CN113670896A - Method for measuring sulfur content in steel rolling oily sludge - Google Patents
Method for measuring sulfur content in steel rolling oily sludge Download PDFInfo
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- CN113670896A CN113670896A CN202110984410.4A CN202110984410A CN113670896A CN 113670896 A CN113670896 A CN 113670896A CN 202110984410 A CN202110984410 A CN 202110984410A CN 113670896 A CN113670896 A CN 113670896A
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 75
- 239000011593 sulfur Substances 0.000 title claims abstract description 75
- 238000000034 method Methods 0.000 title claims abstract description 52
- 239000010802 sludge Substances 0.000 title claims abstract description 49
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 48
- 239000010959 steel Substances 0.000 title claims abstract description 48
- 238000005096 rolling process Methods 0.000 title claims abstract description 41
- 239000012086 standard solution Substances 0.000 claims abstract description 42
- 239000000243 solution Substances 0.000 claims abstract description 41
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000001035 drying Methods 0.000 claims abstract description 28
- 230000029087 digestion Effects 0.000 claims abstract description 22
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000000227 grinding Methods 0.000 claims abstract description 13
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 13
- 238000010304 firing Methods 0.000 claims abstract description 11
- 238000011282 treatment Methods 0.000 claims abstract description 10
- 238000007873 sieving Methods 0.000 claims abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 23
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 19
- 238000009616 inductively coupled plasma Methods 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000004458 analytical method Methods 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000011159 matrix material Substances 0.000 claims description 6
- 230000020477 pH reduction Effects 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 239000000779 smoke Substances 0.000 claims description 5
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 5
- 239000012498 ultrapure water Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 4
- 238000004364 calculation method Methods 0.000 claims description 3
- 230000010354 integration Effects 0.000 claims description 3
- 229920003023 plastic Polymers 0.000 claims description 3
- 239000004033 plastic Substances 0.000 claims description 3
- 238000004064 recycling Methods 0.000 abstract description 2
- 238000005008 domestic process Methods 0.000 abstract 1
- 238000012544 monitoring process Methods 0.000 abstract 1
- 150000003463 sulfur Chemical class 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 48
- 239000003153 chemical reaction reagent Substances 0.000 description 9
- 238000001514 detection method Methods 0.000 description 8
- 229910052742 iron Inorganic materials 0.000 description 7
- 239000003921 oil Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000007865 diluting Methods 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000012216 screening Methods 0.000 description 3
- 239000002910 solid waste Substances 0.000 description 3
- 230000003595 spectral effect Effects 0.000 description 3
- 238000009628 steelmaking Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000002372 labelling Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000005097 cold rolling Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 238000005098 hot rolling Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000006101 laboratory sample Substances 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000014593 oils and fats Nutrition 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010731 rolling oil Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
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Abstract
The invention discloses a method for measuring sulfur content in steel rolling oily sludge, which comprises the following steps: (1) drying and grinding: drying the sample, grinding and sieving; (2) low-temperature firing: firing in a muffle furnace at a low temperature; (3) digestion: adding nitric acid and perchloric acid for digestion treatment; (4) acidifying: acidifying the digestion solution to obtain a solution to be detected; (5) standard solution: preparing a sulfur series standard solution; (6) detecting by an instrument: measuring the content of sulfur element in the solution to be measured; (7) and (4) calculating a result: and calculating the content of sulfur element in the sample according to a formula. The method provided by the invention fills the technical blank of the domestic method for measuring the sulfur content in the steel rolling oily sludge, is simple to operate, has accurate results, and has important significance for monitoring the sulfur element content in the steel rolling oily sludge during subsequent recycling.
Description
Technical Field
The application relates to the technical field of chemical analysis, in particular to a method for measuring sulfur content in steel rolling oily sludge.
Background
Steel rolling wastewater generated by hot rolling, acid washing, cold rolling and other process flows in a steel plant contains small-particle iron scales and various lubricating oils. After steel rolling wastewater is subjected to the procedures of precipitation, filtration, cooling and the like, solid waste containing iron scales (commonly called as iron scales) and various oils and fats is obtained, and the solid waste is often called as steel rolling oily sludge. The components of the fertilizer are iron scale, grease substances, moisture, a small amount of oxides of silicon, aluminum and calcium and harmful impurities of phosphorus and sulfur. In recent years, in response to the national full recycling of solid waste resources, steel mills pay more attention to the subsequent treatment of steel rolling oily sludge, and the most common method is to reuse the oil sludge as a steel smelting raw material after a series of treatments. The steel rolling oily sludge contains a certain amount of sulfur, and the sulfur element can generate adverse effects on the mechanical property, corrosion resistance and weldability of steel, so the sulfur element is often used as a harmful impurity in the steel making process and the content needs to be strictly controlled.
