CN106918488B - The method for quick identification of raw silks of fresh cocoons and dried cocoon raw silk - Google Patents
The method for quick identification of raw silks of fresh cocoons and dried cocoon raw silk Download PDFInfo
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- G01N9/00—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity
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Abstract
The invention discloses the method for quick identification of a kind of raw silks of fresh cocoons and dried cocoon raw silk, its operating procedure is: 1) handling fresh cocoon or dried cocoon raw silk fiber with acetone washing, then washed with distilled water to it；2) neopelex, organic silicon defoamer and distilled water are hybridly prepared into test fluid；3) fresh cocoon or dried cocoon raw silk fiber are cut into several staple fibers and tied up；4) under conditions of normal atmosphere, 18-22 DEG C of temperature, relative humidity are 60-68%, raw silk fiber is put down gently to the liquid level center in test fluid in parallel and starts simultaneously at timing, record fresh cocoon or dried cocoon raw silk natural subsidence to beaker bottom time, if the sedimentation time was less than 300 seconds, then determine that it is raw silks of fresh cocoons, if the sedimentation time is greater than 300 seconds, dried cocoon raw silk is determined that it is.The method of the present invention have it is easy to operate, it is low in cost, be easy accurate judgement the advantages that, can factory and laboratory inspection work in promote.
Description
Technical field
The present invention relates to silk inspection and testing technologies, the specially method for quick identification of raw silks of fresh cocoons and dried cocoon raw silk.
Background technique
Fresh silk cocoon is without drying, high temperature cocoon cooking, raw made of direct filature after only being handled by vacuum hot water infiltration
Silk, referred to as raw silks of fresh cocoons.Conversely, fresh silk cocoon by high temperature cocoon drying, certain time storage, high temperature cocoon cooking and reel silk from cocoons raw silk, then
Referred to as dried cocoon raw silk.Since fresh cocoon reeling process is less, saves energy consumption and throwing byproduct can be made full use of --- silkworm chrysalis, tool
There are certain economic advantages, so that fresh cocoon reeling is more prevalent in the raw silks main producing region such as Guangxi.Although the price of raw silks of fresh cocoons is low
Cleanliness and obvolvent index in dried cocoon raw silk, but due to raw silks of fresh cocoons is poorer than dried cocoon raw silk, between the two there is
The difference of character and service performance, especially raw silks of fresh cocoons break end in weaving process, fuzziness, and strand paper is split, fabric dyeing
The probability that dyeing defect occurs in color is higher than dried cocoon raw silk.
In recent years, raw silk industry pretends to be dried cocoon raw silk and silk production to look forward in the prevalence of reeling enterprises using raw silks of fresh cocoons
Industry transaction, seeks the bad phenomenon of high profit, and the accurate identification of fresh silk and dried cocoon silk is related to reeling enterprises and silk production
The interests of enterprise and trade disputes between the two.But since two kinds of raw silk appearance surfaces are identical, protein fibre is complicated, although
Numerous domestic scientific research at present, quality inspection organization propose several methods for identifying two kinds of raw silks, such as pass through scanning electron microscopic observation raw silk
The surface particles characteristic of unknown sample identifies fresh silk and dried cocoon silk is (a kind of to examine raw silks of fresh cocoons by scanning electron microscope
Method, application number 201410379015.3)；The fresh and dried class of raw silk is judged by the whiteness for detecting position sample with color measurement instrument
Type, biggish whitness index average value is raw silks of fresh cocoons, and whitness index average value is lesser, and for raw silks of fresh cocoons, (colour photometer is examined fresh
The method of cocoon raw silk)；Compare the raw silks of fresh cocoons of same source and the sericin degumming loss percentage of dried cocoon raw silk or silk gum solution concentration
Size (a method of identify raw silks of fresh cocoons and dried cocoon raw silk by silk gum dissolution characteristics, 201510039141.9) uses gel
The length (a method of identify raw silks of fresh cocoons and dried cocoon raw silk by sericin gel characteristic, 201510037780.1) of time is come
Distinguish raw silks of fresh cocoons and dried cocoon raw silk, above method exist be only capable of the different fresh and dried performance raw silks of two kinds of same sources of difference which
It is a be dried cocoon which be fresh cocoon, be unable to a kind of fresh and dried performance of unknown raw silk of chance decision, and as dried cocoon Fresh cocoon grading is equal
Smaller compared with Gao Shiqi surface cleanliness difference and color difference, the accuracy for determining its fresh and dried type by microscope and whiteness method is
It is very low low.Therefore these types of method poor, narrow application range, ineffective disadvantage in the presence of identification accuracy.
