본 연구는 꼭두서니와 그 표준 색소인 알리자린으로 염색한 직물에 조건적 퇴화를 유도하고, 가스 크로마토그라피 질량분석기(GC-MS)를 이용해 퇴화물을 분석하여 이를 선행연구에서 밝혀진 표준 알리자린 색소의 퇴화물과 비교함으로써 대조구로서의 꼭두서니 염료의 정보를 완성하는데 그 목적을 둔다. 아울러 퇴화 전후 염직물의 색차를 측정하여 조건퇴화에 따른 색의 변화를 조사하였다. 퇴화조건은 상온 (RT), 저온$(7^{\circ}C)$ (LT), 고온$(100^{\circ}C)$(OV)의 세 종류의 온도 조건과 염료 폐수처리 용도로 활용되고 있는 $H_2O_2/UV$법 (PER)을 사용하였다. 퇴화시간은 6시간, 24시간, 48시간, 1주, 2주, 4주 각각을 측정하였다. 꼭두서니와 알리자린 염직물 모두 퇴화 전후의 시료에서 alizarin(10.1분)이 검출되었다. 꼭두서니와 알리자린 염직물 모두 퇴화 후 benzoic acid(4.7분), 2,4-di-tert-butylphenol(6.8분), phthalic anhydride(5.8분)가 검출되었다. 꼭두서니와 알리자린 염직물 모두 퇴화 후 붉은색과 노란색이 감소하였다. 꼭두서니 염직물보다 알리자린 염직물의 경우 퇴화 전후의 색차가 더 심하였다. 그러나 가장 퇴화조건이 강한 PER퇴화조건 하에서는 꼭두서니 염직물의 색차가 1주 경과 후에도 매우 심하게 나는 것을 볼 수 있었다. 본 연구의 결과꼭두서니와 그 표준 색소로 염색한 직물이 퇴화할 경우에도 선행연구에서 밝혀진 알리자린의 퇴화물인 benzoic acid, 2,4-di-tert-butylphenol, phthalic anhydride가 검출됨을 확인하였다. 따라서 이들 화합물은 갈변되어 고유의 색을 알 수 없는 출토복식의 염료를 판정할 때 꼭두서니 염료의 사용여부를 확인할 수 있는 대조구 화합물로 사용될 수 있을 것으로 사료된다. 퇴화 전후의 색차에 대한 측정결과는 퇴화에 따른 염료의 색 변화에 대한 결과이다 출토복식의 갈변현상은 염료의 변색과 더불어 토양 유기물에 의한 착색도 기인하므로, 출토복식의 색상 변화를 실질적으로 조사하기 위해서는 본 연구의 결과와 함께 토양유기물에 의한 착색에 대한 연구가 병행되어야 할 것으로 본다
본 연구는 꼭두서니와 그 표준 색소인 알리자린으로 염색한 직물에 조건적 퇴화를 유도하고, 가스 크로마토그라피 질량분석기(GC-MS)를 이용해 퇴화물을 분석하여 이를 선행연구에서 밝혀진 표준 알리자린 색소의 퇴화물과 비교함으로써 대조구로서의 꼭두서니 염료의 정보를 완성하는데 그 목적을 둔다. 아울러 퇴화 전후 염직물의 색차를 측정하여 조건퇴화에 따른 색의 변화를 조사하였다. 퇴화조건은 상온 (RT), 저온$(7^{\circ}C)$ (LT), 고온$(100^{\circ}C)$(OV)의 세 종류의 온도 조건과 염료 폐수처리 용도로 활용되고 있는 $H_2O_2/UV$법 (PER)을 사용하였다. 퇴화시간은 6시간, 24시간, 48시간, 1주, 2주, 4주 각각을 측정하였다. 꼭두서니와 알리자린 염직물 모두 퇴화 전후의 시료에서 alizarin(10.1분)이 검출되었다. 꼭두서니와 알리자린 염직물 모두 퇴화 후 benzoic acid(4.7분), 2,4-di-tert-butylphenol(6.8분), phthalic anhydride(5.8분)가 검출되었다. 꼭두서니와 알리자린 염직물 모두 퇴화 후 붉은색과 노란색이 감소하였다. 꼭두서니 염직물보다 알리자린 염직물의 경우 퇴화 전후의 색차가 더 심하였다. 그러나 가장 퇴화조건이 강한 PER퇴화조건 하에서는 꼭두서니 염직물의 색차가 1주 경과 후에도 매우 심하게 나는 것을 볼 수 있었다. 본 연구의 결과꼭두서니와 그 표준 색소로 염색한 직물이 퇴화할 경우에도 선행연구에서 밝혀진 알리자린의 퇴화물인 benzoic acid, 2,4-di-tert-butylphenol, phthalic anhydride가 검출됨을 확인하였다. 따라서 이들 화합물은 갈변되어 고유의 색을 알 수 없는 출토복식의 염료를 판정할 때 꼭두서니 염료의 사용여부를 확인할 수 있는 대조구 화합물로 사용될 수 있을 것으로 사료된다. 퇴화 전후의 색차에 대한 측정결과는 퇴화에 따른 염료의 색 변화에 대한 결과이다 출토복식의 갈변현상은 염료의 변색과 더불어 토양 유기물에 의한 착색도 기인하므로, 출토복식의 색상 변화를 실질적으로 조사하기 위해서는 본 연구의 결과와 함께 토양유기물에 의한 착색에 대한 연구가 병행되어야 할 것으로 본다
The purpose of this investigation was to investigate the degradation products of the dye component extracted from madder dyed fabrics using the GC-MS analysis and to evaluate the change of color due to degradation treatment. Four different degradation protocols were used in this study,; refrigeratio...
