CN109142124A - A kind of improved modified acrylic fibre qualitative and quantitative analysis method - Google Patents
A kind of improved modified acrylic fibre qualitative and quantitative analysis method Download PDFInfo
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- CN109142124A CN109142124A CN201811003911.4A CN201811003911A CN109142124A CN 109142124 A CN109142124 A CN 109142124A CN 201811003911 A CN201811003911 A CN 201811003911A CN 109142124 A CN109142124 A CN 109142124A
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Abstract
The invention discloses a kind of improved modified acrylic fibre is qualitative, quantitative analysis method, it successively include following processing step: qualitative → sampling → drying weighing → dissolution → drying weighing → calculating, it is characterized in that, in the qualitative step, process comprising nitric acid is added into fiber, in this process, after nitric acid is added, if it is determined that the form of fiber is breaking morphology, then dissolved using cyclohexanone as solvent in subsequent dissolving step, if it is determined that the form of fiber is swelling form, then dissolved using acetone as solvent in subsequent dissolving step.The present invention dexterously according to it is qualitative when fiber add the state of nitric acid, to be directed to fiber different solubilising reagent and dissolution conditions, the neoteric acetone method of instant bulging state of different shape performance, breaking morphology cyclohexanone method, flexibility is high, high-efficient, good to personnel safety, the feature of environmental protection is good.
Description
Technical field
It is qualitative, quantitative that the invention belongs to textile inspection fields more particularly to a kind of improved modified acrylic fibre
Analysis method.
Background technique
In the prior art, for modified acrylic fibre, the principle of qualitative and quantitative analysis method is: with nearly boiling point
Cyclohexanone reagent modified acrylic fibre is dissolved from the mixture of known dry mass removal；Residue is collected, clearly
It washes, dry and weighs, with its percentage for accounting for mixture dry mass of revised Mass Calculation, obtain modified poly- third by difference
The quality percentage of alkene nitrile fiber and other fibers.
Specifically, dissolving step is: distilling flask is added in cyclohexanone in the ratio of every gram of sample 100ML, loads onto extraction
Container will first be put into the glass sand core crucible for having installed sample and perforated baffle and being slightly tilted in extraction container.It connects back and stays
Condenser is heated to solution boiling, extracts 60MIN, at least recycles 12 times per hour.Extraction takes out extraction appearance after terminating cooling
Device takes out glass sand core crucible and takes out perforated baffle, with the excess 3 or 4 in the 50% ethyl alcohol cleaning crucible for being pre-heated to 60 DEG C
It is secondary, it is then cleaned with 60 DEG C of 1L water, cleaning operation is not aspirate, and allows liquid to aspirate again after gravity emptying, finally, drying
Crucible and residue cooling are simultaneously weighed.As a result it calculates and indicates to provide according to GB/T 2910.1.
But the test process, there are the following problems: 1, the time that test needs is long, and low efficiency: only test period is with regard to big
In 1H；2, poor to people's safety: cyclohexanone is inflammable toxic, and when test uses the cyclohexanone of 156 DEG C of nearly boiling point as solubilising reagent,
Although testing in extractor, there is also security risks, additionally while technician wears a gas mask, the volatilization of reagent is still
There is certain harm to body；3, environmental safety is poor: the storage of waste liquid after test, because its property is inflammable toxic in case of broken
It the case where bottle, can cause environmental pollution, not environmentally.
Based on the above issues, people need to find safer and more reliable, efficient, environmentally friendly detection method.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of a kind of safe, reliable, efficient, environmentally friendly improved modifications
Polyacrylonitrile fibre qualitative and quantitative analysis method is to pass through the morphologic appearance of fiber from the qualitative step that fiber content is tested
To use any solubilising reagent and test condition when determining dissolving step.
