CN103712880B - Sericin content in silk rapid detection system and detection method - Google Patents
Sericin content in silk rapid detection system and detection method Download PDFInfo
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- CN103712880B CN103712880B CN201210378044.9A CN201210378044A CN103712880B CN 103712880 B CN103712880 B CN 103712880B CN 201210378044 A CN201210378044 A CN 201210378044A CN 103712880 B CN103712880 B CN 103712880B
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Abstract
The entitled sericin content in silk rapid detection system of the present invention and detection method, be related to content of silk gum in a kind of silk account for silk quality than method for fast measuring.Detection method includes：1. pure silk glue, the foundation of fibroin standard hot weight-loss database；2. tested silk is specifying the weightlessness in temperature rise rate and temperature range with inhaling exothermic characteristic curve；3. a pair experiment curv is standardized；4. silk gum and fibroin and tested silk are drawn by weight-loss curve in specified for temperature ranges and obtain the weightless graph of a relation of three kinds of materials；5. thus three curves constitute two isolated areas and are defined as region 1 (Area1, pure silk glue is constituted with tested silk) and region 2 respectively (Aare2 is made up of tested silk with pure silk element)；6. the area in this two region is calculated respectively, and the ratio of zoning area 1 and total area (region area 1+ region areas 2)；7. thus obtain the gum content KTG of tested silk；8. the silk gum content under standard environment can also be converted into as requested.
Description
Technical field
The present invention relates to textile technology field, more particularly to a kind of quick detection system detected to silk content of silk gum
System and detection method.The significant advantage of one of this method is once-through operation and can save balance and the process for repeating to weigh.
Technical background
China is exactly the big country of a silk production since ancient times, and the Silk Road is even more that China has been made referrals into the whole world.
There is the Chinese Silk quality production scale of document announcement to rank first in the world, 2,007 500,000 tons or so of silk cocoons of annual output (account for world production total
Amount 80%)；More than 70,000 tons of raw silk (account for world production total amount 60%), silk yield accounts for 45% left side of Gross World Product
It is right.Silk is that China can dominate one of only a few advantageous agricultural product of international market.
Silk is made up of two monofilament, and its main body is fibroin, external sheath silk gum.Silk gum is mainly by misaligned
Amorphism silk gum globulin is constituted, and wherein serine, aspartic acid and Glycine Levels are higher, and relative mass is respectively reached
33.43%th, 16.71% and 13.49%, the structure for passing through disulfide bond containing two peptide chains in molecule.The two of sericin
Level structure is practically free of αhelix based on random coil, and containing part β conformations.Most pigment, grease, wax
It is present in inorganic salts etc. in silk gum.To prepare fiber-spinnable, all or part of silk gum is necessarily removed for silk.
Process in silk processing removing silk gum and grease is call concise, is most basic one of the technique of Silk Industry, after all
Continuous processing suffers from conclusive influence, for example, the not enough easily dyeing flower of degumming, irregular, the excessive then feel of degumming of dye in terms of dyeing
It is too poor.
The conventional method of measurement of the existing technology to natural silk degumming rate is：
(1) gravimetric method, that is, determine reduction rate, this method precision is high, but required time is long.It is concise preceding and concise
Afterwards, in 20 DEG C of room temperature, under conditions of relative humidity 60%, the moisture content of silk is kept into poised state.Determine weight at that time.
Thus degumming rate can be calculated.If measuring the degumming rate of silk using the method, the need for balance, whole process is completed extremely
Rare more than 24 hours.Therefore, the method can not contain to the silk gum on natural silk degumming degree or silk in real time in process of production
Amount is monitored.
(2) still an alternative is that the silk gum tinctorial yield different from fibroin after the coloring of colouring, i.e. subjective observation, conventional
Colouring agent is carmine method.This method operation is relatively easy, it is not necessary to carry out sample balance, whole test process can be in phase
To being completed in the shorter time, but precision is not high, and measurement result can only be for qualitative analysis.
Therefore, a kind of content of silk gum of silk is relatively accurately obtained, following behaviour is generally performed according to traditional method
Make process：
1. after silk is balanced, weigh and obtain original weight；
2. silk is put into hot water, chemical assistant can also be added and carry out heating degumming；
3. after complete process 2, being tested with above-mentioned colouring, lay equal stress on if colouring agent not exclusively, is cleaned in degumming
Multiple step 2, until complete degumming
4. cleaning nett silk, it is dehydrated, dries, and be balanced in standard environment.
