1. 背景與簡(jiǎn)介
催化劑轉(zhuǎn)換器的內(nèi)部陶瓷蜂窩結(jié)構(gòu)涂有含有Pt,Pd和Rh的修補(bǔ)基面涂層,同時(shí)還可以存在其他元素以使催化轉(zhuǎn)化器受益。商業(yè)上,能夠回收鉑族貴金屬有助于滿足新的需求。 汽車催化轉(zhuǎn)化器占鉑和鈀需求的一半以上,占銠需求的大部分。 知道催化劑材料的貴金屬含量對(duì)于回收物能夠正確定價(jià)其材料至關(guān)重要
便攜式X射線熒光(XRF)光譜儀Compass 200 XRF可快速,準(zhǔn)確地現(xiàn)場(chǎng)測(cè)定催化劑粉末中的貴金屬,從而大程度地提高測(cè)試通量和利潤(rùn)。
2. 儀器測(cè)量條件
為催化劑分析設(shè)定了工廠優(yōu)化的測(cè)試條件。 這項(xiàng)行業(yè)可靠的技術(shù)可實(shí)現(xiàn)低檢測(cè)限和高精度的貴金屬高速檢測(cè)。
1. 測(cè)試步驟和性能
3.1樣品準(zhǔn)備
樣品的制備只需簡(jiǎn)單地將一塊催化轉(zhuǎn)化器的蜂窩磨碎,用研杵和研缽將其精細(xì)研磨,然后將所得粉末放入裝有Mylar薄膜的樣品杯中。 將樣品杯裝入指南針XRF分析儀的樣品室中進(jìn)行測(cè)量。
3.1.1 將樣品搗碎并研磨
3.1.2 將研磨過的樣品放入使用特殊薄膜的樣品杯中
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3.1.3 將樣品放入Compass200中準(zhǔn)備測(cè)試
3.2 準(zhǔn)確性研究
>>標(biāo)準(zhǔn)樣品制備
為了研究Compass 200的準(zhǔn)確性,進(jìn)行了2種認(rèn)證參考材料的分析。 將測(cè)試的參考標(biāo)準(zhǔn)樣品壓碎,干燥并篩分至恒定大小,均質(zhì)化,然后以帶有特殊薄膜的樣品中再放到分析儀中。 為了獲得準(zhǔn)確而有代表性的結(jié)果,需要樣品制備。 直接試圖分析陶瓷蜂窩的表面可能會(huì)產(chǎn)生誤導(dǎo)性的結(jié)果。
>>經(jīng)驗(yàn)校準(zhǔn)
“ 催化劑標(biāo)定模式"是根據(jù)指南針XRF分析儀中的EC算法預(yù)先校準(zhǔn)的,因此,在開箱即用后即可直接使用。 為了減少基體效應(yīng)對(duì)元素的影響,應(yīng)用了康普頓散射峰校正。
下面的結(jié)果顯示了使用150秒測(cè)量時(shí)間可以從該方法獲得的準(zhǔn)確性和精確度
>測(cè)試結(jié)果和標(biāo)樣值對(duì)比
標(biāo)準(zhǔn)樣品 | Std 01 | Std 02 | ||
ppm | 標(biāo)準(zhǔn)值 | 測(cè)定值 | 標(biāo)準(zhǔn)值 | 測(cè)定值 |
Pt | 285 | 287 | 406 | 396 |
Pd | 128 | 134 | 48 | 55 |
Rh | 23 | 20 | 51 | 42 |
XRF設(shè)備的另一個(gè)重要參數(shù)是分析的可重復(fù)性。 每次150秒對(duì)樣品進(jìn)行7次測(cè)量。 pt,pd和rh含量的平均值,標(biāo)準(zhǔn)偏差(Std Dev)和相對(duì)標(biāo)準(zhǔn)偏差(RSD)由以下數(shù)據(jù)計(jì)算得出
>連續(xù)測(cè)量7次同一樣品
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.結(jié)論
Compass 200 XRF提供了一種精確,快速且易于使用的快篩檢測(cè)方法,用于確定已制備的汽車催化劑樣品中Pt,Pd和Rh的含量。 鉑族元素的高價(jià)值使得對(duì)這些元素的準(zhǔn)確測(cè)定具有重要的商業(yè)意義。
指南針XRF光譜儀提供了最少的樣品制備和快速,現(xiàn)場(chǎng)分析廢舊汽車催化劑的解決方案
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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