What the present invention was realized particular by following technical scheme:
A kind of improved modified acrylic fibre qualitative and quantitative analysis method successively includes following processing step: qualitative → to take
Sample → drying weighing → dissolution → drying weighing → calculating, in the qualitative step, the mistake comprising nitric acid is added into fiber
Journey after nitric acid is added, if it is determined that the form of fiber is breaking morphology, is then adopted in subsequent dissolving step in this process
It uses cyclohexanone to be dissolved as solvent, if it is determined that the form of fiber is swelling form, is then used in subsequent dissolving step
Acetone is dissolved as solvent.
Preferably, as needed, between qualitative → sampling, being additionally provided with pretreatment process.
Emphasis of the invention is that discovery can use acetone in course of dissolution as solvent to dissolve those in qualitative progress
The modified acrylic fibre being swollen is shown as after nitric acid is added, this discovery is derived from sample pretreatment usually, if general
There are some non-fibrous materials on sample, tester needs to carry out pretreatment removal non-fibrous material with reagent to ensure to test knot
The accuracy of fruit.When once encountering modified acrylic fibre and the blended sample of polyester fiber, tester because of experience not
Foot has selected after going pretreatment with 50 DEG C of water-baths of acetone (to may be otherwise and regard operation error as, tester is to prepare originally
With 50 DEG C of water process 30MIN), it is found that modified acrylic fibre all dissolves only remaining polyester fiber in raw sample, it is subsequent to look into
It reads data and finds that 50 DEG C of acetone solvents do not damage polyester fiber, it is contemplated that being applied.
After inventor has found the new acetone method, can all be dissolved for all modified acrylic fibres, but it is real
Find that modified acrylic fibre is not dissolved in some sample residues in the course of dissolution of border, using the qualitative hair of microscope
Existing such modified acrylic fibre is that breaking state is presented after adding nitron.
In qualitative blind sample, if containing acrylic fibers in sample, nitric acid solvent can be added dropwise in tester, because modified poly- third
Alkene nitrile fiber and polyacrylonitrile fibre belong to acrylic fibers, add nitric acid to be to determine that the fiber in blind sample is modified polyacrylonitrile fibre
Dimension or polyacrylonitrile fibre.Under discovery as above, inventor is observed, after different modified acrylic fibres have added nitric acid
One meet together show swelling and fracture two states.Finally, inventor is had found by test of many times, in course of dissolution, acetone
It can be used to be dissolved in these modified acrylic fibres that solvent swelling state is shown as in qualitative step plus after nitric acid, to surplus
Cofibre does not damage, can not be molten for showing as those of fracture modified acrylic fibre in qualitative step plus after nitric acid
Solution, therefore consider to make the invention.
The detailed process of the qualitative step is: qualitative step is executed according to FZ/T 01057.3-2007, by appropriate fiber
It is evenly laid out on glass slide, in addition a drop transparent medium covered, pays attention to that bubble cannot be brought into, is placed on biomicroscope
Objective table on, under the conditions of 100 times~500 times of amplification factor observe fiber vertical face and cross section shapes, control fiber
Standard photographs and morphologic description identify the classification of unknown fiber.
Preferably, being comprised the concrete steps that using acetone as what solvent was dissolved: (1) sample being put into container, pressed
The acetone of 100ML~200ML is added according to every gram of sample, prevents incomplete dissolution data inaccuracy, shakes container and be impregnated with sample,
30MIN ± 5MIN is continuously shaken in 50 DEG C of ± 5 DEG C of water-baths, why selects temperature, firstly because modified poly- third at a temperature of this
Alkene nitrile fiber can be completely dissolved, secondly in view of all laboratory work times have always 50 DEG C ± 5 DEG C of shaking bath,
Heating, cooling is not needed, the time is saved；The selection of time is also when using for reference commonly to test in GB/T 2910-2009 standard
Between, modified polypropylene fiber can be completely dissolved by being primarily due to 30min；Then solution is fallen off, residue stays in container
In, the container known to another dry mass filters the solution poured out；(2) with synthermal acetone by staying in step (1)
Residue in container is washed into container known to dry mass before, then dries, is cooling and weigh, calculating as a result and
It indicates to provide to execute by GB/T 2910.1.