Powder sample is such as placed on moisture analyser by other two kinds of discrimination methods, in the case where setting drying temperature, when interval
Between record example weight change sequence；Datagram is generated to the weight change sequence data of collected sample, is become according to feature
Change situation and completes sample identification (a kind of detection method of raw silks of fresh cocoons, 201510236987.1)；Sample is subjected to efficient liquid phase
Chromatography, to obtain the efficient liquid phase chromatographic analysis of the efficient liquid phase chromatographic analysis result of standard items, sample to be tested respectively
As a result；When the efficient liquid phase chromatographic analysis result of sample to be tested is compared with the efficient liquid phase chromatographic analysis result of standard items, have more
When at least one existing characteristic component peak, determine that sample to be tested is raw silks of fresh cocoons；Conversely, then determining sample to be tested for dried cocoon raw silk.
(method for quickly identifying fresh cocoon reel silk from cocoons raw silk and dried cocoon reel silk from cocoons raw silk, 201510446043.7).Both methods is although can be with
Determine a kind of fresh and dried type of unknown sample, but first method needs to establish complicated database, second method needs
Influence of the accuracy of test stone product, database and standard items to result is very big, and both discrimination methods are excessively complicated,
Expensive instrument and equipment and complicated operating process, higher cost are needed, and is not suitable with and is pushed away in silk production enterprise
Wide application.
Therefore, a kind of simple, efficient, quick, easy-operating fresh cocoon and dried cocoon raw silk discrimination method letter are to be developed.
Summary of the invention
Technical problem to be solved by the invention is to provide the method for quick identification of raw silks of fresh cocoons and dried cocoon raw silk, this method
Have the advantages that simple, efficient, quick, easy to operate, accuracy is high, and cost is relatively low, it is easy to operate, it is good using adaptability,
Be conducive to promote in factory and laboratory inspection work.
The present invention solves above-mentioned technical problem with following technical solution:
The method for quick identification of raw silks of fresh cocoons of the present invention and dried cocoon raw silk, including following operating procedure:
1) raw silk is pre-processed: at room temperature, handles fresh cocoon or dried cocoon raw silk fiber using acetone washing first
Dimension is taken out after 2 minutes, then reuses distilled water and carries out washing 3 times to it, and places it in temperature 18-under normal atmosphere
22 DEG C, relative humidity be 60-68%, moisture equilibrium at dry side 12 hours or more；
2) it prepares test fluid: neopelex, organic silicon defoamer and distilled water is hybridly prepared into test fluid,
Wherein the concentration of neopelex is 3.5mmol/L, and the mass concentration of organic silicon defoamer is 0.025%, and mixing is equal
It is stand-by after standing 2 hours after even；
3) it prepares raw silk test sample: several short fibres will be cut by above-mentioned pretreated fresh cocoon or dried cocoon raw silk fiber
Dimension, every fiber weigh about 0.05mg, then 4-12 fibers are neatly bundled into a branch of, total weight 0.2mg-0.6mg；
4) differential test process: in normal atmosphere, 18-22 DEG C of temperature, the environmental condition that relative humidity is 60-68%
Under, the above-mentioned raw silk fiber by having tied up is put down gently in parallel in the liquid level center of test fluid simultaneously respectively using clean tweezers
Start simultaneously at timing, record fresh cocoon or dried cocoon raw silk natural subsidence to beaker bottom time, if the sedimentation time is less than 300
Second, then raw silks of fresh cocoons are determined that it is, if the sedimentation time is greater than 300 seconds, determine that it is dried cocoon raw silk.
It is 6.0-7.0, specific gravity 1.0 that the test fluid of the step 2), which adjusts pH value,.
The method of the present invention has easy to operate, and low in cost, the advantages that being easy accurate judgement, and cost is relatively low, is easy
Operation, it is good using adaptability, it is suitable for the raw material that the production of this enterprise needs convenient for the selection of silk weaving enterprise, is conducive in factory and reality
It tests in the inspection work of room and promotes.
Specific embodiment
The method for quick identification (hereinafter referred to as discrimination method) of raw silks of fresh cocoons of the present invention and dried cocoon raw silk, including pre- raw silk are pre-
Four steps such as treatment process, the preparation of test fluid, the preparation of raw silk test sample, differential test process.Wherein in test fluid
Main component be neopelex (SDBS) and organic silicon defoamer；Test fluid appearance is colourless transparent liquid, pH
Value is about 6.0-7.0, and specific gravity is approximately 1.0；Differential test process mainly investigates static balance time of the raw silk in test fluid.
