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首页> 外文期刊>Fuel >A new sample preparation method for crude or fuel oils by mineralization utilizing single reaction chamber microwave for broader multi-element analysis by ICP techniques
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A new sample preparation method for crude or fuel oils by mineralization utilizing single reaction chamber microwave for broader multi-element analysis by ICP techniques

机译：一种利用单反应室微波进行矿化的原油或燃料油样品制备的新方法，以ICP技术进行更广泛的多元素分析

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The objective of this study was to develop an effective and routine single sample preparation method to accurately and precisely analyze multiple elements (up to 57) in crude oils using both an inductively coupled plasma-optical emission spectrometer (ICP-OES) for high abundance elements and a triple quadrupole-inductively coupled plasma-mass spectrometer (QQQ-ICP-MS) (or ICP-MS) for low abundance trace and ultra-trace elements. A critical aspect of this study was to develop a single sample preparation method that could be effective in analyzing the largest number of quantifiable elements with instruments used in tandem to cover a wider and more practical combined dynamic range. Three sample preparation techniques were investigated and tested, including high pressure combustion with strong-acid digestion, high pressure and high temperature strong-acid digestion within Parr bombs, and high temperature and high pressure digestions in a Single Reaction Chamber (SRC) microwave. For the combustion method, no element showed recovery above 75%, thus this method was deemed unacceptable for accurate and precise analysis of crude oil. Average recoveries ranging from 94% to 106% for 19 analytes were achieved with high pressure and high temperature acid digestion within Parr bombs. A drawback of the method, however, was a rather small sample sizes (100 mg) that could be achieved without venting, which places limitations on detection and quantitation limits of large numbers of low abundance analytes in natural crude oils. The best of the SRC microwave-assisted acid digestion tests, however, was also shown to be acceptable for 19 analytes using a certified organometallic standard, with average recoveries ranging from 93% to 113%. Because of rapid sample throughput and the larger sample sizes (1.2 g sample size per digestion session) that can be accommodated with the single reaction chamber microwave digestion technique, better method detection and quantification limits and high precision on a range of low abundance elements could be achieved. We also then successfully tested the recovery of 53 elements with this SRC microwave method by adding a multi-element spike to Conostan base oil. This optimum SRC digestion method tested was then used to examine a NIST natural crude oil research material (NIST RM 8505) in an attempt to quantify up to 57 elements. The mean vanadium concentration (mass fraction) is reported as 390 +/- 0.4 mu g/g, the mean value of 5 replicate digestions by our method, which agrees well with the recommended value for the only element recommended for NIST 8505 of 390 +/- 10 mu g/g. The number of quantified analytes for the RM 8505 was further extended to a total of 52 elements with RSDs <5% for 38 elements, between 5% and 10% for 10 elements, and between 10% and 15.6% for 4 elements, all of which met our acceptability limits set at <= 20% RSD. Of the 57 elements analyzed in RM 8505, certain elements B, Nb, and W, although above method quantitation limits, were judged unacceptable because RSDs were >= 31.4%, whereas Ag and Tl were below method quantitation limits, and their RSDs were >= 44.2% and judged unacceptable. However, these elements have been quantified in other natural crude oils with higher abundances, which indicates that up to 57 elements can be potentially assessed in crude oils or refined oils with this method. The NIST RM 8505 crude oil reported here and others are being evaluated as potential natural crude oil standards to provide references values for more routine multi-element analysis.
机译：这项研究的目的是开发一种有效且常规的单一样品制备方法，以使用电感耦合等离子体光发射光谱仪（ICP-OES）对高丰度元素进行准确而精确地分析原油中的多种元素（最多57种）以及用于低丰度痕量和超痕量元素的三重四极杆电感耦合等离子体质谱仪（QQQ-ICP-MS）（或ICP-MS）。这项研究的一个关键方面是开发一种单一的样品制备方法，该方法可以有效地利用串联使用的仪器来分析最大数量的可量化元素，从而涵盖更广泛，更实际的组合动态范围。研究和测试了三种样品制备技术，包括采用强酸消化的高压燃烧，帕尔炸弹内的高压和高温强酸消化，以及在单反应室（SRC）微波中的高温和高压消化。对于燃烧方法，没有元素显示出高于75％的回收率，因此，该方法被认为无法进行准确而精确的原油分析。在Parr炸弹中进行高压和高温酸消解后，对19种分析物的平均回收率从94％到106％。但是，该方法的一个缺点是无需排气即可获得很小的样品量（100毫克），这限制了天然原油中大量低丰度分析物的检测和定量限。但是，还证明了最佳的SRC微波辅助酸消解试验对于使用认证的有机金属标准物的19种分析物是可以接受的，平均回收率在93％至113％之间。由于快速的样品通量和单反应室微波消解技术可容纳的更大样品量（每个消解时间为1.2 g样品量），因此可以实现更好的方法检测和定量限以及对一系列低丰度元素的高精度实现。然后，通过向Conostan基础油中添加多元素加标，我们还成功地通过这种SRC微波方法测试了53种元素的回收率。然后，将这种经过测试的最佳SRC消解方法用于检查NIST天然原油研究材料（NIST RM 8505），以尝试量化多达57种元素。据报告，钒的平均浓度（质量分数）为390 +/- 0.4μg / g，这是根据我们的方法进行的5次重复消化的平均值，与NIST 8505推荐的唯一元素390 +的推荐值非常吻合-/ 10克/克。 RM 8505的定量分析物数量进一步扩展到总共52种元素，其中38种元素的RSD <5％，10种元素的5％至10％，4种元素的10％至15.6％。符合我们设定为<= 20％RSD的可接受范围。在RM 8505中分析的57种元素中，某些元素B，Nb和W尽管高于方法定量限，但由于RSD> = 31.4％，而Ag和Tl低于方法定量限且其RSD，因此被认为是不可接受的。 = 44.2％，被判定为不可接受。但是，这些元素已在其他丰度更高的天然原油中进行了定量，这表明使用此方法可在原油或精炼油中潜在评估多达57种元素。本文和其他报告中所报告的NIST RM 8505原油正在作为潜在的天然原油标准进行评估，以为更常规的多元素分析提供参考值。

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