5. completing after balance, weigh, by the weight difference calculating silk before and after degumming containing de- rate.
Similarly, the introduction of professional standard FZ/T40004-2009 silks gum content test method is also provided in boiling temperature
Under, to stripping 30 minutes in 0.5g/L Na2C03 solution, this process thinks complete degumming after repeating degumming three times, passes through
Balance weighing calculates its gum content
As can be seen here, the measurement of traditional raw silk content of silk gum is a quite cumbersome process, and many due to existing
The process of secondary sampling and dye penetrant inspection, measurement accuracy is also difficult to control to.But this index again with later all processing technologys
There is close contact with product quality.This, which says, is not provided to raw silk content of silk gum in GB/T1797-2008 Raw silk sdandards
Although this bright index is extremely important, also it is the absence of effective means and goes to be controlled by.
The content of the invention
In contrast to the cumbersome of traditional silk gum content detection method, the present invention reports a kind of fast simple inspection herein
Survey method, so as to significantly shorten detection time, eliminates the error that the human factor in measurement process is caused as best one can.
Once-through operation obtains final result.
The key principle of the present invention is that raw silk is, by silk gum, the moieties of fibroin two composition, to make use of silk gum, fibroin and life
The composition of its protein of these three materials of silk and the difference of content cause its in thermogravimetric measurement process it is weightless
Speed and temperature spot it is inconsistent so as to inferring that calculating obtains the gum content in raw silk.
Specific detection method is described in detail as follows：
(1) to carrying out thermogravimetric analysis from the pure natural silk of different sources, Various Seasonal；
(2) to carrying out thermogravimetric analysis from the pure silk glue of different sources, Various Seasonal；
It is as follows about the method that obtains pure silk glue and fibroin：
1. then the silk is cleaned with pure 100-120 DEG C of degumming of hot water 60 minutes with hot water.This process can be repeated several times
(preferably 3 times) are until colouring shows complete degumming.
2. retaining degumming liquid, silk gum powder is made after concentration.It is spray-dried or freeze-drying is all that one kind can selecting technology.
Resulting fibroin silk gum is subjected to thermogravimetric analysis measurement.Various commercial thermogravimetric measuring instrument all can be used, and it heats up
Speed control is in 5-20 DEG C of scope, and preferably 10 DEG C/per minute, heating temperature range is 20-550 degree；Static atmosphere, ceramics or agate
Nao crucibles.Measurement the data obtained deposit database is available for the measurement of same specification raw silk in the future to do standard.Fig. 1 is typical silk heat
Weight curve map.We can be obtained before being warming up to 120 DEG C from figure, and the quality of silk has an obvious weightless process,
This process may be considered the evaporation process of institute's water content in silk.Afterwards, occurs one about between 150 DEG C to 200 DEG C
With respect to the process of constant weight.This represents that almost material is not decomposed because of the rise of temperature in this course.Next
Occurs obvious weightless process again.This phenomenon is same to be observed in the thermogravimetric measurement process of silk gum and fibroin.Difference
It is in different in weightless again initial temperature and weight loss rate.The present invention also exactly carries out raw silk using this difference and contains glue
The calculating of rate.
(3) traditional silk gum (optional) containing rate of the silk is measured with gravimetric method
This step work is option.Can be by tradition by the weight difference front and rear during silk gum fibroin is prepared to raw silk
Method obtain its silk gum containing rate, for further analysis is used from now on.The raw silk in standard environment is obtained it is possible thereby to calculate
Gum content.
(4) silk gum fibroin thermogravimetric change curve standard database is set up according to (1) to (3)
According to foregoing description, we can set up in standard database, database the explanation contained to raw silk specification, silk
The thermogravimetric measurement result of plain silk gum and traditional silk gum contain rate.
(5) thermogravimetric analysis is carried out to tested silk；
By unified thermogravimetric measuring method, carry out thermogravimetric analysis direct to raw silk, and obtain measurement result.Then phase is selected
The standard silk gum answered calculates the gum content of tested silk with fibroin curve and tested silk curve.