The method for quick identification of raw silks of fresh cocoons of the present invention and dried cocoon raw silk, the specific operation method is as follows:
1. raw silk pretreating process: at room temperature, handling fresh cocoon or dried cocoon raw silk fiber 2 using acetone washing first
It is taken out after minute, then reuses distilled water and carry out washing 3 times to it, and place it in temperature 18-22 under normal atmosphere
DEG C, relative humidity be 60-68%, moisture equilibrium at dry side 12 hours or more；
2. the preparation of test fluid: weighing the organosilicon defoaming of the neopelex (SDBS), 0.05g of certain mass
Agent and 200ml distilled water are added in the beaker of 250ml, and stand-by after standing 2 hours after being mixed uniformly, wherein SDBS's is dense
Degree is 3.5mmol/L；
3. the preparation of raw silk test sample: several short fibres will be cut by above-mentioned pretreated fresh cocoon or dried cocoon raw silk fiber
Dimension, every fiber weighs about 0.05mg, is then neatly bundled into 4-12 root fiber a branch of, and total weight is about 0.2mg-0.6mg.
4. differential test process: in normal atmosphere, 18-22 DEG C of temperature, the environmental condition that relative humidity is 60-68%
Under, it is put down gently above-mentioned in parallel by the raw silk fiber tied up in the liquid level center of test fluid respectively using clean tweezers
(avoiding contacting influence sedimentation with walls of beaker) simultaneously starts simultaneously at timing, records fresh cocoon or dried cocoon raw silk natural subsidence to beaker bottom
Time then determine wherein the sedimentation time is greater than 300 seconds if the sedimentation time less than 300 seconds, determines that it is raw silks of fresh cocoons
It is dried cocoon raw silk.
The method of the present invention have it is easy to operate, it is low in cost, the advantages that being easy accurate judgement, suitable convenient for the selection of silk weaving enterprise
Together in the raw material that the production of this enterprise needs, be conducive to promote in factory and laboratory inspection work.
It is the application example of the method for the present invention below, the sample raw silk of use is that Guangxi difference reeling enterprises produce not
Ad eundem (3A~5A) raw silk, raw silk processing result are seen below shown in table 1.
The discrimination method operating procedure of embodiment 1, use is as follows:
Step 1, raw silk pretreating process: at room temperature, first using acetone washing processing raw silk fiber (sample 1)
Taken out after 2 minutes, then reuse distilled water and carry out washing 3 times to it, and place it under normal atmosphere 20.0 DEG C of temperature,
Relative humidity 65.0%, moisture equilibrium at dry side 12 hours；
Step 2, the neopelex (SDBS) of certain mass, the organosilicon of 0.05g the preparation of test fluid: are weighed
Defoaming agent and 200ml distilled water are added in the beaker of 250ml, stand-by after standing 2 hours after being mixed uniformly, wherein SDBS
Concentration be 3.5mmol/L；
Step 3, it the preparation of raw silk test sample: will be cut by above-mentioned pretreated raw silk fiber (sample 1) several short
Fiber, every fiber weigh about 0.05mg, are then neatly bundled into 12 fibers a branch of, and total weight is about 0.6mg.
Step 4, differential test process: under normal atmosphere, 20.0 DEG C of temperature, the environmental condition of relative humidity 65.0%,
The above-mentioned raw silk fiber (sample 1) by having tied up is put down gently in parallel in the liquid level of test fluid respectively using clean tweezers
Centre (avoiding contacting influence sedimentation with walls of beaker) simultaneously starts simultaneously at timing, final raw silk fiber (sample 1) natural subsidence to beaker
The time of bottom is 35 seconds, thus can determine that sample 1 is raw silks of fresh cocoons.
Embodiment 2, operating procedure is as follows:
1. step 1 is identical as the step 1 of embodiment 1, the raw silk fiber sample is sample 2, and moisture equilibrium at dry side condition is: temperature
Degree be 19.0 DEG C, relative humidity 62.0%, moisture equilibrium at dry side 18 hours.
2. step 2 is identical as the step 2 of embodiment 1.
3. step 3 is identical as the step 3 in embodiment 1, the raw silk fiber sample is sample 2.
4. step 4 is identical as the step 4 in embodiment 1, the raw silk fiber sample is sample 2, the environmental condition of use
Be: temperature is 19.0 DEG C, relative humidity 62.0%, the time of final raw silk fiber (sample 2) natural subsidence to beaker bottom
It is 36 seconds, thus can determine that sample 2 is raw silks of fresh cocoons.
