CN102565113A - Method for measuring dimethylbenzene soluble matter content in polypropylene powder material - Google Patents
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Abstract
The invention provides a method for measuring dimethylbenzene soluble matter content in a polypropylene powder material. The method comprises the following steps of: constructing polypropylene powder material nuclear magnetic standard curves with different signs; taking the polypropylene powder material to be measured, and preparing a sample to be measured; testing the sample to be measured by adopting a nuclear magnetic resonance spectrometer, and obtaining a nuclear magnetic signal intensity value of the sample to be measured; searching the polypropylene powder material standard curve with the sign corresponding to the sign of the sample to be measured; and searching a dimethylbenzene soluble matter content value corresponding to the nuclear magnetic signal intensity value of the sample to be measured from the standard curve, and taking the dimethylbenzene soluble matter content value as the dimethylbenzene soluble matter content value in the polypropylene powder material. According to the measurement method, the pretreatment time of the sample is shortened; the method is easy to operate, is accurate in test result, has the characteristics of environment friendliness, high efficiency and energy conservation, and is suitable for application of middle-controlled analysis in industrial production of polypropylene powder materials.
Description
Technical field
The present invention relates to the analytical test technical field, the assay method of xylene soluble part in a kind of polypropylene powder.
Background technology
The classic method of measuring xylene soluble part content in the polypropylene all is that utilization GB chemical solvent method GB/T24282-2009 measures, its process comprise xylene preparation, carry out the experiments of measuring that blank assay is measured xylene impurity content and sample; When testing sample is tested, if needed, sample is carried out dried; Xylene soluble part Determination on content process comprises twice drying, a plurality of steps such as cool off, weigh before and after extraction and the extraction in the polypropylene, and by GB 2412-2009 regulation, the time that only extracts just reaches more than the 6h.Though adopt the novel extraction device can the extraction time be foreshortened to 1h, still need 6～7h total analysis time.And test used xylene and generally contain tangible evaporation residue and other impurity compositions; So, need do blank assay to the xylene solution of experiment usefulness for whether the used xylene of confirmatory experiment contains tangible evaporation residue and other impurity compositions.As receive the influence of complicated process control factor, and also need check again, consuming time longer, therefore, and chemical solvent method complicated operation, sense cycle is long, and the manpower and materials of labor are inappropriate for the middle control analysis of production run.
Summary of the invention
The present invention aims to provide xylene soluble part Determination on content method in a kind of polypropylene powder, and to solve prior art chemical solvent extraction complicated operation, sense cycle is long, problems such as the manpower and materials of labor.
To achieve these goals, according to an aspect of the present invention, xylene soluble part Determination on content method in a kind of polypropylene powder is provided, has may further comprise the steps: the nuclear magnetic signal typical curve of setting up the polypropylene powder of the different trades mark; Get polypropylene powder to be measured, test sample is treated in preparation; Adopt nuclear magnetic resonance spectrometer to treat test sample and test, obtain the nuclear magnetic signal intensity level of treating test sample; Search the nuclear magnetic signal typical curve of the polypropylene powder of the corresponding trade mark according to the trade mark of treating test sample; And the corresponding xylene soluble part content value of nuclear magnetic signal intensity level of from the nuclear magnetic signal typical curve, searching and treat test sample, as the xylene soluble part content value in the polypropylene powder.
Further, the typical curve of polypropylene powder obtains through following steps: A. gets the many parts of polypropylene powders with different xylene soluble part content of the same trade mark, preparation standard appearance; B. adopt nuclear magnetic resonance spectrometer that each standard sample is tested, obtain the nuclear magnetic signal intensity level of each standard sample, and set up typical curve according to xylene soluble part content value in each standard sample and nuclear magnetic signal intensity level; And C. repeating step A and B, set up the typical curve of various trade mark polypropylene powders.
