阅读说明：本技术 一种冷轧油泥废弃物中铁含量的检测方法 (Method for detecting iron content in cold rolling oil sludge waste ) 是由 刘尚超 张垒 王丽娜 苏磊 刘璞 于 2020-08-31 设计创作，主要内容包括：本发明涉及冷轧油泥废弃物中铁含量的检测方法,制备油泥试样；将油泥试样与乙腈溶液混合,并进行震荡,过滤,得到滤渣A；将滤渣A与丙酮试剂混合,并进行震荡,过滤,得到滤渣B；将滤渣B与浓盐酸混合,并搅拌静置,过滤,得到滤液；用去离子水对滤液进行定容,制得待测溶液；用原子吸收光谱仪在特定波长下测定待测溶液中铁元素的吸光度；计算待测冷轧油泥铁元素的含量。选取具有代表性的冷轧油泥试样,先后加入一定量的乙腈和丙酮溶剂,过滤后再入盐酸酸溶定容制备成待测溶液,用原子吸收光谱仪测定待测溶液中铁吸光度,并计算出冷轧油泥中的铁含量,解决了目前冷轧油泥中的铁含量无法检测技术难题。(The invention relates to a method for detecting the iron content in cold rolling oil sludge waste, which comprises the following steps of preparing an oil sludge sample; mixing an oil sludge sample with an acetonitrile solution, oscillating, and filtering to obtain filter residue A; mixing the filter residue A with an acetone reagent, oscillating and filtering to obtain filter residue B; mixing the filter residue B with concentrated hydrochloric acid, stirring, standing and filtering to obtain a filtrate; using deionized water to perform constant volume on the filtrate to prepare a solution to be detected; measuring the absorbance of the iron element in the solution to be measured by using an atomic absorption spectrometer under a specific wavelength; and calculating the content of the iron element of the cold rolling oil sludge to be detected. Selecting a representative cold-rolled oil sludge sample, sequentially adding a certain amount of acetonitrile and acetone solvents, filtering, adding hydrochloric acid for acid dissolution and volume fixing to prepare a solution to be detected, measuring the iron absorbance in the solution to be detected by using an atomic absorption spectrometer, and calculating the iron content in the cold-rolled oil sludge, thereby solving the technical problem that the iron content in the existing cold-rolled oil sludge cannot be detected.)

1. A method for detecting the iron content in cold rolling oil sludge waste is characterized by comprising the following specific steps:

s100, preparing an oil sludge sample;

s200, mixing the oil sludge sample with an acetonitrile solution, oscillating, and filtering to obtain filter residue A;

s300, mixing the filter residue A with an acetone reagent, oscillating, and filtering to obtain a filter residue B;

s400, mixing the filter residue B with concentrated hydrochloric acid, stirring, standing and filtering to obtain a filtrate;

s500, using deionized water to perform constant volume on the filtrate to prepare a solution to be detected;

s600, measuring the absorbance of the iron element in the solution to be measured by using an atomic absorption spectrometer under a specific wavelength;

s700, calculating the content of the cold-rolled fatlute iron element to be measured, wherein the calculation formula is as follows: w ═ Vx (a + b × As/(V)₁×C×10000)，

In the formula:

w is the iron content in the cold rolling oil sludge, and the unit is percent;

V₁dividing the volume of the sample solution, wherein the unit is ml;

v is the volume of deionized water and the unit is ml;

c is the mass of the oil sludge sample, and the unit is g;

a is the background equivalent concentration in μ g;

b is the conversion of the absorbance of the iron element to the mass, and the unit is mu g/cps;

AS is the absorbance of iron in the solution to be measured, and the unit is cps;

the background equivalent concentration a and the absorbance of the iron element to the mass conversion b are determined by a working curve equation of the relationship between the mass of the iron element and the absorbance of the iron element at a specific wavelength.

2. The method for detecting the iron content in the cold rolling oil sludge waste according to claim 1, wherein the step S200 is specifically as follows:

adding 1-3 g of oil sludge sample into a container containing 10-50 ml of acetonitrile solution, carrying out ultrasonic oscillation for 1-5 h, and filtering the solution by using qualitative slow-speed filter paper to obtain filter residue A.

