CN107917885B - Method for detecting nickel, manganese and cadmium in sulfuric acid - Google Patents
Method for detecting nickel, manganese and cadmium in sulfuric acid Download PDFInfo
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- CN107917885B CN107917885B CN201711142014.7A CN201711142014A CN107917885B CN 107917885 B CN107917885 B CN 107917885B CN 201711142014 A CN201711142014 A CN 201711142014A CN 107917885 B CN107917885 B CN 107917885B
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- 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
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- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
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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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Abstract
The invention discloses a method for detecting nickel, manganese and cadmium in sulfuric acid, which comprises the following steps: 1) preparation of standard solutions: weighing nickel, cadmium or manganese, and preparing standard solution by hydrochloric acid; 2) preparing a sample to be tested: sucking 10.00-30.00 ml of a sulfuric acid sample to be detected, injecting the sulfuric acid sample into a beaker, adding 0.05-0.15 g of anhydrous sodium carbonate, heating the sulfuric acid sample to be nearly dry, cooling the sulfuric acid sample, adding a small amount of hot water, dropwise adding 1-2 ml of (1+1) hydrochloric acid, dissolving residues, transferring the residues into a 50ml volumetric flask, diluting the residues to a scale with water, and detecting the residues; 3) and (3) determining a sample to be tested: measuring the absorbance value of the standard solution prepared in the step 1) by using a flame atomic absorption spectrophotometry, establishing a working curve, measuring the absorbance value of nickel, cadmium or manganese elements to be measured in a sample to be measured, and obtaining the concentration of the elements to be measured according to the working curve. The invention fills the deficiency of the detection method of nickel, manganese and cadmium impurity elements in the domestic sulfuric acid standard.
Description
Technical Field
The invention belongs to the technical field of heavy metal detection, and particularly relates to a method for detecting nickel, manganese and cadmium in sulfuric acid.
Background
Sulfuric acid for a storage battery is a main raw material of a lead-acid storage battery. In the production process of the storage battery, a large number of stainless steel facilities are introduced due to the use of appliances, a production line and the like, metal impurities such as nickel, manganese, cadmium and the like are inevitably brought into a sulfuric acid preparation and use system to cause pollution due to direct acid containing or acid liquor contact in the facilities, and the impurities seriously affect the later performance and the environment-friendly discharge requirement of the storage battery. Various domestic sulfuric acid standards (industrial sulfuric acid, analytically pure sulfuric acid, electrolyte for lead-acid storage batteries and the like) only have corresponding requirements on the contents of iron, arsenic, lead and copper, do not have requirements on the contents of manganese, nickel and cadmium, and have no detection method for nickel, manganese and cadmium impurity elements in the domestic sulfuric acid standards.
Disclosure of Invention
The invention aims to solve the problems and provide a method.
The invention adopts the technical scheme for solving the technical problems that:
a method for detecting nickel, manganese and cadmium in sulfuric acid is characterized by comprising the following steps:
1) preparation of standard solutions: weighing nickel, cadmium or manganese, and preparing standard solution by hydrochloric acid;
2) preparing a sample to be tested: sucking 10.00-30.00 ml of a sulfuric acid sample to be detected, injecting the sulfuric acid sample into a beaker, adding 0.05-0.15 g of anhydrous sodium carbonate, heating the sulfuric acid sample to be nearly dry, cooling the sulfuric acid sample, adding a small amount of hot water, dropwise adding 1-2 ml of (1+1) hydrochloric acid, dissolving residues, transferring the residues into a 50ml volumetric flask, diluting the residues to a scale with water, and detecting the residues;
3) and (3) determining a sample to be tested: measuring the absorbance value of the standard solution prepared in the step 1) by using a flame atomic absorption spectrophotometry, establishing a working curve, measuring the absorbance value of nickel, cadmium or manganese elements to be measured in a sample to be measured, and obtaining the concentration of the elements to be measured according to the working curve.
The method for preparing the standard solution in the step 1) comprises the following steps: weighing 0.5000g of metallic nickel, cadmium or manganese, placing the metallic nickel, cadmium or manganese in a beaker, adding 20ml of (1+1) hydrochloric acid, heating the mixture until the metallic nickel, cadmium or manganese is completely dissolved, steaming the mixture to a small volume, cooling the mixture, adding 20ml of (1+1) hydrochloric acid, boiling the mixture to dissolve salts, transferring the mixture into a volumetric flask with water, and fixing the volume.
The method for establishing the working curve in the step 3) comprises the steps of taking three parts of standard solution, respectively placing the three parts of standard solution into a 50ml volumetric flask, adding 2ml (1+1) of hydrochloric acid, diluting the three parts of standard solution to a scale with water, shaking up the three parts of standard solution, adjusting the three parts of hydrochloric acid to zero with water, respectively measuring the absorbance values of the standard solution, and automatically establishing the working curve by an instrument.
