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XRF荧光光谱仪应用于三元催化测试---分析汽车催化剂中的铂钯铑元素

更新时间:2021-08-03      点击次数:2239

EDXRF能量色散光谱仪Compass200在三元催化测试中的应用---测试催化剂中的铂钯铑贵金属元素

1. 背景与简介

催化剂转换器的内部陶瓷蜂窝结构涂有含有PtPdRh的修补基面涂层同时还可以存在其他元素以使催化转化器受益。商业上,能够回收铂族贵金属有助于满足新的需求。 汽车催化转化器占铂和钯需求的一半以上,占铑需求的大部分。 知道催化剂材料的贵金属含量对于回收物能够正确定价其材料至关重要

便携式X射线荧光(XRF光谱仪Compass 200 XRF可快速,准确地现场测定催化剂粉末中的贵金属,从而大程度地提高测试通量和利润。 


2. 仪器测量条件

为催化剂分析设定了工厂优化的测试条件。 这项行业可靠的技术可实现低检测限和高精度的贵金属高速检测。

1. 测试步骤和性能

3.1样品准备

样品的制备只需简单地将一块催化转化器的蜂窝磨碎,用研杵和研钵将其精细研磨,然后将所得粉末放入装有Mylar薄膜的样品杯中。 将样品杯装入指南针XRF分析仪的样品室中进行测量。

3.1.1 将样品捣碎并研磨

3.1.2 将研磨过的样品放入使用特殊薄膜的样品杯中

 

3.1.3 将样品放入Compass200中准备测试

3.2 准确性研究

>>标准样品制备

为了研究Compass 200的准确性,进行了2种认证参考材料的分析。 将测试的参考标准样品压碎,干燥并筛分至恒定大小,均质化,然后以带有特殊薄膜样品中再放到分析仪中。 为了获得准确而有代表性的结果,需要样品制备。 直接试图分析陶瓷蜂窝的表面可能会产生误导性的结果。

>>经验校准

催化剂标定模式"是根据指南针XRF分析仪中的EC算法预先校准的,因此,在开箱即用后即可直接使用。 为了减少基体效应对元素的影响,应用了康普顿散射峰校正。

 

下面的结果显示了使用150秒测量时间可以从该方法获得的准确性和精确度

>测试结果和标样值对比

标准样品

Std 01

Std 02

ppm

标准值

测定值

标准值

测定值

Pt

285

287

406

396

Pd

128

134

48

55

Rh

23

20

51

42

XRF设备的另一个重要参数是分析的可重复性。 每次150秒对样品进行7次测量。 ptpdrh含量的平均值,标准偏差(Std Dev)和相对标准偏差(RSD)由以下数据计算得出

>连续测量7次同一样品

Sample Name

Rh

Pd

Pt

Sample4#-1

35.188

175.501

242.849

Sample4#-2

36.788

167.881

248.067

Sample4#-3

36.063

171.135

244.861

Sample4#-4

36.750

166.669

248.872

Sample4#-5

33.925

177.190

246.872

Sample4#-6

34.488

167.501

250.849

Sample4#-7

35.188

174.281

246.067

Average

35.484

171.451

246.920

Std Dev

1.0982

4.2556

2.6491

RSD

3.09%

2.48%

1.07%

 

 

 

5.结论

Compass 200 XRF提供了一种精确,快速且易于使用的快筛检测方法,用于确定已制备的汽车催化剂样品中PtPdRh量。 铂族元素的高价值使得对这些元素的准确测定具有重要的商业意义。

指南针XRF光谱仪提供了最少的样品制备和快速,现场分析废旧汽车催化剂的解决方案

 

EDXRF fluorescence spectrometer COMPASS 200 is used to analyze and test the precious metals Pt, Pd and Rh in the catalyst

1. Background and introduction

The internal ceramic honeycomb structure of the catalyst converter is coated with a washcoat containing Pt, Pd and Rh. Other elements may also be present to benefit the catalytic converter. Commercially, being able to recover platinum group metals (PGM) can help meet new demands. Automotive catalytic converters account for more than half of platinum and palladium demand and the majority of rhodium demand. Knowing the PGM content of the catalyst material is essential for recyclables to be able to price their materials correctly


The portable X-ray fluorescence (XRF) Compass 200 XRF can quickly and accurately determine the precious metals in the catalyst powder on site, thereby maximizing test throughput and profit.


Sample preparation


The sample preparation simply grinds a piece of catalytic converter honeycomb, grinds it finely with a pestle and mortar, and then puts the resulting powder into a sample cup containing Mylar film. Load the sample cup into the sample chamber of the compass XRF analyzer for measurement.

Accuracy study


>>Standard sample preparation


In order to study the accuracy of Compass 200, two types of certification reference materials were analyzed. The test reference standard sample is crushed, dried and sieved to a constant size, homogenized, and then packed into the analyzer in a cup with a polyester film. In order to obtain accurate and representative results, sample preparation is required. Attempting to analyze the surface of the ceramic honeycomb may produce misleading results.


>>Experience Calibration


"Car catalyst" is pre-calibrated according to the EC algorithm in the compass xrf analyzer, so it can be used directly out of the box. In order to reduce the influence of the matrix effect on the elements, Compton scattering peak correction is applied.


Note: To extend the calibration range (for example, to include different matrices, extend the element calibration range, or add new elements of interest), other standards can be easily added to the existing calibration.

In conclusion


Compass 200 XRF provides an accurate, fast, and easy-to-use alternative method for determining the amount of Pt, Pd, and Rh in prepared automotive catalyst samples. The high value of platinum group elements makes the accurate determination of these elements of great commercial significance.


Compass XRF analyzer provides quick, on-site analysis of waste car catalyst information with minimal samples



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