Method for detecting content of titanium powder in waste residue after biological treatment of spraying waste gas

Abstract

The invention discloses a method for separating and detecting the content of titanium dioxide and titanium powder in waste residues after biological treatment of spraying waste gas. According to the method, the content of titanium atoms is detected according to the national standard inductively coupled plasma atomic emission spectrometry, then the content of titanium dioxide is detected by combining an X-ray fluorescence spectrum with a two-step acid selective dissolution method, and the content of titanium powder in the waste residues is obtained by subtracting numerical values detected twice. The detection process comprises the following steps: 1, detecting the total content of titanium atoms according to the national standard inductively coupled plasma atomic emission spectrometry; 2, detecting the content of titanium dioxide by combining an X-ray fluorescence spectrum with a two-step acid selective dissolution method; and 3, calculating the real content of the titanium powder in the waste residue by subtracting the numerical values detected twice, namely the content of the titanium powder = the total content of the titanium atoms-the content of the titanium dioxide. The method can solve the problem that the titanium powder and the titanium dioxide in the waste residues cannot be distinguished in the detection method provided by the existing national standard, and has important environmental protection and hazardous waste treatment significance.

Description

Technical Field

[0001] The present invention belongs to the technical field of waste residue detection after biological treatment of spraying waste gas, and relates to a detection method for distinguishing the content of titanium dioxide and titanium powder in waste residue after biological treatment of spraying waste gas, that is, a method for separating and detecting the content of titanium dioxide and titanium powder in waste residue after biological treatment of spraying waste gas. Background Art

[0002] Titanium dioxide (TiO 2 ) is a common additive in coatings and is widely used in the spraying process. Therefore, the waste residue generated during the treatment of spraying waste gas often contains titanium dioxide. However, due to the relatively stable nature of titanium dioxide, it is almost impossible to convert it into titanium in the traditional waste gas treatment process.

[0003] According to the "Identification of Toxic Substances in Hazardous Waste Identification Standards" (GB 5085.6-2007), titanium powder (CAS: 7440-32-6) is listed as a toxic substance and is detected by inductively coupled plasma atomic emission spectrometry (ICP-AES). However, the existing detection methods cannot distinguish between titanium powder and titanium dioxide in waste. They can only monitor the overall content of titanium, but cannot accurately detect how much of the titanium comes from titanium dioxide and how much comes from titanium alone. This affects the identification of the hazardousness of waste residues. It can be seen that there is an urgent need for a method that can accurately separate and detect the content of titanium dioxide and titanium powder in waste. Summary of the invention

[0004] The purpose of the present invention is to provide a method for effectively distinguishing the content of titanium dioxide and titanium powder in waste residue after biological treatment of spraying waste gas, that is, a method for separating and detecting the content of titanium dioxide and titanium powder in waste residue after biological treatment of spraying waste gas, so as to solve the technical problem that the content of titanium dioxide and titanium powder cannot be distinguished in the prior art. To achieve the above purpose, the technical solution adopted by the present invention is as follows:

[0005] The present invention provides a method for detecting the content of titanium powder in waste slag after biological treatment of spray waste gas as follows: using inductively coupled plasma atomic emission spectrometry and X-ray fluorescence spectroscopy combined with a two-step acid selective dissolution method to respectively detect the total content of titanium atoms and the content of titanium dioxide, and calculating the true content of titanium powder in the waste slag by subtracting the values ​​of the two detections; the detection process steps are as follows:

[0006] (1) Using inductively coupled plasma atomic emission spectrometry (ICP-AES) to determine the total content of titanium atoms in the waste slag;

[0007] (2) The titanium dioxide content in the waste residue was determined by using a specific separation technique, X-ray fluorescence spectroscopy, combined with a two-step acid selective dissolution method;

[0008] (3) The content of titanium powder in the waste slag is obtained by subtracting the content of titanium dioxide in the waste slag from the total content of titanium atoms in the waste slag.

[0009] Specifically, the present invention provides a method for separating and detecting the content of titanium dioxide and titanium powder in waste residue after biological treatment of spray waste gas, which is carried out according to the following steps:

[0010] (1) Detection of total titanium atom content: Inductively coupled plasma atomic emission spectrometry (ICP-AES) is used to detect the total titanium atom content of waste slag samples in accordance with the "Identification Standard for Hazardous Wastes - Identification of Leaching Toxicity" (GB 5085.3-2007). This method can measure the total content of all titanium substances (including titanium dioxide and titanium powder) in waste slag.

[0011] (2) Detection of titanium dioxide content: X-ray fluorescence spectroscopy combined with selective dissolution method is used to detect titanium dioxide in waste residue separately. This method uses two acidic reagents, dilute nitric acid and concentrated sulfuric acid, to selectively dissolve the waste residue in two steps to separate titanium dioxide, and then uses X-ray fluorescence spectroscopy to detect the titanium dioxide content in the solution after dissolution with concentrated sulfuric acid. This method can effectively separate titanium dioxide from waste residue and accurately determine its content through the two-step separation technology of acidic reagents and X-ray fluorescence spectroscopy analysis.

