使用X射线能量色散荧光光谱仪的测试程序和步骤

使用X射线能量色散荧光光谱仪（XRF Analyzer）的测试程序和步骤

1 光谱仪准备

a) 按照仪器的工作说明书给仪器通电，加热设备，按厂家说明书对仪器进行稳定。

b) 确保测试稳定，并按照制造商的说明使检测器稳定

2 校准

a) 根据仪器用户手册的说明，按照第 7 节的说明选择参考样品作为校准样品。样品中的元素

浓度应该不一样。如果校准覆盖的元素多，浓度范围大，则需要大量的校准样品。

由于以下原因，校准样品的数量有所减少：

— 用基本参数法校准（元素小于标准）

— 使用基本参数方法校准（使用具有相似元素的标准）

— 使用基本参数方法分析加经验校准

b) 分析方法校准考虑了光谱的干扰、基体效应等影响，这些都会影响光谱中荧光散射的强度

决心的程度。这些效果的列表可以在本章的附件中找到。

c) 为保证各测量元素的分析性能合格，需选择合适的激发参数，使仪器处于好的状态

测量条件。这些条件是仪器需要的。通常，此信息可以在分析师的说明手册中找到

d) 作为一般准则，推荐方法的用户知道，相互元素谱的干扰和样品间基质的变化将充分影响

对每个分析物结果的准确度、精密度和检测限。例如纯聚乙烯中Cd的检出限可达

至 15mg/Kg，但当存在 10% 溴化合物和/或 2% 锑时，无法达到检测限

3 检测器性能检查

无论设备是否满足要求的性能标准，都需要通过测量认证参考材料或相关参考样品

决定。样品中所含元素的浓度不得大于测试元素筛选限值的3-5倍（见表3）。按参考样本

产品得到的结果必须在样品测试误差的允许范围内。当设备用于分析未知材料时，制造商应提供

标准操作程序 (SOP) 和适当的参考样本。推荐的方法应该保证操作者可以获得高质量的定量分析结果。

4 测试样品的放置

a) 如果待测样品可以放置在台式X射线荧光光谱仪内部的样品室中，并且待测样品被正确测量

位置，可以进行相应的测试。如果待测样品不适合放置在样品室中，则必须将其切割以适合

尺寸易于测量。为了使测试结果有效，必须满足仪器关于样品厚度和质量的要求。

因为非常小的或薄的样品可能不符合这个条件。在这种情况下，这样的小样本（如蜗牛）

线钉）放置在样品杯中，然后进行分析。同样，相似的薄样品应堆叠在一起，以便

足以达到有效分析的最小样品厚度限制。一个总的原则是所有样本必须*

盖住光谱仪的测量窗口。对于聚合物和轻合金，例如 Al、Mg 和 Ti，其厚度至少应为 5mm。

液体的最小厚度为 15 毫米，而其他合金的厚度约为 1 毫米。但由于设备的个体差异，

所需的样本量也不同。光谱仪的操作人员应参考设备手册或遵循制造商的要求。

制备样品的尺寸/质量/厚度。

b) 如果在便携式 XRF 光谱仪上进行测试，必须注意光谱仪的测量窗口应为

测试样品相对并直接接触。小样品或非常薄的样品应按照上述 a) 中提到的方法进行操作。当然

然后使用附件（如果有）进行分析，让操作员可以测量样品杯中的样品。关于最

小样品的尺寸/质量/厚度规定也适用于便携式分析。

c) 如果样品是液体、粉末或球形，或者只是一个小样品，则需要

在样品杯中测量薄膜。处理此窗膜时，请注意不要

触摸其表面以避免弄脏它

5 筛选测试

a) 按规定时间进行测试。

b) 显示和记录分析结果。

6 结果分析

各种类型的 XRF 光度计单独使用，分析方法允许用户将样品分为以下三类之一：

a)“合格"——如果所有元素的定量分析结果均小于表2所列的下限，则该样品为合格。

b) “不合格"——如果全部高于表 2 所列的上限，则样品检测为不合格。

c) “未定"——如果 Hg、Pb 或 Cd 任何元素的定量分析结果在中间区域

或元素Br和Cr的结果高于表2所列的上限，分析结果未定。 也得进步一步研究。 本次测试“未定"

The test procedure and steps of using X-ray energy dispersive fluorescence spectrometer (XRF Analyzer)

1 Spectrometer preparation

a) Power on the instrument according to the working instructions of the instrument, heat the equipment, and stabilize the instrument according to the manufacturer's instructions.

b) Ensure that the test is stable, and make the detector stable according to the manufacturer's instructions

2 calibration

a) According to the instructions in the instrument user manual, follow the description in section 7 to select the reference sample as the calibration sample. Of the elements in the sample

The concentration must be different. If the calibration covers a lot of elements and the concentration range is large, a lot of calibration samples are needed.

