CN106770247B - Method for detecting iron content in industrial sodium hydroxide - Google Patents
Method for detecting iron content in industrial sodium hydroxide Download PDFInfo
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Abstract
The invention discloses a method for detecting iron content in industrial sodium hydroxide. Specifically, the invention adopts a method that a bisphenol A methanol solution is mixed with an iron-containing sodium hydroxide sample, a standard curve of APHA chroma and ferric oxide content is established according to the color development condition, and the ferric oxide content of the sample is obtained by directly testing the chroma. The method has the advantages that the standard curve can be repeatedly manufactured without changing the bisphenol A, the steps are simple, the requirement on avoiding light for the reagent is avoided, and the error is small.
Description
Technical Field
The invention relates to a method for detecting iron content, in particular to a method for measuring the iron content in industrial sodium hydroxide by adopting a colorimetric method.
Background
The industrial sodium hydroxide is a commonly used raw material in the chemical industry, and is particularly used as an important raw material in the production process of bisphenol A type epoxy resin.
The method for detecting the iron content of the industrial sodium hydroxide generally adopts a 1, 10-phenanthroline spectrophotometric method for determining the iron content of the industrial sodium hydroxide in national standard GB/T, and the method is used for detecting Fe in a sample solution3+Reduction to Fe2+Fe at a pH of 4-62+The method has complicated steps when the color is developed with 1, 10-phenanthroline, and the Fe content in the sample is reduced3+Need to be reduced to Fe2+And the measurement after color development is carried out, the time is long, and the solution needs to be stored in dark, and the like.
Therefore, it is necessary to develop a method for testing the iron content in the industrial sodium hydroxide, which can rapidly detect the iron content, has simple steps and high accuracy.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for testing the iron content in industrial sodium hydroxide by adopting a colorimetric method.
The technical purpose of the invention is realized by the following technical scheme:
the method for detecting the iron content in the industrial sodium hydroxide comprises the following steps:
s1: preparing an iron standard solution;
s2: drawing an iron standard curve: preparing Fe with different concentration gradients by using the iron standard solution of the step S12O3Carrying out color reaction on the iron standard solutions with different concentration gradients, bisphenol A, methanol and industrial NaOH solution, and testing the APHA chromaticities corresponding to the iron standard solutions with different concentration gradients; simultaneously carrying out a blank control test to determine the APHA colorimetric value in the blank control; respectively deducting blank APHA chroma from the measured APHA chroma of the iron standard solution, and then drawing Fe2O3Calculating a linear regression equation of the standard curve of the content and the APHA chroma;
s3: iron in commercial NaOH solution: measuring the color APHA value of the sample to be measured, and calculating the weight m by contrasting with the standard curveSample (A)Fe of the sample solution to be measured2O3The content W of (A) is calculated as follows2O3The content is as follows:
Preferably, the preparation method of the iron standard solution comprises the following steps: taking ammonium ferric sulfate dodecahydrate to react with sulfuric acid to generate an iron standard solution, wherein the content of iron in the iron standard solution is equivalent to 0.1mg/mL Fe2O3Standard solutions of amounts.
Specifically, the preparation method of the iron standard solution comprises the following steps: 0.6039g of ammonium ferric sulphate dodecahydrate are taken and the amount is exactly 0.001g, which is then dissolved with 100mL of distilled water, 10mL of 98% strength sulphuric acid are added and the volume is determined with distilled water in a 1000mL volumetric flask. Specifically, the step of drawing the iron standard curve in step S2 is as follows:
1) taking the iron standard solution with different concentration gradients in the step S1 for standby;
2) adding bisphenol A, methanol and industrial NaOH in a weight ratio of 10-12: 18-20: 1 into 1.0-1.5 mL of the iron standard solution in the step 1) with different concentration gradients, and testing APHA chroma; simultaneously performing a blank test, testing the APHA chroma in the blank test, respectively deducting the APHA chroma of the blank test from the APHA chroma of the measured iron standard solution, and then drawing Fe2O3Standard curve of content versus APHA color. The standard curve is drawn after blank is deducted, and since sodium hydroxide is also added into the blank to adjust the pH value, the sodium hydroxide also contains iron, the iron is developed, and the color intensity generated by the blank is deducted from the standard curve.
Preferably, in the step S3, Fe in the sample to be tested2O3The content detection comprises the following specific steps: dissolving bisphenol A and methanol in a weight ratio of 1: 1.8-2, and adding m weight of bisphenol A and methanolSample (A)Preparing the sample to be tested into a solution to be tested, testing the chromaticity APHA value of the solution to be tested, and calculating Fe of the solution to be tested by contrasting with a standard curve2O3And then calculating the iron content in the industrial sodium hydroxide.