It is that, by standard fibroin, silk gum thermogravimetric analysis is bent to carry out raw silk gum content to calculate previous important process using the method
Line is standardized and constituted the basis that tested silk content of silk gum is calculated together with tested silk thermal gravimetric analysis curve：Number
Carried out as follows according to standardisation process：Using inhale quality of the exotherm in 160 degree or so of an exothermic peak starting point as
100%, without water quality, recalculates to measurement gained weight-loss curve and obtains standard curve.Curve such as Fig. 2 after typical standardization
It is shown.
The figure that silk gum after standardization, fibroin and tested silk are constituted forms two areas between 150 to 400 DEG C
Domain, region 1 (Area is 1.) is made up of fibroin curve with tested silk, and region 2 (Area is 2.) is made up of tested silk with silk gum.It is first
Choosing calculates temperature province can be between 160-320 DEG C.Region 1 (Area is 1.) and region 2 are obtained thus, it is possible to calculate (Area is 2.)
Area；It can further calculate and obtain tested silk silk gum system KTG, its computational methods is
It can be converted (optional) with traditional silk gum gum content according to KTG if desired.The method counted can be utilized
Set up KTG and traditional silk gum gum content corresponding relation each other and converted.Example is as shown in Figure 9.
The typical calculation flow chart of the summary present invention is as shown in Figure 3.
Brief description of the drawings
Fig. 1 is typical silk thermogravimetric curve figure
Fig. 2 is typical standard silk gum of the invention, and fibroin standardizes thermogravimetric curve figure with tested silk；
Fig. 3 is content of silk gum calculation flow chart of the present invention；
Fig. 4 is silk gum of the present invention, and fibroin and original Raw silk sdandard thermogravimetric calculate figure.
Fig. 5 is silk gum of the present invention, and fibroin and original raw silk are calculated through standardization thermogravimetric after 80 DEG C of hot water degummings 60 minutes schemes；
Fig. 6 is silk gum of the present invention, and fibroin and original raw silk are calculated through standardization thermogravimetric after 100 DEG C of hot water degummings 60 minutes
Figure；
Fig. 7 is silk gum of the present invention, and fibroin and original raw silk were through 120 DEG C of hot water degummings 60 minutes, with 1.5 DEG C per minute coolings
To 70 DEG C, then with 100 DEG C, standardization thermogravimetric calculates figure after 60 minutes washing process；
Fig. 8 is silk gum of the present invention, and fibroin and original raw silk were through 120 DEG C of hot water degummings 120 minutes, with 1.5 DEG C per minute drops
Temperature is to 70 DEG C, then with 100 DEG C, and standardization thermogravimetric calculates figure after 60 minutes washing process；
Fig. 9 is that survey calculation data and the relation of conventional method measurement raw silk gum content collect in example.
Embodiment
For the practicability of the further real example present invention, we make use of following equipment to carry out multiple authentication, specifically
Expression is in following example.Used equipment is uniformly described below in checking：
Synchronous (synthesis) thermal analyzer (DSC/DTA-TG) STA449C(the resistance to instrument manufacturing of speeding of Germany)
Specialty analysis balance：METTLER AT201ANALYTICAL BALANCE(International
Equipment Trading Ltd)
Assay balance：(the rich electronics technology in Suzhou City has Japanese SHIMADZU (Shimadzu) electronic analytical balances AUY220
Limit company
BUCHI spray dryers：Small spraying drying instrument B-290 (Bu Qi Co., Ltds of Switzerland)
Infrared heat pressure dyeing machine：AHIBA NUANCE TOP SPEED II(Datacolo Inc)
Baking oven memmert：(German beautiful and special Co., Ltd)
Raw silk material is a kind of raw silk that in the market is arbitrarily bought.By the raw silk purchased in infrared heat high pressure dyeing
With pure 120 DEG C of hot water degumming 60 minutes, then cleaned with hot water.This process is repeated 3 times.Until colouring shows complete degumming.
By the degumming liquid of reservation, silk gum powder is made with BUCHI spray dryers after concentration.
Resulting fibroin silk gum is subjected to thermogravimetric analysis measurement on synchronous (synthesis) thermal analyzer.Its programming rate is
Select 10 DEG C/it is per minute, heating temperature range be 30-450 DEG C；Static atmosphere, ceramic crucible.Obtain fibroin silk gum thermogravimetric curve.
This curve will be used as standard curve in follow-up each example.
Meanwhile, in order to further verify the present invention, when carrying out following each example measurements, while being measured with conventional weight method
Its gum content Kw.The test result of two kinds of different measuring methods collects as shown in Figure 9.Regression Analysis Result, which is shown between the two, to be had
Extraordinary correlation.R2 reaches 0.999.