The number of calibration samples has decreased due to the following reasons:

— Calibrate with the basic parameter method (the elements are less than the standard)

— Calibrate with the basic parameter method (using a standard with similar elements)

— Use basic parameter method analysis plus experience to calibrate

b) The analysis method calibration takes into account the interference of the spectrum, matrix effects and other effects, which will affect the intensity of fluorescence scattering in the spectrum

Degree of determination. A list of these effects can be found in the attachment to this chapter.

c) In order to ensure the qualified analytical performance of each measurement element, it is necessary to select the appropriate excitation parameters to make the instrument at the best

Measurement conditions. These conditions are unique to the instrument. Typically, this information can be found in the analyst’s instruction manual

d) As a general guideline, users of the recommended method know that the interference of mutual element spectra and changes in the matrix between samples will fully affect

To the accuracy, precision and minimum detection limit of each analyte result. For example, the detection limit of Cd in pure polyethylene can reach

To 15mg/Kg, but when 10% bromine compound and/or 2% antimony are present, the detection limit cannot be reached

3 Detector performance check

Regardless of whether the equipment meets the required performance standards, it needs to pass measurement certification reference materials or related reference samples to

determine. The concentration of the element contained in the sample must not be greater than 3-5 times the screening limit of the test element (see Table 3). By reference sample

The result obtained by the product must be within the allowable range of the sample test error. When the equipment is used to analyze unknown materials, the manufacturer should provide

A standard operating procedure (SOP) and an appropriate reference sample. The recommended method should ensure that the operator can get high quality

Quantitative analysis results.

4 Placement of test samples

a) If the sample to be tested can be placed in the sample chamber inside the desktop X-ray fluorescence spectrometer, and the sample to be tested is properly measured

Location, you can perform the corresponding test. If the sample to be tested is not suitable for being placed in the sample chamber, it must be cut to fit

The size is easy to measure. In order for the test results to be valid, the minimum requirements of the instrument regarding sample thickness and quality must be met.

Because very small or thin samples may not meet this condition. In this case, such small samples (such as snails)

Wire nails) are placed in a sample cup, and then analyzed. Similarly, similar thin samples should be stacked together so that

Enough to reach the minimum sample thickness limit for effective analysis. A general principle is that all samples must be completely

Cover the measurement window of the spectrometer. For polymers and light alloys such as Al, Mg and Ti, it should be at least 5mm thick.

The minimum thickness for liquids is 15mm, while for other alloys the thickness is about 1mm. However, due to individual differences in equipment,

The required sample size is also different. The operator of the spectrometer should refer to the equipment manual or follow the minimum required by the manufacturer.

Size/mass/thickness to prepare samples.

b) If the test is performed on a portable XRF spectrometer, it must be noted that the measurement window of the spectrometer should be

The test sample is opposite and in direct contact. Small or very thin samples should be operated in accordance with the method mentioned in a) above. Of course

Then use an accessory (if available) for analysis, allowing the operator to measure the sample in the sample cup. About the most

The size/quality/thickness regulations for small samples also apply to portable analysis.

c) If the sample is liquid, powder or spherical, or just a small sample, it needs to be

The film is measured in the sample cup. When handling this window film, be careful not to touch its surface to avoid staining it

5 screening test

a) Test according to the stipulated time.

b) Display and record analysis results.

6 Result analysis

Various types of XRF photometers are used individually, and the analysis method allows users to classify samples into one of the following three categories:

a) "Pass"-if the results of quantitative analysis of all elements are all less than the lower limit listed in Table 2, the sample has been tested Is qualified.

b) "Unqualified"-If all of them are higher than the high limit listed in Table 2, the sample will be unqualified after testing.

c) "Undecided"-if the result of quantitative analysis of any element of Hg, Pb or Cd is in the middle area

Or the results of the elements Br and Cr are higher than the upper limit listed in Table 2, and the analysis result is undecided. Also have to make progress

One-step research. This test is "undecided"