Further, above-mentioned standard sample with treat that the preparation process of test sample comprises: polypropylene powder is dry in vacuum environment, be cooled to room temperature after the drying, form preparation appearance; Take by weighing the preparation appearance of 4.995～5.005g, constant temperature 25～35 minutes makes standard sample or treats test sample.
Further, polypropylene powder dry step in vacuum environment comprises: is that 0.1MPa, temperature are 123～127 ℃ of following dryings 55～65 minutes with polypropylene powder in vacuum tightness.
Further, the process of above-mentioned preparation appearance constant temperature comprises: will prepare appearance 39.5～40.5 ℃ of following constant temperature 28～32 minutes.
Further, above-mentioned steps B further comprises: a. sets up fundamental curve after adopting nmr spectrometer that 3-5 standard sample measured; B. adopt nmr spectrometer that the standard sample that is different among the step a is measured, according to xylene soluble part content value in the standard model that is different among the step a and nuclear magnetic signal intensity level adjustment fundamental curve; And c. repeating step b, till related coefficient＞0.95 of curve, obtain typical curve.
Further, need proofread and correct above-mentioned typical curve.
Further, above-mentioned correction may further comprise the steps: (1) is divided into two parts with polypropylene powder to be measured; (2) first parts through its xylene soluble part content value of chemical solvent method determination method measurement; (3) second part is handled, form standard sample, obtain the nuclear magnetic signal intensity level of this standard sample through nmr spectrometer; (4) according to the nuclear magnetic signal intensity level adjustment typical curve that records in xylene soluble part content value that obtains polypropylene powder to be measured in the step (2) and the step (3); And (5) get different polypropylene powders to be measured, and repeating step (1)-(4) are till related coefficient＞0.95 of typical curve.
Further, every to above-mentioned typical curve at a distance from once proofreading and correct 7-30 day.
The technique effect that the present invention reached is: the mensuration of carrying out xylene soluble part in the polypropylene with nmr spectrometer; Shortened time for sample pretreatment greatly; And it is easy and simple to handle; Test result is accurate, has environmental protection, efficient, energy-conservation, characteristic accurately, is applicable to that the middle control analysis in the polypropylene powder commercial production is used.
Except top described purpose, feature and advantage, the present invention also has other purpose, feature and advantage.To do further detailed explanation to the present invention with reference to embodiment below.
Description of drawings
Figure of description is used to provide further understanding of the present invention, constitutes a part of the present invention, and illustrative examples of the present invention and explanation thereof are used to explain the present invention, does not constitute improper qualification of the present invention.In the accompanying drawings:
Fig. 1 shows the canonical plotting according to embodiments of the invention 1.
Embodiment
To carry out detailed explanation to the technical scheme in the embodiments of the invention below, but following embodiment only is in order to understanding the present invention, and can not limits the present invention, the multitude of different ways that the present invention can be defined by the claims and cover is implemented.
Term among this paper " trade mark " is the classification name to different polypropylene powders, and this mode classification is accepted extensively and used by those skilled in the art.
In a kind of typical embodiment of the present invention, xylene soluble part Determination on content method in a kind of polypropylene powder may further comprise the steps: the nuclear magnetic signal typical curve of setting up the polypropylene powder of the different trades mark; Get polypropylene powder to be measured, test sample is treated in preparation; Adopt nuclear magnetic resonance spectrometer to treat test sample and test, obtain the nuclear magnetic signal intensity level of treating test sample; Search the nuclear magnetic signal typical curve of the polypropylene powder of the corresponding trade mark according to the trade mark of treating test sample; And the corresponding xylene soluble part content value of nuclear magnetic signal intensity level of from the nuclear magnetic signal typical curve, searching and treat test sample, as the xylene soluble part content value in the polypropylene powder.
The nmr spectrometer that in said method, is adopted is existing procucts, it has quick and precisely, easy and simple to handle, amount of samples is few and the advantage of environmental protection, is suitable for the mensuration of projects such as isotacticity, melting index, molecular weight.According to the character of nuclear magnetic resonance, adopt different stimulating frequencies, and signal sampled just can obtain different data.Therefore utilize the corresponding relation between NMR signal and the xylene extraction value, just can obtain the linear relationship curve of a y=a+bx, can accurately measure the content of the xylene soluble part in the polypropylene thus.
