CN101968422A - Method for nondestructively detecting viscosity of nitro-cotton - Google Patents
Method for nondestructively detecting viscosity of nitro-cotton Download PDFInfo
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- CN101968422A CN101968422A CN 201010264674 CN201010264674A CN101968422A CN 101968422 A CN101968422 A CN 101968422A CN 201010264674 CN201010264674 CN 201010264674 CN 201010264674 A CN201010264674 A CN 201010264674A CN 101968422 A CN101968422 A CN 101968422A
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Abstract
The invention relates to a method for nondestructively detecting the viscosity of nitro-cotton. The method comprises the following steps of: a, selecting a nitro-cotton sample with viscosity representativeness so as to form a sample set and acquiring the spectrum of the sample in the sample set, wherein the viscosity range is between 0.6 and 2,000 s and the spectrum scanning range is between 800 and 2,500 nanometers; b, establishing a prediction model according to the spectrum and viscosity value of the sample; c, acquiring the spectrum of an unknown nitro-cotton sample so as to obtain the spectrum of the unknown sample; and d, inputting the spectrum of the unknown sample into the prediction model for analysis and computation so as to obtain the viscosity value of the unknown nitro-cotton sample. The invention has the advantages that: the method is easy to operate, has high measuring speed and is environmentally-friendly.
Description
Technical field
The present invention relates to a kind of detection method of nitrocotton viscosity, especially a kind of method of utilizing spectral analysis technique nitrocotton viscosity to be carried out Non-Destructive Testing.
Background technology
Nitrocotton claims nitrocellulose again, and the formal name used at school cellulose nitrate is to be prepared through esterification by refining cotton linter and nitration acids.
Nitrocotton is the filmogen that is widely used in aspects such as coating, printing ink, leather gloss agent and nail polish, table tennis.With the nitrocotton is that the coating that raw material is made has had lasting weatherability, the compatible and best quick-drying of better resin concurrently, and for woodwork coating, it has more beyond challenge advantage.
Nitrocotton is divided into different specifications according to its nitro content and viscosity number, is applied to different fields, and is as shown in table 1.
Table 1: the cotton current techique standard of industry nitration
The assay method of tradition viscosity:, represent the viscosity of nitrocotton with the steel ball of the measuring 10 inches institute's elapsed times that in filling an inch diameter viscosity tube of nitrocellulose solution, fall.
Assay method:, press the listed mass percent concentration preparation of table 2 100～200g solution with dry nitrocotton according to different viscosities.The viscosimetric analysis of industrial nitrocotton, the nitrocotton concentration of needs preparation variable concentrations, concentration is respectively 12.2%, 20.0%, 25.0%, is hereinafter referred to as " A method ", " B method ", " C method ".
Table 2
Earlier in bottle, add a sample that takes by weighing during preparation, add toluene and ethanol again, sample is soaked into fully after, add ethyl acetate again.With lid bottle is tightened, made nitrocotton be dissolved into uniform solution fully with the method for shaking or rotate.
Above-mentioned solution is injected clean viscosity tube, and solution height should surpass last groove 30mm, and plug is with stopper, the mouth of pipe upwards, insulation is no less than 30min in 25.0 ± 0.5 ℃ glass water drum, wait not have bubble after, get clean steel ball and freely fall from the viscosity tube center of top.When steel ball declines supreme groove at solution, start stopwatch, when reducing to down scale, stop stopwatch, the record falling sphere time, be accurate to 0.1s.
Nitrocellulose solution by preparation different quality percent concentration, utilize A method, B method and C method can measure the viscosity of nitrocotton well, but also have the following disadvantages:
1, the viscosimetric analysis of industrial nitrocotton, the nitrocotton concentration of needs preparation variable concentrations consumes all ingredients, can not reclaim after reagent uses up, and environment is caused harmful effect; And toluene belongs to hypertoxic class organic solvent, contacts this type of reagent for a long time, and is bigger to human body harm;
Need use the solution of nitrocotton preparation variable concentrations when 2, measuring nitrocotton viscosity, tested nitrocotton sample part is destroyed;
3, the method for employing obtain solution is measured nitrocotton viscosity length consuming time, efficient is low, can't adapt to the real-time detection of industry spot.
Summary of the invention
In order to solve above-mentioned deficiency of the prior art, the invention provides a kind of fast, the measuring method of harmless, simple determination nitrocotton viscosity.