At present, no relevant standard method exists for measuring sulfur element in steel rolling oily sludge, a gravimetric method is common for the analytical means of sulfur content in solid powder substances, but the defects of large manual operation error and complicated steps exist, and the method is not suitable for measuring low-sulfur content samples; the sulfur element is also determined by adopting a high-frequency induction combustion infrared absorption method, but dust generated by high-temperature oxygen blowing in the detection process of the powder sample is easily adsorbed on a furnace head, so that the gas path is blocked, and the accuracy of the detection result is influenced. In recent years, with the development of instrument application technologies, inductively coupled plasma emission spectrometers and atomic absorption spectrometers are also tried to be applied to component analysis of solid powder samples, but a large amount of oil substances exist in steel rolling oily sludge samples, so that instrument detection cannot be directly performed, the consumption of chemical reagents in the conventional acid dissolution pretreatment method is too large, and the method is easy to cause harm to the operating environment and the physical health of detection personnel. Therefore, the conventional detection means cannot meet the requirement of measuring the sulfur content in the steel rolling oily sludge.
In order to solve the technical problem, the invention provides a method for measuring the sulfur content in steel rolling oily sludge. The method is simple and convenient to operate, has high result accuracy, reduces the dosage of chemical reagents in the detection process, and can meet the requirement of measuring the sulfur content in the steel rolling oily sludge while meeting the requirement of environmental protection.
Disclosure of Invention
The invention aims to provide a method for measuring the content of sulfur element in steel rolling oily sludge, which overcomes the defects in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme: a method for measuring the content of sulfur element in steel rolling oil-containing sludge comprises the following steps:
step 1: drying and grinding: taking back the sample on site, drying in a drying box, grinding and sieving;
step 2: low-temperature firing: drying and grinding the sample, and then burning at low temperature;
and step 3: digestion: weighing 0.1000-0.2000 g of sample, adding 20-30 mL of dilute nitric acid and 3-5 mL of perchloric acid, performing digestion treatment on the sample in an electric furnace at 150-200 ℃, heating the sample until perchloric acid smoke is emitted, and taking down the sample when the volume of the digestion solution is 0.5-1 mL;
and 4, step 4: acidifying: dissolving the digestion solution with 3-5 mL of pure water, adding 10mL of dilute hydrochloric acid for acidification, and fixing the volume to a 100mL volumetric flask to obtain a solution to be detected;
and 5: standard solution: taking 6 100mL volumetric flasks, respectively adding 10mL of dilute hydrochloric acid, adding an iron element standard solution with the same content as the sample as a matrix solution, and finally adding a sulfur element standard solution to prepare a series of standard solutions for drawing a standard curve;
and 5: standard solution: taking n 100mL volumetric flasks, respectively adding 10mL of dilute hydrochloric acid, then adding an iron element standard solution with the content similar to that of the sample as a matrix solution, and finally accurately transferring sulfur element standard solutions with different volumes to prepare a sulfur element series standard solution with a mass concentration gradient;
step 6: detecting by an instrument: measuring a series of standard solutions by using an inductively coupled plasma emission spectrometer, establishing a standard curve, and measuring the solution to be measured according to phase synchronization steps to obtain the content of sulfur elements in the solution to be measured;
and 7: and (4) calculating a result: the sulfur element content calculation formula of the oily sludge sample is as follows:
in the formula:
omega (S) -sulfur content in the oily sludge sample,%;
c, obtaining the concentration of sulfur element in the solution to be detected from the working curve, mg/L;
v, determining the volume of the solution to be detected to be the volume mL;
m-weighing the mass of the oily sludge sample, g;
preferably, in step 1, the drying process includes: the drying temperature is 105-110 ℃, and the drying time is 2-3 h; after grinding, the particle size of the ground and filtered by a metal mesh screen is 120 meshes.
