“考古”陶片中酒类残留的分析检测

通过对陶器中酒类残留的检测分析,介绍了化学技术手段在考古工作中的应用。在实验中,学生通过萃取、抽滤、离心、旋转蒸发等实验步骤提取酒的标志物——有机酸,并对其进行高效液相色谱(HPLC)检测,最后结合陶片的考古背景分析陶片的可能用途。该实验依托于考古化学这一新兴交叉学科,面向化学、考古学等专业的学生开设,有助于学生了解并掌握分析化学中样品分离和制备、液相色谱分析等基本概念与操作,并对考古学的研究内容形成一定认识。     

环境介质与生物样品中三氯生残留检测方法研究进展

综述了环境介质与生物样品中三氯生残留的检测方法研究进展。检测方法有气相色谱-质谱法、液相色谱法、液相色谱-质谱联用以及分光光度法、酶联免疫分析方法和电化学法等。气相色谱-质谱法检测三氯生线性关系良好，检出限、定量限低，精密度、准确度较高，但样品需要衍生化前处理，操作较为复杂。液相色谱法操作相对于气相色谱-质谱法更为简便，且具有选择性强、线性范围宽、定量准确和精密度高等优点，目前高效液相色谱法是大多数实验室的首选。液相色谱-质谱法是在液相色谱的基础上，采用质谱法对样品中的三氯生残留进行定性定量，定量准确，检出限低。其他方法的使用率较低，但也可满足环境介质与生物样品中三氯生残留的检测。目前乃至未来的一段时间内，环境介质及生物样品中三氯生残留的检测方法将以色谱-质谱法为主。目前仪器检测技术条件已经相对成熟，因此应积极寻找适合不同样品的前处理方法，使检测结果更加准确和精确，实验过程更加快捷方便。     

气相色谱-负化学离子源质谱法在食品安全分析中的应用

气相色谱-负化学源质谱法(GC-NCI-MS)技术被广泛应用于环境、人体组织、食品等样品中污染物的定性分析和定量测定.综述了近年来气相色谱-负化学源质谱技术在食品安全分析如农药残留、兽药残留和污染物测定中的应用.     

气相色谱法测定五水硫酸铜的脱水机理

目前,许多学校化学系开设的“配位化学”实验中一般采用了经典的差热—热重法检测配合物热分解过程的实验。气相色谱作为一种常用的分析测试手段,对于非分析专业的学生来说,除了在基础分析化学课程中有所涉及外,很少有动手实践的机会。把气相色谱引入配位化学实验,既可以使学生巩固前面课程所学气相色谱原理及操作方法,同时也使学生了解到色谱法在无机化学领域     

食品中氟虫腈的残留量的气相色谱负化学源检测方法

氟虫腈(Fipronil),商品名锐劲特(Regent),是一种苯基吡唑类杀虫剂.目前,国内只有以GC/ECD方式测定植物性食品中氟虫腈残留的气相色谱法的文献报道~([1～4]).有关多类食品中氟虫腈残留量的GC/MS检验方法的报道尚未见.本实验研究了菠菜、藕、草莓、花生、鸡肉、猪肉、鳕鱼、蜂蜜、大麦和酱油等食品中氟虫腈残留量测定的样品前处理方法,采用了常量和微量化法结合的样品前处理技术,有效去除样品中油脂、蛋白质和色素等杂质的干扰.采用气相色谱-负化学源质谱联用法(GC-NCL~-MS)进行检测.     

气相色谱-负化学离子源质谱联用法测定植物性产品中多组分农药残留量

通过气相色谱-负化学离子源质谱技术建立了同时检测18种农药残留的分析方法. 样品经正己烷和丙酮混合溶剂及正己烷提取后, 用活性炭-中性氧化铝混合小柱净化, 再由气相色谱-负化学离子源质谱分时段选择离子监测技术进行测定. 一次进样就能得到18种农药残留结果;各农药在0.005、 0.01和0.02 mg/kg 3个添加水平的平均回收率在70.2%～115.3%之间, RSD<12%, 检出限为0.01～6 μg/kg, 方法可应用于8种植物性产品中的农残检测.     