The purpose of this investigation was to investigate the degradation products of the dye component extracted from madder dyed fabrics using the GC-MS analysis and to evaluate the change of color due to degradation treatment. Four different degradation protocols were used in this study,; refrigeration at $7^{\circ}C$ (LT), room temperature (RT), oven treatment at $100^{\circ}C$ (OV), and $H_2O_2/UV(PER)$ method. Degradation times for each thermal system were 6 hour, 24 hour, 48 hour, 1 week, 2 week, 4 week. Alizarin was detected from the control and degraded samples of both alizarin dyed and madder dyed fabrics. Benzoic acid, 2, 4-di-tert-butylphenol, phthalic anhydride were detected as the degradation products for both alizarin dyed and madder dyed fabrics. The result suggest that these products can be used as the fingerprints of GC-MS analysis for the identification of madder dye in archaeological textiles. Both alizarin dyed and madder dyed samples became less red and less yellow after degradation. In the PER degradation system madder dyed sample showed the greatest color difference even after 1 week of degradation treatment. Further research is necessary for investigating the color change in the exhumed textiles, which is caused by the dual action of dye fading and the staining of organic matters in the soil.
The purpose of this investigation was to investigate the degradation products of the dye component extracted from madder dyed fabrics using the GC-MS analysis and to evaluate the change of color due to degradation treatment. Four different degradation protocols were used in this study,; refrigeration at $7^{\circ}C$ (LT), room temperature (RT), oven treatment at $100^{\circ}C$ (OV), and $H_2O_2/UV(PER)$ method. Degradation times for each thermal system were 6 hour, 24 hour, 48 hour, 1 week, 2 week, 4 week. Alizarin was detected from the control and degraded samples of both alizarin dyed and madder dyed fabrics. Benzoic acid, 2, 4-di-tert-butylphenol, phthalic anhydride were detected as the degradation products for both alizarin dyed and madder dyed fabrics. The result suggest that these products can be used as the fingerprints of GC-MS analysis for the identification of madder dye in archaeological textiles. Both alizarin dyed and madder dyed samples became less red and less yellow after degradation. In the PER degradation system madder dyed sample showed the greatest color difference even after 1 week of degradation treatment. Further research is necessary for investigating the color change in the exhumed textiles, which is caused by the dual action of dye fading and the staining of organic matters in the soil.
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문제 정의
Considering the complex nature of the madder extraction, the question rises to whether the same degradation products of standard alizarin reported in the previous literature(Ahn & Obendorfe 2004) are observed in madder dyed textiles, which is the ultimate form of standard comparable to archaeological textiles. Based on the above questions, the purpose of this investigation was to investigate the degradation products of the dye component extracted from madder dyed fabrics and to evaluate the change of color due to degradation treatment. Comparisons will be made between the degradation products detected from the present investigation and those identified in our previous research on the degradation of standard alizarin.
This paper deals with the identification of degradation products in the madder dyed textiles. The investigation is part of our continuing effort for the identification of dyes in badly faded textiles of archaeological origin. In our previous study(Ahn & Obendorfe 2004), we have designed and experimented the two major degradation conditions, thermal and H2O2/UV treatments, in order to indirectly simulate the burial induced fading observed in archaeological textiles.
