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Method for measuring content of sulfur in steel rolling oily sludge

A technology of sulfur content and oil sludge, which is applied in the field of chemical analysis, can solve the problems of gas circuit blockage, large human operation errors, cumbersome steps, etc., and achieve the effects of reducing consumption, shortening service life, and easy operation

Pending Publication Date: 2021-11-19
INST OF RES OF IRON & STEEL JIANGSU PROVINCE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, there is no relevant standard method for the determination of sulfur in oily sludge from rolling mills. For the analysis of sulfur content in solid powder substances, the gravimetric method is commonly used, but it has the disadvantages of large human error and cumbersome steps, and is not suitable for low-sulfur Determination of content samples; there is also a high-frequency induction combustion infrared absorption method for the determination of sulfur elements, but the dust generated by high-temperature oxygen blowing of powder samples is easily adsorbed on the furnace head during the detection process, causing blockage of the gas path and affecting the accuracy of the detection results
In recent years, with the development of instrument application technology, inductively coupled plasma emission spectrometer and atomic absorption spectrometer have also been tried to be applied to the composition analysis of solid powder samples, but there are a lot of oily substances in the oily sludge samples of steel rolling, which cannot be directly analyzed. Instrument testing, the consumption of chemical reagents in the conventional acid dissolution pretreatment method is too large, and it is easy to cause harm to the operating environment and the health of testing personnel
Therefore, conventional detection methods cannot satisfy the determination of sulfur content in oily sludge from steel rolling.

Method used

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  • Method for measuring content of sulfur in steel rolling oily sludge
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  • Method for measuring content of sulfur in steel rolling oily sludge

Examples

Experimental program
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Effect test

Embodiment 1

[0040] A method for measuring the sulfur content in steel rolling oily sludge, the specific implementation steps of the measuring method are as follows:

[0041] (1) Drying and grinding: Retrieve steel rolling oily sludge sample 1# on site, place it in a drying oven, dry at 110°C for 2 hours, and pass the sample through a 120-mesh metal mesh screen after drying and grinding;

[0042] (2) Burning at low temperature: take the sample obtained in step (1), put it in a muffle furnace and burn it at 450°C for 1.5h;

[0043] (3) Digestion: Weigh 0.1000 g of the sample obtained in step (2), add 20 mL, 50% dilute nitric acid, and 3 mL perchloric acid, and carry out digestion treatment on a 180° C. When the volume of the digestion solution is 0.5-1mL, remove it;

[0044] (4) Acidification: dissolve the digestion solution with 5mL of water, add 10mL of dilute hydrochloric acid to acidify, and dilute to a 100mL volumetric flask to obtain the solution to be tested, and make a reagent blan...

Embodiment 2

[0057] A method for measuring the sulfur content in steel rolling oily sludge, the specific steps of the method for the determination are as follows:

[0058] (1) Drying and grinding: Retrieve steel rolling oily sludge sample 2# in the drying oven, dry at 105°C for 3 hours, and pass the sample through a 120-mesh metal mesh screen after drying and grinding;

[0059] (2) Burning at low temperature: take the sample obtained in step (1), put it in a muffle furnace and burn it at 500°C for 1.5h;

[0060] (3) Digestion: Weigh 0.2000 g of the sample obtained in step (2), add 30 mL, 50% dilute nitric acid, and 5 mL perchloric acid, carry out digestion treatment on a 200° C. When the volume of the digestion solution is 0.5-1mL, remove it;

[0061] (4) Acidification: Dissolve the digestion solution with 3mL of water, add 10mL of dilute hydrochloric acid to acidify, and dilute to a 100mL volumetric flask to obtain the solution to be tested, and make a reagent blank along with the sample...

Embodiment 3

[0068] A method for measuring the sulfur content in steel rolling oily sludge, the specific steps of the method for the determination are as follows:

[0069] (1) Drying and grinding: Retrieve steel rolling oily sludge sample 3# on site and place it in a drying oven, dry at 110°C for 2.5 hours, and pass the sample through a 120-mesh metal mesh screen after drying and grinding;

[0070] (2) Burning at low temperature: take the sample obtained in step (1), put it in a high-temperature furnace and burn at 480°C for 2 hours;

[0071] (3) Digestion: Weigh 0.1500 g of the sample obtained in step (2), add 30 mL, 50% dilute nitric acid, and 4 mL perchloric acid, carry out digestion treatment on a 160° C. When the volume of the digestion solution is 0.5-1mL, remove it;

[0072] (4) Acidification: dissolve the digestion solution with 5mL of water, add 10mL of dilute hydrochloric acid to acidify, and dilute to a 100mL volumetric flask to obtain the solution to be tested, and make a reag...

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Abstract

The invention discloses a method for measuring the content of sulfur in steel rolling oily sludge. The method comprises the following steps: (1) drying and grinding: drying a sample, grinding and sieving; (2) low-temperature firing: performing low-temperature firing in a muffle furnace; (3) digestion: adding nitric acid and perchloric acid for digestion treatment; (4) acidification: acidifying the digestion solution to obtain a solution to be detected; (5) preparing standard solutions: preparing sulfur element series standard solutions; (6) instrument detection: determining the content of the sulfur element in the solution to be detected; and (7) result calculation: calculating the content of the sulfur element in the sample according to a formula. The method provided by the invention fills the technical blank of a method for measuring the sulfur content in the steel rolling oily sludge in China, is simple to operate and accurate in result, and has important significance on monitoring the sulfur content in the steel rolling oily sludge during subsequent recycling.

Description

technical field [0001] The application relates to the technical field of chemical analysis, in particular to a method for determining the sulfur content in oily sludge from steel rolling. Background technique [0002] The steel rolling waste water produced by steel mills in hot rolling, pickling, cold rolling and other processes contains small particles of iron oxide scale and various lubricating oils. After precipitation, filtration, cooling and other processes, the steel rolling wastewater is solid waste containing iron oxide scale (commonly known as iron scale) and various greases. This kind of solid waste is often called steel rolling oily sludge. Its ingredients are iron oxide scale, oily substances, water, a small amount of oxides of silicon, aluminum, calcium, and harmful impurities phosphorus and sulfur. In recent years, in response to the country's full recovery and utilization of solid waste resources, steel mills have paid more and more attention to the follow-up...

Claims

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Application Information

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IPC IPC(8): G01N21/73G01N1/44G01N1/28
CPCG01N21/73G01N1/44G01N1/286G01N1/28G01N2001/2866
Inventor 董礼男周莉莉张继明朱春要
Owner INST OF RES OF IRON & STEEL JIANGSU PROVINCE
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