关于蔬果农药残留现象的实践调研

厦门大学化学化工学院"一点一滴"实践队结合所学专业知识,针对果蔬农药残留现象进行了实践调研。通过对不同背景市民进行的调查访问,了解到他们对农药残留的认识及日常采用的去除办法存在一定疑惑。在大量文献调研的基础上,总结目前农药残留的检测手段,从中筛选并优化适合本次实践活动的测定方法。对部分去除农药残留的方法进行实验检验,根据测定结果给出相应的建议。本次实践活动将所学专业知识运用于实际,培养和提高了学生的实践能力和综合素质。     

仪器分析综合实验:固相微萃取纤维的制备及在有机氯农药富集和分析中的应用*

设计了一个综合性仪器分析实验:固相微萃取纤维的制备及应用。实验内容包括微孔有机聚合物固相微萃取纤维的制备、红外光谱表征、固相微萃取实验条件优化和气相色谱测定有机氯农药含量等4个部分。通过综合运用多种仪器分析实验手段,加深了学生对分离富集技术的了解,巩固了学生对仪器分析课程中的气相色谱法、红外光谱法相关内容的掌握,培养学生构建一个完整、科学的仪器分析操作流程,形成综合性思维能力。     

非正常食用油的在线甲基化-气相色谱测定及模式识别分析研究

建立了食用油中脂肪酸组成的在线水解甲基化-气相色谱测定方法,分析了20余种常用食用油与非正常食用油样品。将1μL(3 mg/mL)油脂样品与2μL衍生化试剂四甲基氢氧化铵(TMAH,25%甲醇溶液)加入裂解器,在350℃下,油脂加水分解瞬间衍生化成相应的脂肪酸甲酯。基于气相色谱图上分离鉴定到的10个共有峰的相对强度,建立了食用油的气相色谱指纹图谱。结合化学模式识别即主成分分析和系统聚类分析对合格食用油和非正常食用油样品的色谱图进行了识别分析。结果表明,建立的指纹图谱结合模式识别技术可以较好的区分合格食用油与非正常食用油样品。     

GC-MS法检测牛肉中拟除虫菊酯的残留量

建立了柱层析法/气相色谱(GC)-负化学离子源(NCI)质谱检测牛肉中7种常用拟除虫菊酯杀虫剂残留的方法.样品经乙腈提取,通过中性氧化铝层析柱净化后,再由气相色谱-负化学离子源质谱选择离子监测技术(SIM)进行测定.7种菊酯类农药标准溶液在10～1 000 μg/L范围内线性关系良好,r2均大于0.997,在10、20...     

The use of FT-IR as a screening technique for organic residue analysis of archaeological samples

A range of archaeological samples have been examined using FT-IR spectroscopy. These include suspected coprolite samples from the Neolithic site of Catalh?yük in Turkey, pottery samples from the Roman site of Silchester, UK and the Bronze Age site of Gatas, Spain and unidentified black residues on pottery sherds from the Roman sites of Springhead and Cambourne, UK. For coprolite samples the aim of FT-IR analysis is identification. Identification of coprolites in the field is based on their distinct orange colour; however, such visual identifications can often be misleading due to their similarity with deposits such as ochre and clay. For pottery the aim is to screen those samples that might contain high levels of organic residues which would be suitable for GC-MS analysis. The experiments have shown coprolites to have distinctive spectra, containing strong peaks from calcite, phosphate and quartz; the presence of phosphorus may be confirmed by SEM-EDX analysis. Pottery containing organic residues of plant and animal origin has also been shown to generally display strong phosphate peaks. FT-IR has distinguished between organic resin and non-organic compositions for the black residues, with differences also being seen between organic samples that have the same physical appearance. Further analysis by GC-MS has confirmed the identification of the coprolites through the presence of coprostanol and bile acids, and shows that the majority of organic pottery residues are either fatty acids or mono- or di-acylglycerols from foodstuffs, or triterpenoid resin compounds exposed to high temperatures. One suspected resin sample was shown to contain no organic residues, and it is seen that resin samples with similar physical appearances have different chemical compositions. FT-IR is proposed as a quick and cheap method of screening archaeological samples before subjecting them to the more expensive and time-consuming method of GC-MS. This will eliminate inorganic samples such as clays and ochre from GC-MS analysis, and will screen those samples which are most likely to have a high concentration of preserved organic residues.     

