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X-ray fluorescence analysis method for determining element sulphur with different valence in cement

A technology of X-ray and analytical method, which is applied in the field of X-ray fluorescence analysis to determine sulfur elements in different valence states in cement, and achieves the effect of being simple and easy to implement and saving the measurement process.

Active Publication Date: 2014-08-06
CHINA TEST & CERTIFICATION INT GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] This shows that in the prior art, there is no scheme that only adopts X-ray fluorescence analysis method to measure the sulfur of sulfate and the sulfur of sulfide in cement

Method used

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  • X-ray fluorescence analysis method for determining element sulphur with different valence in cement
  • X-ray fluorescence analysis method for determining element sulphur with different valence in cement
  • X-ray fluorescence analysis method for determining element sulphur with different valence in cement

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Experimental program
Comparison scheme
Effect test

Embodiment

[0076] 1. Preparation of calibration samples

[0077] (1) Preparation of sulfide-free calibration samples

[0078] Select cement clinker standard samples or cement standard samples confirmed to be free of sulfides, and select sulfates, such as gypsum for cement. Take one piece of cement (or cement clinker) and one piece of gypsum for cement, mix the two in an appropriate proportion, and grind them to an appropriate fineness with a vibrating mill. Prepare n (n>2) calibration samples in this way, and the samples are denoted as SNi (i=1,2,…,n). Perform a fixed value determination of SO3 in these n (n>2) calibration samples. Since the standard sample is used and the gypsum is added quantitatively, the content of the hexavalent sulfur element in each of the above calibration samples is known, that is, the content of sulfate sulfur in the sample C SO3 is known.

[0079] (2) Preparation of calibration samples of sulfide-containing cement.

[0080] Select cement standard samples,...

example 1

[0090] 1. Preparation of calibration samples

[0091] (1) Preparation of sulfide-free calibration samples

[0092] Select a cement clinker sample confirmed to be free of sulfides and a cement gypsum, and grind them into powders first, then quantitatively mix them in an appropriate proportion, and grind them with a vibrating mill for 60 seconds, so as to prepare 8 calibration samples. Take about 5 grams of sample, use boric acid as a cushion layer, use 20 tons of force, hold the pressure for 30 seconds, and make the calibration sample into a powder tablet. The X-ray fluorescence intensity was measured for each calibration sample, and the sulfur trioxide in 8 calibration samples was determined. The results of the determination are shown in Table 1.

[0093] Table 1

[0094]

[0095] (2) Preparation of calibration samples of sulfide-containing cement.

[0096] Add an appropriate amount of iron sulfide or sodium sulfide to any cement standard sample, mix and grind for 60 sec...

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Abstract

The invention relates to an X-ray fluorescence analysis method for determining element sulphur with different valences in cement. The method comprises the following steps: preparing a test sample into pressed pellets and measuring net strength of K alpha ray and K beta ray of element sulfur in the pressed pellets by using an X-ray fluorescence spectrometer; and calculating the sulfur content of sulfides in the test sample according to the following formula: Ik beta / K beta SO3-Ik alpha / K alpha SO3=KS=*CS=, and the sulfur content of sulfides in the test sample according to the following formula: CSO3=(IKalpha-KalphaS=*CS=) / KalphaSO3. The method provided by the invention can directly determine content of element sulphur with different valences in the cement through the X-ray fluorescence analysis method, and is more simple and easy to use; therefore, the method suitable for practical application.

Description

technical field [0001] The invention relates to a cement sample testing technology, in particular to a method for measuring sulfur elements in different valence states in cement by X-ray fluorescence analysis. Background technique [0002] The sulfur element in cement mainly exists in the form of sulfate and sulfide, but at present, the determination of sulfide sulfur and sulfate sulfur in cement adopts chemical methods. The result of X-ray fluorescence analysis (XRF) is total sulfur, which is the sum of sulfate sulfur and sulfide sulfur. Only when it is confirmed that there is no sulfide sulfur in the cement, the XRF measurement result can be used as the result of cement sulfate sulfur, otherwise it is necessary to determine the sulfide sulfur by chemical method and then subtract the total sulfur to calculate the sulfate sulfur. [0003] It can be seen that in the prior art, there is no scheme that only adopts the X-ray fluorescence analysis method to measure the sulfur of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N23/223
Inventor 刘玉兵戴平闫冉赵鹰立韩蔚马振珠
Owner CHINA TEST & CERTIFICATION INT GRP CO LTD