Carry out the mensuration of xylene soluble part in the polypropylene with nmr spectrometer; Shortened time for sample pretreatment greatly, and easy and simple to handle, and test result is accurate; Have environmental protection, efficient, energy-conservation, characteristic accurately, be applicable to that the middle control analysis in the polypropylene powder commercial production is used.
The typical curve of polypropylene powder obtains through following steps among the present invention: A. gets the many parts of polypropylene powders with different xylene soluble part content of the same trade mark, preparation standard appearance; B. adopt nuclear magnetic resonance spectrometer that each standard sample is tested, obtain the nuclear magnetic signal intensity level of each standard sample, and set up typical curve according to xylene soluble part content value in each standard sample and nuclear magnetic signal intensity level; And C. repeating step A and B, set up the typical curve of various trade mark polypropylene powders.
Use the polypropylene of xylene soluble part content value in the known polypropylene to prepare a large amount of standard models, and set up typical curve according to these standard models.For example adopt the polypropylene that obtains accurate xylene soluble part content value through the chemical solvent method.Adopt this mode to set up the accuracy that typical curve not only can promote the pairing numerical value of this typical curve, but also the flow process that can simplify the operation.In actual application; The performance of the polypropylene powder of the different trades mark is different; Therefore be directed against the polypropylene powder of the different trades mark; Need on nmr spectrometer, set up the typical curve of corresponding trade mark polypropylene powder, test getting final product under only need working document when xylene soluble part content is measured in to the polypropylene powder of this trade mark in corresponding standard curve.
Among the present invention standard sample with treat that the preparation process of test sample comprises: polypropylene powder is dry in vacuum environment, be cooled to room temperature after the drying, form preparation appearance; Take by weighing the preparation appearance of 4.995～5.005g, constant temperature 25～35 minutes makes standard sample or treats test sample.Dry polypropylene powder not only can make the moisture evaporation in the polypropylene powder but also can avoid powder oxidized test result that influences in dry run in vacuum environment; And; The preparation appearance that obtains after dry need be carried out constant temperature before test; So that the working temperature of sample temperature and nmr spectrometer adapts, so not only guaranteed precision of test result but also protected instrument not receive the influence of sample.
Preferably; Polypropylene powder is that 0.1MPa, temperature are 123～127 ℃ of following dryings 55～65 minutes in vacuum tightness among the present invention; Under this vacuum condition; Moisture in the polypropylene powder can volatilize fast, and control has promptly guaranteed that effect that powder can reach sufficiently dry avoided the easy problem of oxidation of polypropylene powder under the long hot conditions again drying time in 55～65 minutes.
Preferably, will prepare appearance among the present invention 39.5～40.5 ℃ of following constant temperature 28～32 minutes.The optimum working temperature of nmr spectrometer is 39.5～40.5 ℃, therefore, needs to treat that the temperature of test sample and the temperature of nmr spectrometer are consistent, and help guaranteeing the accuracy of testing result.
The step that the present invention sets up typical curve further comprises: a. sets up fundamental curve after adopting nmr spectrometer that 3-5 standard sample measured; B. adopt nmr spectrometer that the standard sample that is different among the step a is measured, according to xylene soluble part content value in the standard model that is different among the step a and nuclear magnetic signal intensity level adjustment fundamental curve; And c. repeating step b, till related coefficient＞0.95 of curve, obtain typical curve.The fundamental curve that is obtained by few sample can not be used for accurately measuring xylene soluble part content value in the polypropylene powder; Through a series of data of measuring of different samples are adjusted fundamental curve; Completion is just calculated in the foundation of typical curve when the related coefficient of fundamental curve＞0.95, serves as to be only accurately according to measuring the result who obtains with this typical curve.
