioned in ice chest by calibration set sample, keeps 4 DEG C of temperature, and treats that sample temperature reaches stable shape
State.
Step 4: contact with sample surfaces with reflective near infrared probe, the near infrared spectrum data of acquisition correction collection sample.
Step 5: at a temperature of sample is placed on 15 DEG C and 25 DEG C, treat that sample temperature reaches steady statue, use above-mentioned step
Same probe and method described in rapid 4, acquisition correction sample sets spectrum.Fig. 2 show the primary light of different oil sands sample
Spectrum example.
Step 6: to above-mentioned steps 3, the near infrared spectrum gathered in 4,5, carries out baseline correction and first differential processes,
Spectrum after processing is carried out pivot analysis (PCA), rejects unusual sample spot, eventually form modeling spectroscopic data collection.Fig. 3
For pretreated oil-sand spectrum.Fig. 4 is the singular point in calibration set pivot analysis figure.
Step 7: to the oil-sand testing metallic sodium content of calibration set in pretreated modeling spectroscopic data collection and above-mentioned steps 2
Value, sets up, by partial least square method (PLS), the calibration model being associated between metallic sodium content with near infrared spectrum.Choosing
The modeling wavelength band taken is that 1339-1459nm and 1667-1958nm is collectively as modeling wave band.Fig. 5 is respectively oil-sand
Metallic sodium modeling frequency scope.Fig. 6 is the least square coefficient of calibration model.
Step 8: pop one's head in identical reflective near infrared, collects the near infrared spectrum of checking collection sample.The temperature of checking collection sample
Degree requires between 4-25 DEG C.Actual temp need not do and accurately measure and record.According to the quantitative correction set up in step 7
Its metallic sodium content of model prediction, compares measured value and the predictive value of this sample metal sodium content.Calibration model correlation coefficient is
87%, mean square error be 23.49 (mg/L) Fig. 7 be checking collection sample lab analysis value and this method model predication value
Relatively.
Step 9: gather the spectrum of oil-sand to be measured, utilizes the calibration model that step above-mentioned 7 is set up, it was predicted that go out oil-sand to be measured gold
Belonging to the content of sodium, the correlation coefficient of actual analysis value and predictive value is 88.80%, and mean square error is 29.15 (mg/L).
Claims (6)
1. the measuring method of metallic sodium content in an oil-sand based near infrared spectrum, it is characterised in that, comprise the steps:
(1) oil sands sample is gathered: gather the oil sands sample under different geological conditions, and be classified as calibration set and checking collection；
(2) measure Gold Samples and belong to sodium content: the content of metallic sodium, record during method measures all oil sands sample according to the traditional standard
Data；
(3) collection of spectrum: be positioned under specified temp by calibration set sample, waits that sample temperature reaches steady statue；With reflection
Formula near-infrared probe contacts with sample surfaces, gathers the near infrared spectrum data of sample；The placement temperature of change sample, gathers not
Spectrum under synthermal；
(4) pretreatment and the singular point of spectrum is rejected: to the near infrared spectrum gathered in above-mentioned (3), carry out baseline correction and single order
Differential processes, and the spectrum after processing is carried out pivot analysis (PCA), rejects unusual sample spot, eventually form modeling spectroscopic data
Collection；
(5) quantitative calibration models is set up: to the oil-sand metallic sodium content of calibration set in pretreated modeling spectroscopic data collection and (2)
Measured value, chooses specific spectrum frequency range, is set up between metallic sodium content and near infrared spectrum by partial least square method (PLS)
The calibration model being associated；
(6) checking of calibration model: pop one's head in identical reflective near infrared, collects the near infrared spectrum of checking collection sample, according to step
(5) quantitative calibration models set up in predicts its metallic sodium content, compares measured value and the predictive value of this sample metal sodium content, and
According to actual error requirement, calibration model is optimized；
(7) testing sample analysis: gather the spectrum of oil-sand to be measured, utilizes the calibration model that step (5) and step (6) are set up, in advance
Measure the content of oil-sand metallic sodium to be measured.
The measuring method of metallic sodium content in oil-sand the most according to claim 1, it is characterised in that step (3) is described, oil
Sand sample product need not any Chemical Pretreatment, directly with near-infrared reflection formula probe contacts sample surfaces, to measure its near infrared light
Modal data.
The measuring method of metallic sodium content in oil-sand the most according to claim 1, it is characterised in that step (3) is described, will
Sample is as specified temp and treats that it reaches steady statue, gathers near infrared spectrum；After temperature is placed in change, gather different temperatures
Lower spectroscopic data.
The measuring method of metallic sodium content in oil-sand the most according to claim 1, it is characterised in that step (4) is described, light
Spectrum preprocess method is baseline and first derivative；Singular data based on pivot analysis (PCA) is rejected.
The measuring method of metallic sodium content in oil-sand the most according to claim 1, it is characterised in that step (5) is described, builds
Mould near infrared band is the combination of 1339-1459nm and 1667-1958nm, or wave band 1302-2124nm, or wave band
1900-2343nm。
The measuring method of metallic sodium content in oil-sand the most according to claim 1, it is characterised in that step (5) is described, will
Spectroscopic data oil-sand testing metallic sodium content value sets up calibration model by partial least square method (PLS)；Optimal main cause subnumber is by handing over
The predictive residual error sum of squares (PRESS) of proof method gained determines mutually.
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| CN201610521997.4A CN105954228A (en) | 2016-07-04 | 2016-07-04 | Method for measuring content of sodium metal in oil sand based on near infrared spectrum |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106290242A (en) * | 2016-11-07 | 2017-01-04 | 江南大学 | The near infrared spectrum quick test method of magnesium element content in oil-sand |
| CN106442402A (en) * | 2016-11-07 | 2017-02-22 | 江南大学 | Method for rapidly detecting content of calcium element in oil sand on basis of near infrared spectrum |
| CN106525766A (en) * | 2016-11-07 | 2017-03-22 | 江南大学 | Near infrared spectrum measurement method for potassium content in oil sand |
| CN106525755A (en) * | 2016-11-07 | 2017-03-22 | 江南大学 | Oil-sand pH value testing method based on near infrared spectroscopy technology |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106290242A (en) * | 2016-11-07 | 2017-01-04 | 江南大学 | The near infrared spectrum quick test method of magnesium element content in oil-sand |
| CN106442402A (en) * | 2016-11-07 | 2017-02-22 | 江南大学 | Method for rapidly detecting content of calcium element in oil sand on basis of near infrared spectrum |
| CN106525766A (en) * | 2016-11-07 | 2017-03-22 | 江南大学 | Near infrared spectrum measurement method for potassium content in oil sand |
| CN106525755A (en) * | 2016-11-07 | 2017-03-22 | 江南大学 | Oil-sand pH value testing method based on near infrared spectroscopy technology |
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