CN111521612B - 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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CN111521612B
CN111521612B CN202010564594.4A CN202010564594A CN111521612B CN 111521612 B CN111521612 B CN 111521612B CN 202010564594 A CN202010564594 A CN 202010564594A CN 111521612 B CN111521612 B CN 111521612B
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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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    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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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 with round cross sections are selected as reference substances, the lyocell fiber blended product is selected as a sample to be tested, the reference substances and the sample to be tested are mixed to prepare a mixed sample, the mixed sample is subjected to pretreatment to prepare an observation sample piece, the diameter and the number of the 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 then the content proportion of the lyocell fibers and other fibers in the sample to be tested is obtained. The invention can rapidly 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 raw material, has similar structural composition as cotton, has better hygroscopicity and air permeability than cotton fiber, and is the fiber with the best hygroscopicity and air permeability in chemical fiber. The cotton fiber blended fabric has the advantages of softness, smoothness, good air permeability, comfort in wearing, bright color, good color fastness and the like. As three typical representatives of regenerated cellulose fibers, viscose fibers, modal fibers and lyocell fibers are widely used.
Current methods applied to quantitative analysis of natural cellulose fiber and regenerated cellulose fiber blended products include chemical analysis 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 actual test work: the instability of the d value of the damage degree of the natural cellulose fiber (cotton), incomplete dissolution of the regenerated cellulose fiber, inconsistent influence degree of dyeing of a blended product on the dissolution performance and the like, so that the fluctuation of a test result is larger, and related research work mainly focuses on optimizing a dissolution scheme (reagent concentration, temperature, time and the like), adding stripping treatment to a dark color sample and the like.
Aiming at the problems of quantitative chemical analysis methods of natural cellulose fiber and regenerated cellulose fiber blended products, some detection mechanisms apply a microscope method in FZ/T01101-2008 'physical method for measuring fiber content', so as to solve the quantitative analysis problems of cotton and regenerated cellulose fiber. The microscopy in FZ/T01101 is to distinguish various fibers by using a microscope, measure the diameter or the sectional area of the fibers, and respectively calculate indexes such as the mass content of the fibers by combining the number and the density of the various fibers. 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 fiber, so that a mode of measuring the cross section area of the fiber is generally adopted, and the defect that the measuring process is complicated and the time is long is overcome, so that some detecting mechanisms convert the fiber diameter to obtain the fiber correction coefficient by measuring the fiber diameter. In the actual detection process, due to the diversity and complexity of regenerated cellulose fiber samples, the correction coefficients of Modal and viscose of different brands and production enterprises are huge in difference, and the error of a test result is easy to be larger.
Disclosure of Invention
Aiming at the defects of the prior art, the invention discloses a quantitative analysis method for fiber content in a lyocell fiber blended product, which can rapidly 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 fiber content in a lyocell fiber blend product, comprising the following steps:
step S1: selecting yarns of fibers with circular cross sections as reference objects, selecting lyocell fiber blended products as samples to be tested, and mixing the reference objects and the samples to be tested to prepare mixed samples;
step S2: slicing the mixed sample to prepare an observation sample slice, and respectively measuring the diameters and the numbers of the lyocell fibers in the reference object and the lyocell fiber blended product by using a microscopic method;
step S3: obtaining the mass ratio coefficient of the lyocell fiber and the reference in the mixed sample, and further obtaining the content ratio of the lyocell fiber and other fibers in the sample to be detected.