Preferably, in the step 2, the low-temperature burning process is as follows: the ignition temperature is 400-500 ℃, and the ignition time is 1.5-2 h.
Preferably, in the step 3, the concentration of the dilute nitric acid is 1.42g/cm3The concentration of the perchloric acid is 1.67g/cm3。
Preferably, in the step 3, the volume fraction of the dilute nitric acid is 50%.
Preferably, in the steps 4 and 5, the concentration of the dilute hydrochloric acid is 1.18g/cm3The volume fraction was 50%.
Preferably, in the step 5, the concentration of the standard solution of the iron element is 2.0000g/L, and the concentration of the standard solution of the sulfur element is 1000 mg/L.
Preferably, in the step 5, the number of the n 100mL volumetric flasks is 4-8, and the gradient range of the mass concentration of the sulfur element in the series of standard solutions covers the mass concentration of the sulfur element in the solution to be measured.
Preferably, in step 6, the operating conditions of the inductively coupled plasma emission spectrometer are as follows: the radio frequency power is 1150W, the auxiliary air flow is 0.5L/min, the cooling air flow is 15L/min, the atomizer flow is 0.75L/min, the analysis pump speed is 50r/min, the sample washing time is 10s, and the integration time is 30 s.
Preferably, in step 6, the wavelength selected when the inductively coupled plasma emission spectrometer measures the intensity of sulfur in the solution is 182.034 nm.
Preferably, the pure water is ultrapure water, and the volumetric flask is a plastic volumetric flask.
The invention has the beneficial effects that:
(1) the determination method provided by the invention removes the water and oil in the sample by drying and low-temperature firing treatment, effectively avoids the blockage phenomenon caused to the central tube of the ICP instrument device when detecting oil substances, and the blockage can directly influence the accuracy of the detection result and shorten the service life of the instrument.
(2) According to the determination method, after low-temperature ignition, the sample is digested by nitric acid and perchloric acid, and a small amount of residual organic matters are removed, so that the sample is completely converted into an inorganic aqueous solution, the operation is simple and convenient, the consumption of chemical reagents is reduced, and the requirement for determining the sulfur content in the steel rolling oily sludge can be met while the environment-friendly requirement is met.
(3) The method fills the technical blank of the analysis method of the sulfur element content in the steel rolling oily sludge in China, and has important guiding significance for controlling the sulfur element content when the steel rolling oily sludge is recycled as a steel making raw material.
Detailed Description
Technical solutions in the embodiments of the present invention will be described in detail below, and it is apparent that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The invention adopts the following instruments and reagents in the following method:
the instrument equipment comprises: inductively coupled plasma emission spectrometer (iCAP6300 sreis , usa); an electric heating air blast drying box (FT101A (S) P-3 type, Zhenjianfengtai laboratory sample preparation equipment Co., Ltd.); high temperature muffle furnace (model N31/H, Naberterm, Germany); electronic balance (XP204, mettler-toledo); ultra pure water apparatus (Millipore, USA).
All reagents are superior pure: nitric acid (1.42 g/cm)3) (ii) a Perchloric acid (1.67 g/cm)3) (ii) a Hydrochloric acid (1.18 g/cm)3) (ii) a Iron element standard solution (2.0000g/L, preparation method: weighing 2.0000g high purity iron, placing in 250mL beaker, addingAdding 50mL of hydrochloric acid solution (1+1), heating at low temperature for dissolving, dropwise adding nitric acid for acidification, boiling at low temperature for removing nitrogen oxides, cooling, transferring into a 1000mL volumetric flask, diluting with water to a scale, and shaking up); standard solution of elemental sulfur (1000mg/L, national iron and Steel materials testing center iron and Steel research institute). All the test instruments are used after being soaked for 24 hours by hydrochloric acid with the volume fraction of 5 percent and then rinsed for three times by ultrapure water. All volumetric flasks are plastic volumetric flasks. The pure water is ultrapure water. The working conditions of the inductively coupled plasma emission spectrometer are as follows: the radio frequency power is 1150W, the auxiliary air flow is 0.5L/min, the cooling air flow is 15L/min, the atomizer flow is 0.75L/min, the analysis pump speed is 50r/min, the sample washing time is 10s, the integration time is 30s, and the automatic observation mode is adopted.