More preferably, the container in the step (1) is tool plug conical flask or other can obtain the instrument of identical result.
More preferably, container known to the dry mass in the step (1) is glass sand core crucible or other can obtain phase
With the instrument of result.
More preferably, before the baking process of the step (2), container known to the dry mass of residue will also be filled
Being air-dried on 20 ~ 30MIN or sample in ventilation device can't smell peculiar smell, this operation can be by the acetone on residue
Taste volatilization, very heavy taste is had because directly being dried, in baking oven.
The beneficial effects of the present invention are:
The present invention dexterously according to it is qualitative when fiber add the state of nitric acid, to be directed to the fiber of different shape performance with different molten
Reagent and dissolution conditions are solved, the neoteric acetone method of instant bulging state, breaking morphology cyclohexanone method, flexibility is high, especially
It has the advantages that
1. saving human resources, every part of sample test period saves general 1H, improves staff efficiency and houses market competitiveness；
2. improving the safety of tester, guarantee employee's health of human body；
3. sample segment replaces cyclohexanone solvent with acetone solvent, when reducing waste liquid storage due to leakage caused by environment it is dirty
Dye.
Detailed description of the invention
The present invention is described in detail by following specific embodiments and drawings for ease of explanation,.
Fig. 1 is flow diagram of the invention；
Fig. 2 is state diagram of the modified acrylic fibre before nitron is added dropwise；
Fig. 3 is the state that modified acrylic fibre modified acrylic fibre after nitron is added dropwise becomes solvent swelling state
Figure.
Specific embodiment
By taking the blended sample of modified acrylic fibre and polyacrylonitrile fibre as an example:
As shown in Figure 1, a kind of improved modified acrylic fibre qualitative and quantitative analysis method, successively walks comprising following technique
It is rapid: qualitative → sampling → drying weighing → dissolution → drying weighing → calculating, in the qualitative step, comprising into fiber plus
Enter the process of nitric acid, in this process, after nitric acid is added, if it is determined that the form of fiber is breaking morphology, then subsequent molten
It is dissolved using cyclohexanone as solvent in solution step, if it is determined that the form of fiber is swelling form, then in subsequent dissolution
It is dissolved using acetone as solvent in step.
As needed, between qualitative → sampling, it is additionally provided with pretreatment process.
The detailed process of the qualitative step is: qualitative step is executed according to FZ/T 01057.3-2007, by appropriate fiber
It is evenly laid out on glass slide, in addition a drop transparent medium covered, pays attention to that bubble cannot be brought into, is placed on biomicroscope
Objective table on, under the conditions of 100 times~500 times of amplification factor observe fiber vertical face and cross section shapes, control fiber
Standard photographs and morphologic description identify the classification of unknown fiber.
It is comprised the concrete steps that: (1) sample being put into container, according to every gram of sample as what solvent was dissolved using acetone
The acetone of 100ML~200ML is added, prevents incomplete dissolution data inaccuracy, shakes container and be impregnated with sample, at 50 DEG C ± 5 DEG C
30MIN is continuously shaken in water-bath, why selects temperature, firstly because modified acrylic fibre can be complete at a temperature of this
Dissolution does not need heating, drop secondly in view of all laboratory work times have always 50 DEG C ± 5 DEG C of shaking bath
Temperature saves the time；The selection of time is also to use for reference the common testing time in GB/T 2910-2009 standard, is primarily due to
30min can be completely dissolved modified polypropylene fiber；Then solution is fallen off, residue stays in a reservoir, with another drying
Container known to quality filters the solution poured out；(2) with synthermal acetone by the residue stayed in a reservoir in step (1)
It washes into container known to dry mass before, then dries, cools down and weigh, GB/T is pressed in calculating and expression as a result
2910.1 regulation executes.
