CN109642858A - 制备用于激光诱导击穿光谱术的样品的方法 - Google Patents

制备用于激光诱导击穿光谱术的样品的方法 Download PDF

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CN109642858A
CN109642858A CN201680088653.7A CN201680088653A CN109642858A CN 109642858 A CN109642858 A CN 109642858A CN 201680088653 A CN201680088653 A CN 201680088653A CN 109642858 A CN109642858 A CN 109642858A
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托马斯·尼古拉吉森
丹尼尔·亚丁
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Abstract

一种制备用于激光诱导击穿光谱术(LIBS)的有机材料样品的方法(2)，包括以下步骤：获得颗粒状有机材料的步骤(4)；将在颗粒状有机材料中的至少一部分颗粒状有机材料成型为样品团块的步骤(6)；以及灼烧有机材料的步骤(8，8’)，优选仅在待进行LIBS分析的表面处进行灼烧(8)。任选地，该方法(2)包括压制经灼烧的样品团块以固结包括经灼烧的上表面的材料的步骤(10)。

Description

制备用于激光诱导击穿光谱术的样品的方法
本发明涉及制备用于激光诱导击穿光谱(LIBS)分析的样品的方法，并且尤其涉及制备用于LIBS分析的固体有机材料样品的方法。
LIBS是一种光谱化学技术，它使用具有非常短的脉冲持续时间(通常在几纳秒和几飞秒之间)的脉冲激光聚焦在样品上，以产生超过10,000开尔文的瞬时温度。
在这种环境中，一部分样品被转化成等离子体，化学键被破坏，产生电子激发的原子和离子。这些受激发的物种发出取决于构成元素的特定波长的辐射。
通过分析由等离子体发射的光，可以根据所关注的组成元素特征发射波长识别所关注的组成元素，并通过测量其特征发射波长处的光强度来测量所关注的组成元素的浓度。
理想地，特征发射波长的强度仅取决于样品中存在的相关组成元素的量。然而，众所周知，样品性质的变化(即，其中发现组成元素的基质的物理或化学性质的变化)会影响相关组成元素的特征发射波长的强度。这个问题(通常被称为“基质效应”)，在本领域是众所周知的，并且是限制LIBS准确性的因素。
为了使用LIBS进行正确分析，样品等等应该是同质的。通常，天然存在的有机材料样品(诸如，植物材料样品)不是天然均匀的，因此它们必须被加工成均匀的样品。为此，通常通过研磨、切碎或粉碎，首先将有机材料分解成未固结的微粒或颗粒，然后通过将颗粒材料成型为样品团块，将颗粒样品转化成单个实心单元。成型通常通过将颗粒材料压制成固结单元、通过将环氧树脂或其它粘合剂与样品混合并固化以成型样品团块、或压制和添加粘合剂的组合来完成。
然而，即使使用极细的粉末，在样品的有机基质中的不均匀性也可能经常残留。随着颗粒尺寸的增加，最终样品的不均匀性也经常增加。
从US7663749中已知，提供了一种LIBS系统，用于测量非均匀样品的组成元素的量，其中，使用由CCD摄像头获取的图像，将样品分成多个域。然后对每个域进行LIBS分析，并且根据每个域的LIBS分析以及该域与整个样品的相对体积，计算样品的所关注的元素浓度。通过将分析限于各种离散域，任何基质效应都减少了，并且浓度分析的整体精度也提高了。
其他LIBS系统(诸如，在US8319964中描述的LIBS系统)采用第一激光器烧蚀样品，并且采用第二激光器对烧蚀羽状物进行LIBS分析。这种LIBS分析通常是在远离烧蚀部位的位置进行的，并且载气将烧蚀羽状物输送到该部位，进行LIBS分析。由于等离子体的LIBS分析与烧蚀事件解耦，因此任何基质效应会被减少。
这种系统通常构造起来更加复杂，因此更加昂贵。
本发明的目的是减轻对固体有机材料的LIBS分析的基质效应。
根据本发明的第一方面，提供了制备用于激光诱导击穿光谱术(LIBS)的植物材料样品的方法，包括以下步骤：获得颗粒状有机材料；以及例如通过将颗粒状有机材料压制成型为固结块，将颗粒状有机材料中的至少一部分成型为样品团块；其中，该方法还包括烧灼有机材料的步骤。
在一些实施例中，仅对使用LIBS分析的样品团块的表面执行灼烧步骤。
