CN110057811B - Method for rapidly judging whether mulberry silk is grafted or not - Google Patents
Method for rapidly judging whether mulberry silk is grafted or not Download PDFInfo
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- CN110057811B CN110057811B CN201811257960.0A CN201811257960A CN110057811B CN 110057811 B CN110057811 B CN 110057811B CN 201811257960 A CN201811257960 A CN 201811257960A CN 110057811 B CN110057811 B CN 110057811B
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- 235000008708 Morus alba Nutrition 0.000 title claims abstract description 33
- 240000000249 Morus alba Species 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 16
- 239000000523 sample Substances 0.000 claims abstract description 43
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 36
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 16
- 239000013074 reference sample Substances 0.000 claims abstract description 13
- 238000005303 weighing Methods 0.000 claims abstract description 10
- 239000003086 colorant Substances 0.000 claims description 2
- 239000012488 sample solution Substances 0.000 abstract description 8
- 238000001514 detection method Methods 0.000 abstract description 4
- 238000012360 testing method Methods 0.000 abstract description 4
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 2
- 238000010998 test method Methods 0.000 abstract 1
- 241000628997 Flos Species 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 125000000524 functional group Chemical group 0.000 description 3
- 150000001413 amino acids Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 108090000765 processed proteins & peptides Proteins 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000002411 thermogravimetry Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 229920000578 graft copolymer Polymers 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000002076 thermal analysis method Methods 0.000 description 1
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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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to a detection method of a silk product, in particular to a method for judging whether silk is grafted or not. The invention discloses a method for rapidly judging whether mulberry silk is grafted, which comprises the following steps: 1) weighing mulberry silk reference samples and measured samples, putting the mulberry silk reference samples and the measured samples into corresponding beakers, weighing concentrated hydrochloric acid or phosphoric acid with the same concentration according to the same bath ratio, and pouring the concentrated hydrochloric acid or phosphoric acid into the beakers of the reference samples and the measured samples to dissolve the mulberry silk reference samples and the measured samples into light yellow transparent silk solution; 2) observing the color change of the two silk solutions within 3-48 hours, and if the solution color of the detected sample is consistent with that of the reference sample and is the same purple, indicating that the detected sample is ungrafted mulberry silk; if the purple degree of the tested sample solution is obviously lighter than that of the reference sample or is still a faint yellow solution, the tested sample is the grafted mulberry silk. The test method is simple, the dosage of the tested sample is small, and the test can be carried out quickly; does not need complex equipment and reagents, and has low cost.
Description
Technical Field
The invention relates to a detection method of a silk product, in particular to a method for judging whether silk is grafted or not.
Background
The silk is protein fiber, is used as a textile clothing material, has good skin-friendly property, excellent moisture absorption and air permeability and heat retention property, is a high-grade raw material for clothing, clothes and bedding, and particularly has a higher proportion when being used for silk wadding quilts. However, because the cost of silk is high, individual silk fabrics, silk floss or bedding and clothing manufacturers graft and weigh the silk in order to reduce the cost of the silk floss. After the silk is grafted and weighted, chemical components of the silk comprise chemical graft polymers with different contents besides natural silk protein, the physical and chemical properties, the processing property and the service performance of the silk are changed, in addition, the price of the silk raw material is high, and the introduction of the chemical polymers impacts the price system of the market.
At present, except for producers, common users and consumers are difficult to judge whether the purchased silk floss is the grafted silk floss, and a detection department does not have a proper and standardized detection method at present. Although chinese patent (CN 201510303852) "a method for detecting silk grafting ratio" reports that the silk grafting ratio is measured by thermogravimetry, and product quality identification and component identification are performed. However, the method needs a thermogravimetric analysis instrument to gradually heat the silk sample to 700 ℃, and needs a more professional thermal analysis knowledge and a mathematical analysis method such as deconvolution, so that the method is not substantially applied in the industry at present.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for rapidly judging whether mulberry silk is grafted, which is simple, convenient and rapid, has low test cost, and enables silk users and consumers to conveniently and qualitatively detect whether the mulberry silk is grafted.