Embodiment 3, operating procedure is as follows:
1. step 1 is identical as the step 1 of embodiment 1, the raw silk fiber sample is sample 3, and moisture equilibrium at dry side condition is: temperature
Degree be 21.0 DEG C, relative humidity 68.0%, moisture equilibrium at dry side 16 hours.
2. step 2 is identical as the step 2 of embodiment 1.
3. step 3 is identical as the step 3 of embodiment 1, the raw silk fiber sample is sample 3.
4. step 4 is identical as the step 4 of embodiment 1, the raw silk fiber sample is sample 3, and the environmental condition of use is:
Temperature is 21.0 DEG C, relative humidity 68.0%.The time of final raw silk fiber (sample 3) natural subsidence to beaker bottom is 40
Second, it thus can determine that sample 3 is raw silks of fresh cocoons.
Embodiment 4
1. step 1 is identical as the step 1 of embodiment 1, the raw silk fiber sample is sample 4, and moisture equilibrium at dry side condition is: temperature
Degree be 20.0 DEG C, relative humidity 66.0%, moisture equilibrium at dry side 20 hours.
2. step 2 is identical as the step 2 in embodiment 1.
3. step 3 is identical as the step 3 in embodiment 1, the raw silk fiber sample is sample 4.
4. step 4 is identical as the step 4 in embodiment 1, the raw silk fiber sample is sample 4, the environmental condition of use
Be: temperature is 20.0 DEG C, relative humidity 66.0%.Time of final raw silk fiber (sample 4) natural subsidence to beaker bottom
Greater than 300 seconds, it thus can determine that sample 4 is dried cocoon raw silk.
Embodiment 5
1. step 1 is identical as the step 1 of embodiment 1, the raw silk fiber sample is sample 5, and moisture equilibrium at dry side condition is: temperature
Degree be 20.0 DEG C, relative humidity 65.0%, moisture equilibrium at dry side 14 hours.
2. step 2 is identical as the step 2 of embodiment 1.
3. step 3 is identical as the step 3 of embodiment 1, the raw silk fiber sample is sample 5.Raw silk fiber (sample 5) is cut
At several staple fibers, every fiber weighs about 0.05mg, is then neatly bundled into 4 fibers a branch of, and total weight is about 0.2mg.
4. step 4 is identical as the step 4 of embodiment 1, the raw silk fiber sample is sample 5, and the environmental condition of use is:
Temperature is 20.0 DEG C, relative humidity 65.0%.The time of final raw silk fiber (sample 5) natural subsidence to beaker bottom is greater than
300 seconds, it thus can determine that sample 5 is dried cocoon raw silk.
Embodiment 6
1. step 1 is identical as the step 1 of embodiment 1, the raw silk fiber sample is sample 6, and moisture equilibrium at dry side condition is: temperature
Degree be 18.0 DEG C, relative humidity 65.0%, moisture equilibrium at dry side 24 hours.
2. step 2 is identical as the step 2 of embodiment 1.
3. step 3 is identical as the step 3 of embodiment 1, the raw silk fiber sample is sample 6.
4. step 4 is identical as the step 4 of embodiment 1, the raw silk fiber sample is sample 6, and the environmental condition of use is:
Temperature is 18.0 DEG C, relative humidity 65.0%.The time of final raw silk fiber (sample 6) natural subsidence to beaker bottom is greater than
300 seconds, it thus can determine that sample 6 is dried cocoon raw silk.
Embodiment 7
1. step 1 is identical as the step 1 of embodiment 1, the raw silk fiber sample is sample 7, and moisture equilibrium at dry side condition is: temperature
Degree be 22.0 DEG C, relative humidity 68.0%, moisture equilibrium at dry side 18 hours.
2. step 2 is identical as the step 2 of embodiment 1.
3. step 3 is identical as the step 3 of embodiment 1, the raw silk fiber sample is sample 7.Raw silk fiber (sample 7) is cut
At several staple fibers, every fiber weighs about 0.05mg, is then neatly bundled into 8 fibers a branch of, and total weight is about 0.5mg.
4. step 4 is identical as the step 4 of embodiment 1, the raw silk fiber sample is sample 7, and the environmental condition of use is:
Temperature is 22.0 DEG C, relative humidity 68.0%.The time of final raw silk fiber (sample 7) natural subsidence to beaker bottom is 22
Second, it thus can determine that sample 7 is raw silks of fresh cocoons.
Embodiment 8
1. step 1 is identical as the step 1 of embodiment 1, the raw silk fiber sample is sample 8, and moisture equilibrium at dry side condition is: temperature
Degree be 20.0 DEG C, relative humidity 60.0%, moisture equilibrium at dry side 24 hours.
2. step 2 is identical as the step 2 of embodiment 1.