对样品表面进行烧灼(也称为炭化)导致有机样品基质的热化学分解。对于随后的LIBS分析，热化学分解有两个影响；1)矿物的发射线更强，因为元素更容易电离；2)定量元素丰度分析的准确性得到提高，因为在比较不同植物材料时，经烧灼的基质在化学成分方面比未烧灼的基质具有更多的共同点。
有用的但不是必需的是，样品团块被压制成型，并在表面受到这种灼烧之后被再次压制。这为LIBS分析提供了一个紧凑、相对平坦的表面。
根据本发明的第二方面，提供了一种执行激光诱导击穿光谱术(LIBS)的方法，包括以下步骤：根据本发明第一方面的方法制备有机材料样品；将激光束脉冲导向有机材料样品的经烧灼的表面，以产生等离子体烧蚀事件；以及对在等离子体烧蚀事件中产生的等离子体发射的光进行光谱分析，以根据有机材料样品中所关注的组成元素的特征发射波长，识别出有机材料样品中所关注的组成元素。
通过考虑参考附图中的绘图所作出的根据本发明的方法和系统的一个或更多个示例性实施例的以下描述，将更好地理解这些和其他的优点和特征，其中：
图1显示了示出本发明的方法的实施例的流程图；
图2饲料和大豆的经烧灼的和未经烧灼的样品的比较LIBS光谱；以及
图3饲料样品在不同烧灼持续时间下的比较LIBS光谱。
将参照图1描述根据本发明的方法的说明性实施例。
方法2的第一步骤4通常包括获得颗粒状有机材料。在特定的实施例中，植物材料的样品(是来自植物本身的材料或者是使用这种材料制造的材料(诸如，动物饲料、面粉或食品))被加工成未固结的颗粒(例如，通过切碎、研磨或粉碎该材料)。该过程可以手动实现(例如，使用研钵和研杵)或者机械实现(例如，使用研磨机或粉碎机)，并且可以可选地在材料干燥后完成。
第二步骤6通常包括将在第一步骤4中获得的颗粒状材料的至少一部分成型为样品团块。在一个特定的实施例中，颗粒状有机材料(例如，植物材料)被装载到端部敞开的圆柱形模具中，并且压力被施加到该材料上，以便成型固结颗粒状植物材料的样品团块，该样品团块优选地被保存在模具中，以帮助保持结构完整性并提高操作的容易性。如此成型的团块呈现出暴露的端面，在该端面处，将进行LIBS分析。可以采用常规的液压实验室压丸机来成型样品团块。
第三步骤8通常包括灼烧颗粒状有机材料。在实施例中，该步骤是在成型样品团块的步骤6之后进行的，并且包括将热量仅施加到颗粒的暴露端面。在可选的实施例中，可以在成型步骤6之前(例如，在获得颗粒状有机材料的步骤4之后)对有机材料进行灼烧步骤8’。
在成型样品团块的步骤6之后执行灼烧步骤8的实施例中，执行第四步骤10。这个第四步骤10通常包括压制(或再压制)样品团块。在该步骤10中，将压力施加于样品团块，以便固结该材料，这成型样品团块的经灼烧的暴露端面。在成型步骤6处采用的压机合宜地用于这个压制(或再压制)样品团块的步骤10。
通过首先获得颗粒状植物材料(4)；然后将颗粒状植物材料压制成型用于LIBS分析的具有暴露端面的样品颗粒(6)；然后灼烧暴露的端面(8)；以及最后在呈现样品以供LIBS分析之前再次压制经灼烧的暴露端面(10)，根据上面参照图1描述的方法(2)制备出样品。LIBS分析是对在所得样品团块中的每个样品团块的经灼烧的暴露端面执行的。本质上，这是通过将激光束脉冲导向有机材料样品的经灼烧的表面以产生等离子体烧蚀事件、并对在等离子体烧蚀事件中产生的等离子体发射的光进行光谱分析，以根据有机材料样品的所关注的组成元素的特征发射波长识别该有机材料样品中所关注的组成元素来实现的。图2示出了针对混合定量饲料(a)中钠(Na)、在混合定量饲料(b)中的钙(Ca)、针对大豆(c)中的钾(K)以及针对大豆(d)中的磷(P)，由LIBS系统的光谱仪对经灼烧的(实线)和未灼烧的(虚线)样品团块生成的光谱。可以看出，与其中的每个样品中的元素相关联的光谱特征都在经灼烧的样品颗粒中得到增强。
在图3中针对钙(Ca)示出了灼烧持续时间对根据图1的、并且其包括在灼烧后再压制样品团块的步骤10的方法生产出的混合饲料定量的样品团块的经灼烧的暴露端面的LIBS光谱的影响。在每个压制阶段2、10，将每平方厘米5吨施加到模具中的植物材料上九十秒。以下面五个不同的灼烧级别进行LIBS分析：(a)“不灼烧”(即，根据图1的方法进行，直到并且包括将有微粒的混合饲料定量压制成型为样品团块的步骤6)；(b)“正常灼烧”(即，根据目测，当团块的暴露的上表面变黑时，灼烧停止)；(c)“严重灼烧”(相比于正常灼烧，灼烧时间是其两倍)；和(d)“最严重的灼烧”(相比于正常灼烧，灼烧时间是其三倍)。
从图3可以看出，随着灼烧的持续时间增加(即，从(a)到(c))，由于Ca引起的LIBS光谱信号的强度增加。当灼烧强度增加并且超过某一灼烧级别(在严重(c)和最严重(d)灼烧持续时间之间)时，强度开始收敛，LIBS光谱信号的强度开始降低。因此，可以通过实验容易地确定特定基质的最优灼烧时间和/或灼烧温度。