[0012] (3) Calculation of titanium powder content: The actual content of titanium powder in the waste slag is calculated by subtracting the values ​​of the two tests, that is, titanium powder content = total titanium atom content - titanium dioxide content. This calculation method can accurately reflect the content of titanium powder in the waste slag, solving the problem that titanium dioxide and titanium powder cannot be distinguished in the prior art.

[0013] Furthermore, the titanium dioxide content detection method of step (2) is specifically as follows: first use dilute nitric acid (mass concentration 5%-10%) to dissolve titanium substances other than titanium dioxide in the waste residue, then filter the solution and retain the filter residue (waste residue). The filtered filter residue (waste residue) contains the remaining titanium dioxide, and then use concentrated sulfuric acid to dissolve the titanium dioxide in the filter residue (waste residue). Finally, use X-ray fluorescence spectroscopy to determine the titanium dioxide content in the solution after dissolution with concentrated sulfuric acid.

[0014] Furthermore, in step (2), before the titanium dioxide content is detected, the waste residue sample is placed in a quartz crucible and the sample is preliminarily calcined at a temperature of about 500-600° C. for 1-2 hours to remove moisture and volatile substances.

[0015] Furthermore, in step (2), 15-30 mL of dilute nitric acid with a mass concentration of 5%-10% is added to 1 g of the calcined waste residue sample, heated to 80-90° C., and reacted for 20-30 minutes to dissolve titanium substances (elemental titanium) in the waste residue except titanium dioxide.

[0016] Furthermore, in step (2), 10-15 mL of concentrated sulfuric acid is added to the solid waste residue (filter residue) after dissolving and filtering with dilute nitric acid, and the mixture is heated to 110-130° C. until the solid waste residue is completely dissolved, at which time the titanium dioxide is completely converted into titanium ions in the solution; pure titanium dioxide is used to prepare a standard substance, a calibration curve is established, and a mixture of elemental titanium and titanium dioxide is used as a comparison standard, and the content of the titanium dioxide part after acid dissolution is determined on an XRF (X-ray fluorescence spectrometer).

[0017] Beneficial effects of the present invention:

[0018] The detection method for distinguishing the content of titanium dioxide and titanium powder in waste residue after biological treatment of spraying waste gas solves the problem that the existing standard cannot distinguish titanium powder and titanium dioxide.

[0019] The method provided by the present invention can effectively distinguish the content of titanium dioxide and titanium powder in the waste residue after the biological treatment of spray waste gas, and solves the problem of inaccurate detection in the prior art. By accurately measuring the content of titanium dioxide and titanium powder in the waste residue, the danger of the waste residue can be more accurately evaluated, thereby providing a scientific basis for the treatment of the waste residue and environmental protection.

[0020] The method of the present invention is simple and easy to implement, can be used in combination with existing detection equipment and technology, and has good adaptability and operability. Through this method, the accuracy of hazardous waste identification and waste residue management can be effectively improved, and contributions can be made to environmental protection and public safety. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 It is a schematic diagram of the implementation process of the method for separating and detecting the content of titanium dioxide and titanium powder in waste residue after biological treatment of spray waste gas of the present invention. DETAILED DESCRIPTION

[0022] The present invention is further described in detail below in conjunction with the accompanying drawings and specific embodiments.

[0023] Example 1

[0024] The present invention provides a method for separating and detecting the content of titanium dioxide and titanium powder in waste residue after biological treatment of spray waste gas, and the specific implementation steps are as follows (such as Figure 1 shown):

[0025] (1) Waste residue sample collection: Select waste residue samples after biological treatment of spraying waste gas to ensure the representativeness and uniformity of the samples.

[0026] (2) Detection of total titanium atom content: According to the “Identification Standard for Hazardous Wastes - Identification of Leaching Toxicity” (GB 5085.3-2007), the total titanium atom content of the waste residue samples was detected using inductively coupled plasma atomic emission spectrometry (ICP-AES).

[0027] (3) Titanium dioxide content detection: Weigh 1g of waste residue sample accurately to 0.0001g, place it in a quartz crucible, and perform preliminary calcination (about 500°C, 2 hours) to remove moisture and volatile substances. Transfer the calcined sample to a PTFE beaker, add 15mL of dilute nitric acid (10%, w / w), keep it at about 90°C on a hot plate, and heat for 20 minutes to dissolve the elemental titanium. After dissolution, filter the solution and retain the residue (mainly TiO 2 and other insolubles). The filtered solid waste was transferred to another PTFE beaker, 10 mL of concentrated sulfuric acid and 5 mL of hydrofluoric acid (20%, w / w) were added, and heated (about 110°C) until the solid waste was completely dissolved. At this time, titanium dioxide was completely converted into titanium ions in the solution. Standard substances were prepared using pure titanium dioxide to establish a calibration curve. At the same time, mixtures of elemental titanium and titanium dioxide in different proportions were used as comparative samples. The content of titanium dioxide in the acid-dissolved part was determined on an XRF (X-ray fluorescence spectrometer).

