CN111521612A - Quantitative analysis method for fiber content in lyocell fiber blended product - Google Patents

Quantitative analysis method for fiber content in lyocell fiber blended product Download PDF

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CN111521612A
CN111521612A CN202010564594.4A CN202010564594A CN111521612A CN 111521612 A CN111521612 A CN 111521612A CN 202010564594 A CN202010564594 A CN 202010564594A CN 111521612 A CN111521612 A CN 111521612A
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lyocell
sample
fiber
fibers
content
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CN111521612B (en
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袁裕禄
刘艳
钱蕾
顾昊
王惠珍
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Jiangsu Chengxin Inspection Certification Co ltd
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JIANGSU JIANGYIN FIBRES TESTING INSTITUTE
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84—Systems specially adapted for particular applications
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84—Systems specially adapted for particular applications
    • G01N2021/8444—Fibrous material
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P90/00—Enabling technologies with a potential contribution to greenhouse gas [GHG] emissions mitigation
    • Y02P90/30—Computing systems specially adapted for manufacturing

Abstract

The invention discloses a quantitative analysis method for fiber content in a lyocell fiber blended product, which belongs to the field of quantitative analysis of fibers and has the technical scheme that yarns of fibers with circular sections are selected as reference substances, the lyocell fiber blended product is selected as a sample to be detected, the reference substances and the sample to be detected are mixed to prepare a mixed sample, the mixed sample is pretreated to prepare an observation sample piece, the diameters and the number of lyocell fibers in the reference substances and the lyocell fiber blended product are respectively measured by a microscope method, the mass proportion coefficient of the lyocell fibers and the reference substances in the mixed sample is obtained, and further the content proportion of the lyocell fibers and other fibers in the sample to be detected is obtained. The method can quickly and accurately analyze the content of each fiber component in the lyocell fiber blended product.

Description

Quantitative analysis method for fiber content in lyocell fiber blended product
Technical Field
The invention relates to a quantitative analysis method of fiber content, in particular to a quantitative analysis method of fiber content in a lyocell fiber blended product.
Background
The regenerated cellulose fiber takes natural cellulose as a raw material, has a structural composition similar to that of cotton, has better moisture absorption and air permeability than cotton fiber, and is the fiber with the best moisture absorption and air permeability in chemical fiber. Usually blended with cotton fiber, and the blended fabric has the advantages of softness, smoothness, good air permeability, wearing comfort, bright color, good color fastness and the like. Viscose, modal and lyocell fibres are widely used as three representative of regenerated cellulose fibres.
The current methods applied to the quantitative analysis of the blended product of natural cellulose fibers and regenerated cellulose fibers include chemical analysis methods and physical methods. The chemical analysis method relates to a sodium zincate method, a formic acid/zinc chloride method, a hydrochloric acid method, a sulfuric acid method, a mixed acid method and the like. The quantitative chemical analysis method applied to the natural cellulose fiber and regenerated cellulose fiber blended product has the following main problems in the actual test work: the volatility of the test result is large due to unstable d value of damage degree of natural cellulose fibers (cotton), incomplete dissolution of regenerated cellulose fibers, inconsistent influence degree of blended product dyeing on the dissolution performance and the like, and related research work mainly focuses on optimizing a dissolution scheme (concentration of a reagent, temperature, time and the like) and increasing stripping treatment on dark color samples.
Aiming at the problems of the quantitative chemical analysis method of the blended product of the natural cellulose fiber and the regenerated cellulose fiber, some detection mechanisms apply a microscope method in FZ/T01101-. The FZ/T01101 middle microscope method is to use microscope to distinguish various fibers, measure fiber diameter or sectional area, and combine the measured fiber number and density to calculate the fiber quality content and other indexes. Specifically, for a circular cross-section fiber, the fiber diameter was measured; for non-circular cross-section fibers, the fiber cross-sectional area was measured.