The typical curve that the present invention sets up need be proofreaied and correct, and concrete aligning step is: (1) is divided into two parts with polypropylene powder to be measured; (2) first parts through its xylene soluble part content value of chemical solvent method determination method measurement; (3) second part is handled, form standard sample, obtain the nuclear magnetic signal intensity level of this standard sample through nmr spectrometer; (4) according to the nuclear magnetic signal intensity level adjustment typical curve that records in xylene soluble part content value that obtains polypropylene powder to be measured in the step (2) and the step (3); And (5) get different polypropylene powders to be measured, and repeating step (1)-(4) are till related coefficient＞0.95 of typical curve.
Because in the application of typical curve; The variation of nmr spectrometer environment of living in (such as the position of environment temperature, humidity, nmr spectrometer etc.) all can exert an influence to measuring the result; The result error that obtains when the mensuration result and the nuclear magnetic resonance spectrometer method of chemical solvent method is less than 0.1 the time, and typical curve need not proofreaied and correct and can directly measure polypropylene powder; The result error that obtains when the mensuration result and the nuclear magnetic resonance spectrometer method of chemical solvent method need be proofreaied and correct typical curve greater than 0.1 the time, proofreaies and correct and could measure xylene soluble part content in the polypropylene powder after accomplishing.The chemical solvent method is a kind of method of measuring xylene soluble part content in the polypropylene powder comparatively accurately; Therefore with the chemical solvent method typical curve is proofreaied and correct; The correctness of validation criteria curve guarantees to obtain comparatively accurately xylene soluble part content value in the polypropylene powder.
The present invention needs every at a distance from 7-30 day typical curve once being proofreaied and correct.Regularly typical curve is proofreaied and correct according to actual conditions, can accurately be determined the xylene soluble part content value of sample.
To combine the accompanying drawing in the embodiment of the invention below; Technical scheme in the embodiments of the invention is carried out detailed explanation; But following embodiment and accompanying drawing only are in order to understand the present invention; And can not limit the present invention, the multitude of different ways that the present invention can be defined by the claims and cover is implemented.
According to demand of practical production, embodiments of the invention have only been set up the typical curve of L5E89 powder, and the polypropylene powder of this trade mark is carried out the xylene soluble part Determination on content.
Nmr spectrometer model: MARAN-23 type;
Instrument is formed: permanent magnet (23MHz); Sample probe (diameter 26mm); Super MARAN electronic unit; Thermostat (0.1 ℃ of temperature-controlled precision); Workstation.Wherein super MARAN electronic unit comprises pulse producer, frequency generator, radio frequency amplifier, prime amplifier, radio frequency receiver, digital sample.
Use preparation: vacuum drying oven; Multifunction constant temperature case model: MH-2800A; Analytical balance: reading accuracy 0.1mg; Sample hose: Φ 26mm (sample-loading amount 21ml).
The drafting of typical curve:
1) polypropylene powder that to choose seven trades mark be L5E89 is a standard model; This trade mark is the name of group of Shenhua; And accepted extensively by those skilled in the art, these seven standard models are the samples with different xylene soluble part content that measure through the chemical solvent method;
2) utilizing nmr spectrometer sample to be carried out pre-treatment before measuring, be 0.1MPa in vacuum tightness with seven samples; Temperature is in 125 ℃ the vacuum drying oven dry 60 minutes; Then sample is taken out, put into the glass exsiccator and be cooled to room temperature, form seven preparation appearance; Take by weighing the preparation appearance of different quality, constant temperature obtained standard specimen 1, standard specimen 2, standard specimen 3...... standard specimen 6, standard specimen 7 in 30 minutes in 39.7 degrees centigrade thermostat.The quality of seven standard models and see table 1 through the xylene soluble part content value that the chemical solvent method is measured;
3) on nmr spectrometer, standard model is tested; " working curve rules " according to nmr spectrometer operate; After standard specimen 1, standard specimen 2 and standard specimen 3 test completion, obtain three different nuclear magnetic signal intensity levels; With this nuclear magnetic signal intensity level is ordinate, and the xylene soluble part content value is that horizontal ordinate is set up fundamental curve;
4) successively standard specimen is tested, after accomplishing to standard specimen 7 tests, the related coefficient of fundamental curve reaches 0.96, and typical curve is set up and accomplished, and stops the test to standard model.The nuclear magnetic signal intensity level of standard specimen 1 to standard specimen 7 is seen table 1.