The invention has the beneficial effects that: a flame atomic absorption spectrophotometry is utilized to monitor various acid and water impurities in incoming sulfuric acid and production process control, a nickel, manganese and cadmium analysis method is established, and the defect of a nickel, manganese and cadmium impurity element detection method in the domestic sulfuric acid standard is filled. According to the detection method, the sodium carbonate can be used for forming carbonate with nickel, manganese and cadmium in sulfuric acid to prevent the carbonate from volatilizing in the heating process, so that the accuracy of a detection result is ensured. And the reliability and the accuracy of the method are fully checked through data comparison of a multiple ratio test and a recovery rate test.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to be limiting.
Example 1
1 Main instruments and reagents
1.1 atomic absorption spectrophotometer model WFX-320, instrument operating conditions (see Table 1):
TABLE 1 working conditions of the apparatus
1.2 hollow cathode lamp of nickel (Ni), manganese (Mn) and cadmium (Cd).
1.3 hydrochloric acid: (1+1) solution (i.e. concentrated hydrochloric acid mixed with water at a volume of 1: 1)
1.4 anhydrous sodium carbonate: and (5) analyzing and purifying.
1.5 Standard storage solutions of Nickel (Ni), manganese (Mn), cadmium (Cd) (1 mg/ml): accurately weighing 0.5000g of metal nickel, cadmium and manganese (99.99 percent), respectively placing the metal nickel, the cadmium and the manganese into a 150 ml beaker, adding 20ml of (1+1) hydrochloric acid, heating the metal nickel, the cadmium and the manganese to be completely dissolved, steaming the metal nickel and the manganese to be small in volume, cooling the metal nickel, the cadmium and the manganese, then adding 20ml of (1+1) hydrochloric acid, boiling the metal nickel, the cadmium and the manganese to be dissolved in salt, respectively transferring the metal nickel, the cadmium and the manganese into a 500. The standard storage solution contains 1mg of nickel, manganese and cadmium per ml.
1.6 intermediate standard solutions of nickel (Ni), manganese (Mn), cadmium (Cd) (50 μ g/ml): 5ml of the standard stock solution prepared above (1mg/ml) was transferred into 100ml volumetric flasks, diluted to the mark with 2% HCl and shaken well.
2 detection of sulfuric acid samples
The method comprises the following steps:
1) preparation of samples to be tested
Accurately sucking 10.00-30.00 ml of a sample by using a pipette, injecting the sample into a beaker, adding 0.05-0.15 g of anhydrous sodium carbonate, heating the sample to be nearly dry, cooling the sample, adding a small amount of hot water, dropwise adding 1-2 ml of (1+1) hydrochloric acid, dissolving residues, transferring the residue into a 50ml volumetric flask, washing the beaker by using water for 3-5 times, diluting the sample to a scale, shaking the sample uniformly, and measuring the sample to be measured. A blank test was made with the sample.
2) Sample assay
Predicting the absorbance value of the sample prepared in the step 1) under the optimal working condition of the instrument, then placing three parts of the prepared intermediate standard solution (enabling the absorbance value of the test solution to be in the absorbance value of the working curve) in a 50ml volumetric flask respectively in the linear range of the working curve (see table 1), adding 2ml (1+1) of hydrochloric acid, diluting with water to scale, and shaking up. And (5) adjusting zero by water, respectively measuring the absorbance values of the standard solutions, and automatically establishing a working curve.
Then, the ABS/CONC bond is pressed to convert the absorbance and the concentration, the blank solution is adjusted to zero, and the concentration value (microgram/milliliter) of the element to be detected in the test solution is measured. If the absorbance value A of the solution to be measured exceeds the absorbance value corresponding to the upper limit concentration of the working curve, the test solution should be diluted, or the sampling amount is reduced, so that the absorbance value is in the range of the working curve.
3) Calculation of analysis results
The contents of nickel, manganese and cadmium are calculated according to the following formula:
in the formula:
c, measuring the concentration of the element to be measured in the test solution, namely microgram/milliliter;
v-volume of test solution, ml;
m-sample mass, g;
a-content of element to be measured,%.
Example 2 detection of Nickel, manganese, cadmium in sulfuric acid samples and accuracy verification of the detection method
First, detection of nickel, manganese and cadmium in sulfuric acid sample and method reliability verification-multiple ratio test
For a batch of 171014 sulfuric acid (acid density 1.8114 g/cm)3) The same sample was aspirated for different volumes, and the sample was prepared and tested according to the method in example 1.