MALDI‐FT‐ICR‐MS for archaeological lipid residue analysis

Soft‐ionization methods are currently at the forefront of developing novel methods for analysing degraded archaeological organic residues. Here, we present little‐used soft ionization method of matrix assisted laser desorption/ionization‐Fourier transform‐ion cyclotron resonance‐mass spectrometry (MALDI‐FT‐ICR‐MS) for the identification of archaeological lipid residues. It is a high‐resolution and sensitive method with low limits of detection capable of identifying lipid compounds in small concentrations, thus providing a highly potential new technique for the analysis of degraded lipid components. A thorough methodology development for analysing cooked and degraded food remains from ceramic vessels was carried out, and the most efficient sample preparation protocol is described. The identified components, also controlled by independent parallel analysis by gas chromatography‐mass spectrometry (GC‐MS) and gas chromatography‐combustion‐isotope ratio mass spectrometry (GC‐C‐IRMS), demonstrate its capability of identifying very different food residues including dairy, adipose fats as well as lipids of aquatic origin. The results obtained from experimentally cooked and original archaeological samples prove the suitability of MALDI‐FT‐ICR‐MS for analysing archaeological organic residues. Sample preparation protocol and identification of compounds provide future reference for analysing various aged and degraded lipid residues in different organic and mineral matrices.     

Analysis of oil used in late Roman oil lamps with different mass spectrometric techniques revealed the presence of predominantly olive oil together with traces of animal fat.

The lipid fraction of residues in ancient oil lamps found at the archaeological site of Sagalassos (south-west Turkey) was analysed by gas chromatography (GC) coupled to mass spectrometry (MS). The identification of plant sterols and long chain alcohols suggested that a vegetable oil was used in these lamps. The lipid sample was also analysed with reversed-phase liquid chromatography (LC) coupled to MS with atmospheric pressure chemical ionization (APCI). The identification of TAG's detected with LC-APCI-MS showed that predominantly olive oil was used as a fuel for the antique oil lamps. The presence of large quantities of multiply unsaturated triacylglycerol (TAG) and traces of saturated TAG indicated that also other oils and animal fat were added. Summarizing, the analysis of TAG's with LC-APCI-MS in lipid extracts of ancient ceramics proved to be a valuable method to reconstitute the original contents.     

Optically stimulated luminescence dating of pottery from Turkey

In this study, the potential of optically stimulated luminescence (OSL) dating for archaeological potteries was investigated. Firstly, recently purchased OSL and alpha counter systems were calibrated. Then, archaeological sherds taken from Dat?a-Burgaz (Mu?la, Turkey) archaeological site of archaic and classical period (700-400 BC) were dated. Samples were prepared by the fine grain technique and paleodose was found by using the additive dose technique. The annual doses of uranium and thorium were determined by using the alpha counter. The potassium, which has no alpha activity, was determined by atomic absorption spectrometry. The age of the sherds was found to be 2340+/-190 years which is in good agreement with the archaeological evidence involving figurines and coins obtained in the same level.     

An integrated analytical approach for characterizing an organic residue from an archaeological glass bottle recovered in Pompeii (Naples, Italy)

Within the framework of an Italian research project aimed at studying organic residues found in archaeological objects from the Roman period, the chemical composition of the contents of several glass vessels recovered from archaeological sites from the Vesuvian area (Naples, Italy) was investigated. In particular, this paper deals with the study of an organic material found in a glass bottle from the archaeological site of Pompeii using a multi-analytical approach, including FT-IR, direct exposure mass spectrometry (DE-MS) and GC-MS techniques. The overall results suggest the occurrence of a lipid material of vegetable origin. The hypothesis that the native lipid material had been subjected to a chemical transformation procedure before being used is presented and discussed.     