For achieving the above object, the present invention adopts following technical scheme:
A kind of Non-Destructive Testing nitrocotton method of viscosity may further comprise the steps:
A, selection have the representational nitrocotton sample of viscosity to form sample sets, and range of viscosities is 0.6～2000s;
Collected specimens is concentrated the spectrum of sample, and the spectral scan scope is 800～2500nm;
B, spectrum per sample and viscosity number are set up forecast model;
The spectrum of c, the unknown nitrocotton sample of collection obtains unknown sample spectrum;
D, unknown sample spectrum input forecast model is carried out analytical calculation, obtain the viscosity number of unknown nitrocotton sample.
As preferably, in step a, selecting has the representational nitrocotton sample of viscosity to form and measure the corresponding sample sets of type respectively, measures type and is respectively A method, B method and C method;
Collected specimens is concentrated the spectrum of sample, forms respectively and the corresponding spectra collection of measurement type;
In step b, set up respectively and the corresponding forecast model of measurement type;
In steps d, the measurement type that the identification unknown sample is fit to; The corresponding forecast model of measurement type selecting according to identification carries out analytical calculation to unknown sample spectrum, obtains the viscosity number of unknown nitrocotton sample.
As preferably, in steps d, the forecast model of setting up among the unknown sample spectrum input step b is carried out analytical calculation, obtain unknown sample and measure type viscosity number one to one;
The measurement type that the identification unknown sample is fit to;
Unknown sample and this are measured the viscosity number of the corresponding viscosity number of type as unknown nitrocotton sample.
Further, the concrete steps of the measurement type that the identification unknown sample is fit to are: all samples spectrum among unknown sample spectrum and the step a is mated, with the good spectrum of the relative matching degree of described unknown sample spectrum, the measurement type under the sample that it is corresponding is as the suitable measurement type of unknown sample in the identification all samples spectrum.
As preferably, the library of spectra that all spectrum among the step a are formed is optimized.
As preferably, to being optimized with A method, B method and the corresponding spectra collection of C method respectively.
Further, described optimization is meant: library of spectra or the concentrated spectrum of corresponding spectrum are mated, select the good similar spectrum of matching degree, keep in the similar spectrum, and with all the other rejectings, upgrade library of spectra or corresponding spectra collection.
As preferably, the characteristic absorption wave band of choosing sample when setting up forecast model is: 1000～1800nm.
As preferably, the range of viscosities of the nitrocotton sample that adopts when setting up forecast model is 0.9～227s.
Further, when setting up forecast model, adopt multivariate calibration methods.
The assay method of the nitrocotton viscosity that the spectral analysis that the present invention adopts combines with Chemical Measurement has following beneficial effect:
1, introduces spectral technique first, be used to measure nitrocotton viscosity, opened up the new method of nitrocotton viscosimetric analysis;
2, this method is simple to operate, cost of determination is low, and finding speed is fast, can determine apace whether to be measured batch nitrocotton meets the requirements, and is fit to industrial online application;
3, before measure spectrum, nitrocotton does not need to dissolve joins the sample step, environmentally friendly.
Description of drawings
Fig. 1 is the process flow diagram that detects nitrocotton viscosity method among the embodiment 1.
Embodiment
Embodiment 1
See also Fig. 1, a kind of Non-Destructive Testing nitrocotton method of viscosity may further comprise the steps:
A, selection nitrocotton sample sets and collected specimens spectrum, concrete steps are as follows:
A1, according to the viscosity number scope, select to form and measure the corresponding sample sets A collection of type, B collection and C collection by the representational nitrocotton sample of viscosity, wherein, the measurement type is respectively A method, B method and C method; The A collection comprises 270 by the viscometric sample of A method, and the viscosity number distribution gradient of sample; The B collection comprises 50 by the viscometric sample of B method, and the viscosity number distribution gradient of sample; The C collection comprises 60 by the viscometric sample of C method, and the viscosity number distribution gradient of sample; The range of viscosities of nitrocotton is between 0.6～2000s, and the range of viscosities of the sample that present embodiment is chosen is 0.9～227s;
A2, collection respective sample are concentrated the diffuse reflection spectrum of sample:
With the white pottery porcelain is background, utilizes spectroanalysis instrument collected specimens spectrum, and the spectral scan scope is 800～2500nm, and scanning times is 30 times;