Example 1
A method for measuring the sulfur content in steel rolling oily sludge comprises the following specific implementation steps:
(1) drying and grinding: taking a steel rolling oily sludge sample No. 1 back on site, placing the sample in a drying box, drying the sample for 2 hours at 110 ℃, and screening the dried and ground sample through a 120-mesh metal screen;
(2) low-temperature firing: putting the sample obtained in the step (1) into a muffle furnace, and burning for 1.5h at 450 ℃;
(3) digestion: weighing 0.1000g of the sample obtained in the step (2), adding 20mL of dilute nitric acid with concentration of 50% and 3mL of perchloric acid, performing digestion treatment on an electric hot plate at 180 ℃, heating until perchloric acid smoke is emitted, and taking down the sample when the volume of the digestion solution is 0.5-1 mL;
(4) acidifying: dissolving the digestion solution with 5mL of water, adding 10mL of dilute hydrochloric acid for acidification, and fixing the volume to a 100mL volumetric flask to obtain a solution to be detected, wherein a reagent blank is made along with a sample;
(5) standard solution: taking 5 100mL volumetric flasks, respectively adding 10mL of dilute hydrochloric acid, then adding 30mL of iron element standard solution as a matrix solution, and finally respectively adding 0mL, 0.10mL, 0.50mL, 1.00mL and 3.00mL of sulfur element standard solution. Diluting with water to scale, shaking, and making into series of standard solutions with mass concentration shown in Table 1.
TABLE 1 Mass concentration of sulfur in standard solution series
| Serial number | S(mg/L) |
| Blank 0 | 0.00 |
| 1 | 1.00 |
| 2 | 5.00 |
| 3 | 10.00 |
| 4 | 30.00 |
(6) Drawing a standard curve: and (3) measuring the relative strength of the series of standard solutions in the step (5) by using an inductively coupled plasma emission spectrometer, drawing a standard working curve, and leading the linear correlation coefficient of the sulfur element analysis spectral line to be more than 0.999.
(7) And (4) calculating a result: the sulfur element content calculation formula of the oily sludge sample is as follows:
in the formula:
omega (S) -sulfur content in the oily sludge sample,%;
c, obtaining the concentration of sulfur element in the solution to be detected from the working curve, mg/L;
v, determining the volume of the solution to be detected to be the volume mL;
m-weighing the mass of the oily sludge sample, g;
example 2
A method for measuring the sulfur content in steel rolling oily sludge comprises the following specific steps:
(1) drying and grinding: taking a steel rolling oily sludge sample No. 2 back on site, placing the sample in a drying box, drying the sample for 3 hours at 105 ℃, and screening the dried and ground sample through a 120-mesh metal screen;
(2) low-temperature firing: putting the sample obtained in the step (1) into a muffle furnace, and burning for 1.5h at 500 ℃;
(3) digestion: weighing 0.2000g of the sample obtained in the step (2), adding 30mL of dilute nitric acid with concentration of 50% and 5mL of perchloric acid, performing digestion treatment on an electric hot plate at 200 ℃, heating until perchloric acid smoke is emitted, and taking down the sample when the volume of the digestion solution is 0.5-1 mL;
(4) acidifying: dissolving the digestion solution with 3mL of water, adding 10mL of dilute hydrochloric acid for acidification, and fixing the volume to a 100mL volumetric flask to obtain a solution to be detected, wherein a reagent blank is made along with a sample;
(5) standard solution: taking 6 100mL volumetric flasks, respectively adding 10mL of dilute hydrochloric acid, then adding 40mL of iron element standard solution as a matrix solution, and finally respectively adding 0mL, 0.10mL, 0.50mL, 1.00mL, 2.00mL and 5.00mL of sulfur element standard solution. Diluting with water to scale, shaking, and making into series of standard solutions with mass concentration shown in Table 2.
TABLE 2 Mass concentration of sulfur in standard solution series
| Serial number | S(mg/L) |
| Blank 0 | 0.00 |
| 1 | 1.00 |
| 2 | 5.00 |
| 3 | 10.00 |
| 4 | 20.00 |
| 5 | 50.00 |
(6) Drawing a standard curve: and (3) measuring the relative strength of the series of standard solutions in the step (5) by using an inductively coupled plasma emission spectrometer, drawing a standard working curve, and leading the linear correlation coefficient of the sulfur element analysis spectral line to be more than 0.999.