The method comprises the following specific steps of: three volumes of sample, 10.00ml, 20.00ml, 30.00ml, were accurately pipetted, 3 replicates for each volume were set up and separately injected into the beaker. Respectively adding 0.05g, 0.10g and 0.15g of anhydrous sodium carbonate into 3 repeated samples with the volume of 10.00ml and 30.00ml, heating to be nearly dry, cooling, adding a small amount of hot water, respectively dropwise adding 1, 1.5 and 2ml of (1+1) hydrochloric acid, dissolving residues, transferring to a 50ml volumetric flask, washing a beaker with water for 3-5 times, diluting to a scale, shaking up, and measuring. Respectively adding 0.10g of anhydrous sodium carbonate into 3 repeated samples with the volume of 20.00ml, heating to be nearly dry, cooling, adding a small amount of hot water, dropwise adding 2ml of (1+1) hydrochloric acid, dissolving residues, transferring to a 50ml volumetric flask, washing a beaker with water for 3-5 times, diluting to a scale, shaking up, and testing.
The results of the test on three volumes of replicate samples are shown in table 2:
TABLE 2 concentrations of Ni, Mn and Cd in samples to be tested prepared with different sulfuric acid volumes
The results of the sample multiple ratio experiment are shown in table 3, and it can be seen that the results do not change with the sampling amount, the error of the results is small, and the method is proved to be reliable.
Table 3: sample multiple ratio test results
Second, accuracy verification of detection method-recovery test
In order to examine the accuracy of the method, only the standard recovery rate of the metal elements is tested, and the results are shown in table 4.
And respectively carrying out recovery rate tests on samples of different batches, wherein the recovery rates are more than 98%, which shows that the pretreatment method adopted by the samples is successful, and the treated matrix has no obvious influence on the determination of nickel (Ni), manganese (Mn) and cadmium (Cd), thereby proving that the selected determination method is feasible.
Table 4: results of recovery test
The analytical method for measuring nickel, manganese and cadmium in sulfuric acid by acetylene-flame atomic absorption, which is established by the invention, fully tests the reliability and accuracy of the method by comparing the data of a multiple ratio test and a recovery rate test, and proves that the analytical method is feasible.
Claims (2)
1. A method for detecting nickel, manganese and cadmium in sulfuric acid is characterized by comprising the following steps:
1) preparation of standard solutions: weighing 0.5000g of metal nickel, cadmium or manganese, placing the metal nickel, cadmium or manganese in a beaker, adding 20ml of (1+1) hydrochloric acid, heating the solution until the solution is completely dissolved, steaming the solution to a small volume, cooling the solution, adding 20ml of (1+1) hydrochloric acid, boiling the solution to dissolve salts, transferring the solution into a volumetric flask and fixing the volume by using water;
2) preparing a sample to be tested: sucking 10.00-30.00 ml of a sulfuric acid sample to be detected, injecting the sulfuric acid sample into a beaker, adding 0.05-0.15 g of anhydrous sodium carbonate, heating the sulfuric acid sample to be nearly dry, cooling the sulfuric acid sample, adding a small amount of hot water, dropwise adding 1-2 ml of (1+1) hydrochloric acid, dissolving residues, transferring the residues into a 50ml volumetric flask, diluting the residues to a scale with water, and detecting the residues; the density of the sulfuric acid sample to be detected is 1.8114g/cm3；
3) And (3) determining a sample to be tested: measuring the absorbance value of the standard solution prepared in the step 1) by using a flame atomic absorption spectrophotometry, establishing a working curve, measuring the absorbance value of nickel, cadmium or manganese elements to be measured in a sample to be measured, and obtaining the concentration of the elements to be measured according to the working curve.
2. The method for detecting nickel, manganese and cadmium in sulfuric acid as claimed in claim 1, wherein the method for establishing the working curve in step 3) comprises the steps of taking three standard solutions, respectively placing the three standard solutions in a 50ml volumetric flask, adding 2ml (1+1) hydrochloric acid, diluting with water to scale, shaking up, adjusting to zero with water, respectively measuring absorbance values of the standard solutions, and automatically establishing the working curve by an instrument.
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| CN103760218A (en) * | 2014-01-13 | 2014-04-30 | 福建兴朝阳硅材料股份有限公司 | Method for rapidly measuring trace boron impurities in polysilicon |
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| JP2008309767A (en) * | 2007-05-11 | 2008-12-25 | Horiba Ltd | Method for decomposing solid sample and method for determining quantity of chrome using the same |
| CN101609040A (en) * | 2009-07-16 | 2009-12-23 | 江苏双登集团有限公司 | Method for continuously measuring iron, copper and manganese in sulfuric acid by flame atomic absorption method |
| CN104165856A (en) * | 2014-09-02 | 2014-11-26 | 吉林化工学院 | Method for testing content of nickel in industrial sulfuric acid by flame atomic absorption spectroscopy method |
| CN104697983B (en) * | 2015-03-18 | 2017-08-01 | 河北金木药业集团有限公司 | The detection method of heavy metal lead, cadmium, arsenic, copper in a kind of prepared slices of Chinese crude drugs |
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| CN103760218A (en) * | 2014-01-13 | 2014-04-30 | 福建兴朝阳硅材料股份有限公司 | Method for rapidly measuring trace boron impurities in polysilicon |
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