The a certain nitrocotton sample that A is concentrated is positioned on the sample disc and spreads out, and the rotary sample dish is gathered its diffuse reflection spectrum with above-mentioned spectrometer; Other nitrocotton sample that A is concentrated carries out same operation, obtains the diffuse reflection spectrum of respective sample; The set of the diffuse reflection spectrum of all samples that the above-mentioned A that records is concentrated is as collecting with the corresponding A spectrum of A method;
The B collection concentrates the spectra collection step of corresponding nitrocotton sample identical with A collection corresponding steps with C, obtains collecting with B method and the corresponding diffuse reflection spectrum collection of C method B spectrum respectively and C spectrum collection;
All spectrum are carried out pre-service: to spectrum carry out smoothly, pre-service such as differentiate, polynary scatter correction, the conversion of calibration normal variate, remove redundant information to greatest extent and eliminate the spectrum deviation that various disturbing factors cause, and upgrade A spectrum collection, B spectrum collection and C spectrum collection;
All samples spectrum forms library of spectra;
B, set up forecast model:
Selecting the characteristic absorption wave band is 1000～1800nm;
Adopt partial least square method, compose the viscosity number that the spectrum of concentrating reaches sample corresponding with it, set up the multiple regression forecasting model, be the A model corresponding with the A method by the A after upgrading;
The establishment step of B spectrum collection and C spectrum collection corresponding model and A compose that to collect corresponding steps identical, obtain respectively and B method and C method corresponding forecast model B model and C model;
C, adopt spectrometer described in the step a2 to gather the spectrum of unknown nitrocotton sample, and the method among a is carried out pre-service to spectrum set by step, obtains unknown sample spectrum;
D, obtain the viscosity number of sample, concrete steps are as follows:
The measurement type that d1, identification unknown sample are fit to: the spectrum in unknown sample spectrum and the library of spectra is mated, calculate the mahalanobis distance between the spectrum; Identify in the library of spectra spectrum with unknown sample spectrum mahalanobis distance minimum, the measurement type that the measurement type under the sample that it is corresponding is fit to as unknown sample;
D2, according to the measurement type of identification, select corresponding forecast model that unknown sample spectrum is carried out analytical calculation, obtain the viscosity of unknown nitrocotton sample, thereby determine the specification of unknown nitrocotton sample according to table 1.
Adopt the method for present embodiment that 10 parts of blind samples of unknown nitrocotton (viscosity number is known) are carried out the viscosity prediction, as shown in table 3.By the result as seen, the viscosity that adopts the nitrocotton sample that the inventive method records and tradition dissolve that to join the result that quadrat method (being A method, B method and C method) records more consistent, and residual error is less, can determine the specification of corresponding nitrocotton more exactly.Show that the present invention has higher mensuration accuracy, as a kind of non-destructive and assay method fast, practical measurement result is an acceptable.
Table 3
The present invention introduces spectral analysis technique, is used to measure nitrocotton viscosity, has opened up the new method of nitrocotton viscosimetric analysis; Method of the present invention is simple to operate simultaneously, finding speed is fast, can determine apace whether to be measured batch nitrocotton meets the requirements, and is fit to industrial online application; Simultaneously when measuring unknown sample viscosity, do not need nitrocotton dissolved and join the sample step, environmentally friendly.
Embodiment 2
A kind of Non-Destructive Testing nitrocotton method of viscosity, different with embodiment 1 described detection nitrocotton method of viscosity is:
In step a, the library of spectra that all samples spectrum is formed is optimized: the spectrum in the library of spectra is mated, calculate the mahalanobis distance between the spectrum; Select the good similar spectrum of matching degree according to the mahalanobis distance between the spectrum, keep in the similar spectrum, and all the other spectrum are rejected, upgrade library of spectra;
To A spectrum collection, B spectrum collection and C spectrum collection and the spectrum in the library of spectra after upgrading carry out pre-service.
The benefit of optimizing library of spectra is to remove redundant information, picks out representative spectrum, so that when input unknown sample spectrum, can find out the spectrum that is complementary with it apace.
Embodiment 3
A kind of Non-Destructive Testing nitrocotton method of viscosity, different with embodiment 2 described detection nitrocotton method of viscosity is:
In step a, the spectrum that library of spectra was rejected when optimizing is concentrated in corresponding A spectrum collection or B spectrum collection or C spectrum simultaneously and is rejected, and upgrades A spectrum collection and/or B spectrum collection and/or C spectrum collection, to pick out representative spectrum, to save the modelling time;
In step b, according to upgrading and pretreated A spectrum collection, B spectrum collection and C spectrum collection are set up corresponding forecast model A model, B model and C model.
