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Method for detecting zirconium content in chromium-free passivation solution

A detection method and a chromium-free passivation technology, applied in the field of analytical chemistry, can solve the problems of low accuracy of measurement results, complex processing technology, large acid consumption, etc., to meet production detection requirements, low operating cost, and high measurement accuracy. Effect

Pending Publication Date: 2022-03-18
CHINA FIRST AUTOMOBILE
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the Mg present in the passivation solution 2+ , Zn 2+ and Fe 3+ Plasma will cause certain interference to the measurement of zirconium content in the passivation solution, so the zirconium content in the passivation solution cannot be accurately measured, resulting in reduced passivation effect of the passivation solution
[0004] CN110243810A discloses a method for testing zirconium content in conversion coatings on the surface of metal materials. The method uses a standard test plate containing zirconium and a quality control panel corrected by an X-ray fluorescence spectrometer, and combines the X-ray fluorescence spectrometer to measure the content of zirconium in the conversion coating on the surface of metal materials. Element determination parameters, quantitative analysis of the zirconium element in the conversion coating on the surface of the metal material, the method is complicated in processing technology, uses more reagents, and is not suitable for industrial production
[0005] CN104614365A discloses an inductively coupled plasma atomic emission spectrometry for determining chromium and zirconium in copper-chromium-zirconium alloys. The method dissolves samples with nitric acid and sulfuric acid, and uses inductively coupled plasma atomic emission spectrometry to measure the chromium in copper-chromium-zirconium alloys. and zirconium content, this method consumes a lot of acid, it is difficult to control the interference of impurity elements in the sample, and the accuracy of the measurement results is relatively low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] This embodiment provides a detection method for zirconium content in a chromium-free passivation solution, the detection method comprising the following steps:

[0068] (1) After adding 10 mL of nitric acid solution with a molar concentration of 7 mol / L to 10 mL of passivation solution for acid treatment, carry out ion exchange purification by 732 cation exchange resin to obtain the test solution, which includes: Zr 4+ 60mg / L, Ca 2+ 35mg / L, Mg 2+ 130mg / L, Zn 2+ 25mg / L and Fe 3+ 15mg / L;

[0069] (2) Take 10 mL of zirconium standard solutions with mass concentrations of 1 mg / L, 2 mg / L, 3 mg / L, 4 mg / L and 5 mg / L respectively and add 10 mL of nitric acid solution with a molar concentration of 7 mol / L, and The power is 1150W, the cooling air flow is 15L / min, the carrier gas flow is 0.8L / min, the auxiliary air flow is 0.2L / min, the integration time is 60s, the pump speed is 2L / min, the observation height is 15mm, and the observation method is Carry out inductively couple...

Embodiment 2

[0073] This embodiment provides a detection method for zirconium content in a chromium-free passivation solution, the detection method comprising the following steps:

[0074] (1) After adding 10 mL of nitric acid solution with a molar concentration of 6 mol / L to 10 mL of passivation solution for acid treatment, carry out ion exchange purification by 732 cation exchange resin to obtain the test solution, which includes: Zr 4+ 45mg / L, Ca 2+ 36mg / L, Mg 2+ 125mg / L, Zn 2+ 38mg / L and Fe 3+ 14mg / L;

[0075] (2) Take 10mL of zirconium standard solutions with mass concentrations of 2mg / L, 4mg / L, 6mg / L, 8mg / L and 10mg / L respectively, and add 10mL of nitric acid solution with a molar concentration of 6mol / L respectively. The power is 1100W, the cooling air flow is 20L / min, the carrier gas flow is 0.7L / min, the auxiliary air flow is 0.1L / min, the integration time is 70s, the pump speed is 1L / min, the observation height is 16mm, and the observation method is Carry out inductively cou...

Embodiment 3

[0079] This embodiment provides a detection method for zirconium content in a chromium-free passivation solution, the detection method comprising the following steps:

[0080] (1) After adding 10 mL of nitric acid solution with a molar concentration of 8 mol / L to 10 mL of passivation solution for acid treatment, carry out ion exchange purification by 732 cation exchange resin to obtain the test solution, including: Zr in the passivation solution 4+ 76mg / L, Ca 2+ 32mg / L, Mg 2+ 134mg / L, Zn 2+ 12mg / L and Fe 3+ 18mg / L;

[0081] (2) Take 10 mL of zirconium standard solutions with mass concentrations of 1 mg / L, 3 mg / L, 5 mg / L, 7 mg / L and 9 mg / L respectively and add 10 mL of nitric acid solution with a molar concentration of 8 mol / L, and The power is 1200W, the cooling air flow is 10L / min, the carrier gas flow is 0.9L / min, the auxiliary air flow is 0.3L / min, the integration time is 50s, the pump speed is 3L / min, the observation height is 13mm, and the observation method is Carry...

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Abstract

The invention relates to a method for detecting the content of zirconium in a chromium-free passivation solution, and the method comprises the following steps: (1) the passivation solution is subjected to acid treatment and ion exchange purification in sequence to obtain a solution to be detected, the acid solution for acid treatment comprises a nitric acid solution, and the molar concentration of the nitric acid solution is 6-8 mol / L; (2) preparing a zirconium standard solution and carrying out zirconium content analysis to obtain a detection model; and (3) carrying out zirconium content analysis on the to-be-detected solution obtained in the step (1), and carrying out calculation through the detection model obtained in the step (2) to obtain the zirconium content of the passivation solution. The detection method provided by the invention has the advantages of simple operation, fewer reagents, repeated determination and higher determination precision, and meets the production and detection requirements.

Description

technical field [0001] The invention relates to the field of analytical chemistry, in particular to a method for detecting zirconium content in a chromium-free passivation solution. Background technique [0002] Passivation solution refers to a solution that can make the metal surface passivate, and is generally used for post-plating treatment of galvanized, cadmium or other coatings. The purpose of passivation solution treatment is to form a surface state on the surface of the coating that can prevent the normal reaction of the metal, improve its corrosion resistance, and increase the aesthetics of the product. Traditionally, hexavalent chromium passivation process has been used, but hexavalent chromium is one of the most toxic heavy metals identified so far. It is highly carcinogenic and causes blood diseases, bone diseases, early hair loss, premature skin aging and other problems, and Chromium accumulates in the environment for a long time and will endanger human health....

Claims

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Application Information

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IPC IPC(8): G01N21/73G01N1/34
CPCG01N21/73G01N1/34
Inventor 王慧娟寇英达李宇升孙硕雷蕾温家德刘兴宝孙凯付新
Owner CHINA FIRST AUTOMOBILE
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