CN106525743A - New method and device for measuring calcium carbonate content in paper sheet based on optical sensor - Google Patents
New method and device for measuring calcium carbonate content in paper sheet based on optical sensor Download PDFInfo
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- CN106525743A CN106525743A CN201611176462.4A CN201611176462A CN106525743A CN 106525743 A CN106525743 A CN 106525743A CN 201611176462 A CN201611176462 A CN 201611176462A CN 106525743 A CN106525743 A CN 106525743A
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- 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
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Abstract
The invention relates to the technical field of calcium carbonate content measurement and discloses a new method and device for measuring calcium carbonate content in a paper sheet based on an optical sensor. The device comprises an acidizing reaction tank, a precipitator storage tank, metering pumps, a solution mixer, an optical detection system and a computer, wherein the acidizing reaction tank is used for dispersing the paper sheet and adding acid for acidizing; the optical detection system is equipped with a colorimetric dish; the acidizing reaction tank and the precipitator storage tank are respectively communicated with the solution mixer through pipelines with valves and metering pumps; the solution mixer is communicated with the colorimetric dish; and a liquid outlet is formed in the colorimetric dish. According to the method, the paper sheet is acidized, and then the acidized solution is subjected to spectrum detection, so that the calcium carbonate content in the paper sheet can be acquired. The device disclosed by the invention has a simple structure, the operation is simple and convenient, the detection working strength is greatly improved, and the error of manual operation is reduced; the accurate measurement for the calcium carbonate content in the paper sheet can be quickly realized; and the detection result is high in accuracy and precision.
Description
Technical field
The present invention relates to the technical field that calcium carbonate content is determined, more particularly to a kind of based on optical pickocff
New method and device that paper calcium carbonate content is determined.
Background technology
With regard to the measure of calcium carbonate content in paper, traditional method be by calcination after, the survey to ash in paper pulp
Determine method, the method is the national standard method determined to the calcium carbonate retention rate in paper, the method needs high-temperature calcination, if
Operation is continuous, easily there is the danger scalded, also higher to time requirement in addition, due to being that filler is calcined, it may not be possible to
Combustion calcination time and calcination temperature is accurately held very much, the problems such as calcining inequality can be caused.And complex operation, the time required to determining
It is long.And also have the assay method for using such as ion-chromatographic determination calcium ion content now, mainly by chromatography of ions to calcium
Ion detected, the method for the content by calculating Calcium Carbonate.This method advantage is substantially, easy to detect, but for actual life
There is no need in product, because ion chromatograph price is higher, increased unnecessary production cost.EDTA titrimetrys are by carbon
Sour calcium is reacted completely with hydrochloric acid, writes down the consumption of hydrochloric acid, then titrates remaining hydrochloric acid with EDTA, and total hydrochloric acid consumption subtracts EDTA and disappears
The hydrochloric acid content of consumption, the result of gained are exactly the hydrochloric acid content of Calcium Carbonate consumption, are obtained by equation of the Calcium Carbonate with hydrochloric acid reaction
The amount of Calcium Carbonate.Though it is faster than traditional method, similarly there is flaw, mainly determination step is complicated, the sample of survey
The characteristic of all over products can not be reflected, and it is larger to there is error.
The content of the invention
The technical problem to be solved in the present invention is to overcome drawbacks described above, there is provided a kind of paper carbon based on optical pickocff
The device of sour determination of calcium content.
Another object of the present invention is to provide the new side that a kind of paper calcium carbonate content based on optical pickocff is determined
Method.
The present invention is achieved through the following technical solutions：
The device that a kind of paper calcium carbonate content based on optical pickocff is determined, including for disperseing paper and acid adding acid
The acidification reaction groove of change, precipitant accumulator tank, dosing pump, solution mixer, the Systems for optical inspection for being provided with cuvette and calculating
Machine, the acidification reaction groove and precipitant accumulator tank respectively by being provided with the pipeline communication solution mixer of valve and dosing pump,
Solution mixer connects cuvette, and the cuvette is provided with liquid outlet.
The present invention is dissolved into the calcium carbonate solid subparticle in paper in water phase initially with the method for acidifying；So
Afterwards, solution is separated from fiber suspension, and a large amount of bubbles for producing in removing solution；Solution to be detected after purification
Jing after quantitatively mixing with precipitant, in the form of not producing gas, moment generates the stable calcium salt solid of particle diameter again；Finally, use
The content of the quantitative calcium salt solid particle of method of fluorescence detector.