Embodiment 4
A kind of Non-Destructive Testing nitrocotton method of viscosity, different with embodiment 1 described detection nitrocotton method of viscosity is:
In step a, optimize A spectrum collection: the spectrum that the A spectrum is concentrated mates, and calculates the mahalanobis distance between the spectrum; Select the good similar spectrum of matching degree according to the mahalanobis distance between the spectrum, keep in the similar spectrum, and all the other spectrum are rejected, upgrade A spectrum collection;
The optimization step of B spectrum collection and C spectrum collection is identical with A spectrum collection corresponding steps, B spectrum collection after obtaining respectively upgrading and C spectrum collection;
In step b, according to upgrading and pretreated A spectrum collection, B spectrum collection and C spectrum collection are set up corresponding forecast model A model, B model and C model.
Embodiment 5
A kind of Non-Destructive Testing nitrocotton method of viscosity, different with embodiment 1 described detection nitrocotton method of viscosity is:
In steps d, obtain the viscosity number of sample, concrete steps are as follows:
D1, with obtain among the unknown sample spectrum input step b respectively with the corresponding A model of A method, B method and C method, B model and C model, obtain the viscosity number of unknown sample under A method, B method and C method;
The measurement type that d2, identification unknown sample are fit to: unknown sample spectrum and all samples spectrum are mated, calculate the mahalanobis distance between the spectrum; Identify in all spectrum the spectrum with unknown sample spectrum mahalanobis distance minimum, the measurement type that the measurement type under the sample that it is corresponding is fit to as unknown sample;
D3, select the corresponding viscosity number of measurement type determined with steps d 2 in the steps d 1 viscosity number, thereby determine the specification of unknown nitrocotton sample according to table 1 as unknown sample.
In practical operation, have this situation and take place: promptly the client knows the specification that unknown sample is general in advance, knows its pairing measurement type, but does not know the viscosity number that sample is concrete; Then can be according to the method for present embodiment, the client is from the viscosity number of unknown sample under A method, B method and C method that is drawn by steps d 1, select to measure the corresponding viscosity number of type, thereby determine the specification of unknown nitrocotton sample according to table 1 with the unknown sample known to it.
Extract 10 blind samples of nitrocotton, known its viscosity actual value is measured the method for nitrocotton sample and is verified to present embodiment.The checking result sees also table 4.By the result as seen, the final viscosity value of the sample that records according to the method for present embodiment is consistent with sample viscosity actual value, and the viscosity number that the method by present embodiment of illustrating records sample is an acceptable.
Table 4
Above-mentioned embodiment should not be construed as limiting the scope of the invention.Key of the present invention is: concentrate the spectrum of nitrocotton sample and corresponding with it viscosity number to set up forecast model per sample, the spectrum of unknown nitrocotton sample is inputed in the above-mentioned forecast model, calculate the viscosity number of unknown nitrocotton sample by analysis, thereby determine the specification of unknown nitrocotton sample.Under the situation that does not break away from spirit of the present invention, any type of change that the present invention is made all should fall within protection scope of the present invention.
Claims (10)
1. Non-Destructive Testing nitrocotton method of viscosity may further comprise the steps:
A, selection have the representational nitrocotton sample of viscosity to form sample sets, and range of viscosities is 0.6～2000s;
Collected specimens is concentrated the spectrum of sample, and the spectral scan scope is 800～2500nm;
B, spectrum per sample and viscosity number are set up forecast model;
The spectrum of c, the unknown nitrocotton sample of collection obtains unknown sample spectrum;
D, unknown sample spectrum input forecast model is carried out analytical calculation, obtain the viscosity number of unknown nitrocotton sample.
2. Non-Destructive Testing nitrocotton method of viscosity according to claim 1 is characterized in that:
In step a, selecting has the representational nitrocotton sample of viscosity to form and measure the corresponding sample sets of type respectively, measures type and is respectively A method, B method and C method;
Collected specimens is concentrated the spectrum of sample, forms respectively and the corresponding spectra collection of measurement type;
In step b, set up respectively and the corresponding forecast model of measurement type;
In steps d, the measurement type that the identification unknown sample is fit to; The corresponding forecast model of measurement type selecting according to identification carries out analytical calculation to unknown sample spectrum, obtains the viscosity number of unknown nitrocotton sample.
3. Non-Destructive Testing nitrocotton method of viscosity according to claim 2 is characterized in that:
In steps d, the forecast model of setting up among the unknown sample spectrum input step b is carried out analytical calculation, obtain unknown sample and measure type viscosity number one to one;
The measurement type that the identification unknown sample is fit to;
Unknown sample and this are measured the viscosity number of the corresponding viscosity number of type as unknown nitrocotton sample.