[0028] (4) Calculation of titanium powder content: Based on the above two test results, the titanium powder content in the waste slag is calculated by subtracting the titanium dioxide content from the total titanium atom content.

[0029] (5) Data analysis and evaluation: Based on the test results, the composition of the waste residue is analyzed, its hazard is assessed, and appropriate disposal measures are taken.

[0030] Through the above steps, the content of titanium dioxide and titanium powder in the waste slag can be accurately detected, providing strong support for the subsequent treatment and environmental management of the waste slag.

[0031] Example 2

[0032] The present invention provides a method for separating and detecting the content of titanium dioxide and titanium powder in waste residue after biological treatment of spraying waste gas, which is suitable for treating spraying waste gas containing a large amount of quartz sand or abrasive in the spraying liquid. The specific implementation steps are as follows (such as Figure 1 shown):

[0033] (1) Waste residue sample collection: Select waste residue samples after biological treatment of spraying waste gas to ensure the representativeness and uniformity of the samples.

[0034] (2) Detection of total titanium atom content: According to the “Identification Standard for Hazardous Wastes - Identification of Leaching Toxicity” (GB 5085.3-2007), the total titanium atom content of the waste residue samples was detected using inductively coupled plasma atomic emission spectrometry (ICP-AES).

[0035] (3) Titanium dioxide content detection: Weigh 1g of waste residue sample accurately to 0.0001g, place it in a quartz crucible, and perform preliminary calcination (about 550°C, 1.5 hours) to remove moisture and volatile substances. Transfer the calcined sample to a PTFE beaker, add 20mL of dilute nitric acid (8%), and heat on a hot plate at about 85°C for 25 minutes to dissolve the elemental titanium. After dissolution, filter the solution and retain the residue (mainly TiO 2 and other insolubles). Transfer the filtered solid waste to another PTFE beaker, add 12 mL of concentrated sulfuric acid and 6 mL of hydrofluoric acid (20%, w / w). Heat (about 120°C) until the solid waste is completely dissolved. At this time, the titanium dioxide is completely converted into titanium ions in the solution. Use pure titanium dioxide to prepare standard substances and establish a calibration curve. At the same time, use mixtures of elemental titanium and titanium dioxide in different proportions as comparative samples. Measure the content of the titanium dioxide part after acid dissolution on an XRF (X-ray fluorescence spectrometer).

[0036] (4) Calculation of titanium powder content: Based on the above two test results, the titanium powder content in the waste slag is calculated by subtracting the titanium dioxide content from the total titanium atom content.

[0037] (5) Data analysis and evaluation: Based on the test results, the composition of the waste residue is analyzed, its hazard is assessed, and appropriate disposal measures are taken.

[0038] Through the above steps, the content of titanium dioxide and titanium powder in the waste slag can be accurately detected, providing strong support for the subsequent treatment and environmental management of the waste slag.

[0039] Example 3

[0040] The present invention provides a method for separating and detecting the content of titanium dioxide and titanium powder in waste residue after biological treatment of spray waste gas, and the specific implementation steps are as follows (such as Figure 1 shown):

[0041] (1) Waste residue sample collection: Select waste residue samples after biological treatment of spraying waste gas to ensure the representativeness and uniformity of the samples.

[0042] (2) Detection of total titanium atom content: According to the “Identification Standard for Hazardous Wastes - Identification of Leaching Toxicity” (GB 5085.3-2007), the total titanium atom content of the waste residue samples was detected using inductively coupled plasma atomic emission spectrometry (ICP-AES).

[0043] (3) Titanium dioxide content detection: Weigh 1g of waste residue sample accurately to 0.0001g, place it in a quartz crucible, and perform preliminary calcination (about 600°C, 1 hour) to remove moisture and volatile substances. Transfer the calcined sample to a PTFE beaker, add 30mL of dilute nitric acid (5%), and heat on a hot plate at about 80°C for 30 minutes to dissolve the elemental titanium. After dissolution, filter the solution and retain the residue (mainly TiO 2 and other insolubles). Transfer the filtered solid waste to another PTFE beaker, add 15mL of concentrated sulfuric acid and 8mL of hydrofluoric acid (if the sample contains silicon), and heat (about 110°C) until the solid waste is completely dissolved. At this time, titanium dioxide is completely converted into titanium ions in the solution. Use pure titanium dioxide to prepare standard substances and establish a calibration curve. At the same time, a mixture of elemental titanium and titanium dioxide is used as a comparison standard. Determine the content of titanium dioxide in the acid-dissolved part on an XRF (X-ray fluorescence spectrometer).

