高温燃烧-水蒸气吸收-离子色谱法测定纺织品中的有机卤化物

建立了高温燃烧-水蒸气吸收-离子色谱同时测定纺织品中有机氟、有机氯、有机溴和有机碘的分析方法.首先采用振荡方式去除纺织品中的无机卤化物得到试样,之后通过设计一种新型的高温燃烧吸收装置,采用程序升温方式对试样进行高温氧化燃烧、裂解及气化,产生的游离态卤素和卤化氢等气体被水蒸气吸收并完全转化为无机卤素阴离子,冷凝收集后用离...     

微库仑法测定固体样品中的可吸附有机卤化物

建立了一种固体样品中可吸附有机卤化物(AOX)的分析方法。通过恒温条件下的混合振荡提取固体样品中的有机卤化物,利用活性碳对有机卤化物进行富集,采用微库仑法对AOX进行检测。对比振荡吸附柱压滤法和振荡吸附抽滤法分析结果,表明柱压滤法在系统空白值、回收率和精密度方面都要优于抽滤法,其系统空白值为0.44μg(Cl-),空白加标回收率为93.8%~99.0%。利用本方法对沉积物和土壤中的AOX进行了测定。     

氧弹燃烧-离子色谱法测定高分子聚合物的卤素离子

采用氧弹燃烧法对塑料样品进行燃烧,用碳酸钠作为吸收液进行吸收,建立了离子色谱法分离测定微量卤素离子的方法.离子色谱条件为:IonPac AS22离子交换柱,碳酸盐等度淋洗,抑制型电导检测.用该方法对塑料颗粒和塑料瓶盖中的氯离子进行测定,加标回收率分别为92.25%～95.68%、92.37% ～95.52%.     

高温燃烧-离子色谱测定导电胶中氯和溴

采用高温燃烧吸收仪与离子色谱仪联用技术，建立了测定导电胶中卤素含量的方法。优化的实验条件为：燃烧炉温度为800℃，样品质量为0.1 g，以0.05 mol/L氢氧化钠为吸收液，0.02 mol/L氢氧化钾为淋洗液，采用抑制型电导检测器检测。氯、溴离子质量浓度在1～50 mg/L范围内与对应色谱峰面积线性关系良好，氯离子的线性相关系数r=0.999 7，检出限为5.4 mg/kg，加标的平均回收率为101.2%；溴离子线性相关系数r=0.999 7，检出限为8.6 mg/kg，加标的平均回收率为100.2%。与传统氧弹燃烧-离子色谱法相比，该法无需对样品进行固化处理，进样方便、快捷，可用于导电胶样品中卤素含量的测定。     

离子色谱法测定铜粉中的卤素离子

用离子色谱法测定了铜粉中卤素的含量. 采用酸溶法溶解固体铜粉样品以提取其中的卤化物, 然后分别除去过量的铜离子和硫酸根离子, 排除干扰, 以达到进样要求. 优化了溶解酸、 H2O2及其用量、淋洗液及流速等实验条件. 该方法加标平均回收率为97.4%～102.1%, 可用于实际铜粉样品的测定.     

氧弹燃烧-离子色谱法测定电子产品连接线中的卤素

建立了氧弹燃烧法处理电子产品连接线,离子色谱测定样品中卤素的分析方法。选用TSK-gelSuperIC-AZ阴离子分析柱,以NaHCO3(7.5mmol/L)+Na2CO3(1.1mmol/L)为流动相等度洗脱,抑制电导检测。结果表明,该条件下F-浓度在0.02～2mg/L,Cl-和Br-浓度在0.05～5mg/L范围内峰面积与浓度的线性关系良好(r>0.999),实际样品中卤素回收率为90.52%～97.24%,样品测定结果相对标准偏差均为0.73%～2.01%(n=5)。应用氧弹燃烧-离子色谱法测定电子产品连接线中的卤素离子,方法简便、快捷,测定结果准确。     

高温热水解离子色谱法快速同时测定粘土中的卤素

建立高温热水解分解粘土样品,离子色谱快速同时测定其中的氟、氯、溴和碘含量的方法。优化了影响粘土高温热水解的主要参数,得到以下最佳测定条件:2.0 g粘土,反应温度1000℃,停留时间10 min,样品与催化剂V2O5质量比为1∶1,空气流量90 mL/min,15 mL 5.4 mmol/L Na2CO3和5.1 mmol/L NaHCO3混合溶液为粘土释放卤素的吸收液;考察了粘土高温热水解后卤素的赋存形态。结果表明,这些卤素在吸收液中以F!、Cl!、Br!和I!形式存在,且能被离子色谱很好地分离。粘土样品较好的卤素加标回收率和较小的相对标准偏差及土壤标准物质中卤素的评估说明本方法的准确度和精密度良好。分析了4个粘土样品,氟、氯、溴和碘的检出限分别为0.030,0.043,0.09和0.13#g/g,本方法简单、可靠、低消耗和快速,每小时可分析5个样品,可同时分析粘土和其它无机基质中的氟、氯、溴和碘的含量。     