Based on above step, the present invention need not carry out prolonged high temperature sintering to sample, also without headspace gas
The costliness instrument such as chromatograph makees detector, the efficiency for drastically increasing detection, the hardware input cost for reducing detection.
Further, the Systems for optical inspection includes light source, optical fiber and imageing sensor (such as CCD or CMOS) etc..
Further, drainage screen is provided with the acidification reactor, be provided with and match somebody with somebody with external drive equipment in the drainage screen
The agitator for disperseing paper for closing, the drainage screen are provided with acid solution input duct.
Further, dashpot is additionally provided between the acidification reactor and solution mixer.Dashpot can remove solution
In due to acidifying generate great amount of carbon dioxide bubble, to improve the accuracy of detection.Preferably, it is additionally provided with and goes out liquid with cuvette
The waste liquid tank of mouth connection.
Further, the mixed pipe line that the solution mixer is included three-way valve and is connected with three-way valve, it is preferable that described
Mixed pipe line is to strengthen turbulent flow, prevent the spiral pipeline or female thread pipeline of pipeline blockage.
Further, the agitator is magnetic stir bar, propeller mixer or turbine type agitator.
A kind of detection method of the device that paper calcium carbonate content based on optical pickocff is determined, comprises the following steps：
S1. paper is reacted with acid solution, obtains solution to be detected；
S2. detect the absorbance A of precipitant solution0；
S3. detect the absorbance A of solution to be detected1；
S4. calcium carbonate content in paper is calculated according to standard curve；
Wherein, the foundation of standard curve：According to above-mentioned steps, paper in S1 is replaced with into Calcium Carbonate, determine different quality
The absorbance A that obtained of Calcium Carbonate1, the standards calibration curve being shown below is drawn according to linear fit：
W=a (A1-A0)+b
In formula：W Calcium Carbonate quality, g；The slope of a, b standard correction equation and intercept, g.
In paper, calcium carbonate content is calculated：
In formula：Y paper calcium carbonate contents, %；M detections paper quality used；D paper it is dry
Degree, %.
Further, the detection method of the device that a kind of paper calcium carbonate content based on optical pickocff is determined, including
Following steps：
S1. the paper of certain mass is torn up, is put in acidification reaction groove (4), is subsequently adding a certain amount of acid solution；
Paper is mixed homogeneously by turn on agitator (3) with acid solution, obtains pulp suspension；
S2. the precipitant in precipitant accumulator tank (8) is delivered to three-way valve by Open valve (9) and dosing pump (10)
(11), in, into mixed pipe line (12) and cuvette (13), eventually enter into waste liquid tank (14)；The Single wavelength of Systems for optical inspection or
The light that multi wave length illuminating source (15) sends, determines the absorbance of precipitant in cuvette, computer (17) record absorbance data
A0；
S3. agitator (3), Open valve (5) is closed, after filter screen (2) filtration, solution to be detected enters pulp suspension
Enter dashpot (6)；Valve (7) is opened, and the solution to be detected after degasification and the precipitant in precipitant accumulator tank (8) are with certain
Flow-rate ratio mixes in three-way valve (11), enters cuvette (13), finally after being further sufficiently mixed in mixed pipe line (12)
Into waste liquid tank (14)；Systems for optical inspection detects solution to be detected, and computer (17) records the absorbance A of solution to be detected1；
S4. calcium carbonate content in paper is calculated according to standard curve.
The detection method of the device that the paper calcium carbonate content based on optical pickocff is determined, also including following step
Suddenly：
S5. after detection is finished, valve (9) and dosing pump (10) is closed, cleaning agitator (3), drainage screen (2) and acidifying are anti-
Answer groove (4)；And clear water in backward reactive tank, is added, clear water enters waste liquid tank (14) after overall pipeline；Close all valves
And dosing pump, detection terminates.
Preferably, the precipitant is oxalic acid or Soluble oxalate saline solution；The oxalate concentration of the precipitant is
0.05-5mol/L；Preferably, Soluble oxalate salt is Disodium oxalate., potassium oxalate, ammonium oxalate or magnesium oxalate etc..
Preferably, the hydrogen ion concentration of the acid solution is 0.05～2mol/L.The acid solution is hydrochloric acid solution
Deng the acid solution for not producing precipitation with calcium ion.