Preferably, the industrial NaOH is replaced with the sample to be tested in step S2.
The invention has the beneficial effects that:
compared with the prior detection technology, the invention has the following beneficial effects:
after the corresponding standard substance is prepared, the method is generally used for detecting the sample only for about 10min, and the method has good reproducibility and no light-shielding requirement on the reagent. And the same 1, 10-phenanthroline spectrophotometric method needs 30-60 min, and has the requirement of keeping out of the sun for the reagent. By using the method to detect the sample, a large amount of time can be saved, the analysis efficiency is improved, the detection result is accurate, and the rapid and accurate feeding detection is guaranteed.
Drawings
FIG. 1 is a diagram of a standard curve and a regression equation according to the present invention.
Detailed Description
The required instruments of the invention:
a colorimeter;
electronic analytical balance (accurate to 0.0001g) for accurate weighing of ferric ammonium sulfate dodecahydrate (NH)4Fe(SO4)2·12H2O) weight;
volumetric flask: 1000ml of 100 ml;
a cuvette: the optical path length is 5 cm.
In order to make the objects, technical solutions and advantages of the present invention more apparent, preferred embodiments of the present invention are described in detail below.
The invention relates to a method for testing the iron content in industrial sodium hydroxide by adopting a colorimetric method, which comprises the following steps:
implementation steps of detection method
(1) Preparation of iron Standard solution
0.6039g of ammonium ferric sulfate dodecahydrate (NH) are taken4Fe(SO4)2·12H2O ] to the accuracy of 0.001g, 100mL of distilled water was dissolved in a 200mL beaker, 10mL (98% by mass) of sulfuric acid was added, and the volume was determined in a 1000mL volumetric flask using distilled water. The solution was equivalent to 0.1mg/mL Fe2O3Standard solutions of amounts.
(2) Drawing of iron standard curve
1) Sequentially taking 2mL, 4mL, 6mL, 8mL, 12mL, 16mL and 20mL of the iron standard solution in the step (1), adding distilled water into a 100mL volumetric flask to fix the volume to 100mL, and uniformly mixing;
2) 20.0g of bisphenol A (analytical grade) was weighed, 40.0g of methanol (analytical grade) was added, 2.0g of industrial NaOH was added, 1.0mL of the above constant volume solution was added, and the concentration of the obtained solution was equivalent to Fe2O3In an amount of0.002mg, 0.004mg, 0.006mg, 0.008mg, 0.012mg, 0.016mg and 0.020 mg.
The reaction principle of the color reaction is as follows:
blank control was also performed: 20.0g bisphenol A (analytical grade) were weighed, 40.0g methanol (analytical grade) were added, 2.0g technical NaOH was added, and Fe was not added2O3Standard solution, measuring APHA color.
3) Then testing the APHA chroma of the solution obtained in the step 2) in a colorimeter, deducting the APHA chroma value of a blank control, and then drawing Fe2O3The standard curve of the content versus APHA color and the linear regression equation thereof were calculated as shown in fig. 1. And each Fe in the standard curve2O3The results of the contents versus APHA color are given in table 1:
TABLE 1 respective Fe in the standard curve2O3Results of the content corresponding to APHA color
| Fe2O3Content (mg) | 0.002 | 0.004 | 0.006 | 0.008 | 0.012 | 0.016 | 0.020 |
| Chroma (APHA) | 10.1 | 20.7 | 29.3 | 38.2 | 55.6 | 74.0 | 88.8 |
(3) Sample detection
20g of bisphenol A (analytical grade) are weighed out, 40g of methanol (analytical grade) are added, and after dissolution, 2.0g of the sample to be tested (recorded weight m) are addedSample (A)2.011), preparing a solution to be tested, testing the chromaticity APHA value (27.8APHA) in a spectrophotometer, and calculating Fe in the solution to be tested in a standard curve2O3The content of W (W ═ 0.0057 mg).
And (4) calculating a result:
second, method precision verification
The precision and sample spiking recovery of the method of the invention were verified as follows:
1. standard curve precision test
Separately determining Fe2O3The colorimetric values of the standard solutions with the contents of 0.008 and 0.016mg are respectively 6 times. The results of the precision tests are shown in Table 2 by comparison with the standard curve
TABLE 2 results of precision test
2. Recovery rate of sample by adding standard
20g bisphenol A (analytical grade) was weighed out and 40g methanol (analytical grade) was added, dissolved and addedSample A2.0 g (record weight m)Sample (A)2.011), preparing two parts of solution to be detected, and adding Fe into one part of the solution2O3At a level of 0.012mg (spiked sample A), the APHA values were measured in a colorimeter and the spiked recoveries were calculated as shown in Table 3.