氧弹燃烧-离子色谱法测定电子产品中卤素

采用氧弹燃烧法对试样进行燃烧,然后用水作为吸收液进行吸收,提出了离子色谱法分离测定电子产品中卤素含量的方法。以Metrosep A Supp 4型阴离子分析柱为离子交换柱,以1.8mmol·L~(-1)碳酸钠-1.7mmol·L~(-1)碳酸氢钠溶液为淋洗液等度洗脱。3种卤素离子氟离子、氯离子和溴离子的方法检出限(3S/N)依次为4.0,5.6,20.5μg·L~(-1)。该方法已用于电子产品中卤素的测定。     

柱前衍生-气相色谱/质谱-选择离子法测定纺织品中烷基酚的方法研究

建立了纺织品中壬基酚和辛基酚的提取与含量测定方法.纺织品样品经以CH2Cl2为萃取液的超声提取、衍生化后,采用气相色谱/质谱-选择离子定量分析方法,对4-壬基酚同分异构体总量和4-n-辛基酚进行了定量检测.通过实验对前处理条件、衍生化条件、色谱条件、选择离子等作了优化.该方法的加标回收率为80.73%～99.78%,相对标准偏差小于5%.方法适用于纺织品中烷基酚的含量分析.     

超声辅助-固相分散溶液提取离子色谱法测定染发剂中的9种染料中间体

建立了提取和清洗整合成一步的超声辅助-固相分散溶液提取离子色谱法测定染发剂中的9种染料中间体的方法。样品基质经分散后,测定组分进入溶液,油脂溶解在正己烷中,干扰化合物被分散剂吸附。在振荡、超声和加热的协同作用下,9min内快速完成提取,具有高的样品处理效率。用离子色谱法测定商业染发剂中的中间体以确定方法的提取效率。方法的线性范围为0.2～100mg/L,检出限0.019～0.048mg/L,回收率85.0%～107.0%,相对标准偏差0.3%～3.7%。实验结果表明,方法简单、可靠,适用于大批量样品的常规分析。     

Solid Phase Micro-extraction – Gas Chromatography–Mass Spectrometry to Characterize Pyrolysis Products from Textiles

Headspace solid phase micro-extraction gas chromatography–mass spectrometry (HS-SPME GC–MS) was used for identifying thermally labile volatile compounds from cotton, wool, polyester, olefin, silk, and acrylic. Volatile compounds were generated from the textiles using a pyrolysis apparatus prior to GC–MS. Pyrolysis temperatures ranged from 190 to 550°C. Each textile displayed a unique chromatogram containing compounds that were consistent with the chemical structure of the textile. Experimental parameters that were investigated included the temperature, sample size, and sampling time to determine their effect on the number and intensity of peaks in the chromatograms as well as to identify optimum conditions for analysis. Heating of each sample was achieved using a resistively heated Pt wire. Full pyrolysis at 550°C of the textiles appeared to give the best results in terms of peak height relative to background. A range of sample sizes (0.02–1.5?mg) were used and, generally, ≤0.02?mg was used for identifying the textiles. The reproducibility of retention times for selected compounds in the chromatograms was less than 1% relative standard deviation. The combination with mass spectrometry provided valuable structural information.     

ICP-OES determination of metals present in textile materials

The aim of this work was to quantify the content of elements present in textile materials since it is known that textiles containing metals may represent a health hazard to consumers. Determination of metal content can be also useful to the textile industry since some metals present in textiles may contribute to problems during textile production. Extraction of metals from different textile materials was performed in an artificial acidic sweat solution according to the Öko Tex standard for materials coming into direct contact with the skin. After extraction from textile products made of cotton, flax, wool, silk, viscose, and polyester materials, all elements were determined by means of inductively coupled plasma-optical emission spectrometry (ICP-OES). Results in the sweat extracts (minimum-maximum in μg/mL) were: Al 0.11-1.58, Cd 0.02-0.05, Cr 0.01-0.32, Cu 0.05-1.95, Mn 0.01-2.17, and Ni 0.05-0.10. Concentrations of other elements were bellow detection limits. The total amount of metals present was determined after microwave assisted acidic digestion of textile materials with 7 M nitric acid. According to the results, the majority of the detected elements were below the concentration limits given by the Öko Tex, and for this reason the textile materials investigated do not represent a health hazard to consumers.     