In order to achieve the purpose, the method for rapidly judging whether the mulberry silk is grafted comprises the following specific steps:
1) weighing mulberry silk reference samples and measured samples, putting the mulberry silk reference samples and the measured samples into corresponding beakers, weighing concentrated hydrochloric acid or phosphoric acid with the same concentration according to the same bath ratio, and pouring the concentrated hydrochloric acid or phosphoric acid into the beakers of the reference samples and the measured samples to dissolve the mulberry silk reference samples and the measured samples into light yellow transparent silk solution; the mulberry silk reference sample is an ungrafted mulberry silk sample, and the bath ratio is 1: 30-200, wherein the concentration of concentrated hydrochloric acid is not less than 36%, and the concentration of phosphoric acid is not less than 83%;
2) observing the color change of the two silk solutions within 3-48 hours, and if the solution color of the detected sample is consistent with that of the reference sample and is the same purple, indicating that the detected sample is ungrafted mulberry silk; if the purple degree of the solution of the tested sample is obviously lighter than that of the reference sample or still is a light yellow solution, the tested sample is grafted mulberry silk; the larger the difference between the solution colors of the measured sample and the reference sample is, the higher the grafting ratio of the measured sample is.
Preferably, the concentration of the concentrated hydrochloric acid is 36-38%.
Preferably, the concentration of the phosphoric acid is 83-88%.
The ungrafted mulberry silk can be rapidly hydrolyzed into peptide or amino acid in concentrated hydrochloric acid or phosphoric acid to form a light yellow solution, the solution gradually changes color along with the further action of the concentrated hydrochloric acid or the phosphoric acid on functional groups in the peptide or the amino acid, and the purple solution is formed after a certain time. And for the grafted weight-increased mulberry silk, although the grafted weight-increased mulberry silk can be rapidly hydrolyzed in concentrated hydrochloric acid or phosphoric acid, a part of functional groups and the grafting agent generate chemical reaction to form covalent bonds, so that the functional groups which can be further acted by the concentrated hydrochloric acid or the phosphoric acid are reduced, and the solution has small or basically no color change after the same time. Therefore, whether the mulberry silk is grafted and weighted or not and the weight increasing degree can be qualitatively judged according to the color change degree of the solution after the mulberry silk is dissolved in concentrated hydrochloric acid or phosphoric acid for a certain time.
Compared with the prior art, the invention has the beneficial effects that:
1. the testing method is simple, the dosage of the tested sample is small, and the test can be carried out quickly;
2. does not need complex equipment and reagents, and has low cost.
Drawings
FIG. 1 is a comparison of the color of the solutions of the grafted silk sample and the ungrafted silk sample of example 1.
FIG. 2 is a comparison of the color of the solutions of the grafted silk sample and the ungrafted silk sample of example 2.
FIG. 3 is a comparison of the color of the solutions of the grafted silk sample and the ungrafted silk sample in example 3.
FIG. 4 is a comparison of the color of the solutions of the silk samples tested and the ungrafted silk samples of example 4.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example 1:
1) weighing 2 parts of grafted silk sample and 1 part of ungrafted silk sample, respectively putting the weighed grafted silk sample and ungrafted silk sample into containers, and respectively adding concentrated hydrochloric acid with the concentration of 36% into 3 containers according to the bath ratio of 1:100 to dissolve the silk; wherein the grafted silk samples are numbered as 01 and 03, and the ungrafted silk samples are numbered as 02;
2) observing the color of the solution after 48 hours, wherein the result shows that the ungrafted silk sample solution is purple and the grafted silk sample solution is faint yellow; as shown in fig. 1.
Example 2:
1) weighing 1 part of ungrafted silk sample and 2 parts of grafted silk sample, respectively putting the weighed materials into containers, respectively adding concentrated hydrochloric acid with the concentration of 38% into 3 containers according to the bath ratio of 1:30, and dissolving silk; wherein the number of the ungrafted silk sample is 01B, and the number of the grafted silk samples are 02B and 03B;
2) observing the color of the solution after 3 hours, wherein the result shows that the ungrafted silk sample solution is purple and the grafted silk sample solution is faint yellow; as shown in fig. 2.
Example 3:
1) taking 1 part of ungrafted silk sample and 4 parts of grafted silk sample (wherein the grafting rates of 2 parts of samples are the same), weighing, respectively putting into containers, respectively adding phosphoric acid with the concentration of 85% into 5 containers according to the bath ratio of 1:100, and dissolving silk; the number of the ungrafted silk sample is 00, and the number of the grafted silk sample is 01P, 02P, 03P and 04P (wherein, the grafting rates of 01P and 03P are the same, the grafting rate is 12 percent, and the grafting rate of 04P is the highest and is 35 percent);
2) observing the color of the solution after 16 hours, wherein the result shows that the ungrafted silk sample solution is purple, the silk sample with low grafting rate is purple, the silk sample with the same grafting rate of the 01P and 03P samples is the same in color, and the solution with high grafting rate of 04P is faint yellow; as shown in fig. 3.
