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A method for dissolving magnesium metaphosphate for plasma spectrometry detection

A technology of plasma spectroscopy and magnesium metaphosphate, which is applied in the field of ion spectrometry to detect magnesium metaphosphate impurity elements to prepare its solution samples, can solve the problems of difficult measurement, increased background, large interference, etc., and reduce the lower limit of detection of the analysis. Ease of operation and improved analytical sensitivity

Active Publication Date: 2020-10-30
HUBEI NEW HUAGUANG NEW INFORMATION MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The weak point of existing method one is that a large amount of alkali is introduced in the melting, which is unfavorable to the sample introduction system and easily causes the atomizer to be blocked; the use of silver crucible will introduce certain copper ions
In the method, 0.1-0.2 grams of magnesium metaphosphate is weighed, so that the detection impurity concentration is too low, which is not conducive to detection
[0006] The disadvantages of using the magnesium metaphosphate sample solution prepared by the above method to detect trace impurities by plasma spectrometry are: 1. The procedures are cumbersome; 2. The sample solution contains a higher concentration of salt, which increases the background in the plasma spectrometry , great interference
Moreover, the nebulizer is easy to block, which makes the measurement difficult

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1: take by weighing 0.5000 gram glassy powder Mg (PO 3 ) 2 , with a purity of 99.9% and a particle size of less than 200 mesh, put it in a 250ml dry beaker, add 5ml of superior pure concentrated perchloric acid with a weight percentage of ≥72% and 5ml of superior pure concentrated sulfuric acid with a weight percentage of ≥98% , heated at low temperature to slightly boiling, and kept for 60-120 minutes. Let cool afterwards. Carefully add pure water to dilute, dissolve, cool, transfer to a 50ml volumetric flask, dilute to the mark with water, shake well, and obtain a magnesium metaphosphate solution for testing with an inductively coupled plasma spectrometer.

Embodiment 2

[0023] Embodiment 2: take by weighing 0.5000 gram of non-glass state powder Mg (PO 3 ) 2 , with a purity of 99.7% and a particle size of less than 200 mesh, put it in a 100ml dry quartz beaker, add 3ml of superior pure concentrated perchloric acid with a weight percentage of ≥72% and 3ml of superior pure perchloric acid with a weight percentage of ≥98% Concentrated sulfuric acid, heated at low temperature to slightly boiling 200-350°C, kept for 1-2 hours, a large number of needle-shaped crystals precipitated, and the solution was clear and not turbid. Let cool afterwards. Carefully add distilled water to dilute, dissolve, cool, transfer to a 50ml volumetric flask, dilute with water to the mark, shake well and set aside.

Embodiment 3

[0024] Embodiment 3: take by weighing 0.5000 gram glassy powder Mg (PO 3 ) 2 , with a purity of 99.4% and a particle size of less than 200 mesh, put it in a 50ml conical flask, add 2ml of superior pure concentrated perchloric acid with a weight percentage ≥ 72% and 3ml of superior pure concentrated sulfuric acid with a weight percentage ≥ 98% , Heated at low temperature to slightly boiling 200-350°C, kept for 1-2 hours, a large number of needle-like crystals precipitated. Let cool afterwards. Carefully add distilled water to dilute, dissolve, cool, transfer to a 50ml volumetric flask, dilute with water to the mark, shake well and set aside.

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Abstract

The name of the present invention is a method for dissolving magnesium metaphosphate by plasma spectrometry. It belongs to the technical field of plasma detection of magnesium metaphosphate. It mainlysolves the problem that the existing method has a complicated procedure and the sample solution contains a relatively high concentration of salt. Its main features are: (img file='DEST_PATH_IMAGE001.TIF' wi='19' he='24' / ) placing the magnesium metaphosphate powder sample into a dry beaker, adding enough concentrated perchloric acid and thick Sulfuric acid; (img file='645275DEST_PATH_IMAGE002.TIF'wi='19' he='23' / ) then heating at low temperature, slightly boiling to clear, cooling, diluting to the mark and shaking, to obtain the magnesium metaphosphate test sample solution. According to the method for dissolving magnesium metaphosphate by plasma spectroscopy, the magnesium metaphosphate sample solution prepared by the method of the invention has low salt content, small spectral backgroundand is suitable for measuring trace impurity elements in magnesium metaphosphate.

Description

technical field [0001] The invention belongs to the technical field of plasma spectrometry detection of magnesium metaphosphate, and in particular relates to a method for preparing a solution sample of magnesium metaphosphate when detecting impurity elements of magnesium metaphosphate by plasma spectrometry. Background technique [0002] Inductively Coupled Plasma-Atomic Emission Spectrometer (ICP-AES) is a commonly used plasma spectrometry detection equipment. It has high analytical sensitivity, wide linear range and low background, and is an effective method for the determination of trace elements in solution. [0003] The general method that existing preparation plasma spectrometry detects impurity solution sample in magnesium metaphosphate is: 1, the magnesium metaphosphate sample powder of 1 gram solid is placed in silver crucible, then adds 2 gram sodium hydroxide in crucible, Gradually rise to 700 ° C to melt, soak in hot water, acidify with nitric acid, and dilute t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/73
CPCG01N21/73
Inventor 杨斌李庆峰高晓芳邬理凡王德国
Owner HUBEI NEW HUAGUANG NEW INFORMATION MATERIALS CO LTD
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