3. The method for detecting the iron content in the cold rolling oil sludge waste as claimed in claim 2, wherein the addition amount of the acetonitrile solution is 30 ml.

4. The method for detecting the iron content in the cold rolling oil sludge waste according to claim 2, wherein the step S300 specifically comprises:

and adding the filter residue A into a container filled with 10-50 ml of acetone reagent, carrying out ultrasonic oscillation for 1-5 hours, and filtering the solution by using qualitative slow filter paper to obtain a filter residue B.

5. The method for detecting the iron content in the cold rolling oil sludge waste as claimed in claim 4, wherein the addition amount of the acetone reagent is 30 ml.

6. The method for detecting the iron content in the cold rolling oil sludge waste according to claim 4, wherein S400 specifically comprises:

and adding 10-30 ml of 37% concentrated hydrochloric acid into the container, adding the filter residue B into the container, stirring for 20-30 min, standing for 30min, and filtering the solution by using qualitative slow filter paper to obtain a filtrate.

7. The method for detecting the iron content in the cold rolling oil sludge waste according to claim 6, wherein the adding amount of the concentrated hydrochloric acid is 20 ml.

8. The method for detecting the iron content in the cold rolling oil sludge waste according to claim 6, wherein the S500 is specifically:

and transferring the filtrate into a container with the volume of 200ml, fixing the volume of the filtrate in the container with the volume of 200ml to a scale with deionized water, and shaking up to obtain the solution to be detected.

9. The method for detecting the iron content in the cold rolling oil sludge waste according to claim 8, wherein the step S600 specifically comprises:

and measuring the absorption intensity of iron in the solution to be measured by an atomic absorption spectrometer when the wavelength is 248.3 nm.

10. The method for detecting the content of iron in cold rolling oil sludge waste according to claim 9, wherein the background equivalent concentration a and the absorbance of the iron element to mass conversion b in S700 are determined by a working curve equation of a relationship between the mass of the iron element and the absorbance of the iron element at a specific wavelength, and specifically comprise:

accurately and respectively transferring 0, 1.00, 3.00, 5.00, 7.00, 10.00 and 10.00ml of iron standard solution with the mass concentration of 100 mu g/ml by using a suction pipe, placing the iron standard solution in a corresponding 100ml container, respectively fixing the volume of the iron standard solution in the container to a scale by using deionized water, and then shaking up;

respectively measuring the absorption intensity of iron at a wavelength of 248.3nm by using an atomic absorption spectrometer;

according to the mass of iron in the standard solution, calculating a unary linear regression equation of a working curve of the relationship between the mass of the iron and the absorbance of the iron by a computer, and determining the values of a and b in m ═ a + b × As, wherein in the regression equation:

m is the mass of iron, and the unit is mug;

a is the background equivalent concentration in μ g;

b is the conversion of the absorbance of the iron to the mass, and the unit is mu g/cps;

as is the absorbance of iron in cps.

Technical Field

The invention relates to the technical field of environmental protection analysis, in particular to a method for detecting iron content in cold rolling oil sludge waste.

Background

The cold-rolled oil sludge is a product filtered by a magnetic filter in the process of purifying and recycling emulsion in a cold rolling factory, and is a mixture of iron powder, rolling oil, a small amount of water and other impurities, hundreds of cold rolling factories exist in China, a medium-sized cold rolling factory can generate about 400kg of cold-rolled oil sludge every day, and in the early stage, the cold-rolled oil sludge is treated as industrial solid waste in the metallurgical industry, or is buried or combusted, and basically no relevant report of reutilization exists.

With the vigorous development of solid waste resource utilization in China in recent years, cold-rolled oil sludge is gradually resource-utilized, and the iron and oil in the cold-rolled oil sludge are recovered. The precondition of recovery is that the physicochemical properties of the cold rolling oil sludge are clearly known, for example, the iron content of the cold rolling oil sludge not only influences the selection of a resource utilization process of the cold rolling oil sludge, but also directly influences the utilization value of the cold rolling oil sludge, so that the accurate detection of the iron content of the cold rolling oil sludge is of great importance.