Embodiment 1
As shown in figure 4, by raw silk purchased in market by 10 DEG C of programming rate/per minute, heating temperature range is 30-450 DEG C；It is static
Atmosphere, ceramic crucible carries out thermogravimetric measurement.Its measurement result merges silk gum, and fibroin generates silk gum, fibroin and original raw silk together
Standardize thermogravimetric and calculate figure.
It can calculate and obtain by preceding method：
Area 1.=288.47, Area 1.+2.=865, KTG%=33.35 and conventional method calculate gained raw silk and contain
Glue rate is Kw%=25.00
Embodiment 2
On the basis of experiment one, in order to test the raw silk of a variety of different gum contents, the present invention will be used in example one
After raw silk was with 80 DEG C of hot water degummings 60 minutes, removing unit sub-wire glue.Determine parameter by example one again and carry out thermogravimetric measurement.Marked
Measurement result after standardization is as shown in Figure 5.
It can calculate and obtain by preceding method：
Area 1.=280.41, Area 1.+2.=865, KTG%=32.42 and conventional method calculate gained raw silk and contain
Glue rate is Kw%=24.56
Embodiment 3
On the basis of experiment one, in order to test the raw silk of a variety of different gum contents, the present invention will be used in example one
After raw silk was with 100 DEG C of hot water degummings 60 minutes, removing unit sub-wire glue.Determine parameter by example one again and carry out thermogravimetric measurement.Obtain
Measurement result after standardization is as shown in Figure 6.
It can calculate and obtain by preceding method：
Area 1.=240.93, Area 1.+2.=865, KTG%=27.85 and conventional method calculate gained raw silk and contain
Glue rate is Kw%=18.91
Embodiment 4
On the basis of experiment one, in order to test the raw silk of a variety of different gum contents, the present invention will be used in example one
Raw silk is cooled to 70 DEG C, then with 100 DEG C, wash within 60 minutes, removing unit with 120 DEG C of hot water degummings 60 minutes with 1.5 DEG C per minute
Sub-wire glue.Determine parameter by example one again and carry out thermogravimetric measurement.Measurement result after being standardized is as shown in Figure 7.
It can calculate and obtain by preceding method：
Area 1.=54.64, Area 1.+2.=865, KTG%=6.32 and conventional method calculate gained raw silk and contain glue
Rate is Kw%=2.16
Embodiment 5
On the basis of experiment one, in order to test the raw silk of a variety of different gum contents, the present invention will be used in example one
Raw silk is cooled to 70 DEG C, then with 100 DEG C, wash within 60 minutes, removing unit with 120 DEG C of clocks of hot water degumming 120 with 1.5 DEG C per minute
Sub-wire glue.Determine parameter by example one again and carry out thermogravimetric measurement.Measurement result after being standardized is as shown in Figure 8.
It can calculate and obtain by preceding method：
Area 1.=46.98, Area 1.+2.=865, KTG%=5.43 and conventional method calculate gained raw silk and contain glue
Rate is Kw%=1.58.