3. step 3 is identical as the step 3 of embodiment 1, the raw silk fiber sample is sample 8.
4. step 4 is identical as the step 4 of embodiment 1, the raw silk fiber sample is sample 8, and the environmental condition of use is:
Temperature is 20.0 DEG C, relative humidity 60.0%.The time of final raw silk fiber (sample 8) natural subsidence to beaker bottom is greater than
300 seconds, it thus can determine that sample 8 is dried cocoon raw silk.
The qualification result of the fiber sample of 1 embodiment 1-8 of table
The result shows that using the method for the present invention for identifying eight kinds of fresh cocoons and when dried cocoon raw silk sample, determine result with
Actual fibers property is consistent.
The present invention is defoamed using raw silks of fresh cocoons and dried cocoon raw silk containing neopelex (SDBS) and organosilicon
The length of sedimentation time identifies raw silks of fresh cocoons and dried cocoon raw silk in the test fluid of agent, this method have it is quick, easy to operate, at
The advantages that this is cheap, efficient, accuracy is high is a kind of effective raw silks of fresh cocoons and dried cocoon raw silk identification method.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (3)
1. the method for quick identification of a kind of raw silks of fresh cocoons and dried cocoon raw silk, which is characterized in that including following operating procedure:
1) raw silk is pre-processed: at room temperature, handles fresh cocoon using acetone washing first or dried cocoon raw silk fiber 2 divides
It is taken out after clock, then reuses distilled water and carry out washing 3 times to it, placed it in after washing under normal atmosphere in temperature 18-22
DEG C, relative humidity be 60-68%, moisture equilibrium at dry side 12 hours or more；
2) it prepares test fluid: neopelex, organic silicon defoamer and distilled water is hybridly prepared into test fluid, wherein
The concentration of neopelex is 3.5 mmol/L, and the mass concentration of organic silicon defoamer is 0.025%, after mixing
It is stand-by after standing 2 hours；
3) it prepares raw silk test sample: several staple fibers will be cut by above-mentioned pretreated fresh cocoon or dried cocoon raw silk fiber, often
Root fiber weighs about 0.05 mg, then 4-12 fibers are neatly bundled into it is a branch of, total weight be the mg of 0.2 mg-0.6；
4) it differential test process: under normal atmosphere, 18-22 DEG C of temperature, the environmental condition that relative humidity is 60-68%, uses
Clean tweezers are put down the raw silk fiber that above-mentioned process has been tied up gently liquid level center in test fluid respectively in parallel and are opened simultaneously
Beginning timing, record fresh cocoon or dried cocoon raw silk natural subsidence to beaker bottom time, if the sedimentation time less than 300 seconds, is sentenced
Fixed its is raw silks of fresh cocoons, if the sedimentation time greater than 300 seconds, determines that it is dried cocoon raw silk.
2. the method for quick identification of raw silks of fresh cocoons and dried cocoon raw silk according to claim 1, which is characterized in that the step 2
Test fluid adjust pH value be 6.0-7.0, specific gravity 1.0.
3. the method for quick identification of raw silks of fresh cocoons and dried cocoon raw silk according to claim 1, which is characterized in that the step 1)
The time of moisture equilibrium at dry side is 12-24 hours.
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| CN107576609A (en) * | 2017-09-27 | 2018-01-12 | 中国计量大学 | A kind of raw silk cohesion detection means and its application method |
| CN109490123A (en) * | 2018-11-02 | 2019-03-19 | 广西出入境检验检疫局检验检疫技术中心 | Identify the obvolvent test method of dried cocoon raw silk |
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| CN103091165A (en) * | 2013-01-18 | 2013-05-08 | 浙江大学 | Method for testing fresh cocoon raw silk by monofilament stretching |
| CN104865151A (en) * | 2015-05-11 | 2015-08-26 | 广西科技大学 | Fresh cocoon raw silk detection method |
| CN106526040A (en) * | 2016-11-12 | 2017-03-22 | 浙江理工大学 | Method for identifying fresh cocoon/dried cocoon raw silk based on GC or GC-MS technology |
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|---|---|---|---|---|
| CN103091165A (en) * | 2013-01-18 | 2013-05-08 | 浙江大学 | Method for testing fresh cocoon raw silk by monofilament stretching |
| CN104865151A (en) * | 2015-05-11 | 2015-08-26 | 广西科技大学 | Fresh cocoon raw silk detection method |
| CN106526040A (en) * | 2016-11-12 | 2017-03-22 | 浙江理工大学 | Method for identifying fresh cocoon/dried cocoon raw silk based on GC or GC-MS technology |
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