The revolution of the agitator is 50～1500rpm, and mixing time is 5～30min.
The Detection wavelength of the Systems for optical inspection is 350～900nm.The light path of the cuvette is 0.5～10cm.
Preferably, it is 0.1%～1.0% that the slurry of the pulp suspension is dense.
Preferably, in S3, solution to be detected is 1 with the flow-rate ratio of precipitant：0.01～100.
Compared with now with technology, the invention has the advantages that：
The present invention provides the device that a kind of employing spectrographic method quickly determines Calcium Carbonate in paper, and the apparatus structure is simple, behaviour
Make easy, greatly improve the working strength of detection, reduce manually-operated error.It is high for obtaining accuracy and precision
Testing result provides important guarantee.
The result relative error detected by testing result and 211 standard methods of TAPPI T of the present invention in ± 5%,
There was no significant difference, and the detection time of the method is less than 35min, and comparison with standard detection method substantially increases detection
Efficiency.
The retention data of Calcium Carbonate in paper-making process can quickly be obtained by the method for the present invention, be quickly applied to
In the adjustment of production technology, improve production efficiency and product quality.
Description of the drawings
Fig. 1 is the structural representation of the device that the paper calcium carbonate content based on optical pickocff is determined.
Wherein, 1 acid solution input duct；2 drainage screens；3 agitators；4 acidification reaction grooves；5,9 valves；
6 dashpots；7 dosing pumps；8 precipitant accumulator tanks；10 dosing pumps；11 three-way valve；12 mixed pipe lines；13 ratios
Color ware；14 waste liquid tanks；15 light sources；16 optical fiber；17 computers.
Specific embodiment
The present invention is further illustrated with reference to specific embodiment.Unless stated otherwise, adopt in the embodiment of the present invention
Raw material and method are the routinely commercial raw material in this area and conventional use of method.
Embodiment 1
The device that a kind of paper calcium carbonate content based on optical pickocff is determined, including for disperseing paper and acid adding acid
The acidification reaction groove 4 of change, precipitant accumulator tank 8, solution mixer, the Systems for optical inspection and computer that are provided with cuvette 13
17, acidification reaction groove 4 and precipitant accumulator tank 8 are respectively by being provided with the pipeline communication solution mixer of valve and dosing pump, molten
Liquid mixer connects cuvette 13, and cuvette 13 is provided with liquid outlet, and liquid outlet connects waste liquid tank 14 by pipeline.
The mixed pipe line 12 that solution mixer is included three-way valve 11 and is connected with three-way valve 11.Mixed pipe line 12 is mixed for current stabilization
The spiral pipeline of cooperation.
Systems for optical inspection includes light source 15, optical fiber 16, CCD etc..
Drainage screen 2 is provided with acidification reactor 4, is provided with the cooperation of external drive equipment for disperseing paper in drainage screen 2
The agitator 3 opened, agitator 3 are magnetic stir bar, propeller mixer or turbine type agitator.Drainage screen 2 is provided with acidity
Solution input duct 1.
Dashpot 6 is additionally provided between acidification reactor 4 and solution mixer.Pipe between acidification reaction groove 4 and dashpot 6
Road is provided with valve 5.Dosing pump 7 is provided between dashpot 6 and three-way valve 11.Precipitant accumulator tank 8 and three-way valve 11 are by pipe
Road is connected, and the pipeline of connection is provided with valve 9 and dosing pump 10.
A kind of detection method of the device that paper calcium carbonate content based on optical pickocff is determined, comprises the following steps：
S1. the paper of 0.1g is torn up, be put in acidification reaction groove 4,100mL concentration is subsequently adding for 0.05mol/L's
Hydrochloric acid solution.Turn on agitator 3, revolution 50rpm stir 15min, paper are mixed homogeneously with acid solution, obtain slurry dense
0.1% pulp suspension.