Table 1
| Quality (g) | The xylene soluble part content value | The nuclear magnetic signal intensity level | |
| Standard specimen 1 | ?5.02 | 1.18 | 395.48 |
| Standard specimen 2 | ?5.05 | 1.47 | 425.72 |
| Standard specimen 3 | ?5.02 | 1.81 | 469.71 |
| Standard specimen 4 | ?5.01 | 2.45 | 518.85 |
| Standard specimen 5 | ?5.01 | 2.49 | 546.09 |
| Standard specimen 6 | ?5.02 | 2.61 | 523.35 |
| Standard specimen 7 | ?5.01 | 2.98 | 538.65 |
With xylene content value in the table 1 is horizontal ordinate x; The nuclear magnetic signal intensity level that measures is set up typical curve y=ax+b for ordinate y; The slope a=85.97 of typical curve, b=304.16 utilizes this typical curve to calculate the xylene soluble part content value of testing sample through nmr spectrometer.
Embodiment 1
Polypropylene powder raw material to be measured: L5E89 powder 1,4.998g;
Test sample is treated in preparation: with L5E89 powder 1, the vacuum drying oven of putting into vacuum tightness and be 0.1MPa, temperature and be 125 ℃ kept vacuum 60 minutes; Then sample is taken out, put into the glass exsiccator and cool off, extremely near room temperature; Take by weighing the sample that quality is 4.998g, put into the formation in 30 minutes of thermostat constant temperature and treat test sample 1.Utilize nmr spectrometer to treat test sample 1 and test, to this sample horizontal survey five times, the mean value of five measurement results is seen table 2 and table 3.
Embodiment 2
Polypropylene powder raw material to be measured: L5E89 powder 2., 5.000g;
Test sample is treated in preparation: with L5E89 powder 2, putting into vacuum tightness is that 0.1MPa, temperature are 123 ℃ vacuum drying oven, keeps vacuum 65 minutes; Then sample is taken out, put into the glass exsiccator and cool off, extremely near room temperature.Weighing sample 5.000g puts into the formation in 32 minutes of thermostat constant temperature and treats test sample 2.Utilize nmr spectrometer to treat test sample 2 and test, to this sample horizontal survey five times, the mean value of five measurement results is seen table 3.
Embodiment 3
Polypropylene powder raw material to be measured: L5E89 powder 3,5.005g;
Test sample is treated in preparation: with L5E89 powder 3, putting into vacuum tightness is that 0.1MPa, temperature are 127 ℃ vacuum drying oven, keeps vacuum 55 minutes; Then sample is taken out, put into the glass exsiccator and cool off, extremely near room temperature.Weighing sample 5.005g puts into the formation in 28 minutes of thermostat constant temperature and treats test sample 3.Utilize nmr spectrometer to treat test sample 3 and test, to this sample horizontal survey five times, the mean value of five measurement results is seen table 3.
Comparative Examples 1
Polypropylene powder raw material to be measured: with embodiment 1;
Utilize GB/T 24282-2009 chemical solvent method to measure xylene soluble part content in the polypropylene:
Getting L5E89 powder 1 drying is 70 ℃ dry 20 minutes of vacuum drying chamber at pressure less than the 13.3kp temperature, the dried sample of weighing 2.0g then, logical nitrogen protection; In 180 ℃ of refluxed 30 minutes with sample dissolution in xylene, cooling is 15 minutes under the state of nature, the mixed liquor that will be dissolved in xylene is then put into the water-bath constant temperature of 25 ℃ of constant temperature; After 30 minutes this mixed solution is filtered, get transparent filtrating, draw 100ml filtrating and put into the aluminium box; In 140-150 ℃ of evaporation process 30 minutes once more, behind the evaporate to dryness of waiting to filtrate, put into the logical nitrogen oven dry of vacuum drying oven 1 hour; Weigh after taking out the room temperature cooling, do four parallel appearance simultaneously.
