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Method for determining content of hydrofluoric acid in nitric acid-hydrofluoric acid pickling solution

The technology of a hydrofluoric acid type acid and a determination method is applied in the field of analysis and testing of electroplating solutions, which can solve problems such as many operation steps, and achieve the effects of low cost, accurate and consistent detection results, and convenient detection process.

Inactive Publication Date: 2017-05-31
江南工业集团有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has many steps, the test cycle takes 2 days, and the heavy metal lead that pollutes the environment is used.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0030] (2) Preparation of fluorine standard stock solution: Weigh 2.0985g of benchmark pure sodium fluoride (accurate to 0.0001g) after drying at 105°C for 2h and cooling in a desiccator, dissolve it in water, dilute to 1000mL, shake well, Stored in a polyethylene bottle, the concentration of fluorine in this solution converted to hydrofluoric acid is 1mg / mL;

[0031] (3) Preparation of fluorine standard solution A: Pipette 1.00mL of fluorine standard stock solution into a 100mL volumetric flask, add water to the mark, shake well, store in a polyethylene bottle, and convert the fluorine content in this solution into hydrofluoric acid The concentration is 0.01mg / mL;

[0032] (4) Preparation of fluorine standard solution B: Pipette 5.00mL of fluorine standard stock solution into a 100mL volumetric flask, add water to the mark, shake well, store in a polyethylene bottle, and convert the fluorine content in this solution into hydrofluoric acid The concentration is 0.05mg / mL;

[...

Embodiment 2

[0046] The same method as in Example 1 was adopted, except that Sample 1 was replaced with Sample 2.

[0047] Through measurement and calculation, the content of hydrofluoric acid in sample 2 is 2.72g / L.

Embodiment 3

[0049] The same method as in Example 1 was adopted, except that Sample 1 was replaced with Sample 3.

[0050] Through measurement and calculation, the content of hydrofluoric acid in sample 3 was obtained to be 3.05g / L.

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Abstract

The invention discloses a method for determining a content of hydrofluoric acid in a nitric acid-hydrofluoric acid pickling solution. The method comprises the steps of preparing a sodium citrate-sodium nitrate total ion strength buffer solution, preparing a fluorine standard storage solution, preparing a fluorine standard solution A and a fluorine standard solution B, preparing a test sample solution, preparing a fluorine standard application solution A and a fluorine standard application solution B, preparing a test sample application solution, mounting an ion meter, calibrating a slope when in concentration measurement, measuring the concentration, calculating the content of the hydrofluoric acid of a test sample and the like. By adopting the precision ion meter, a fluorine ion selective electrode is adopted as an indicator electrode which is inserted into a solution to be detected together with a reference electrode, so that an electrochemical system for determination is formed; a concentration mode is selected, and a two-point calibration is adopted; and by adding the total ion strength buffer solution, the influence of interference ions and acidity can be eliminated, and the content of the hydrofluoric acid in the test solution is directly determined. The determination method is simple, convenient, rapid and environment-friendly in the detection process, low in expense and cost, accurate and consistent in detection results, and capable of supporting the maintenance and quality control of the acid pickling solution.

Description

technical field [0001] The invention relates to a method for measuring hydrofluoric acid content in a nitric acid-hydrofluoric acid type pickling solution, belonging to the field of analysis and testing of electroplating solutions. Background technique [0002] The mixture of nitric acid and hydrofluoric acid has loosening ability and strong dissolution. Widely used to remove heat-treated scale on lead, stainless steel, nickel- and iron-based alloys, titanium, zirconium, and certain cobalt-based alloys. The technical parameters of a titanium alloy pickling solution are HF: 10g / L~50g / L; HNO 3 : 150g / L~200g / L. At present, the domestic method for determining the hydrofluoric acid content in the nitric acid-hydrofluoric acid type pickling solution is to add lead nitrate and sodium chloride to the neutral solution to separate the fluoride ion in the form of lead fluoride chloride, and then dissolve it with nitric acid. , to generate chloride ions, react with silver nitrate to ...

Claims

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Application Information

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IPC IPC(8): G01N27/26
CPCG01N27/26
Inventor 许自强任志忠胡德意罗臻葵许成尹公晖谭琳叶甜甜
Owner 江南工业集团有限公司
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