Further, 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 the subsequent slice, and finishing the reference object into a straight beam-shaped yarn, so that the two ends of the yarn are level, and the length of the beam-shaped yarn is more than 10cm for standby;
step S1.2: the length of the sample to be measured is kept consistent with the length of the reference object, the sample to be measured is weighed according to the weight ratio of the reference object to the sample to be measured of 0.9:1.9-1.1:2.1, the sample to be measured is arranged into a straight beam shape, and two ends of the sample to be measured are flush for standby;
step S1.3: and (3) adjusting and aligning the two ends of the reference object and the sample to be tested in the step S1.1 and the step S1.2, 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 fiber to other fibers in the step S3 comprises the following steps:
step S3.1: calculating mass ratio coefficients of the lyocell fiber and the reference in the mixed sample according to a formula (1):
Figure BDA0002547212490000031
λ lyocell reference The mass ratio coefficient of the lyocell fiber in the mixed sample and the reference is as follows;
n lyocell Measuring the number of lyocell fibers in the mixed sample;
d 2 richcelEr The average value of the square of the diameter of lyocell fibers in a mixed sample is expressed in square micrometers (μm) 2 )；
ρ Lyocell To mix the density of lyocell fibers in a sample, the unit is grams per cubic centimeter (g/cm) 3 )；
n Reference object Measuring the number of reference objects in the mixed sample;
d 2 reference object The mean value of the square of the diameter of the reference in the mixed sample is expressed in square micrometers (μm) 2 )；
ρ Reference object To mix the density of the reference in the sample, the unit is grams per cubic centimeter (g/cm) 3 )；
Step S3.2: calculating according to formulas (2) and (3) to obtain the mass percentage of the lyocell fiber and other fiber components in the mixed sample:
P lyocell ＝λ Lyocell reference ×P Reference object (2)
P Other components ＝100-P Lyocell -P Reference object (3)
P Lyocell The mass content (%) of the lyocell fiber in the mixed sample;
P reference object The mass content (%) of the reference in the mixed sample;
P other components For mixing the mass content (%) of the fiber components other than the lyocell fiber and the reference in the sample;
step S3.3: calculating according to formulas (4) and (5) to obtain the mass content (%) of the lyocell fibers and other fiber components in the sample to be tested:
Figure BDA0002547212490000032
P final other Components ＝100-P Final lyocell (5)
P Final lyocell The mass content (%) of the lyocell fiber in the sample to be detected;
P final other Components The mass content (%) of other fiber components except the lyocell fiber in the sample to be detected;
step S3.4: and the final test result of the sample to be tested is the arithmetic average value of the two parallel test results, if the difference of the two parallel test results is more than 3%, a third observation sample piece is measured, and finally, the average value of the three test results is taken.
In summary, 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 proportion of each component in the sample to be tested by combining a microscope test method.
2. The test method established by the invention has the advantages of simple and convenient test process, easy operation and less time consumption, and can reduce test errors caused by correction coefficients, thereby improving the accuracy of test results.
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FIG. 1 is a schematic flow chart of a quantitative analysis method established by the invention;
FIG. 2 is a schematic flow chart of the preparation of a mixed sample according to the present invention.
Detailed Description
The following describes specific embodiments of the present invention with reference to the drawings.
FIG. 1 is a flow chart of the quantitative analysis method of the present invention. As shown in fig. 1, first, a fiber having a circular cross section is selected as a reference, and the reference and a sample to be measured are uniformly mixed to prepare a mixed sample. The mixed sample was subjected to pretreatment to prepare a sample observation piece, and the diameters and the number of the reference substance and the lyocell fibers were measured by a microscope method. And calculating the mass ratio coefficient of the lyocell fibers and the reference in the mixed sample, and further obtaining the content of each fiber in the sample to be detected.