Xylene solution to experiment usefulness is done blank assay: in xylene, add antioxidant 1010; Stirring makes antioxidant be dissolved in the xylene fully; With transfer pipet 200mL xylene is pipetted in the 250mL volumetric flask; Be poured in the funnel, splash in the 250mL volumetric flask, all be collected up to all solution through filter paper; The aluminium dish is put in the baking oven, 200 ℃ dry 30 minutes down, in exsiccator, be cooled to room temperature, after the constant weight with its quality of analytical balance weighing; Pipette 100mL filtrating to load weighted aluminium dish with transfer pipet.It is on 145 ℃ of controllable temperature heating plates that the aluminium dish is put into temperature, slowly is being heated to the approaching drying of residue in the aluminium dish under the nitrogen protection; It is in 100 ℃ of vacuum drying chambers 1 hour that the aluminium dish is put into temperature.Take out the aluminium dish in exsiccator with aluminium dish cool to room temperature, and weigh promptly to get and test with xylene evaporation residue and other impurity quality.
Deduct the measured value that result that experiment obtains with xylene evaporation residue and other impurity contents is this Comparative Examples 1 with xylene soluble part content in the L5E89 powder 1 that experiment is recorded, measurement result is seen table 2 and table 3.
Comparative Examples 2
Polypropylene powder raw material to be measured: with embodiment 2;
Measuring method: with Comparative Examples 1, measurement result is seen table 3.
Comparative Examples 3
Polypropylene powder raw material to be measured: with embodiment 3;
Measuring method: with Comparative Examples 1, measurement result is seen table 3.
Table 2
Table 3
Table 2 is the mensuration result of embodiment 1 and Comparative Examples 1.Measure the result in the comparison sheet 2, the data that embodiment 1 obtains with the nuclear magnetic resonance spectrometer method are all measured with the chemical solvent method about the mean value of moral data in Comparative Examples and are fluctuateed, and both mean value relative errors (2.17%) are less.
Table 3 is that embodiment and Comparative Examples are measured correlation data as a result, and the relative error of three groups of embodiment explains that all less than 3% to obtain data accuracy with nuclear magnetic resonance spectrometer higher in the table 3.
From above description; Can find out; The above embodiments of the present invention have realized following technique effect: utilize assay method of the present invention to shorten time for sample pretreatment greatly, and also easy and simple to handle, test result is accurate; Have environmental protection, efficient, energy-conservation, characteristic accurately, be applicable to that the middle control analysis in the polypropylene powder commercial production is used.
The above is merely the preferred embodiments of the present invention, is not limited to the present invention, and for a person skilled in the art, the present invention can have various changes and variation.All within spirit of the present invention and principle, any modification of being done, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. xylene soluble part Determination on content method in the polypropylene powder is characterized in that, may further comprise the steps:
Set up the nuclear magnetic signal typical curve of the polypropylene powder of the different trades mark;
Get polypropylene powder to be measured, test sample is treated in preparation;
Adopt nuclear magnetic resonance spectrometer that the said test sample of treating is tested, obtain the said nuclear magnetic signal intensity level of treating test sample;
Search the said polypropylene powder nuclear magnetic signal typical curve of the corresponding trade mark according to the said trade mark of test sample of treating; And
From said nuclear magnetic signal typical curve, search and the said corresponding xylene soluble part content value of nuclear magnetic signal intensity level of treating test sample, as the xylene soluble part content value in the said polypropylene powder to be measured.