Cotton fiber, modal fiber and viscose fiber are non-circular fibers, so a mode of measuring the cross section of the fiber is generally adopted, the defects are that the measuring process is complicated, and the time consumption is long, so some detection mechanisms solve the problems by measuring the diameter of the fiber and converting the diameter of the fiber to obtain a fiber correction coefficient. In the actual detection process, due to the diversity and complexity of regenerated cellulose fiber samples, the difference of correction coefficients of modal and viscose of different brands and production enterprises is huge, and the error of a test result is easily caused to be larger.
Disclosure of Invention
Aiming at the defects of the prior art, the invention discloses a quantitative analysis method for the fiber content in a lyocell fiber blended product, which can quickly and accurately analyze the content of each fiber component in the lyocell fiber blended product.
The technical scheme adopted by the invention is as follows:
a quantitative analysis method for the fiber content in a lyocell fiber blended product comprises the following steps:
step S1: selecting yarns of fibers with circular cross sections as reference objects, selecting a lyocell fiber blended product as a sample to be tested, and mixing the reference objects and the sample to be tested to prepare a mixed sample;
step S2: slicing the mixed sample to prepare an observation sample piece, and respectively measuring the diameter and the number of the lyocell fibers in the reference object and the lyocell fiber blended product by using a microscope method;
step S3: and obtaining the mass proportion coefficient of the lyocell fibers and the reference substance in the mixed sample, and further obtaining the content proportion of the lyocell fibers and other fibers in the sample to be detected.
Further, the preparation of the mixed sample in step S1 includes the following steps:
step S1.1: weighing a reference object suitable for the weight of subsequent slices, and finishing the reference object into straight bunched yarns, so that the two ends of the yarns are flush, and the length of the bunched yarns is more than 10cm for later use;
step S1.2: keeping the length of the sample to be detected consistent with that of the reference object, weighing the sample to be detected according to the weight ratio of the reference object to the sample to be detected of 0.9: 1.9-1.1: 2.1, arranging the sample to be detected into a straight beam shape, and enabling two ends of the sample to be detected to be level for later use;
step S1.3: and (3) adjusting and aligning the reference object in the step (S1.1) and the sample to be detected at two ends, and uniformly mixing to obtain a mixed sample.
Further, the reference object in step S1 is a fiber having a circular cross section.
Further, the method for obtaining the content ratio of the lyocell fibers to other fibers in the step S3 includes the steps of:
step S3.1: the mass ratio coefficient of the lyocell fibers to the reference substance in the mixed sample was calculated according to the formula (1):
Figure BDA0002547212490000031
λreference substance of LyocellThe mass proportion coefficient of the lyocell fiber in the mixed sample and a reference substance is calculated;
nlyocellThe number of the lyocell fibers in the mixed sample was measured for counting;
d2 lyocellThe average of the squares of the diameters of the lyocell fibers in the mixed sample is given in units of square micrometers (μm)2)；
ρLyocellThe density of the lyocell fibers in the mixed sample is given in grams per cubic centimeter (g/cm)3)；
nReference objectMeasuring the number of reference substances in the mixed sample;
d2 reference objectThe mean value of the square of the diameter of the reference in the mixed sample is given in square micrometers (. mu.m)2)；
ρReference objectThe density of the reference in the mixed sample is given in grams per cubic centimeter (g/cm)3)；
Step S3.2: the mass percentages of the lyocell fibers and other fiber components in the mixed sample are calculated according to the formulas (2) and (3):
Plyocell＝λReference substance of Lyocell×PReference object(2)
POther Components＝100-PLyocell-PReference object(3)
PLyocellThe content (%) of lyocell fiber in the mixed sample;
Preference objectThe mass content (%) of the reference substance in the mixed sample;
Pother ComponentsMass content (%) of the other fiber components except for lyocell fiber and the reference in the mixed sample;
step S3.3: and (3) calculating according to the formulas (4) and (5) to obtain the mass content (%) of the lyocell fibers and other fiber components in the sample to be detected:
Figure BDA0002547212490000032
Pfinal other Components＝100-PFinal lyocell(5)
PFinal lyocellThe mass content (%) of the lyocell fiber in the sample to be tested;
Pfinal other ComponentsThe mass content (%) of the other fiber components except the lyocell fiber in the sample to be measured;
step S3.4: and if the difference of the two parallel test results is more than 3%, determining a third observation sample piece, and finally taking the average value of the three test results.