Example 4:
1) taking 2 parts of blind sample silk and 1 part of non-grafted silk reference sample, weighing, respectively putting into containers, respectively adding concentrated hydrochloric acid with the concentration of 37% into 3 containers according to the bath ratio of 1:200, and dissolving the silk; the serial numbers of the two blind sample silks are respectively 01C and 02C, and the serial number of the ungrafted silk reference sample is CC;
2) observing the color of the solution after 8 hours, wherein the result shows that the color of the sample solution with the number of 02C is purple consistent with that of the reference sample solution with the number of CC, and the silk sample is ungrafted silk; if the sample solution with the number of 01C is light yellow, the silk sample is grafted silk; as shown in fig. 4.
The above examples are only specific embodiments of the present invention. The present invention is not limited to the above embodiments, and many variations are possible. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the present invention are to be considered within the scope of the invention.
Claims (3)
1. A method for rapidly judging whether mulberry silk is grafted is characterized by comprising the following steps: the method comprises the following specific steps:
1) weighing mulberry silk reference samples and measured samples, putting the mulberry silk reference samples and the measured samples into corresponding beakers, weighing concentrated hydrochloric acid or phosphoric acid with the same concentration according to the same bath ratio, and pouring the concentrated hydrochloric acid or phosphoric acid into the beakers of the reference samples and the measured samples to dissolve the mulberry silk reference samples and the measured samples into light yellow transparent silk solution; the mulberry silk reference sample is an ungrafted mulberry silk sample, and the bath ratio is 1: 30-200, wherein the concentration of concentrated hydrochloric acid is not less than 36%, and the concentration of phosphoric acid is not less than 83%;
2) observing the color change of the two silk solutions within 3-48 hours, and if the solution color of the detected sample is consistent with that of the reference sample and is the same purple, indicating that the detected sample is ungrafted mulberry silk; if the purple degree of the solution of the tested sample is obviously lighter than that of the reference sample or still is a light yellow solution, the tested sample is grafted mulberry silk; the larger the difference between the solution colors of the measured sample and the reference sample is, the higher the grafting ratio of the measured sample is.
2. The method for rapidly judging whether mulberry silk is grafted according to claim 1, wherein the method comprises the following steps: the concentration of the concentrated hydrochloric acid is 36-38%.
3. The method for rapidly judging whether mulberry silk is grafted according to claim 1, wherein the method comprises the following steps: the concentration of the phosphoric acid is 83-88%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811257960.0A CN110057811B (en) | 2018-10-26 | 2018-10-26 | Method for rapidly judging whether mulberry silk is grafted or not |
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| CN201811257960.0A CN110057811B (en) | 2018-10-26 | 2018-10-26 | Method for rapidly judging whether mulberry silk is grafted or not |
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| CN110057811A CN110057811A (en) | 2019-07-26 |
| CN110057811B true CN110057811B (en) | 2021-11-02 |
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| JP2002066315A (en) * | 2000-08-30 | 2002-03-05 | National Institute Of Agrobiological Sciences | Adsorbent material for harmful substance, harmful substance desorption process and method for quantitative determination of endocrine disruptor |
| CN1410437A (en) * | 2002-02-11 | 2003-04-16 | 李学军 | Method of producing silk peptide, silk amino acid by acid hydrolysis of natural silk |
| CN1687755A (en) * | 2005-04-27 | 2005-10-26 | 苏州大学 | Testing reagent and identification method for natural colored mulberry silk |
| CN1693574A (en) * | 2005-06-21 | 2005-11-09 | 苏州大学 | Method of plasma grafting weight gaining for silk fibre |
| CN101671402A (en) * | 2009-10-20 | 2010-03-17 | 东华大学 | Preparation method of cyclodextrin derivatives capable of grafting silk fabric |
| CN101881776A (en) * | 2010-06-12 | 2010-11-10 | 苏州大学 | Quantitative analysis method for identifying mulberry silk and tussah silk |
| CN102313734A (en) * | 2011-08-02 | 2012-01-11 | 湖南大学 | Method for determining content of active hydroxyl in natural fibre by titration method |
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| WO2016100721A1 (en) * | 2014-12-17 | 2016-06-23 | Tufts University | Injectable, flexible hydroxyapatite-silk foams for osteochondral and dental repair |
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2018
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| CN101671402A (en) * | 2009-10-20 | 2010-03-17 | 东华大学 | Preparation method of cyclodextrin derivatives capable of grafting silk fabric |
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