CN101281188B - Method for detecting dissolving pulp methyl fiber based on indirect method - Google Patents
Method for detecting dissolving pulp methyl fiber based on indirect method Download PDFInfo
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- CN101281188B CN101281188B CN2008100444825A CN200810044482A CN101281188B CN 101281188 B CN101281188 B CN 101281188B CN 2008100444825 A CN2008100444825 A CN 2008100444825A CN 200810044482 A CN200810044482 A CN 200810044482A CN 101281188 B CN101281188 B CN 101281188B
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Abstract
The invention discloses an automatization dissolving pulp methy fiber testing method and detector, in order to resolve the large artificial error and long analyzing time problem in the prior method using an artificial indirect method to test the dissolving pulp methy fiber. The invention adopts potassium dichromate to oxidize organics in the filtrate sample into carbon dioxide, and then excessive potassium dichromate in the sample filtrate is measuring after oxygenation. The analytical error resulting from individual reason can be decreased and the analyzing time can be cut short by adopting the invention.
Description
Technical field
The present invention relates to the pulp methyl fiber detection technique, adopt indirectly specifically pulp methyl fiber is carried out the method that robotization detects.
Background technology
Detecting pulp methyl fiber at present mainly is to adopt manual analysis.Comprise indirect method and direct method, indirect method claims volumetric method again, the direct method method that weighs again.Indirect method detects principle: each component of non-cellulose in the working sample, gained sum as a result deduct from 100 and are content of cellulose, testing process: claim partly fibre-calculating in separation (mercerization the processings)-filtration-mensuration filtrate of sample-fiber; Direct method detects principle: utilize chemical reagent (17.5% NaOH) to handle sample, make non-cellulose stripping wherein and obtain alpha-cellulose, testing process: claim the separation (mercerization processing) of sample-fiber-wash sample-oven dry-weighing-calculating.
May be when gravimetric method is analyzed because of washing in the clean and mercerization processing procedure because of there is big artificial error in individual reason, existing sample constant weight drying mode time length and influence production control; When volumetric method is analyzed during because of endpoint because of there is big artificial error in individual reason, also exist than mistake, as spectrophotometric method because of analytical approach self.For further dwindling personal error and detection time, the fine testing process of first is carried out very necessity of robotization, instrumentation mensuration.
Summary of the invention
The present invention is intended to detect the problem that personal error is big, analysis time is long in the method for pulp methyl fiber at existing artificial indirect method, a kind of robotization pulp methyl fiber detection method based on indirect method is proposed, and the robotization detector that this method adopted, with the analytical error that reduces to cause and shorten analysis time owing to individual reason.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
Pulp methyl fiber detection method based on indirect method is characterized in that:
A, adopt potassium dichromate to make organism in the filtrate sample (that is: dissolved β, gamma cellulose) be oxidized to carbon dioxide;
B, measure after the oxidation excessive potassium dichromate in the sample filtrate then.
Adopt microwave that filtrate sample is heated to quicken half fine oxidizing process before the said method A step.
In the said method B step, adopt the potassium dichromate oxidation reductometry, adopt, and be terminal point to being purple with the l ferrous ammonium sulfate solution titration of demarcation newly with the agent of giving instruction of ferrous Ling-Fei Luo quinoline.
In the said method B step, adopt and stop the method automatic potentiometric titration forever, select Fe for use
3+/ Fe
2+Electrodes selective is determined titration end-point.
Step is as follows: drop into sample, Weighing system weighs up its quality and imports data into data transmission processing system, computer is handled data, calculate the required alkali lye consumption of the photochemical processing of sample filaments (calculating) by 2 gram sample 30ml alkali lye amounts, then information feedback is arrived automatic control system, be metered into alkali lye by miniature volume pump and carry out the mercerization processing.The mercerization processing finishes the back filters, and automatic ration (can control container by overflow achieves the goal) pipettes filtrate mensuration, and titration is adopted and stopped the method automatic potentiometric titration forever.Data after the titration are imported data transmission processing system processing and output result into.
Then can calculate the potassium dichromate amount that oxidation stripping hemicellulose is consumed after measuring excessive potassium dichromate.Rule of thumb data 1mol potassium dichromate can be calculated the fine content of first by following formula by oxidation 0.00675g half fibre:
The fine %=[1-CV*0.00675/G of first] * 100%
The concentration of c-potassium dichromate in the formula, mol/l
The volume of the potassium dichromate that v-consumes, ml
The example weight that G-takes by weighing, g
Based on the pulp methyl fiber detector of indirect method, comprise following four parts:
Weighing system: be made up of large face plate, mass sensor, quality instrument, mass sensor is sent to the quality instrument with quality signal and changes into electric signal and import computing machine again into and handle.