[0044] (4) Calculation of titanium powder content: Based on the above two test results, the titanium powder content in the waste slag is calculated by subtracting the titanium dioxide content from the total titanium atom content.

[0045] (5) Data analysis and evaluation: Based on the test results, the composition of the waste residue is analyzed, its hazard is assessed, and appropriate disposal measures are taken.

[0046] Through the above steps, the content of titanium dioxide and titanium powder in the waste slag can be accurately detected, providing strong support for the subsequent treatment and environmental management of the waste slag.

Claims

1. A method for detecting the content of titanium powder in waste residue after biological treatment of spray waste gas, characterized in that: The total content of titanium atoms and the content of titanium dioxide were detected by inductively coupled plasma atomic emission spectrometry and X-ray fluorescence spectroscopy combined with a two-step acid selective dissolution method. The actual content of titanium powder in the waste slag was calculated by subtracting the values ​​of the two tests. The detection process steps are as follows: (1) Using inductively coupled plasma atomic emission spectrometry (ICP-AES) to determine the total content of titanium atoms in the waste slag; (2) Using a specific separation technique, X-ray fluorescence spectroscopy combined with a two-step acid selective dissolution method, the titanium dioxide content in the waste residue was determined; (3) The content of titanium powder in the waste slag is obtained by subtracting the content of titanium dioxide in the waste slag from the total content of titanium atoms in the waste slag.

2. The method for detecting the content of titanium powder in waste residue after biological treatment of spraying waste gas according to claim 1, characterized in that: Follow these steps: (1) Detection of total titanium atom content: Inductively coupled plasma atomic emission spectrometry (ICP-AES) was used to detect the waste slag sample in accordance with the national standard GB 5085.3-2007 to determine the total content of titanium atoms in the waste slag; (2) Detection of titanium dioxide content: The titanium dioxide content in the waste residue is further detected by using X-ray fluorescence spectroscopy combined with a two-step acid selective dissolution method; this method uses two acidic reagents, dilute nitric acid and concentrated sulfuric acid, to selectively dissolve the waste residue in two steps to separate titanium dioxide, and then uses X-ray fluorescence spectroscopy to detect the titanium dioxide content in the waste residue; (3) Calculation of titanium powder content: The actual content of titanium powder in the waste slag is calculated by subtracting the values ​​of the first two tests, that is, titanium powder content = total content of titanium atoms - titanium dioxide content.

3. The method for detecting the content of titanium powder in waste residue after biological treatment of spraying waste gas according to claim 2 is characterized in that: The titanium dioxide content detection method of step (2) is specifically as follows: first use dilute nitric acid to dissolve titanium substances other than titanium dioxide in the waste residue, then filter the solution and retain the waste residue. The filtered waste residue contains the remaining titanium dioxide, and then use concentrated sulfuric acid to dissolve the titanium dioxide in the waste residue. Finally, use X-ray fluorescence spectroscopy to determine the titanium dioxide content in the solution dissolved with concentrated sulfuric acid.

4. The method for detecting the content of titanium powder in waste residue after biological treatment of spraying waste gas according to claim 2, characterized in that: In step (2), the dilute nitric acid is a dilute nitric acid with a mass concentration of 5%-10%.

5. The method for detecting the content of titanium powder in waste residue after biological treatment of spraying waste gas according to claim 3 is characterized in that: In step (2), before the titanium dioxide content is detected, the waste residue sample is placed in a quartz crucible and the sample is preliminarily calcined at a temperature of 500-600° C. for 1-2 hours.

6. The method for detecting the content of titanium powder in waste residue after biological treatment of spraying waste gas according to claim 5, characterized in that: Add 15-30 mL of dilute nitric acid with a mass concentration of 5%-10% to 1 g of the calcined waste residue sample, heat to 80-90° C., react for 20-30 minutes, and dissolve titanium substances including elemental titanium in the waste residue except titanium dioxide.

7. The method for detecting the content of titanium powder in waste residue after biological treatment of spraying waste gas according to claim 6 is characterized in that: After dissolving the filtered solid waste residue in dilute nitric acid, add 10-15 mL of concentrated sulfuric acid and heat to 110-130° C. until the solid waste residue is completely dissolved.

8. The method for detecting the content of titanium powder in waste residue after biological treatment of spraying waste gas according to claim 7 is characterized in that: Pure titanium dioxide was used to prepare standard substances and establish a calibration curve. A mixture of elemental titanium and titanium dioxide was used as a comparative standard. The content of the titanium dioxide part after acid dissolution was determined on an X-ray fluorescence spectrometer.

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