In conclusion, the invention has the following beneficial effects:
1. the invention selects a fiber with a circular section as a reference object, uniformly mixes the reference object and a sample to be tested to prepare a mixed sample, and then respectively calculates the content ratio of each component in the sample to be tested by combining a microscope testing method.
2. The testing method established by the invention has simple and convenient testing process, easy operation and less time consumption, and can reduce the testing error brought by the correction coefficient, thereby improving the accuracy of the testing result.
Drawings
FIG. 1 is a schematic flow diagram of the quantitative analysis method established in the present invention;
FIG. 2 is a schematic flow chart of the preparation of the mixed sample in the present invention.
Detailed Description
The following describes embodiments of the present invention with reference to the drawings.
FIG. 1 is a schematic flow chart of the quantitative analysis method of the present invention. As shown in fig. 1, a fiber having a circular cross section is selected as a reference material, and the reference material and a sample to be measured are uniformly mixed to prepare a mixed sample. The mixed sample was pretreated to prepare a sample observation piece, and the diameters and the number of the reference substance and lyocell fibers were measured by a microscope. And calculating to obtain the mass proportion coefficient of the lyocell fibers and the reference substance in the mixed sample, and further obtaining the content of each fiber in the sample to be detected.
In which like parts are designated by like reference numerals. It should be noted that the terms "front," "back," "left," "right," "upper" and "lower" used in the following description refer to directions in the drawings, and the terms "bottom" and "top," "inner" and "outer" refer to directions toward and away from, respectively, the geometric center of a particular component.
Example 1:
a quantitative analysis method for fiber content in a lyocell fiber blended product selects a sample 1, a sample 2 and a sample 3 as three to-be-detected samples blended by lyocell fibers with different proportions, wherein the to-be-detected samples are lyocell and cotton blended fibers, and then the fiber content in the three to-be-detected samples is respectively analyzed through the following steps, which comprise the following steps:
step S1: a yarn of a round-section fiber is selected as a reference substance, the solubility of the reference substance is different from that of lyocell fiber, the reference substance selected in the embodiment is polyester fiber, and a mixed sample is prepared according to the following steps:
step S1.1: selecting polyester fiber as a reference object, weighing the reference object suitable for the weight of subsequent slices, and finishing the reference object into straight bunched yarns, so that the two ends of the yarns are flush, the length of a sample to be detected is consistent with that of the reference object, the length of the bunched yarns is more than 10cm, and the moisture absorption balance is regulated according to the specification of CB/T6529 for later use;
step S1.2: keeping the length of the sample to be tested consistent with that of the reference object, weighing the sample to be tested according to the weight ratio of the reference object to the sample to be tested of 1:2, arranging the sample to be tested into a straight beam shape, enabling two ends of the sample to be tested to be flush, and humidifying according to the specification of CB/T6529 until moisture absorption is balanced for later use;
step S1.3: and (3) adjusting and aligning the reference object in the step (S1.1) and the sample to be detected at two ends, and uniformly mixing to obtain a mixed sample. The mixed sample yarn bundle was placed near one end into the jaw of a Hawski slicer. The cut end was cut off flush with scissors at a position near the other end, and then cut with a blade at a position close to the same side surface of the slicer. Reserving the yarn bundle, splitting, drying, weighing and converting into official moisture regain to obtain the mass content P of the reference substance fiber in the mixed sampleReference object(％)。
Step S2: and (3) slicing the mixed sample, cutting short fibers with the length of about 0.4mm from the slicer in the step S1.3, transferring the short fibers onto a cover glass, dripping liquid paraffin, and fully stirring and uniformly mixing. And the short fibers are uniformly spread to prepare an observation sample piece. The worker put the observation sample pieces on a microscope stage, measured the diameters and the numbers of the reference and lyocell fibers respectively by a microscope method, 200 fibers were measured for each fiber, the total number of fibers was 1500, and the measurement of two observation sample pieces was repeated.