Sample preparation (mercerization processing) system: form by reagent system, mixing arrangement (forming) and filtrate disposal system by peristaltic pump, container.After sample and classes of agents automatically added, peristaltic pump fully mixed reagent with sample and leaves standstill mercerization then, after finishing sample is separated with solvent (classes of agents).
Automatic control system: quantitatively add reagent system and form by data transmission processing system, (the program control miniature volume pump of computer control, valve).Automatically calculate the alkali lye amount of adding according to sample weighting amount, and control the automatic gauge adding of addition and other reagent automatically.
Automatic potentiometric titration control system: form by reagent system (with identical in the sample processing system), automatic titration system.In the titration process, oxidation state changes with the ratio of going back ortho states in the solution, and current potential changes thereupon, and when the current potential indication was reached home, computing machine to control system, stopped titration with signal feedback automatically.
Equipment work process and principle:
Weighing system weighs up its sample quality and imports data into automatic control system, computer is handled data, calculate the required alkali lye consumption of the photochemical processing of sample filaments, be metered into alkali lye or quantitatively add (end product is proofreaied and correct by coefficient) by miniature volume pump then, under programmed control, start peristaltic pump and automatically alkali lye and the abundant mixing of sample are carried out the mercerization processing by overflow control container.The mercerization processing finishes the back and filters, automatic ration (can control container by overflow achieves the goal) pipettes filtrate to the filtrate disposal system, automatic ration (can control container by overflow achieves the goal) adds potassium dichromate again under programmed control, sulfuric acid oxidation half fibre quantitatively adds phosphoric acid and distilled water then, automatic ration (achieving the goal by overflow control container) pipettes solution again under automatic control system, with iron ammonium sulfate filtrate is measured again, titration is adopted and is stopped the method automatic potentiometric titration forever (in titration process, oxidation state changes with the ratio of going back ortho states in the solution, current potential changes thereupon), timely with the magnetic stirrer agitating solution in titration process to react fully, when the current potential indication is reached home, computing machine to control system, stops signal feedback titration and imports endpoint data into data transmission processing system handling and export the result automatically.The operating control signal of pump and valve, time control signal etc. are controlled by automatic control system in the system.
Beneficial effect of the present invention shows:
One, reduce the analytical error that causes owing to individual reason: since the reading after terminal colour, titration everyone exist difference, thereby produce analytical error or analysis result not parallel.Adopt instrumental analysis then can reduce the analytical error that causes owing to individual reason, instrument error then can be controlled by revising.
Two, shorten analysis time: existing sample drying mode just can reach constant weight for up to 2～3 hours, and partly the fibre time can not surpass half an hour in the titration filtrate.
Description of drawings
Fig. 1 is the inventive method process flow diagram
Fig. 2 is a detector structure principle chart of the present invention
Embodiment
The present invention is directed to existing manual analysis method, proposed the detection method and the detector of robotization.
One, detection method
1, about shortening detection time
Analyze the definition of fine testing process of first and first fibre, the mercerization processing procedure and the mercerization processing time of sample can't be compressed.When direct method detected the first fibre, the shortening time should consider that oven drying is adopted in existing oven dry from drying course, and the constant weight time needs more than 2 hours.If the employing micro-wave vacuum then can shorten drying time (needing about 30 minutes approximately) significantly.
The micro-wave drying processing procedure is exactly by microwave and material direct interaction, and portion is converted into very-high frequency electromagnetic energy the process of heat energy within it.Under the effect of microwave electromagnetic field, the polar molecule in the medium transfers the alternation of following microwave electromagnetic field to and oriented from original thermal motion state, in this microprocess, and the fierce friction of intermolecular generation, microwave energy is converted into the heat in the medium.And water is polar molecule, is to absorb the good medium of microwave.Traditional heat solid material must be in the environment of a heating, then from outward appearance to inner essence, is conducted into solid interior gradually, need for a long time, and microwave is to infiltrate interior of articles with the light velocity that the time is very short.Drying means such as traditional infrared, hot blast heat inhomogeneously, and energy consumption is big, and drying time is long, and microwave heating time is short, homogeneous heating, and no thermal inertia is easy to control, and the microwave penetration ability reaches 80mm.If then further shortened drying time in microwave and vacuum combination.
2, testing process
When indirect method detects, mainly utilize the oxidation of potassium dichromate to make the organism in the filtrate all be oxidized to carbon dioxide.Measure potassium dichromate excessive in the oxidation rear filtrate then.