At present, the related technology for detecting the iron content of the cold-rolled oil sludge is not found, only the detection for the iron content in the solid waste is found, and the main results are as follows:

the Chinese patent application with application publication number CN201711355651.2 discloses a method for detecting the total iron content of steel slag, which mainly aims at detecting the iron content in solid waste of the steel slag, and the method is completely different from the detection pretreatment of the iron content in cold-rolled oil sludge in the pretreatment process of a sample and is not suitable for detecting the iron content in the cold-rolled oil sludge. Specifically, there are the following problems:

(1) the method is not suitable for detecting the iron content in the cold rolling oil sludge;

(2) the method adopts a magnetic absorption gravimetric method to measure the iron content, and has lower accuracy.

The chinese patent application with application publication No. CN201210506623.7 discloses a method for detecting iron content in photovoltaic glass based on X-ray fluorescence energy spectrum, which uses X-ray fluorescence energy spectrum to detect iron content in photovoltaic glass, and the detection method has the following two problems:

(1) the X-ray fluorescence detector has higher requirement on the cleanliness of a sample, and a detection object in the invention contains a large amount of oil substances and is easy to pollute the instrument;

(2) the standard deviation of the detection of the method is 4.5% -9.0%, and the reliability of the method is poor.

Cold-rolled oil sludge is produced in a large amount in metallurgical enterprises as metallurgical solid waste, more and more metallurgical enterprises utilize the cold-rolled oil sludge as resources, and an effective detection method for the iron content in the cold-rolled oil sludge is lacked in the industry, and a literature report about the detection method for the iron content in the cold-rolled oil sludge is not seen.

Disclosure of Invention

The invention aims to provide a method for detecting the iron content in cold rolling oil sludge waste so as to overcome the defects in the prior art.

The technical scheme for solving the technical problems is as follows: a method for detecting the iron content in cold rolling oil sludge waste comprises the following specific steps:

s100, preparing an oil sludge sample;

s200, mixing the oil sludge sample with an acetonitrile solution, oscillating, and filtering to obtain filter residue A;

s300, mixing the filter residue A with an acetone reagent, oscillating, and filtering to obtain a filter residue B;

s400, mixing the filter residue B with concentrated hydrochloric acid, stirring, standing and filtering to obtain a filtrate;

s500, using deionized water to perform constant volume on the filtrate to prepare a solution to be detected;

s600, measuring the absorbance of the iron element in the solution to be measured by using an atomic absorption spectrometer under a specific wavelength;

s700, calculating the content of the cold-rolled fatlute iron element to be measured, wherein the calculation formula is as follows: w ═ Vx (a + b × As/(V)₁×C×10000)，

In the formula:

w is the iron content in the cold rolling oil sludge, and the unit is percent;

V₁dividing the volume of the sample solution, wherein the unit is ml;

v is the volume of deionized water and the unit is ml;

c is the mass of the oil sludge sample, and the unit is g;

a is the background equivalent concentration in μ g;

b is the conversion of the absorbance of the iron element to the mass, and the unit is mu g/cps;

AS is the absorbance of iron in the solution to be measured, and the unit is cps;

the background equivalent concentration a and the absorbance of the iron element to the mass conversion b are determined by a working curve equation of the relationship between the mass of the iron element and the absorbance of the iron element at a specific wavelength.

Further, S200 specifically is:

adding 1-3 g of oil sludge sample into a container containing 10-50 ml of acetonitrile solution, carrying out ultrasonic oscillation for 1-5 h, and filtering the solution by using qualitative slow-speed filter paper to obtain filter residue A.

Further, the amount of the acetonitrile solution added was 30 ml.

Further, S300 specifically is:

and adding the filter residue A into a container filled with 10-50 ml of acetone reagent, carrying out ultrasonic oscillation for 1-5 hours, and filtering the solution by using qualitative slow filter paper to obtain a filter residue B.