The elemental sulfur results for the samples were calculated as in example 1.
Example 3
A method for measuring the sulfur content in steel rolling oily sludge comprises the following specific steps:
(1) drying and grinding: taking a steel rolling oily sludge sample No. 3 back on site, placing the sample in a drying box, drying the sample for 2.5 hours at 110 ℃, and screening the dried and ground sample through a 120-mesh metal screen;
(2) low-temperature firing: putting the sample obtained in the step (1) into a high-temperature furnace, and burning for 2 hours at 480 ℃;
(3) digestion: weighing 0.1500g of the sample obtained in the step (2), adding 30mL of dilute nitric acid with concentration of 50% and 4mL of perchloric acid, performing digestion treatment on an electric hot plate at 160 ℃, heating until perchloric acid smoke is emitted, and taking down the sample when the volume of the digestion solution is 0.5-1 mL;
(4) acidifying: dissolving the digestion solution with 5mL of water, adding 10mL of dilute hydrochloric acid for acidification, and fixing the volume to a 100mL volumetric flask to obtain a solution to be detected, wherein a reagent blank is made along with a sample;
(5) standard solution: 10mL of dilute hydrochloric acid and 35mL of iron element standard solution are respectively added into 8 100mL volumetric flasks as matrix solutions, and finally 0mL, 0.10mL, 0.20mL, 0.30mL, 0.50mL, 1.00mL, 2.00mL and 3.00mL of sulfur element standard solutions are respectively added. Diluting with water to scale, shaking, and making into series of standard solutions with mass concentration shown in Table 3.
TABLE 3 Mass concentration of sulfur in standard solution series
| Serial number | S(mg/L) |
| Blank 0 | 0.00 |
| 1 | 1.00 |
| 2 | 2.00 |
| 3 | 3.00 |
| 4 | 5.00 |
| 5 | 10.00 |
| 6 | 20.00 |
| 7 | 30.00 |
(6) Drawing a standard curve: and (3) measuring the relative strength of the series of standard solutions in the step (5) by using an inductively coupled plasma emission spectrometer, drawing a standard working curve, and leading the linear correlation coefficient of the sulfur element analysis spectral line to be more than 0.999.
The elemental sulfur results for the samples were calculated as in example 1.
The sulfur content of the steel rolling oily sludge samples of examples 1 to 3 was measured, 10 times of each sample was measured in parallel, precision tests were performed, and the average value and the Relative Standard Deviation (RSD) of the results were calculated, and the results are shown in table 4. The data in Table 4 show that the Relative Standard Deviation (RSD) of elemental sulfur is between 1.83% and 2.75%, and the results are satisfactory.
Table 4 precision measurement results (n ═ 10)
The accuracy of the method of the invention is verified by using a labeling recovery test, and 3 levels of labeling tests are respectively carried out, and the results are shown in Table 5.
TABLE 5 results of recovery measurements with addition of standard
The data in Table 5 show that the recovery rate of sulfur is between 96.00% and 103.0%, and the result is satisfactory.
As can be seen from tables 4 to 5, the method of the present invention has good recovery rate and accuracy, and is favorable for popularization and application. The method of the present invention. Compared with the prior art: the determination method removes the water and oil in the sample by drying and low-temperature burning treatment, effectively avoids the blockage phenomenon caused to the central tube of the ICP instrument device when detecting the oil substances, and the blockage can directly influence the accuracy of the detection result and shorten the service life of the instrument. After low-temperature firing, the sample is digested by nitric acid and perchloric acid, and a small amount of residual organic matters are removed, so that the sample is completely converted into an inorganic aqueous solution, the operation is simple and convenient, the consumption of chemical reagents is reduced, and the requirement for measuring the sulfur content in the steel rolling oily sludge can be met while the environmental protection requirement is met. The method fills the technical blank of the analysis method of the sulfur element content in the steel rolling oily sludge in China, and has important guiding significance for controlling the sulfur element content when the steel rolling oily sludge is recycled as a steel making raw material.
The above-mentioned examples only express the specific embodiments of the present invention, but should not be construed as limiting the scope of the present invention. Any modifications of the present invention which would occur to those skilled in the art and which are within the spirit of the invention are considered to be within the scope of the present invention.