基于香港高中化学学科校本评核的教、学、评活动设计*

化学实验评价对于培养学生的创新意识和化学学科实践能力具有重要意义,尝试借鉴香港高中化学学科校本评核方法设计“教、学、评”活动促进学生化学学习和实验能力发展。介绍了香港高中化学学科校本评核框架及准则,以人教版《化学1》(2003年课标本)“铁盐和亚铁盐”为例,结合2017年课标设计实验评价量表,通过实验活动串联教学任务,以期实现教、学、评目标。通过评价反馈,促使更加科学、全面地评估学生的实验能力表现,为教师的化学教学实践提供改进依据。     

Mass spectrometric methods prove the use of beeswax and ruminant fat in late Roman cooking pots

Lipid extracts of sherds of archaeological late Roman cooking pots were analysed using high temperature-gas chromatography coupled to a mass spectrometer and liquid chromatography with atmospheric pressure chemical ionization mass spectrometer detection (LC-APCI-MS). With these advanced techniques the use of beeswax was shown through identification of the constituting alkanes, mono and diesters. The detection of high amounts of saturated triacylglycerols (TAGs) further indicated that animal fat was processed in these pots. Part of the animal fat was characterised as originating from ruminants due to the presence of trans-fatty acids. The distribution of saturated TAGs and the higher concentration of stearic acid compared to palmitic acid in the transesterified lipid extract indicated that this was sheep fat. The results illustrate how complex mixtures can be unravelled and original contents of ancient ceramic vessels can be determined using specialised analytical equipment.     

Solid-state electrochemical analysis of Inka pottery from Qotakalli archeological site in the Cusco (Perú) area

Journal of Solid State Electrochemistry - A series of sherds from the archeological site of Qotakalli in the area of Cusco (Perú), corresponding to four different Inka periods, were studied by...     

Introducing Field Environmental–Analytical Chemistry in the Quantitative Analysis Laboratory

Advances in instrumentation and technology now provide the ability to perform many quantitative determinations in the field. Additionally, the potential for sample degradation and analyte decomposition make it necessary to determine certain analytes (e.g., dissolved oxygen) in the field when conducting environmental analyses. Unfortunately, field environmental—analytical chemistry is not a substantial portion of the analytical chemistry curriculum at many institutions. Students in lower-level analytical chemistry courses are often non-chemistry science majors, particularly at institutions with small chemistry departments. We report here on an experiment in which field environmental-analytical chemistry is introduced in the quantitative analysis laboratory. In the context of a water quality assessment of a local river, students determine temperature, pH, ORP, nitrate nitrogen, and ammonia nitrogen at several points in the river. The experimental objective is to determine the potential effects local agricultural practices and treated wastewater discharge may be having on the water composition. The pedagogical objective is to expose these students to the difficulties involved in making analytical determinations in unfamiliar and/or disruptive settings.     

杭州老虎洞窑古陶瓷成分的化学计量学研究

用支持向量机算法研究了与杭州老虎洞古陶瓷有关的两个断源、断代问题。作为化学计量学的～种新型分类算法,支持向量机在小样本问题上表现出良好的泛化能力,与特征选择方法结合,可以有效处理样本少,特征多的问题。本研究综合利用支持向量机、特征选择算法和其它化学计量学算法研究了杭州凤凰山麓万松岭附近的古窑遗址和“传世哥窑”的断源、断代问题,证明老虎洞窑与郊坛下窑产品截然不同,万松岭附近地面收集瓷片样本是老虎洞窑宋代地层的瓷片滑落所致,而“传世哥窑”样品可能是老虎洞窑元代时的产品。实验表明：支持向量机算法与化学分析相结合可以成为研究古陶瓷断源和断代问题的一种新方法。