中空纤维液相微萃取-高效液相色谱法测定纺织品中10种含氯苯酚类化合物

建立了中空纤维液相微萃取-高效液相色谱法测定纺织品中10种含氯苯酚类化合物的方法。系统地优化了影响萃取效率的因素,得到的最佳萃取条件为：萃取溶剂为正己烷,接受相NaOH溶液的浓度为0.10 mol/L,萃取时间为60 min,搅拌速度为600 r/min。在最佳萃取条件下,10种含氯苯酚在0.01～1.00 mg/L范围内线性关系良好（r>0.999）,10种含氯苯酚的检出限（信噪比为3）为0.01 mg/kg,富集倍数为95～101。在空白样品中添加0.01、0.05和0.1 mg/kg 3个不同水平的10种含氯苯酚类化合物,其平均回收率为78.8%～105.1%,相对标准偏差为0.3%～7.3%。研究结果表明该方法灵敏度高、简便、准确,可用于纺织品中含氯苯酚类化合物的测定。     

Toward a comprehensive understanding of textiles functionalized with silver nanoparticles

This article provides a comprehensive understanding of development of textiles functionalized with silver nanoparticles (AgNPs). There are three established methods to fabricate textiles functionalized with AgNPs, namely, solution‐immersion, layer‐by‐layer deposition, and sonochemical. In addition, several textile types such as cotton, wool, polyester, silk, cotton/polyester blend, polyamide, and regenerated cellulose have been used for the fabrication. The AgNP deposition mechanism on textiles is mainly due to electrostatic interaction between AgNPs and textile constituents. It was exhibited that the deposition of AgNPs on textiles can transform their textiles colors. In addition, it was demonstrated that the deposition of AgNPs on textiles is not permanent, particularly against washing treatment. Textiles modified with AgNPs have several promising applications such as antibacterial, antifungal, catalyst, electronic devices, water treatment, sun protection, air treatment, and surface‐enhanced Raman scattering, which are comprehensively discussed in this article. Future challenges in fabricating textiles functionalized with AgNPs remain on how this can be carried out to improve long‐term stabilization of AgNPs on textiles to achieve their permanent deposition by employing greener approaches.     

A spectrometric and chromatographic approach to the study of ageing of madder (Rubia tinctorum L.) dyestuff on wool

In this work, the lightfastness of wool textile samples, dyed with madder and its principal components alizarin and purpurin, was investigated using two complementary experimental techniques: absorption and emission UV-vis spectroscopy and chromatography (HPLC-PDA). Spectroscopic techniques were used to follow the time course of ageing, whereas chromatography was applied to determine relative compositional changes that occurred after exposure of wool dyed samples to natural and artificial ageing. The results from the two techniques integrate well each other and provide complementary and useful indications about the sensitivity of the dyed textiles to ageing, showing that purpurin is the principal component responsible for the spectral and chromatic properties of madder as well as for its degradation. The fading of both the fibre and dye is reduced in the presence of alum and in the absence of oxygen. The multi-analytical approach used highlights the potential of the UV-vis spectroscopy for the investigation of dyes on textiles. The great sensitivity of the spectrofluorimetry makes this technique particularly promising for a non-destructive study of dyes on works of art.     

气相色谱-三重四极杆质谱法同时测定纺织品中11种挥发性全氟化合物前体物

以甲醇为提取溶剂,超声辅助提取纺织品中的全氟化合物前体物,建立了一种气相色谱-三重四极杆质谱(GC-MS/MS)法同时测定纺织品中11种挥发性全氟化合物前体物:4种氟调聚物醇(FTOHs)、3种氟调聚丙烯酸酯(FTAs)、2种全氟辛基磺酰胺(FOSAs)和2种全氟辛基磺酰胺乙醇(FOSEs)。考察了超声提取溶剂、提取温度和提取时间对提取效率的影响,最终确定用甲醇为提取溶剂,70 ℃下超声提取60 min,目标物经VF-WAXms毛细管柱(30 m×0.25 mm×0.25 μm)程序升温分离,GC-MS/MS多反应监测(MRM)模式检测,外标法定量。实验结果表明:11种挥发性全氟化合物前体物在10~500 μg/L范围内线性关系良好,相关系数(r)均不低于0.9984;以信噪比为3计算,检出限(LOD)为0.002~0.04 mg/kg;以信噪比为10计算,定量限(LOQ)为0.006~0.1 mg/kg;不同材质纺织品中,11种挥发性全氟化合物前体物在高、中、低3个添加水平下的回收率为73.2%~117.2%,相对标准偏差(RSD)为0.1%~9.4%(n=6)。该方法前处理简单,定性、定量准确,灵敏度高,重现性好,可有效用于纺织品中11种挥发性全氟化合物前体物的同时检测。实际样品分析发现,当前全氟化合物前体物已被应用于纺织品整理当中。该方法的建立对我国纺织品中全氟化合物前体物风险物质的管控和检测标准的制定具有一定的理论和现实意义。     