Claims (10)
1. A method for measuring the sulfur content in steel rolling oily sludge is characterized by comprising the following steps:
step 1: drying and grinding: taking back the sample on site, drying in a drying box, grinding and sieving;
step 2: low-temperature firing: drying and grinding the sample, and then firing at a low temperature;
and step 3: digestion: weighing 0.1000-0.2000 g of sample, adding 20-30 mL of dilute nitric acid and 3-5 mL of perchloric acid, performing digestion treatment on an electric hot plate at 150-200 ℃, heating until perchloric acid smoke emerges, and taking down the solution when the volume of the solution is 0.5-1 mL;
and 4, step 4: acidifying: dissolving the digestion solution with 3-5 mL of pure water, adding 10mL of dilute hydrochloric acid for acidification, and fixing the volume to a 100mL volumetric flask to obtain a solution to be detected;
and 5: standard solution: taking n 100mL volumetric flasks, respectively adding 10mL of dilute hydrochloric acid, then adding an iron element standard solution with the content similar to that of the sample as a matrix solution, and finally accurately transferring sulfur element standard solutions with different volumes to prepare a sulfur element series standard solution with a mass concentration gradient;
step 6: detecting by an instrument: measuring a series of standard solutions by using an inductively coupled plasma emission spectrometer, establishing a standard curve, and measuring the solution to be measured according to phase synchronization steps to obtain the content of sulfur elements in the solution to be measured;
and 7: and (4) calculating a result: the sulfur element content calculation formula of the oily sludge sample is as follows:
in the formula:
omega (S) -sulfur content in the oily sludge sample,%;
c, obtaining the concentration of sulfur element in the solution to be detected from the working curve, mg/L;
v, determining the volume of the solution to be detected to be the volume mL;
m-weighing the mass of the steel rolling oily sludge sample, g.
2. The method for measuring the sulfur content in the steel rolling oily sludge according to claim 1, wherein the method comprises the following steps: in the step 1, the drying and grinding process comprises: the drying temperature is 105-110 ℃, and the drying time is 2-3 h; the granularity of the ground metal mesh screen is 120 meshes.
3. The method for measuring the sulfur content in the steel rolling oily sludge according to claim 1, wherein the method comprises the following steps: the low-temperature firing process in the step 2 comprises the following steps: the ignition temperature is 400-500 ℃, and the ignition time is 1.5-2 h.
4. The method for measuring the sulfur content in the steel rolling oily sludge according to claim 1, wherein the method comprises the following steps: in the step 3, the concentration of the dilute nitric acid is 1.42g/cm3The volume fraction is 50%; the concentration of the perchloric acid is 1.67g/cm3。
5. The method for measuring the sulfur content in the steel rolling oily sludge according to claim 1, wherein the method comprises the following steps: in the steps 4 and 5, the concentration of the dilute hydrochloric acid is 1.18g/cm3The volume fraction was 50%.
6. The method for measuring the sulfur content in the steel rolling oily sludge according to claim 1, wherein the method comprises the following steps: in the step 5, the concentration of the iron element standard solution is 2.0000g/L, and the concentration of the sulfur element standard solution is 1000 mg/L.
7. The method for measuring the sulfur content in the steel rolling oily sludge according to claim 1, wherein the method comprises the following steps: in the step 5, the number of the n 100mL volumetric flasks is 4-8, and the gradient range of the mass concentration of the sulfur element in the serial standard solutions covers the mass concentration of the sulfur element in the solution to be detected.
8. The method for measuring the sulfur content in the steel rolling oily sludge according to claim 1, wherein the method comprises the following steps: in step 6, the operating conditions of the inductively coupled plasma emission spectrometer are as follows: the radio frequency power is 1150W, the auxiliary air flow is 0.5L/min, the cooling air flow is 15L/min, the atomizer flow is 0.75L/min, the analysis pump speed is 50r/min, the sample washing time is 10s, and the integration time is 30 s.
9. The method for measuring the sulfur content in the steel rolling oily sludge according to claim 1, wherein the method comprises the following steps: in the step 6, the wavelength of the sulfur element is selected to be 182.034nm when the inductively coupled plasma emission spectrometer measures the solution.
10. The method for measuring the sulfur content in the steel rolling oily sludge according to claim 1, wherein the method comprises the following steps: the pure water is ultrapure water, and the volumetric flask is the plastics volumetric flask.
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