As shown in Table 1, the test results of the lyocell fibers and the reference material measured in the first test were measured by microscopy by selecting polyester fibers as the reference material, wherein the density of the fibers was checked by the data table in appendix A of FZ/T01101-.
TABLE 1 test results of the first test
Figure BDA0002547212490000061
As shown in Table 2, in order to select the polyester fiber as a reference, the results of the tests of the lyocell fiber and the reference measured in the second test were measured by microscopy, wherein the density of the fiber was checked by the data table in appendix A of FZ/T01101-.
TABLE 2 test results of the second test
Figure BDA0002547212490000062
Step S3: the method comprises the following steps of obtaining a mass proportion coefficient of the lyocell fibers and a reference substance in the mixed sample, and finally obtaining the content proportion of the lyocell fibers and other fibers in the sample to be tested, wherein the method specifically comprises the following steps:
step S3.1: calculating mass proportion coefficients of the lyocell fibers and the reference substance in the mixed sample of the two tests according to the following formula (1);
Figure BDA0002547212490000063
step S3.2: then substituting the data obtained in the step S3.1 into the formulas (2) and (3), and calculating the mass proportion coefficient of the lyocell fibers and the reference substance in the mixed sample;
Plyocell＝λReference substance of Lyocell×PReference object(2)
POther Components＝100-PLyocell-PReference object(3)
Step S3.3: substituting the data in the step S3.2 into the formulas (4) and (5), and calculating to obtain the mass content of the lyocell fibers and the cotton fibers in the sample to be detected, wherein the difference 1 is the difference value between the mass content of the lyocell fibers calculated by adopting the quantitative analysis method and a theoretical value, and the difference 2 is the difference value between the mass content of the lyocell fibers measured by adopting a microscope method and the theoretical value, as shown in Table 3.
Figure BDA0002547212490000071
PFinal other Components＝100-PFinal lyocell(5)
TABLE 3 test results for the individual fiber components
Figure BDA0002547212490000072
As shown in Table 3, in order to select the polyester fiber as a reference, the results of two parallel tests were performed according to the steps S1 and S2. It can be seen that the difference between the mass content of the lyocell fibers measured by the method of the present invention and the theoretical value of the lyocell fibers is within the range of ± 2%, while the difference between the mass content of the lyocell fibers measured by the microscope method and the theoretical value exceeds the range of ± 5%, which indicates the accuracy of the quantitative analysis method established by the present invention, and the content of each fiber component in the lyocell fiber blended product can be rapidly analyzed on the basis of improving the accuracy.
Example 2:
the present embodiment is different from embodiment 1 in that: the test sample to be tested is a blend of lyocell and viscose, and the fiber content of the three samples to be tested is analyzed through the steps, so that the test result is as follows:
TABLE 4 test results of the first test
Figure BDA0002547212490000073
TABLE 5 test results of the second test
Figure BDA0002547212490000081
As shown in table 6, the results of content measurement of each fiber component in sample 1, sample 2 and sample 3, the difference 1 (/%) is the difference between the content of lyocell fiber calculated by the analysis method of the present invention and the theoretical value, and the difference 2 (/%) is the difference between the content of lyocell fiber measured by FZ/01101 microscopic diameter method and the theoretical value, and the data results of difference 1 and difference 2 are compared.
TABLE 6 test results for the individual fiber components
Figure BDA0002547212490000082
As can be seen from the data in Table 6, the difference between the mass content of the lyocell fibers measured by the test method of the present invention and the theoretical value was within. + -. 2%. The difference between the good quality content of the lyocell fibers measured by a microscope method and a theoretical value exceeds the range of +/-4 percent, and the difference 2 of the sample 2 reaches-8.2, which shows that the quantitative analysis method established by the invention can accurately measure the content of each fiber component in the lyocell fiber blended product.
The foregoing description is illustrative of the present invention and is not to be construed as limiting thereof, the scope of the invention being defined by the appended claims, which may be modified in any manner without departing from the basic structure thereof.