2. assay method according to claim 1 is characterized in that, the typical curve of said polypropylene powder obtains through following steps:
A. get many parts of polypropylene powders of the same trade mark, preparation standard appearance with different xylene soluble part content;
B. adopt nuclear magnetic resonance spectrometer that each said standard sample is tested, obtain the nuclear magnetic signal intensity level of each said standard sample, and set up typical curve according to xylene soluble part content value in each said standard sample and said nuclear magnetic signal intensity level; And
C. repeating step A and B set up the said typical curve of various trade mark polypropylene powders.
3. assay method according to claim 2 is characterized in that, said standard sample and the said preparation process of test sample of treating comprise:
Polypropylene powder is dry in vacuum environment, be cooled to room temperature after the drying, form preparation appearance;
Take by weighing the said preparation appearance of 4.995～5.005g, constant temperature 25～35 minutes makes said standard sample or the said test sample of treating.
4. assay method according to claim 3 is characterized in that, said polypropylene powder dry step in vacuum environment comprises:
Is that 0.1MPa, temperature are 123～127 ℃ of following dryings 55～65 minutes with said polypropylene powder in vacuum tightness.
5. assay method according to claim 3 is characterized in that, the process of said preparation appearance constant temperature comprises:
With said preparation appearance 39.5～40.5 ℃ of following constant temperature 28～32 minutes.
6. assay method according to claim 2 is characterized in that, said step B further comprises:
A. after adopting nmr spectrometer that 3-5 said standard sample measured, set up fundamental curve;
B. adopt nmr spectrometer that the standard sample that is different among the step a is measured, adjust said fundamental curve according to xylene soluble part content value in the said standard model that is different among the step a and said nuclear magnetic signal intensity level; And
C. repeating said steps b till related coefficient＞0.95 of said fundamental curve, obtains said typical curve.
7. assay method according to claim 1 is characterized in that, typical curve is proofreaied and correct said typical curve after setting up.
8. assay method according to claim 7 is characterized in that, said correction may further comprise the steps:
(1), is divided into two parts with polypropylene powder to be measured;
(2) first parts through its xylene soluble part content value of chemical solvent method determination method measurement;
(3) second part is handled, form standard sample, obtain the nuclear magnetic signal intensity level of this standard sample through nmr spectrometer;
(4) adjust said typical curve according to the nuclear magnetic signal intensity level that records in xylene soluble part content value that obtains said polypropylene powder to be measured in the said step (2) and the said step (3); And
(5) get different polypropylene powders to be measured, repeating said steps (1)-(4) are till related coefficient＞0.95 of said typical curve.
9. assay method according to claim 7 is characterized in that, and is every at a distance from once proofreading and correct 7-30 day to said typical curve.
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| CN111595885A (en) * | 2019-04-22 | 2020-08-28 | 苏州纽迈分析仪器股份有限公司 | Calibration standard sample for testing fluorine content and sealing method and application thereof |
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| CN104655805A (en) * | 2015-02-13 | 2015-05-27 | 云南中烟再造烟叶有限责任公司 | Method for rapidly measuring content of hot water soluble matter in paper-making reconstituted tobacco production |
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| CN106248711B (en) * | 2015-06-10 | 2018-03-09 | 中国石油天然气股份有限公司 | The assay method of normal heptane the extractives content in polypropylene |
| CN107389719A (en) * | 2017-06-08 | 2017-11-24 | 内蒙古中煤蒙大新能源化工有限公司 | Xylene soluble content method for measuring in a kind of polypropylene powder |
| CN111595885A (en) * | 2019-04-22 | 2020-08-28 | 苏州纽迈分析仪器股份有限公司 | Calibration standard sample for testing fluorine content and sealing method and application thereof |
| CN110927196A (en) * | 2019-12-10 | 2020-03-27 | 南京曙光精细化工有限公司 | Method for evaluating relative content of silane coupling agent polymer |
| CN110927196B (en) * | 2019-12-10 | 2023-05-23 | 南京曙光精细化工有限公司 | Method for evaluating relative content of silane coupling agent polymer |
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