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Determination method of metal antimony in powder samples

A sample, powdery technique for elemental measurement

Active Publication Date: 2015-09-02
贵州东峰锑业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Simultaneously prepare blank sample solution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Step 1. Take 0.5g of the powder foundation sample to be tested, put it in a microwave digestion tank, add digestion reagents, and fully immerse the sample. The digestion reagent is 10 mL of a mixed solution of HNO3 and HF, in which the concentration of HNO3 is 30% (volume percentage), and the concentration of HF is 30% (volume percentage); the volume ratio of the two is 2:1. The specific digestion process is as follows: the 0.5g foundation sample to be tested is fully mixed with the above-mentioned digestion reagent and left to stand for 10 minutes; heated to 100 degrees in a microwave digestion tank and kept at this temperature for 15 minutes; then heated to 150 degrees and kept The temperature is 15 minutes, after cooling to room temperature, dilute to 20mL, shake well, and set aside. Prepare blank sample solution at the same time.

[0019] Step 2. draw calibration curve: get the standard solution that concentration is 0.0,0.2,0.4,0.6,0.8,1.0μg / mL; Measure the spect...

Embodiment 2

[0031] Step 1. Take 0.5g of the powder foundation sample to be tested, put it in a microwave digestion tank, add digestion reagents, and fully immerse the sample. The digestion reagent is 10 mL of a mixed solution of HNO3 and HF, in which the concentration of HNO3 is 20% (volume percentage), and the concentration of HF is 30% (volume percentage); the volume ratio of the two is 2:1. The specific digestion process is as follows: the 0.5g foundation sample to be tested is fully mixed with the above-mentioned digestion reagent and left to stand for 10 minutes; heated to 120 degrees in a microwave digestion tank, and kept at this temperature for 15 minutes; then heated to 150 degrees again, kept The temperature is 15 minutes, after cooling to room temperature, dilute to 20mL, shake well, and set aside. Prepare blank sample solution at the same time.

[0032] Step 2. draw calibration curve: get the standard solution that concentration is 0.0,0.2,0.4,0.6,0.8,1.0μg / mL; Measure the s...

Embodiment 3

[0044] Step 1. Take 0.5g of the powder foundation sample to be tested, put it in a microwave digestion tank, add digestion reagents, and fully immerse the sample. The digestion reagent is 10 mL of a mixed solution of HNO3 and HF, in which the concentration of HNO3 is 30% (volume percentage), and the concentration of HF is 20% (volume percentage); the volume ratio of the two is 2:1. The specific digestion process is as follows: the 0.5g foundation sample to be tested is fully mixed with the above-mentioned digestion reagent and left to stand for 10 minutes; heated to 120 degrees in a microwave digestion tank, and kept at this temperature for 15 minutes; then heated to 150 degrees again, kept The temperature is 15 minutes, after cooling to room temperature, dilute to 20mL, shake well, and set aside. Prepare blank sample solution at the same time.

[0045] Step 2. draw calibration curve: get the standard solution that concentration is 0.0,0.2,0.4,0.6,0.8,1.0μg / mL; Measure the s...

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Abstract

The invention relates to a method for measuring antimony metal in a powder sample. According to method, an inductively coupled plasma (ICP) atomic emission spectrometry is adopted for measuring the content of the antimony metal in the powder sample. The method comprises the steps of: firstly adding a certain amount of mixed solution of HNO3 and HF into the sample with impurity antimony metal, and then carrying out digestion in a digestion tank; heating up to a certain temperature, and then maintaining the constant temperature for a period of time; and then, heating up to another temperature, maintaining the constant temperature for a period of time, and cooling to the room temperature. According to the method, an ICP atomic emission spectrometer is adopted for measuring the content of arsenic, and the experiment parameters can be reasonably selected according to the experiment need during measurement, so that the antimony metal in the environment sample can be conveniently and accurately measured, and the detection limit of 0.01mug / mL, thus meeting the demand of daily life.

Description

Technical field: [0001] The invention relates to the field of element measurement, in particular to the measurement of antimony element in powder samples by ICP plasma atomic emission spectrometry. Background technique: [0002] Powdery samples, such as foundation in cosmetics, are in increasing demand in people's daily life. However, it is often found in the current testing that metal antimony elements that should not appear in these powdery samples appear. Antimony can irritate people's eyes, nose, throat and skin. Continuous exposure can damage the heart and liver function. Inhalation of high levels of antimony can lead to antimony poisoning. Symptoms include vomiting, headache, breathing difficulties, and severe cases may cause death. How to detect the metal antimony element contained in the foundation seems to be very important. There is no more accurate measurement method for antimony element in the existing detection. The present invention uses ICP plasma atomic emis...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/71G01N1/44
Inventor 傅酉付玉生
Owner 贵州东峰锑业股份有限公司