Wherein like parts are designated by like reference numerals. It should be noted that the words "front", "back", "left", "right", "upper" and "lower" used in the following description refer to directions in the drawings, and the words "bottom" and "top", "inner" and "outer" refer to directions toward or 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 three samples 1, 2 and 3 to be tested for the lyocell fiber blending with different proportions, wherein the samples to be tested are fibers blended by lyocell and cotton, and then the fiber content in the three samples to be tested is analyzed through the following steps:
step S1: the yarn of a circular cross-section fiber is selected as a reference, and the solubility of the reference is different from that of the lyocell fiber, and the reference 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 the subsequent slice, and finishing the reference object into straight bunchy yarns, so that the two ends of the yarns are level, the length of a sample to be tested is consistent with that of the reference object, the length of the bunchy yarns is more than 10cm, and the bunchy yarns are subjected to humidity adjustment according to the regulations of CB/T6529 to be in moisture absorption balance for later use;
step S1.2: keeping the length of the to-be-measured sample consistent with the length of the reference object, weighing the to-be-measured sample according to the weight ratio of the reference object to the to-be-measured sample of 1:2, arranging the to-be-measured sample into a straight beam shape, enabling two ends of the to-be-measured sample to be level, and regulating humidity to be in moisture absorption balance according to the regulations of CB/T6529 for later use;
step S1.3: and (3) adjusting and aligning the two ends of the reference object and the sample to be tested in the step S1.1 and the step S1.2, and uniformly mixing to obtain a mixed sample. The mixed sample yarn bundle was placed into the hawk slicer jaw near one end. The sheared ends are trimmed flush with scissors near the other end, discarded, and then cut with a blade at a position that is flush with the same side surface of the slicer. The yarn bundle is reserved, and the mass content P of the reference object fiber in the mixed sample is obtained by splitting, drying, weighing and folding the official moisture regain Reference object (％)。
Step S2: the mixed sample is sliced, short fibers with the length of about 0.4mm are cut from a slicer in the step S1.3, the short fibers are transferred to a cover glass, liquid paraffin is dripped, and the mixture is fully stirred and uniformly mixed. And the short fibers are uniformly spread to prepare an observation sample piece. The worker put the observation sample on a microscope stage, measured the diameter and the number of the reference and lyocell fibers, respectively, using a microscope method, measured 200 fibers each, counted the total number of fibers 1500, and repeatedly measured two observation sample pieces.
As shown in table 1, polyester fibers were selected as a reference, and the results of the first test of lyocell fibers and the reference were measured by a microscopic method, wherein the density of the fibers was checked by the data table in annex a of FZ/T01101-2008.
TABLE 1 test results of the first test
Figure BDA0002547212490000061
As shown in table 2, to select polyester fiber as a reference, the results of the test of lyocell fiber and the reference, measured in the second test, were measured by a microscopic method, wherein the density of the fiber was checked by the data table in annex a of FZ/T01101-2008.
TABLE 2 test results of the second test
Figure BDA0002547212490000062
Step S3: obtaining the mass ratio coefficient of the lyocell fiber and the reference in the mixed sample, and finally obtaining the content ratio of the lyocell fiber and other fibers in the sample to be detected, wherein the method specifically comprises the following steps:
step S3.1: calculating mass ratio coefficients of the lyocell fiber and the reference in the mixed sample of the two tests according to the following formula (1);
Figure BDA0002547212490000063
step S3.2: substituting the data obtained in the step S3.1 into the formulas (2) and (3), and calculating the mass ratio coefficient of the lyocell fiber in the mixed sample to the reference;
P lyocell ＝λ Lyocell reference ×P Reference object (2)
P Other components ＝100-P Lyocell -P Reference object (3)
Step S3.3: substituting the data in step S3.2 into formulas (4) and (5), and calculating to obtain the mass contents of the lyocell fibers and the cotton fibers in the sample to be detected, wherein as shown in table 3, the difference 1 is the difference between the mass content of the lyocell fibers calculated by the quantitative analysis method of the invention and the theoretical value, and the difference 2 is the difference between the mass content of the lyocell fibers measured by a microscopic method and the theoretical value.
Figure BDA0002547212490000071
P Final other Components ＝100-P Final lyocell (5)
TABLE 3 results of testing the fiber components
Figure BDA0002547212490000072
As shown in table 3, to select polyester fiber as a reference, the results of two parallel tests performed according to steps S1 and S2 were obtained. It can be seen that the difference between the mass content of the lyocell fiber measured by the method and the theoretical value of the lyocell fiber is within a range of +/-2%, and the difference between the mass content of the lyocell fiber measured by a microscopic method and the theoretical value exceeds a range of +/-5%, which indicates the accuracy of the quantitative analysis method established by the method, 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:
this embodiment differs from embodiment 1 in that: the test sample is a fiber blended by lyocell and viscose, and then the fiber contents in the three samples to be tested are respectively analyzed through the steps, so that the obtained test results are 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 the content test 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 analytical method of the present invention and the theoretical value, the difference 2 (/%) is the difference between the content of lyocell fiber measured by the FZ/01101 microscopic diameter method and the theoretical value, and the data results of the difference 1 and the difference 2 are compared.