4. according to claim 2 or 3 described Non-Destructive Testing nitrocotton method of viscosity, it is characterized in that: the concrete steps of the measurement type that the identification unknown sample is fit to are: all samples spectrum among unknown sample spectrum and the step a is mated, with the good spectrum of the relative matching degree of described unknown sample spectrum, the measurement type under the sample that it is corresponding is as the suitable measurement type of unknown sample in the identification all samples spectrum.
5. Non-Destructive Testing nitrocotton method of viscosity according to claim 1 is characterized in that: the library of spectra that all spectrum among the step a are formed is optimized.
6. Non-Destructive Testing nitrocotton method of viscosity according to claim 2 is characterized in that: to being optimized with A method, B method and the corresponding spectra collection of C method respectively.
7. according to claim 5 or 6 described Non-Destructive Testing nitrocotton method of viscosity, it is characterized in that: described optimization is meant: library of spectra or the concentrated spectrum of corresponding spectrum are mated, select the good similar spectrum of matching degree, keep in the similar spectrum, and, upgrade library of spectra or corresponding spectra collection with all the other rejectings.
8. Non-Destructive Testing nitrocotton method of viscosity according to claim 1 is characterized in that: the characteristic absorption wave band of choosing sample when setting up forecast model is: 1000～1800nm.
9. Non-Destructive Testing nitrocotton method of viscosity according to claim 1 is characterized in that: the range of viscosities of the nitrocotton sample that adopts when setting up forecast model is 0.9～227s.
10. Non-Destructive Testing nitrocotton method of viscosity according to claim 1 is characterized in that: when setting up forecast model, adopt multivariate calibration methods.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105699255A (en) * | 2016-03-15 | 2016-06-22 | 山东万圣博科技股份有限公司 | Method for rapidly detecting molecular weight of poly-p-phenylene terephthamide resin |
| CN109856013A (en) * | 2017-11-30 | 2019-06-07 | 廊坊立邦涂料有限公司 | A kind of semisolid decorative material workability judgment method of flat surface |
| CN111713745A (en) * | 2020-06-08 | 2020-09-29 | 深圳市康泓威科技有限公司 | Method for detecting and controlling solution viscosity of electronic atomization equipment and electronic atomization equipment thereof |
| CN113959906A (en) * | 2021-11-23 | 2022-01-21 | 北方化学工业股份有限公司 | Viscosity testing method for nitrocotton for coating |
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| WO2007034802A1 (en) * | 2005-09-20 | 2007-03-29 | Sumitomo Electric Industries, Ltd. | Elasticity/viscosity measuring device |
| US7281413B2 (en) * | 2002-11-07 | 2007-10-16 | Edc Biosystems, Inc. | Acoustic method for determining the viscosity and/or surface tension of a liquid |
| CN101726451A (en) * | 2008-10-21 | 2010-06-09 | 冯新泸 | Method for measuring viscosity index of internal combustion engine oil |
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2010
- 2010-08-24 CN CN 201010264674 patent/CN101968422A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7281413B2 (en) * | 2002-11-07 | 2007-10-16 | Edc Biosystems, Inc. | Acoustic method for determining the viscosity and/or surface tension of a liquid |
| WO2007034802A1 (en) * | 2005-09-20 | 2007-03-29 | Sumitomo Electric Industries, Ltd. | Elasticity/viscosity measuring device |
| CN101726451A (en) * | 2008-10-21 | 2010-06-09 | 冯新泸 | Method for measuring viscosity index of internal combustion engine oil |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105699255A (en) * | 2016-03-15 | 2016-06-22 | 山东万圣博科技股份有限公司 | Method for rapidly detecting molecular weight of poly-p-phenylene terephthamide resin |
| CN109856013A (en) * | 2017-11-30 | 2019-06-07 | 廊坊立邦涂料有限公司 | A kind of semisolid decorative material workability judgment method of flat surface |
| CN109856013B (en) * | 2017-11-30 | 2021-09-14 | 廊坊立邦涂料有限公司 | Method for judging construction performance of semi-solid decorative material with flat surface |
| CN111713745A (en) * | 2020-06-08 | 2020-09-29 | 深圳市康泓威科技有限公司 | Method for detecting and controlling solution viscosity of electronic atomization equipment and electronic atomization equipment thereof |
| CN113959906A (en) * | 2021-11-23 | 2022-01-21 | 北方化学工业股份有限公司 | Viscosity testing method for nitrocotton for coating |
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Application publication date: 20110209 |