TABLE 3 recovery of sample spiked
3.1, 10-phenanthroline spectrophotometric control test
Taking a sample to be tested B, C, D, E, testing by adopting the method of the invention, and simultaneously carrying out a contrast test with a 1, 10-phenanthroline spectrophotometry, wherein the results are as follows:
TABLE 4 comparison of the detection method of the present invention with the detection results of 1, 10-phenanthroline spectrophotometry
| Test results (%) | Sample B | Sample C | Sample D | Sample E |
| The method of the invention | 0.00012 | 0.00025 | 0.00032 | 0.00073 |
| 1, 10-phenanthroline spectrophotometric method | 0.00012 | 0.00028 | 0.00031 | 0.00074 |
Through the comparison, the test result of the detection method disclosed by the invention is close to that of 1, 10-phenanthroline spectrophotometry; in terms of detection time, the detection method does not need to repeatedly make a standard curve when the bisphenol A is not changed, the detection result is finished within about 20min, and the 1, 10-phenanthroline spectrophotometry needs 2.5 h.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. Not all embodiments are exhaustive. All obvious changes and modifications which are obvious to the technical scheme of the invention are covered by the protection scope of the invention.
Claims (4)
1. A method for detecting the iron content in industrial sodium hydroxide is characterized by comprising the following steps:
s1: preparing an iron standard solution;
s2: drawing an iron standard curve: preparing Fe with different concentration gradients by using the iron standard solution of the step S12O3Carrying out color reaction on the iron standard solutions with different concentration gradients, bisphenol A, methanol and industrial NaOH solution, and testing the APHA chromaticities corresponding to the iron standard solutions with different concentration gradients; simultaneously carrying out a blank control test to determine the APHA colorimetric value in the blank control; respectively deducting the APHA chroma of the measured iron standard solutionDrawing Fe after blank APHA chroma2O3Calculating a linear regression equation of the standard curve of the content and the APHA chroma;
s3: detecting the iron content in the industrial NaOH solution: measuring the color APHA value of the sample to be measured, and calculating the weight m by contrasting with the standard curveSample (A)Fe of the sample solution to be measured2O3The content W of (A) is calculated as follows2O3The content is as follows:
finally calculating the content of iron in the industrial sodium hydroxide; the step of drawing the iron standard curve of the step S2 is as follows:
1) taking the iron standard solution with different concentration gradients in the step S1 for standby;
2) adding bisphenol A, methanol and industrial NaOH in a weight ratio of 10-12: 18-20: 1 into 1.0-1.5 mL of the iron standard solution in the step 1) with different concentration gradients, and testing APHA chroma; simultaneously performing a blank test, testing the APHA chroma in the blank test, respectively deducting the APHA chroma of the blank test from the APHA chroma of the measured iron standard solution, and then drawing Fe2O3A standard curve of the content and APHA chroma; the preparation method of the iron standard solution comprises the following steps: taking ammonium ferric sulfate dodecahydrate to react with sulfuric acid to generate an iron standard solution, wherein the content of iron in the iron standard solution is equivalent to 0.1mg/mL Fe2O3Standard solutions of amounts.
2. The method for detecting the content of iron in the industrial sodium hydroxide according to claim 1, wherein the preparation steps of the iron standard solution are as follows: 0.6039g of ammonium ferric sulphate dodecahydrate are taken and the amount is exactly 0.001g, which is then dissolved with 100mL of distilled water, 10mL of 98% strength sulphuric acid are added and the volume is determined with distilled water in a 1000mL volumetric flask.
3. The method for detecting the iron content in industrial sodium hydroxide according to claim 1,fe in the sample to be detected in the step S32O3The content detection comprises the following specific steps: dissolving bisphenol A and methanol in a weight ratio of 1: 1.8-2, and adding m weight of bisphenol A and methanolSample (A)Preparing the sample to be tested into a solution to be tested, testing the chromaticity APHA value of the solution to be tested, and calculating Fe of the solution to be tested by contrasting with a standard curve2O3And then calculating the iron content in the industrial sodium hydroxide.
4. The method for detecting the iron content in the industrial sodium hydroxide as claimed in claim 1, wherein the industrial NaOH is replaced with a sample to be detected in the step S2.
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| 基于手持技术的化学研究性学习;王萌萌;《中国优秀硕士学位论文全文数据库社会科学II辑》;20150815;第20-22页 * |
| 建立悬浮法PVC树脂质量管理检测体系的构想;齐树东，张春明等;《中国氯碱》;20111031;第39-42页 * |
| 铁元素分析方法的进展;张琨;《化学分析计量》;20111231;第95-98页 * |
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