Claims (6)

1.一种制备用于激光诱导击穿光谱术(LIBS)的有机材料样品的方法(2)，包括以下步骤：获得颗粒状有机材料(4)；以及将所述颗粒状有机材料中的至少一部分颗粒状有机材料成型为样品团块(6)；其中，所述方法还包括灼烧所述有机材料的步骤(8；8’)。
2.根据权利要求1所述的方法(2)，其中，灼烧所述有机材料的步骤包括仅对所述样品团块的将要受到LIBS分析的表面进行灼烧(8)。
3.根据权利要求2所述的方法(2)，其中，在仅对所述样品团块的表面进行灼烧的步骤(8)之后，提供了压制所述样品团块(6)的另一步骤(10)。
4.根据权利要求1所述的方法(2)，其中，将所述颗粒状有机材料成型为样品团块的步骤(6)包括通过对所述颗粒状有机材料施加压力以成型作为所述样品团块的固结块，来压制所述颗粒状有机材料。
5.根据权利要求1所述的方法(2)，其中，所述有机材料是植物材料。
6.一种执行激光诱导击穿光谱术(LIBS)的方法，包括以下步骤：根据权利要求1至5中任一项所述的方法制备有机材料样品；将激光束脉冲导向有机材料样品的经灼烧的表面，以产生等离子体烧蚀事件；以及对在所述等离子体烧蚀事件中产生的等离子体发射的光进行光谱分析，以根据在所述有机材料样品中所关注的组成元素的特征发射波长识别出在所述有机材料样品中所关注的组成元素。
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