Claims (5)
1. a kind of sericin content in silk detection method, it is characterised in that comprise the following steps：
I. set up the thermogravimetric change curve of different sources, the fibroin of Various Seasonal and silk gum and inhale exotherm standard database；
II. thermogravimetric analysis is carried out to tested silk, records the tested silk data including thermogravimetric curve and suction exotherm；
III. corresponding with tested silk data fibroin normal data and silk gum normal data in selection standard database, calculate quilt
Survey the characterization parameter K of silkTG；
The step I comprises the following steps：
I-1. to from different sources, Various Seasonal pure natural silk carry out thermogravimetric analysis, record include the place of production, season,
Fibroin normal data including thermogravimetric curve and suction exotherm data；
I-2. to from different sources, Various Seasonal silk pure silk glue carry out thermogravimetric analysis, record include the place of production, season,
Silk gum normal data including thermogravimetric curve and suction exotherm data；
The step III comprises the following steps：
III-1. corresponding with tested silk data fibroin normal data and silk gum normal data in selection standard database；
III-2. the suction exotherm being tested in silk data, fibroin normal data and silk gum normal data is analyzed, with
Quality in 160 degree or so of an exothermic peak starting point is used as starting point pair without water quality, and using this as 100% without water quality
Thermogravimetric change curve in tested silk data, fibroin normal data and silk gum normal data is standardized；
III-3. the thermogravimetric in tested silk data, fibroin normal data and the silk gum normal data after standardization is become
Change curve is integrated respectively tries to achieve area, and further obtains the thermogravimetric change curve and tested silk number of fibroin normal data
According to the Area areas 1. that constitute of thermogravimetric change curve and tested silk data thermogravimetric change curve and silk gum normal data
The Area areas 2. that constitute of thermogravimetric change curve；
III-4. the characterization parameter K of tested silk is calculated according to below equationTG：
；
The step I is further comprising the steps of：
I-3. traditional silk gum K containing rate from different sources, the silk of Various Seasonal is measured with gravimetric methodw, and the silk is entered
Row thermogravimetric analysis, record includes the place of production, season, traditional silk gum K containing ratewWith the silk normal data including thermogravimetric curve；
I-4. the silk normal data in the identical place of production and season, silk gum normal data and fibroin standard in selection standard database
Data；
I-5. the suction exotherm in silk normal data, fibroin normal data and silk gum normal data is analyzed, with
Quality during 160 degree or so of an exothermic peak starting point as 100% without water quality, and using this without water quality as starting point to silkworm
Thermogravimetric change curve in silk normal data, fibroin normal data and silk gum normal data is standardized；
I-6. the thermogravimetric in the silk normal data after standardization, fibroin normal data and silk gum normal data is changed
Curve is integrated respectively tries to achieve area, and further obtains the thermogravimetric change curve and silk normal data of fibroin normal data
The Area areas 1. that constitute of thermogravimetric change curve and silk normal data thermogravimetric change curve and silk gum normal data
The areas of the Area that thermogravimetric change curve is constituted 2.；
I-7. the characterization parameter K of silk normal data is calculated and recorded according to below equationTG：
；
I-8. the characterization parameter K of silk normal data is calculatedTGWith traditional silk gum K containing ratewRelation curve；
Described sericin content in silk detection method is further comprising the steps of：
IV. according to the characterization parameter K of silk normal dataTGWith traditional silk gum K containing ratewRelation curve, by the table of tested silk
Levy parameter KTGIt is scaled traditional silk gum K containing ratew。
2. sericin content in silk detection method according to claim 1, it is characterised in that the thermogravimetric analysis parameter is such as
Under：Thermogravimetric measurement is carried out in static atmosphere, heating temperature range is at 20-500 DEG C, and firing rate is at 5-20 DEG C/min.
3. sericin content in silk detection method according to claim 2, it is characterised in that：The thermogravimetric analysis parameter is such as
Under：
Thermogravimetric measurement is carried out in static atmosphere, heating temperature range is at 30-450 DEG C, and firing rate is at 10 DEG C/min.
4. the sericin content in silk detection method according to claim 1 any one, it is characterised in that：The Area 1. and
The calculating temperature provinces of Area 2. are 160-400 DEG C.
5. sericin content in silk detection method according to claim 4, it is characterised in that：The Area 1. with Area 2.
It is 160-320 DEG C to calculate temperature province.
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| CN107421845A (en) * | 2017-09-18 | 2017-12-01 | 山东大学 | A kind of quick analysis and identification Weihai sea cucumber, Russian red ginseng and the method for eggplant ginseng |
| CN107907441A (en) * | 2017-11-13 | 2018-04-13 | 山东大学 | A kind of quick method for differentiating plantain seed and lepidium seed |
| CN111060418B (en) * | 2019-12-16 | 2022-08-02 | 广东溢达纺织有限公司 | Yarn dryness judging method |
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| CN102590012A (en) * | 2011-12-20 | 2012-07-18 | 苏州大学 | Method for measuring gel rate of silk flosses |
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| JPS56125647A (en) * | 1980-03-07 | 1981-10-02 | Toshiba Corp | Thermogravimetric analyzing method and its apparatus |
| CN1828273A (en) * | 2006-03-15 | 2006-09-06 | 东华大学 | Method for determining regenerated silk fibroin water solution concentration |
| CN102042940A (en) * | 2010-11-12 | 2011-05-04 | 中国烟草总公司郑州烟草研究院 | Gradient cracking method for researching compound cracking process |
| CN102590012A (en) * | 2011-12-20 | 2012-07-18 | 苏州大学 | Method for measuring gel rate of silk flosses |
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