Claims (4)

1. A quantitative analysis method for the fiber content in a lyocell fiber blended product is characterized by comprising the following steps:
step S1: selecting yarns of fibers with circular cross sections as reference objects, selecting a lyocell fiber blended product as a sample to be tested, and mixing the reference objects and the sample to be tested to prepare a mixed sample;
step S2: slicing the mixed sample to prepare an observation sample piece, and respectively measuring the diameter and the number of the lyocell fibers in the reference object and the lyocell fiber blended product by using a microscope method;
step S3: and obtaining the mass proportion coefficient of the lyocell fibers and the reference substance in the mixed sample, and further obtaining the content proportion of the lyocell fibers and other fibers in the sample to be detected.
2. The method for quantitatively analyzing the fiber content in a lyocell fiber blended product according to claim 1, wherein: the preparation of the mixed sample in step S1 includes the steps of:
step S1.1: weighing a reference object suitable for the weight of subsequent slices, and finishing the reference object into straight bunched yarns, so that the two ends of the yarns are flush, and the length of the bunched yarns is more than 10cm for later use;
step S1.2: keeping the length of the sample to be detected consistent with that of the reference object, weighing the sample to be detected according to the weight ratio of the reference object to the sample to be detected of 0.9: 1.9-1.1: 2.1, arranging the sample to be detected into a straight beam shape, and enabling two ends of the sample to be detected to be level for later use;
step S1.3: and (3) adjusting and aligning the reference object in the step (S1.1) and the sample to be detected at two ends, and uniformly mixing to obtain a mixed sample.
3. The method for quantitatively analyzing the fiber content in a lyocell fiber blended product according to claim 1, wherein: the reference object in step S1 is a fiber having a circular cross section.
4. The method for quantitatively analyzing the fiber content in a lyocell fiber blended product according to claim 1, wherein: the method for obtaining the content ratio of the lyocell fibers to other fibers in the step S3 includes the steps of:
step S3.1: the mass ratio coefficient of the lyocell fibers to the reference substance in the mixed sample was calculated according to the formula (1):
Figure FDA0002547212480000011
λreference substance of LyocellThe mass proportion coefficient of the lyocell fiber in the mixed sample and a reference substance is calculated;
nlyocellThe number of the lyocell fibers in the mixed sample was measured for counting;
d2 lyocellThe average of the squares of the diameters of the lyocell fibers in the mixed sample is given in units of square micrometers (μm)2)；
ρLyocellThe density of the lyocell fibers in the mixed sample is given in grams per cubic centimeter (g/cm)3)；
nReference objectMeasuring the number of reference substances in the mixed sample;
d2 reference objectThe mean value of the square of the diameter of the reference in the mixed sample is given in square micrometers (. mu.m)2)；
ρReference objectThe density of the reference in the mixed sample is given in grams per cubic centimeter (g/cm)3)；
Step S3.2: the mass percentages of the lyocell fibers and other fiber components in the mixed sample are calculated according to the formulas (2) and (3):
Plyocell＝λReference substance of Lyocell×PReference object(2)
POther Components＝100-PLyocell-PReference object(3)
PLyocellThe content (%) of lyocell fiber in the mixed sample;
Preference objectThe mass content (%) of the reference substance in the mixed sample;
Pother ComponentsMass content (%) of the other fiber components except for lyocell fiber and the reference in the mixed sample;
step S3.3: and (3) calculating according to the formulas (4) and (5) to obtain the mass content (%) of the lyocell fibers and other fiber components in the sample to be detected:
Figure FDA0002547212480000021
Pfinal other Components＝100-PFinal lyocell(5)
PFinal lyocellThe mass content (%) of the lyocell fiber in the sample to be tested;
Pfinal other ComponentsThe mass content (%) of the other fiber components except the lyocell fiber in the sample to be measured;
step S3.4: and if the difference of the two parallel test results is more than 3%, determining a third observation sample piece, and finally taking the average value of the three test results.
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