Method for detecting ancient silk fabric

A technology of silk fabrics and silk fibroin, which is applied in the field of cultural relics detection, can solve problems such as low sensitivity, unsuitability for cultural relics detection, and large influence of impurities, and achieve high sensitivity, excellent sensitization and modifiability, and enhanced sensitivity.

Active Publication Date: 2019-01-11
ZHEJIANG SCI-TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And as an organic polymer material, mulberry silk is easily degraded by light, heat, acid-base, microorganisms, etc., resulting in changes in crystallinity, molecular weight and other structure and properties. Therefore, conventional detection method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1) Weigh 5g of mulberry silk and place it in 180mL of 0.018M sodium carbonate solution, in a water bath for 55 minutes, and the temperature of the water bath is 80°C, take it out and wash it with deionized water three times, and put it in an oven to dry.

[0029] 2) Take 2g of dried silk fibroin, 2.3g of calcium nitrate, add 48mL of formic acid, magnetically stir for 80min, filter and add sodium bicarbonate until the solution is neutral, and use a cellulose dialysis bag with a molecular weight cut-off of 8000 to remove the resulting solution. After dialysis in ionized water for 2 days, and changing the water every 5 hours, the silk fibroin solution was freeze-dried in a vacuum freeze dryer for 2 days, and the obtained silk fibroin was ground into powder for use.

[0030] 3) Take 2.8mL of graphene oxide with a concentration of 5mg / mL, soak it in 0.2M propylenediamine and reflux for 2.8h at 65℃; then, add 5ml of 0.1% (w / v) sodium hexachloroplatinate to the previous After conti...

Embodiment 2

[0040] 1) Weigh 5g of mulberry silk and place it in 200mL of 0.02M sodium carbonate solution, in a water bath for 60 minutes, the temperature of the water bath is 80℃, take it out and wash it with deionized water four times, and put it in an oven to dry.

[0041] 2) Take 2g of dried silk fibroin, 2.5g of calcium nitrate, add 50mL of formic acid, stir with a magnetic force for 90 minutes, filter and add sodium bicarbonate until the solution is neutral, and use a cellulose dialysis bag with a molecular weight cut-off of 9000 to remove the resulting solution. Dialysis in ionized water for 2.5 days and changing the water every 6 hours. After freeze-drying the silk fibroin solution in a vacuum freeze dryer for 2.5 days, the resulting silk fibroin is ground into powder for use.

[0042] 3) Take 3mL of graphene oxide with a concentration of 6mg / mL, soak it in 0.3M propylenediamine and reflux for 3h at 70℃; then, add 5.5ml of 0.1% (w / v) sodium hexachloroplatinate to the previous In the mix...

Embodiment 3

[0052] 1) Weigh 5g of mulberry silk and place it in 220mL of 0.022M sodium carbonate solution, in a water bath for 65 min, and the temperature of the water bath is 80°C, take it out and wash it with deionized water five times, and put it in an oven to dry.

[0053] 2) Take 2g of dried silk fibroin, 2.7g of calcium nitrate, add 52mL of formic acid, stir with a magnetic force for 100min, filter and add sodium bicarbonate until the solution is neutral, and use a cellulose dialysis bag with a molecular weight cut-off of 10,000 to remove the resulting solution. After dialysis in ionized water for 3 days, and changing the water every 7 hours, the silk fibroin solution was freeze-dried in a vacuum freeze dryer for 3 days, and the obtained silk fibroin was ground into powder for use.

[0054] 3) Take 3.2mL of graphene oxide with a concentration of 7mg / mL, soak it in 0.4M propylenediamine and reflux for 3.2h at 75℃; then, add 6ml of 0.1% (w / v) sodium hexachloroplatinum to the previous After...

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PUM

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Abstract

The invention relates to the field of cultural relic detection and discloses a method for detecting an ancient silk fabric. The method comprises the following steps: extracting silk fibroin by adopting formic acid and a calcium nitrate solution system; then preparing a graphene nano compound modified working electrode through a mixed system of graphene oxide, propylene diamine, sodium hexachloroplatinate hexahydrate and sodium borohydride; successively modifying a silkworm silk fibroin antibody and a detected sample on the working electrode; and electrochemically detecting current value respectively, and judging whether the sample is the silk fabric or not through analyzing the changes of the current value. The method provided by the invention is simple to operate and high in sensitivity.

Description

Technical field [0001] The invention relates to the field of cultural relic detection, in particular to a method for detecting ancient silk fabrics. Background technique [0002] China has been a major textile country since ancient times, producing a rich variety of textiles, exquisite craftsmanship, and comfortable and breathable. One of the most prestigious textiles is China's silk, so China is also known as "the country of silk." The main component of silk is mulberry silk, which is mainly composed of silk fibroin and sericin. Silk fibroin is the main component of silk, accounting for about 70% of the total weight. And as an organic polymer material, mulberry silk is easily degraded under the influence of light, heat, acid and alkali, microorganisms, etc., resulting in changes in structure and properties such as crystallinity and molecular weight. Therefore, conventional detection methods have low sensitivity and are interfered by impurities It has a large impact and is not...

Claims

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Application Information

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IPC IPC(8): G01N27/416
CPCG01N27/416
Inventor 王秉李青青刘林帅欧阳毅彭志勤胡智文
Owner ZHEJIANG SCI-TECH UNIV
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