Further, the amount of acetone reagent added was 30 ml.

Further, S400 specifically is:

and adding 10-30 ml of 37% concentrated hydrochloric acid into the container, adding the filter residue B into the container, stirring for 20-30 min, standing for 30min, and filtering the solution by using qualitative slow filter paper to obtain a filtrate.

Further, the amount of concentrated hydrochloric acid added was 20 ml.

Further, S500 specifically is:

and transferring the filtrate into a container with the volume of 200ml, fixing the volume of the filtrate in the container with the volume of 200ml to a scale with deionized water, and shaking up to obtain the solution to be detected.

Further, S600 specifically is:

and measuring the absorption intensity of iron in the solution to be measured by an atomic absorption spectrometer when the wavelength is 248.3 nm.

Further, in S700, the background equivalent concentration a and the absorbance of the iron element to mass conversion b are determined by a working curve equation of a relationship between the mass of the iron element and the absorbance of the iron element at a specific wavelength, specifically:

accurately and respectively transferring 0, 1.00, 3.00, 5.00, 7.00, 10.00 and 10.00ml of iron standard solution with the mass concentration of 100 mu g/ml by using a suction pipe, placing the iron standard solution in a corresponding 100ml container, respectively fixing the volume of the iron standard solution in the container to a scale by using deionized water, and then shaking up;

respectively measuring the absorption intensity of iron at a wavelength of 248.3nm by using an atomic absorption spectrometer;

according to the mass of iron in the standard solution, calculating a unary linear regression equation of a working curve of the relationship between the mass of the iron and the absorbance of the iron by a computer, and determining the values of a and b in m ═ a + b × As, wherein in the regression equation:

m is the mass of iron, and the unit is mug;

a is the background equivalent concentration in μ g;

b is the conversion of the absorbance of the iron to the mass, and the unit is mu g/cps;

as is the absorbance of iron in cps.

The invention has the following beneficial effects:

selecting a representative cold-rolled oil sludge sample, sequentially adding a certain amount of acetonitrile and acetone solvents, filtering, adding hydrochloric acid for acid dissolution and volume fixing to prepare a solution to be detected, measuring the iron absorbance in the solution to be detected by using an atomic absorption spectrometer, and calculating the iron content in the cold-rolled oil sludge, thereby solving the technical problem that the iron content in the existing cold-rolled oil sludge cannot be detected;

the method realizes accurate determination of the iron content in the cold-rolled oil sludge, and has the advantages of high precision of detection data, good accuracy, simple and convenient operation, low labor intensity and strong operability;

the method of the invention also applies modern analytical instrument technology, and has the characteristics of quick measurement, high efficiency, high flux, environmental protection and the like;

the method is wide in linear range, is suitable for accurately analyzing the iron content in the cold-rolled oil sludge within the content range of 0.05-20.00%, and meets the requirements of value identification and resource utilization of the cold-rolled oil sludge on discharge-protecting process parameter control.

Detailed Description

The principles and features of this invention are described below in conjunction with examples which are set forth to illustrate, but are not to be construed to limit the scope of the invention.

A method for detecting the iron content in cold rolling oil sludge waste comprises the following specific steps:

s100, dividing 800g of oil sludge into four parts by a quartering method, and taking about 200g of one part of the oil sludge as an oil sludge sample;

s200, weighing 1-3 g of oil sludge sample by using a ten-thousandth electronic balance, placing the oil sludge sample in a beaker with the volume of 200ml, adding 10-50 ml of acetonitrile solution into the beaker 1, covering a watch glass on the beaker, placing the beaker covered with the watch glass in an ultrasonic oscillator for oscillation for 1-5 hours, taking out the beaker from the ultrasonic oscillator, and filtering the solution in the beaker by using qualitative slow-speed filter paper to obtain filter residue A;