S2. Open valve 9 and dosing pump 10, by the concentration in precipitant accumulator tank for 5.0mol/L sodium oxalate solution with
The flow of 1mL/min is delivered in three-way valve 11, into mixed pipe line 12 and cuvette 13, eventually enters into waste liquid tank 14；Optics
The light that the single wavelength light source (350nm) of detecting system sends, determines the absorbance of sodium oxalate solution in cuvette, computer 17
Record absorbance data A0。
S3. agitator 3, Open valve 5 is closed, after the filtration of filter screen 2, solution to be detected enters degasification to pulp suspension
Dashpot 6；Valve 7 is opened, and the precipitant in the solution to be detected after degasification and precipitant accumulator tank 8 is with 1：0.01 flow-rate ratio
(precipitation agent flux 1mL/min) mixes in three-way valve 11, enters cuvette after being further sufficiently mixed in mixed pipe line 12
13 (light path of cuvette is 0.5cm), eventually enter into waste liquid tank 14；Systems for optical inspection detection detection solution to be detected, calculates
Machine 17 records the absorbance A of testing sample solution1。
S4. calcium carbonate content in paper is calculated according to standard curve.
S5., after detection is finished, valve 9 and dosing pump 10, cleaning agitator 3, drainage screen 2 and acidification reaction groove 4 are closed；And
Clear water, clear water is added to enter waste liquid tank 14 after overall pipeline in backward reactive tank；All valves and dosing pump is closed, is detected
Terminate.
The foundation of standard curve：
The foundation of standard curve：According to above-mentioned steps, paper is replaced with into Calcium Carbonate, determine five different quality levels
The absorbance obtained by Calcium Carbonate, draws the standards calibration curve being shown below according to linear fit：
W=a (A1-A0)+b
In formula：W Calcium Carbonate quality, g；The slope of a, b standard correction equation and intercept, g.
Paper calcium carbonate content is calculated：
In formula：Y paper calcium carbonate contents, %；M detections paper quality used；D paper it is dry
Degree, %.
Embodiment 2～5
Following examples are basically identical with embodiment 1, and difference is：
Experimental result and analysis
By 211 standard methods of TAPPI T, the sample of Example 1～5 is detected that testing result is shown in Table 2 respectively.
Testing result is as follows：
Table 2
| Embodiment | The inventive method, % | Standard method, % | Relative error, % |
| Sample 1 | 40.11 | 39.20 | -2.28 |
| Sample 2 | 35.29 | 36.03 | 2.09 |
| Sample 3 | 11.21 | 11.02 | -1.66 |
| Sample 4 | 5.22 | 5.22 | 0.01 |
| Sample 5 | 23.78 | 22.62 | -4.89 |
Test result indicate that：The relative error of the method and standard detecting method is in ± 5%, there was no significant difference, and
The detection time of the method is less than 35min, and comparison with standard detection method substantially increases the efficiency of detection.
Claims (10)
1. the device that a kind of paper calcium carbonate content based on optical pickocff is determined, it is characterised in that include for disperseing paper
And be acidified with acid acidification reaction groove, precipitant accumulator tank, dosing pump, solution mixer, the optical detection for being provided with cuvette
System and computer, the acidification reaction groove and precipitant accumulator tank it is molten by being provided with the pipeline communication of valve and dosing pump respectively
Liquid mixer, solution mixer connection cuvette, the cuvette are provided with liquid outlet.
2. the device that paper calcium carbonate content according to claim 1 based on optical pickocff is determined, it is characterised in that institute
State, be provided with the drainage screen with the cooperation of external drive equipment for disperseing stirring for paper
Device is mixed, the drainage screen is provided with acid solution input duct.
3. the device that paper calcium carbonate content according to claim 1 based on optical pickocff is determined, it is characterised in that institute
State；Preferably, it is additionally provided be connected with cuvette liquid outlet useless
Liquid bath.
4. the device that paper calcium carbonate content according to claim 1 based on optical pickocff is determined, it is characterised in that institute
State the mixed pipe line that solution mixer is included three-way valve and is connected with three-way valve, it is preferable that the mixed pipe line for strengthen turbulent flow,
Prevent the spiral pipeline or female thread pipeline of pipeline blockage.
5. the device that paper calcium carbonate content according to claim 2 based on optical pickocff is determined, it is characterised in that institute
Agitator is stated for magnetic stir bar, propeller mixer or turbine type agitator.
6. the device that the paper calcium carbonate content according to Claims 1 to 5 any one based on optical pickocff is determined
Detection method, it is characterised in that comprise the following steps：
S1. paper is reacted with acid solution, obtains solution to be detected；
S2. detect the absorbance A of precipitant solution0；
S3. detect the absorbance A of solution to be detected1；
S4. calcium carbonate content in paper is calculated according to standard curve；
Wherein, the foundation of standard curve：According to above-mentioned steps, paper in S1 is replaced with into Calcium Carbonate, determine the carbon of different quality
The absorbance A obtained by sour calcium1, the standards calibration curve being shown below is drawn according to linear fit：
W=a (A1-A0)+b
In formula：W Calcium Carbonate quality, g；The slope of a, b standard correction equation and intercept, g.