Concrete assay method has (1) potassium dichromate oxidation reductometry, adopts indicator to determine titration end-point, but because terminal colour is darker, endpoint is difficult, excessive easily during titration.As select Fe for use
3+/ Fe
2+Electrodes selective adopts and stops method potentiometric titration (current potential is 0.8mv when titration end-point) (list of references " analytical chemistry ", " instrumental analysis ") forever, then can accurately judge terminal point and can realize automatic control.(2) spectrophotometric method (721 type spectrophotometer): adopting wavelength is 620nm (list of references: hemicellulose level cuts into a mountain and collects eastern Yu of chemical fibre mill's gold in the colorimetric method for determining pulp), according to the size of optical density, can record and starch the hemicellulose level that dissolves.The present invention also can adopt red, orange, green, blue, yellow (ROGBY) that organism in the filtrate is analyzed.
Two, robotization detector
When design, can be divided into following several module and carry out, make up according to different schemes then:
1 Weighing system
2 sample preparation (mercerization processing) system
3 chemical reagent and distilled water add control system
4 micro-wave vacuum systems
5 automatic potentiometric titration control system
6 data transmission processing systems
7 module combinations schematic diagrams
When measuring, need do the effect correction of different alkali charges to the fine analysis result of first with indirect method.Half fiber detecting device can adopt automatic control of Electric potentials titration, also can adopt spectrophotometric method to measure automatically.
Claims (1)
1. based on the pulp methyl fiber detection method of indirect method, it is characterized in that:
A, employing potassium dichromate make the organism in the filtrate sample be oxidized to carbon dioxide;
B, measure after the oxidation excessive potassium dichromate in the sample filtrate then;
Adopt microwave that filtrate sample is heated to quicken half fine oxidizing process before the method A step;
In the method B step, adopt the potassium dichromate oxidation reductometry, adopt the agent of giving instruction of ferrous Ling-Fei Luo quinoline, and be terminal point to being purple with the l ferrous ammonium sulfate solution titration of new demarcation;
In the method B step, adopt and stop the method automatic potentiometric titration forever, select Fe for use
3+/ Fe
2+Electrodes selective is determined titration end-point;
Testing process is: claim half fine, calculating in sample, the photochemical processing of filament, filtration, the mensuration filtrate;
Title sample described in the above-mentioned steps, the photochemical processing of filament, filtration are specially as follows: drop into sample, Weighing system weighs up its quality and imports data into data transmission processing system, computer is handled data, calculate the required alkali lye consumption of the photochemical processing of sample filaments, then information feedback is arrived automatic control system, be metered into alkali lye by miniature volume pump and carry out the mercerization processing; The mercerization processing finishes the back filters, and automatic ration pipettes filtrate mensuration, and titration is adopted and stopped the method automatic potentiometric titration forever, and the data after the titration are imported data transmission processing system processing and output result into;
Half fibre, calculating are specially as follows in the mensuration filtrate described in the above-mentioned steps: then calculate the potassium dichromate amount that oxidation stripping hemicellulose is consumed after measuring excessive potassium dichromate, rule of thumb data 1mol potassium dichromate can be calculated the fine content of first by following formula by oxidation 0.00675g half fibre:
The fine %=[1-CV*0.00675/G of first] * 100%
The concentration of c-potassium dichromate in the formula, mol/l
The volume of the potassium dichromate that v-consumes, ml
The example weight that G-takes by weighing, g.
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| CN2008100444825A CN101281188B (en) | 2008-05-30 | 2008-05-30 | Method for detecting dissolving pulp methyl fiber based on indirect method |
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| CN102645513B (en) * | 2012-05-02 | 2014-07-16 | 成都苑东药业有限公司 | Method for determining sodion content in diphosphonic acid monosodium salt compound |
| CN105572260B (en) * | 2016-01-19 | 2018-05-15 | 华南理工大学 | One kind measure dissolving pulp in α-, β-and gamma cellulose content method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6048715A (en) * | 1988-07-08 | 2000-04-11 | Univ. Of British Columbia | Two-phase partition affinity separation system and affinity separated cell-containing composition |
| US6255118B1 (en) * | 1997-06-11 | 2001-07-03 | Nalco Chemical Company | Method for using an all solid-state fluorometer in industrial water system applications |
| CN201251573Y (en) * | 2008-05-30 | 2009-06-03 | 宜宾长毅浆粕有限责任公司 | Detector of alpha cellulose in pulp based on indirect method |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6048715A (en) * | 1988-07-08 | 2000-04-11 | Univ. Of British Columbia | Two-phase partition affinity separation system and affinity separated cell-containing composition |
| US6255118B1 (en) * | 1997-06-11 | 2001-07-03 | Nalco Chemical Company | Method for using an all solid-state fluorometer in industrial water system applications |
| CN201251573Y (en) * | 2008-05-30 | 2009-06-03 | 宜宾长毅浆粕有限责任公司 | Detector of alpha cellulose in pulp based on indirect method |
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