Method for analyzing arsenic content in glass refining agent

An analysis method and clarifier technology, applied in the field of physical and chemical testing, can solve the problems of arsenic volatilization loss, analysis precision reduction, long analysis period, etc., and achieve the effect of avoiding volatilization loss, simple analysis process, sensitive and repeatable

Inactive Publication Date: 2010-01-06
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The analysis method of arsenic usually includes sample processing and determination. For glass clarifier samples, the effective arsenic components usually exist in a low-valence state. During sample processing, traditional wet acid digestion will cause volatilization loss of arsenic. The test results are seriously low; although the traditional alkali fusion decomposition method can meet the test requirements, the processing process is extremely cumbersome and time-consuming, and the analysis cycle is long. At the same time, it will also bring hidden dangers to the entire analysis system due to the introduction of a large amount of sample matrix and digestion flux. , the analysis accuracy is significantly reduced
[0005] The determination of arsenic usually adopts arsenomolybdenum heteropolyacid spectrophoto...

Method used

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  • Method for analyzing arsenic content in glass refining agent
  • Method for analyzing arsenic content in glass refining agent
  • Method for analyzing arsenic content in glass refining agent

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 1. Instruments and reagents

[0033] XS-205 automatic electronic analytical balance (Switzerland, Mettler-Toledo company);

[0034] Vista Axial CCD Simultaneous ICP-AES Spectrometer (USA, Varian company), charge-coupled detector, dispersive system is echelle grating, concentric nebulizer, frequency is 40.68MHz, the instrument is controlled by IBM computer and Varian'sVista software system.

[0035] Instrument working parameters: power 1.1kW, cooling gas flow 15L / min, auxiliary gas flow 1.5L / min, atomizing gas flow 0.8L / min, integration time 5s; repeat times 3 times, stabilization time 20s, sample lifting time 20s , cleaning time 10s, peristaltic pump speed 15rpm; argon purity 99.99%.

[0036] Acidity: HCl is used as the solution medium, and the concentration of HCl is 4% (V / V).

[0037] Analytical spectral line: The measured spectral line of As element is As 193.696nm.

[0038] The concentration of arsenic single element standard solution is 1mg / mL (GSBG62028-90, Nat...

Embodiment 2

[0047] In order to verify the accuracy of the analysis method of the present invention to measure arsenic in the glass clarifier sample and evaluate the precision of the analysis method, the following experiments are carried out on actual samples:

[0048] 1. Detection limit experiment

[0049] Use the sample blank test solution to measure ten times continuously, and calculate the standard deviation of arsenic in the sample blank solution. The results are shown in Table 2.

[0050] Table 2.

[0051] Determining element

Analytical lines

(nm)

Determination result (μg / mL)

standard deviation

3 times the standard deviation

arsenic

193.696

0.025，0.040，0.041，0.033，

0.034，0.037，0.038，0.034，

0.027，0.032

0.005

0.015

[0052] Set 3 times the standard deviation of the arsenic blank solution as the detection limit of arsenic, that is, 0.015 μg / mL is the minimum concent...

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Abstract

The invention discloses a method for analyzing arsenic content in a glass refining agent, which comprises the following steps: processing samples by a potassium permanganate preoxidation-hydrofluoric acid wet digestion method to obtain a sample digestion solution; measuring the content of arsenic in the digestion solution by an inductance coupling plasma atomic emission spectrometry. By using potassium permanganate as a pre-oxidizing agent to carry out routine wet acid digestion on glass refining agent samples, the method can effectively avoid volatilizable loss of low-valent arsenic components in the preliminary processing of the samples, therefore, a routine inductance coupling plasma atomic emission spectrometer can be used to directly measure the content of the effective content-arsenic in the glass refining agent without allocating a hydride generator or an atomic fluorescence spectrometer. The method has the advantages of high operability, high analysis speed, high accuracy and favorable sensitivity and repetitiveness.

Description

technical field [0001] The invention belongs to the technical field of physical and chemical testing, and in particular relates to an analysis and determination method for arsenic content in glass clarifiers. Background technique [0002] In the production of glass industry, commonly used glass clarifiers include nitrates, sulfates, ammonium salts, fluorides, rare earth minerals, arsenic trioxide, antimony trioxide, etc. Among them, rare earth elements (such as cerium oxide) are used as glass clarifiers, which have good clarification effect and low pollution, but the disadvantage is that the price is high, and they are usually only used by some large glass manufacturers. Arsenic oxide and antimony oxide are traditional glass fining agents. Although they are toxic, especially arsenic oxide, they are still widely used in glass production because of their high-efficiency clarifying effect and relatively low price, such as most small enterprises. white arsenic, arsenic-antimony...

Claims

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Application Information

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IPC IPC(8): G01N21/73
Inventor 屈海云陈弈睿
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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