In paper, calcium carbonate content is calculated：
In formula：Y paper calcium carbonate contents, %；M detections paper quality used；The mass dryness fraction of D paper, %.
7. according to claim 6 based on optical pickocff paper calcium carbonate content determine device detection method, its
It is characterised by, comprises the following steps：
S1. the paper of certain mass is torn up, is put in acidification reaction groove (4), is subsequently adding a certain amount of acid solution；Open
Paper is mixed homogeneously by agitator (3) with acid solution, obtains pulp suspension；
S2. Open valve (9) and dosing pump (10), the precipitant in precipitant accumulator tank (8) is delivered in three-way valve (11),
Into mixed pipe line (12) and cuvette (13), waste liquid tank (14) is eventually entered into；The Single wavelength or multi-wavelength of Systems for optical inspection
The light that light source (15) sends, determines the absorbance of precipitant in cuvette, computer (17) record absorbance data A0；
S3. agitator (3), Open valve (5) is closed, after filter screen (2) filtration, solution to be detected enters slow pulp suspension
Jet-bedding (6)；Valve (7) is opened, and the solution to be detected after degasification and the precipitant in precipitant accumulator tank (8) are with certain flow
Than mixing in three-way valve (11), cuvette (13) is entered after being further sufficiently mixed in mixed pipe line (12), is eventually entered into
Waste liquid tank (14)；Systems for optical inspection detects solution to be detected, and computer (17) records the absorbance A of solution to be detected1；
S4. calcium carbonate content in paper is calculated according to standard curve.
8. according to claim 7 based on optical pickocff paper calcium carbonate content determine device detection method, its
It is characterised by, it is further comprising the steps of：
S5., after detection is finished, valve (9) and dosing pump (10), cleaning agitator (3), drainage screen (2) and acidification reaction groove are closed
(4)；And clear water in backward reactive tank, is added, clear water enters waste liquid tank (14) after overall pipeline；Close all valves and meter
Amount pump, detection terminate.
9. according to claim 7 based on optical pickocff paper calcium carbonate content determine device detection method, its
It is characterised by,
The precipitant is oxalic acid or Soluble oxalate saline solution；The oxalate concentration of the precipitant is 0.05-5mol/L；Institute
The hydrogen ion concentration for stating acid solution is 0.05-2mol/L；The slurry of the pulp suspension is dense for 0.1%-1.0%.
10. according to claim 7 based on optical pickocff paper calcium carbonate content determine device detection method, its
It is characterised by, in S3, solution to be detected is 1 with the flow-rate ratio of precipitant：0.01～100.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111965374A (en) * | 2020-08-18 | 2020-11-20 | 江西师范大学 | Automatic equipment for detecting content of multistage acidic polysaccharide in water body and use method thereof |
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| CN103499542A (en) * | 2013-09-30 | 2014-01-08 | 中粮生物化学（安徽）股份有限公司 | Method for detecting calcium ion content of citric acid-containing substance |
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| CN103499542A (en) * | 2013-09-30 | 2014-01-08 | 中粮生物化学（安徽）股份有限公司 | Method for detecting calcium ion content of citric acid-containing substance |
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| CECILE GOMEZ ET AL.: "Continuum removal versus PLSR method for clay and calcium carbonate content estimation from laboratory and airborne hyperspectral measurements", 《GEODERMA》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111965374A (en) * | 2020-08-18 | 2020-11-20 | 江西师范大学 | Automatic equipment for detecting content of multistage acidic polysaccharide in water body and use method thereof |
| CN111965374B (en) * | 2020-08-18 | 2023-10-17 | 江西师范大学 | Automatic equipment for detecting content of multistage acidic polysaccharide in water body and application method of automatic equipment |
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Inventor after: Zhang Yu Inventor after: Hu Huichao Inventor after: Chen Lihui Inventor after: Huang Liulian Inventor before: Hu Huichao Inventor before: Zhang Yu Inventor before: Chen Lihui Inventor before: Huang Liulian |
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