s300, transferring the filter residue A to a beaker, adding 10-50 ml of acetone reagent into the beaker, covering the beaker with a watch glass, placing the beaker covered with the watch glass in an ultrasonic oscillator to oscillate for 1-5 hours, taking out the beaker from the ultrasonic oscillator, and filtering the solution in the beaker by using qualitative slow-speed filter paper to obtain a filter residue B;

s400, transferring the filter residue B to a beaker, adding 10-30 ml of 37% concentrated hydrochloric acid into the beaker, stirring for 20-30 min, standing for 30min, and filtering the solution in the beaker by using qualitative slow-speed filter paper to obtain a filtrate;

s500, transferring the filtrate into a volumetric flask with the volume of 200ml, using deionized water to fix the volume of the filtrate in the volumetric flask with the volume of 200ml to a scale, and shaking up to obtain a solution to be detected;

s600, measuring the absorbance AS of the iron element in the solution to be measured by using an atomic absorption spectrometer under the wavelength of 248.3nm, wherein the atomic absorption spectrometer can adopt an iCAP7400 atomic absorption spectrometer produced by Shimadzu corporation of Japan;

s700, calculating the content of the cold-rolled fatlute iron element to be measured, wherein the calculation formula is as follows: w ═ Vx (a + b × As/(V)₁×C×10000)，

In the formula:

w is the iron content in the cold rolling oil sludge, and the unit is percent;

V₁dividing the volume of the sample solution, wherein the unit is ml;

v is the volume of deionized water and the unit is ml;

c is the mass of the oil sludge sample, and the unit is g;

a is the background equivalent concentration in μ g;

b is the conversion of the absorbance of the iron element to the mass, and the unit is mu g/cps;

AS is the absorbance of iron in the solution to be measured, and the unit is cps;

the background equivalent concentration a and the absorbance of the iron element to the mass conversion b are determined by a working curve equation of the relationship between the mass of the iron element and the absorbance of the iron element at a specific wavelength, and specifically are as follows:

accurately and respectively transferring 0, 1.00, 3.00, 5.00, 7.00, 10.00 and 10.00ml of iron standard solution with the mass concentration of 100 mu g/ml by using a suction pipe, placing the iron standard solution in a corresponding 100ml volumetric flask, respectively metering the iron standard solution in the volumetric flask to a scale by using deionized water, and then shaking up;

respectively measuring the absorption intensity of iron at a wavelength of 248.3nm by using an atomic absorption spectrometer;

according to the mass of iron in the standard solution, calculating a unary linear regression equation of a working curve of the relationship between the mass of the iron and the absorbance of the iron by a computer, and determining the values of a and b in m ═ a + b × As, wherein in the regression equation:

m is the mass of iron, and the unit is mug;

a is the background equivalent concentration in μ g;

b is the conversion of the absorbance of the iron to the mass, and the unit is mu g/cps;

as is the absorbance of iron in cps.

The precision and accuracy of the method are confirmed by the standard addition recovery experiment and the precision experiment of the sample:

performing a standard adding recovery experiment on a sample, adding a certain amount of iron standard solution into the prepared solution to be detected, detecting according to the method of the invention, and calculating the standard adding recovery rate, wherein the test result is shown in the following table 1:

TABLE 1 sample recovery test with addition of standard

Adding iron standard solution	Recovery of iron element	Recovery rate (100%)
			100	98	98.0
300	296	98.67
			500	524	104.8
1000	1029	102.9
			1500	1496	99.73
2000	1984	99.2

The precision experiment was performed to detect the iron content in 3 groups of prepared samples to be tested for 14 times, according to the method, the analysis results are shown in table 2 below:

TABLE 2 sample precision test

As can be seen from tables 1 and 2 above, according to the method for detecting the iron content in the cold-rolled oil sludge waste, the precision of the detection data of the sample is good, the RSD is less than 1.80%, the recovery rate of the iron content in the standard recovery experiment is 98.0-104.8%, the accuracy is high, the problem that the iron content in the cold-rolled oil sludge waste cannot be accurately detected is solved, and the requirements of identifying the iron resource value in the cold-rolled oil sludge and controlling the technological parameters of the resource utilization of the cold-rolled oil sludge are completely met.

Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.