Container in the step (1) is tool plug conical flask or other can obtain the instrument of identical result.
Container known to dry mass in the step (1) is glass sand core crucible or other can obtain identical result
Instrument.
Before the baking process of the step (2), it will also fill container known to the dry mass of residue and divulging information
Device apoplexy dry-air blast, which is done, can't smell peculiar smell on 20 ~ 30MIN or sample, this operation can be by the acetone taste on residue
Road volatilization, very heavy taste is had because directly being dried, in baking oven.
Fig. 2 is state diagram of the modified acrylic fibre before nitron is added dropwise；Fig. 3 is modified acrylic fibre
Modified acrylic fibre becomes the state diagram of solvent swelling state after nitron is added dropwise.
The present invention dexterously according to it is qualitative when fiber add the state of nitric acid, to be directed to the fiber difference of different shape performance
Solubilising reagent and dissolution conditions, the neoteric acetone method of instant bulging state, breaking morphology cyclohexanone method, flexibility
Height especially has the advantages that
1. saving human resources, every part of sample test period saves general 1H, improves staff efficiency and houses market competitiveness；
2. improving the safety of tester, guarantee employee's health of human body；
3. sample segment replaces cyclohexanone solvent with acetone solvent, when reducing waste liquid storage due to leakage caused by environment it is dirty
Dye.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
The change or replacement expected without creative work, should be covered by the protection scope of the present invention.Therefore, of the invention
Protection scope should be determined by the scope of protection defined in the claims.
Claims (6)
1. a kind of improved modified acrylic fibre qualitative and quantitative analysis method, which is characterized in that successively include following technique
Step: qualitative → sampling → drying weighing → dissolution → drying weighing → calculating, in the qualitative step, comprising into fiber
The process of nitric acid is added, in this process, after nitric acid is added, if it is determined that the form of fiber is breaking morphology, then subsequent
It is dissolved using cyclohexanone as solvent in dissolving step, if it is determined that the form of fiber is swelling form, then subsequent molten
It is dissolved using acetone as solvent in solution step.
2. improved modified acrylic fibre qualitative and quantitative analysis method according to claim 1, which is characterized in that
It is comprised the concrete steps that using acetone as what solvent was dissolved: (1) sample being put into container, is added according to every gram of sample
The acetone of 100ML~200ML prevents incomplete dissolution data inaccuracy, shakes container and be impregnated with sample, in 50 DEG C of ± 5 DEG C of water-baths
In continuously shake 30MIN ± 5MIN；Then solution is fallen off, residue stays in a reservoir, known to another dry mass
Container filters the solution poured out；(2) residue stayed in a reservoir in step (1) is washed into before with synthermal acetone
It in container known to dry mass, then dries, cool down and weigh, calculating and expression as a result is held by the regulation of GB/T 2910.1
Row.
3. improved modified acrylic fibre qualitative and quantitative analysis method according to claim 2, which is characterized in that
Container in the step (1) is tool plug conical flask or other can obtain the instrument of identical result.
4. improved modified acrylic fibre qualitative and quantitative analysis method according to claim 2, which is characterized in that
Container known to dry mass in the step (1) is glass sand core crucible or other can obtain the instrument of identical result.
5. improved modified acrylic fibre qualitative and quantitative analysis method according to claim 2, which is characterized in that
Before the baking process of the step (2), container known to the dry mass of residue will be also filled in ventilation device apoplexy
It can't smell peculiar smell on dry 20 ~ 30MIN or sample.
6. improved modified acrylic fibre qualitative and quantitative analysis method according to claim 1, which is characterized in that
As needed, between qualitative → sampling, it is additionally provided with pretreatment process.
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Cited By (1)
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| CN113340764A (en) * | 2021-06-15 | 2021-09-03 | 中国林业科学研究院林产化学工业研究所 | Method for analyzing fiber fraction and fiber bundle content of plant fibers |
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