高效液相色谱法同时测定含脂羊毛中残留的除虫脲和杀铃脲

建立了同时测定含脂羊毛中除虫脲和杀铃脲的反相高效液相色谱方法。样品用正己烷-乙醚混合溶剂提取,经凝胶渗透色谱柱和固相萃取柱净化后,采用反相高效液相色谱-二极管阵列检测器检测,外标法定量。除虫脲和杀铃脲分别在0.41～41 mg/L和0.38～38 mg/L范围内线性关系良好,相关系数分别为0.9996和0.9999。最低检出限:除虫脲为0.22 mg/kg,杀铃脲为0.18 mg/kg;最低定量限:除虫脲为0.73 mg/kg,杀铃脲为0.60 mg/kg。在添加水平为0.76～10.25 mg/kg的除虫脲和杀铃脲时,平均加标回收率为86.3%～96.7%,相对标准偏差为4.2%～8.7%。该方法杂质干扰小、回收率高、重现性好,能够对含脂羊毛中除虫脲和杀铃脲残留量进行准确的定性定量分析。     

Investigation of the flammability of different textile fabrics using micro-scale combustion calorimetry

Evaluating and analyzing the performance of flame retardant (FR) textiles are a critical part of research and development of new FR textiles products by the industry. The testing methods currently used in the industry have significant limitations. Most analytical and testing techniques are not able to measure heat release rate (HRR), the single most important parameter in evaluating the fire hazard of materials. It is difficult to measure HRR of textile fabrics using cone calorimetry because textile fabrics are dimensionally thin samples. The recently developed micro-scale combustion calorimetry (MCC) is able to measure the following flammability parameters for textile using milligram sample sizes: heat release capacity, HRR, temperature at peak heat release rate (PHRR), total heat release and char yield. In this research, we applied MCC to evaluate the flammability of different textile fabrics including cotton, rayon, cellulose acetate, silk, nylon, polyester, polypropylene, acrylic fibers, Nomex and Kevlar. We also studied the cotton fabrics treated with different flame retardants. We found that MCC is able to differentiate small differences in flammability of textile materials treated with flame retardants. We were also be able to calculate the limiting oxygen index (LOI) using the thermal combustion properties of various textile samples measured by the MCC. The calculated LOI data have yielded good agreement with experimental LOI results. Thus, we conclude that MCC is an effective new analytical technique for measuring textile flammability and has great potentials in the research and development of new flame retardants for textiles.     

超高效液相色谱-线性离子阱/静电场轨道阱高分辨质谱法测定纺织品中的游离态致癌芳香胺

建立了超高效液相色谱-线性离子阱/静电场轨道阱高分辨质谱(UPLC-LTQ/Orbitrap MS)同时测定纺织品中24种游离态致癌芳香胺的方法。样品经二氯甲烷超声提取并稀释后,用ZORBAX SB-C₁₈色谱柱(150 mm×2.1 mm, 5 μm)分离,以0.1%甲酸水溶液和甲醇为流动相,电喷雾正离子(ESI⁺)模式电离,以准分子离子峰的精确质量数和保留时间定性,以提取的色谱图峰面积定量。在0.5~500 μg/L范围内,24种芳香胺的线性相关系数(R²) 大于0.99,样品加标回收率为87.8%~105.6%,相对标准偏差为1.6%~3.4%。方法检出限为0.5~1 μg/kg。应用本方法检测山东地区进出口含氨纶纺织品样品14个,在5个样品中检出游离态芳香胺4,4'-二氨基二苯甲烷,含量范围为0.21~25.6 mg/kg。     

新型毛细管内固相萃取-气相色谱法检测纺织品中烷基酚类物质

建立了毛细管内固相萃取(SPE)-气相色谱(GC)检测纺织品中壬基酚和辛基酚含量的分析方法。通过比较4种性质不同固相萃取剂的萃取效果,筛选出对烷基酚(APs)类物质萃取效果最佳的固相萃取剂,将其作为填充物质制作毛细管内固相萃取柱,将毛细管内固相萃取法与气相色谱联用进行分析检测。最佳固相萃取剂为Abselut NEXUS,毛细管内固相萃取最佳条件为:1.2 μL甲醇和1.2 μL超纯水活化,1.2 μL甲醇洗脱,上样速率是0.4 μL/min。该法在较低浓度范围内呈现良好的线性相关性,对烷基酚的富集倍数约为100倍,对辛基酚和壬基酚的检出限分别为3.7 μg/L和4.5 μg/L,加标回收率分别为85.6%~98.2%和83.8%~95.7%,结果表明,此法能够简捷、迅速、有效地检测出纺织品中残留的烷基酚类物质。