TABLE 6 test results for fiber components
Figure BDA0002547212490000082
As can be seen from the data in table 6, the difference between the mass content of lyocell fiber measured by the test method of the present invention and the theoretical value is within ±2%. The difference between the good quality content of the lyocell fiber and the theoretical value measured by a microscope method exceeds the range of +/-4%, 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 above description is illustrative of the invention and not limiting, the scope of the invention being defined by the appended claims, which may be modified in any manner without departing from the basic structure of the invention.

Claims (3)

1. The quantitative analysis method for the fiber content in the lyocell fiber blended product is characterized by comprising the following steps of:
step S1: selecting yarns of fibers with circular cross sections as reference objects, selecting lyocell fiber blended products as samples to be tested, and mixing the reference objects and the samples to be tested to prepare mixed samples;
step S2: slicing the mixed sample to prepare an observation sample slice, and respectively measuring the diameters and the numbers of the lyocell fibers in the reference object and the lyocell fiber blended product by using a microscopic method;
step S3: obtaining the mass ratio coefficient of the lyocell fiber and the reference in the mixed sample, and further obtaining the content ratio of the lyocell fiber and other fibers in the sample to be detected;
the method for obtaining the content ratio of the lyocell fiber to other fibers in the step S3 comprises the following steps:
step S3.1: calculating mass ratio coefficients of the lyocell fiber and the reference in the mixed sample according to a formula (1):
Figure FDA0004100807570000011
λ lyocell reference The mass ratio coefficient of the lyocell fiber in the mixed sample and the reference is as follows;
n lyocell Measuring the number of lyocell fibers in the mixed sample;
d 2 lyocell The average value of the square of the diameter of lyocell fibers in a mixed sample is expressed in square micrometers (μm) 2 )；
ρ Lyocell To mix the density of lyocell fibers in a sample, the unit is grams per cubic centimeter (g/cm) 3 )；
n Reference object Measuring the number of reference objects in the mixed sample;
d 2 reference object The mean value of the square of the diameter of the reference in the mixed sample is expressed in square micrometers (μm) 2 )；
ρ Reference object To mix the density of the reference in the sample, the unit is grams per cubic centimeter (g/cm) 3 )；
Step S3.2: calculating according to formulas (2) and (3) to obtain the mass percentage of the lyocell fiber and other fiber components in the mixed sample:
P lyocell ＝λ Lyocell reference ×P Reference object (2)
P Other components ＝100-P Lyocell -P Reference object (3)
P Lyocell The mass content (%) of the lyocell fiber in the mixed sample;
P reference object The mass content (%) of the reference in the mixed sample;
P other components For mixing the mass content (%) of the fiber components other than the lyocell fiber and the reference in the sample;
step S3.3: calculating according to formulas (4) and (5) to obtain the mass content (%) of the lyocell fibers and other fiber components in the sample to be tested:
Figure FDA0004100807570000021
P final other Components ＝100-P Final lyocell (5)
P Final lyocell The mass content (%) of the lyocell fiber in the sample to be detected;
P final other Components The mass content (%) of other fiber components except the lyocell fiber in the sample to be detected;
step S3.4: and the final test result of the sample to be tested is the arithmetic average value of the two parallel test results, if the difference of the two parallel test results is more than 3%, a third observation sample piece is measured, and finally, the average value of the three test results is taken.
2. The method for quantitatively analyzing the fiber content of the lyocell fiber blend product according to claim 1, characterized in that: 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 the subsequent slice, and finishing the reference object into a straight beam-shaped yarn, so that the two ends of the yarn are level, and the length of the beam-shaped yarn is more than 10cm for standby;
step S1.2: the length of the sample to be measured is kept consistent with the length of the reference object, the sample to be measured is weighed according to the weight ratio of the reference object to the sample to be measured of 0.9:1.9-1.1:2.1, the sample to be measured is arranged into a straight beam shape, and two ends of the sample to be measured are flush for standby;
step S1.3: and (3) adjusting and aligning the two ends of the reference object and the sample to be tested in the step S1.1 and the step S1.2, and uniformly mixing to obtain a mixed sample.
3. The method for quantitatively analyzing the fiber content of the lyocell fiber blend product according to claim 1, characterized in that: the reference in step S1 is a fiber having a circular cross section.
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