This paper deals with the identification of degradation products in the madder dyed textiles. The investigation is part of our continuing effort for the identification of dyes in badly faded textiles of archaeological origin.
가설 설정
5. The color difference was more prominent in alizarin dyed fabrics. In the PER degradation system which is the most accelerated degradation system of the present investigation, madder dyed sample showed the greatest color difference even after 1 week of degradation treatment.
제안 방법
Degradation times for each thermal system were 6 hour, 24hour? 48hour, 1 week, 2week, 4week. For H2O2/UV degradation, 2cmx 10cm size dyed fabrics were immersed in separate vials with 30% H2O2 solution and the vials were placed under the UV lamp (365nm, UVL-18, UVP, Upland CA) at room temperature for 6hour 24hour, 1 week, and 2week.
The purpose of this investigation was to investigate the degradation products of the dye component extracted from madder dyed fabrics using gas chromatography mass spectroscopy and to evaluate the change of color of the dye fabrics after degradation treatment. The results were as follows:
The result of the present investigation suggest that the four degradation products identified in our previous research can be used as the fingerprints of GC- MS analysis for the identification of madder dye in badly faded archaeological textiles. However, further research needs to be carried out in order to investigate the color change in the exhumed textiles which is caused by the dual action of dye fading and the staining of organic substance in the soil.
The assignment of possible degradation products was based on the match with standard mass spectrum available in the GC-MS library database(Agilent Technologies, 2000). The structural assignments of four main degradation products identified by GC-MS analysis were verified further by comparing their MS spectra with those of known chemicals. Color of madder and standard alizarin dyed fabrics were evaluated in terms of CIE Lab data(D65/10) measured with the Macbeth Color-eye 1500/PLUS Color Measurement System with Optiview software version 2.
대상 데이터
Metha- nol(HPLC grade) was purchased from Mal-linckrodt Baker(Paris, KY). 30% H202(ACS reagent grade) was purchased from J. T. Baker(Phillipsburg, NJ). Reagent grade H2SO4 and HCl were purchased from EM Sci- ence(Darmstadt, NJ).
Alizarin(l, 2 dihydroxyanthraquinone, 97% purity) was purchased from Sigma Aldrich(Milwaukee, WI) and used without further purification. Dried madder root was purchased from Korean traditional medicinal market.
Alizarin(l, 2 dihydroxyanthraquinone, 97% purity) was purchased from Sigma Aldrich(Milwaukee, WI) and used without further purification. Dried madder root was purchased from Korean traditional medicinal market.
Potassium aluminum sulfate was purchased from Shinyo Pure Chemicals(Osaka, Japan). Benzoic acid, 2, 4-di-tert-butylphenol, phthalic a가hydride, and dimethyl phthalate were all ACS reagent grades purchased from Sigma Aldrich(Mil- waukee, WI). Silk fabric used for dyeing was standard silk fabric(KS K0905) purchased from Korea Apparel Testing & Research Institute.
Alizarin(l, 2 dihydroxyanthraquinone, 97 % purity) was purchased from Sigma Aldrich(Milwau- kee, WI) and used without further purification. Metha- nol(HPLC grade) was purchased from Mal-linckrodt Baker(Paris, KY). 30% H202(ACS reagent grade) was purchased from J.
성능/효과
3. In both madder dyed and alizarin dyed fabrics, the samples became brighter after degradation treatment and the increase of brightness was greater with degradation progression.
4. After degradation treatment both alizarin dyed and madder dyed samples became less red and less yellow.
후속연구
The usefulness of 1 -phe- nylalamine, methyl ester, 2, 5-peperazinedione, 3- (phenylmethyl)-, and 2, 5-piperazinedione, 3, 6-bis(2- methylphenyl)- in the identification of badly faded archaeological textiles dyed with madder is yet uncertain. However it is important to note their detection in the degradation of our madder and standard alizarin dyed fabrics for further comparative research on silk fabrics dyed with other natural dyestuffs. There were several other products repeatedly detected from our degraded fabric extracts.
The result of the present investigation suggest that the four degradation products identified in our previous research can be used as the fingerprints of GC- MS analysis for the identification of madder dye in badly faded archaeological textiles. However, further research needs to be carried out in order to investigate the color change in the exhumed textiles which is caused by the dual action of dye fading and the staining of organic substance in the soil.
참고문헌 (16)
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