CN112858199A - Method for detecting content of phosphorus in dimer acid - Google Patents
Method for detecting content of phosphorus in dimer acid Download PDFInfo
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- CN112858199A CN112858199A CN202110345206.8A CN202110345206A CN112858199A CN 112858199 A CN112858199 A CN 112858199A CN 202110345206 A CN202110345206 A CN 202110345206A CN 112858199 A CN112858199 A CN 112858199A
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Abstract
The invention provides a method for detecting the content of phosphorus in dimer acid, which comprises the following steps: drawing a standard curve for measuring phosphorus, pretreating a sample, developing the color of a test solution, measuring the absorbance of the sample and calculating the result. The invention provides another method for accurately and efficiently detecting the content of phosphorus in dimer acid, which has low cost and simple and convenient operation.
Description
Technical Field
The invention relates to the technical field of oil detection, in particular to a method for detecting the content of phosphorus in dimer acid.
Background
Dimer acid is an organic synthesis intermediate with wide application, and is applied to various industries such as machinery, automobiles, electronics, motors, aerospace, civil construction, printing, daily chemicals, textiles, ships, coatings and the like. The non-reactive solid dimer acid type polyamide resin is mainly used as a raw material for synthesizing dimer acid type polyamide resin, wherein the non-reactive solid dimer acid type polyamide resin is used as a printing ink production raw material for the most part, and is partially used as a hot melt adhesive in shoe making, electronic industry and automobile industry. The reactive liquid dimer acid type polyamide resin is used as an epoxy resin curing agent, and gives excellent performance to a cured product thereof. In particular to the application in the field of heavy-duty anticorrosive coatings for ships, automobiles and containers. The dimer acid is required to have light color and have strict requirements on inorganic trace elements. The trace iron and the trace phosphorus in the dimer acid applied to ship heavy corrosion prevention are respectively less than 1PPm and less than 10 PPm. .
The dimer acid production develops rapidly in recent years, the yield and the quality are improved year by year, and the application field is continuously expanded. The requirement for the quality of dimer acid is higher and higher, and the control of the phosphorus content in the dimer acid is particularly important. At present, the phosphorus content in the dimer acid can be generally detected by atomic absorption, and the detection method has relatively large equipment investment and high detection cost.
Disclosure of Invention
The invention aims to provide a method for detecting the content of phosphorus in dimer acid, so as to solve the problems.
In order to achieve the purpose, the invention provides the following technical scheme: a method for detecting the content of phosphorus in dimer acid comprises the following steps:
s1, drawing a standard curve for measuring phosphorus: preparing a plurality of bottles of phosphorus-containing standard solution, and drawing a standard curve by taking the absorbance as a vertical coordinate and the phosphorus amount as a horizontal coordinate;
s2, sample pretreatment: adding a catalyst into a sample to be detected for carbonization pretreatment;
s3, color development of the test solution: adding a color developing agent into the sample pretreated in the step S2 for color development;
s4, measuring the absorbance of the sample: measuring the absorbance of the sample obtained after the color development treatment in the step S3 by using a spectrophotometer;
s5, calculating the result: comparing the absorbance obtained in step S4 with the standard curve in step S1, calculating the phosphorus content in the sample according to formula 1),
in the formula:
p-amount of phosphorus found on the standard curve, unit: mg;
V2-volume of sample diluted after ashing, unit: ml;
V1the volume of the test solution taken during color development, unit: ml;
w-sample mass, unit: g.
as a modification of the present invention, in step S1, the drawing of the standard curve includes the steps of:
s1.1, taking 5 volumetric flasks, and preparing 5 standard solutions with phosphorus contents of 0.01mg, 0.02mg, 0.04mg, 0.06mg and 0.08mg respectively;
s1.2, adding 8ml of hydrazine sulfate and 2ml of sodium molybdate sulfuric acid solution into 5 standard solutions, and heating in a boiling hot water bath for 10 minutes;
s1.3, adjusting the wavelength to be zero by using a spectrophotometer at 650nm and a 5cm cuvette with water, and respectively measuring the absorbance of the 5 standard solutions heated in the step S1.2;
and S1.4, drawing a standard curve by taking the absorbance as a vertical coordinate and the phosphorus amount as a horizontal coordinate according to the measurement result in the step S1.3.
As an improvement of the present invention, in step S2, the sample pretreatment specifically includes the following steps:
s2.1, adding 0.2-0.3 g of carbonization-assisting catalyst into a sample, uniformly mixing, and placing in a ceramic crucible;
s2.2, placing the ceramic crucible on a temperature-adjusting electric furnace padded with an asbestos gauze, slowly heating, shaking up the content of the crucible, heating until the content is completely carbonized, and taking down the crucible;
s2.3, transferring the porcelain crucible processed in the step S2.2 into a high-temperature furnace, burning and ashing at 600-700 ℃ for 1.5-2 hours, taking out the crucible, and cooling;
s2.4, placing the porcelain crucible processed in the step S2.3 on an electric furnace, adding 3-5 ml of HCI, heating and stirring until the content is clear, slightly boiling for 1-2 minutes, cooling, transferring the test solution into a 100ml volumetric flask, and uniformly shaking to a constant volume with water.
As an improvement of the invention, in the step 3, the color development of the test solution comprises the following steps:
s3.1, sucking 10ml of the test solution pretreated in the step S2, injecting the test solution into a 50ml volumetric flask, adding 8ml of hydrazine sulfate solution, adding 2ml of sodium molybdate dilute sulfuric acid solution, and shaking up;
and S3.2, placing the test solution processed in the step S3.1 in a boiling water bath, heating for 10 minutes, taking out, cooling to room temperature, fixing the volume with water, and fully shaking up.
As a modification of the present invention, in step S4, the absorbance of the sample obtained after the color development treatment in step S3 is measured with a spectrophotometer at a wavelength of 650nm in a 2cm cuvette with reference to water.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and description, and is in no way intended to limit the invention.
A method for detecting the content of phosphorus in dimer acid comprises the following steps:
s1, drawing a standard curve for measuring phosphorus: preparing a plurality of bottles of phosphorus-containing standard solution, and drawing a standard curve by taking the absorbance as a vertical coordinate and the phosphorus amount as a horizontal coordinate;
s2, sample pretreatment: adding a catalyst into a sample to be detected for carbonization pretreatment;
s3, color development of the test solution: adding a color developing agent into the sample pretreated in the step S2 for color development;
s4, measuring the absorbance of the sample: measuring the absorbance of the sample obtained after the color development treatment in the step S3 by using a spectrophotometer;
s5, calculating the result: comparing the absorbance obtained in step S4 with the standard curve in step S1, calculating the phosphorus content in the sample according to formula 1),
in the formula:
p-amount of phosphorus found on the standard curve, unit: mg;
V2-volume of sample diluted after ashing, unit: ml;
V1the volume of the test solution taken during color development, unit: ml;
w-sample mass, unit: g.
as an embodiment of the present invention, in step S1, the drawing of the standard curve includes the steps of:
s1.1, taking 5 volumetric flasks, and preparing 5 standard solutions with phosphorus contents of 0.01mg, 0.02mg, 0.04mg, 0.06mg and 0.08mg respectively;
s1.2, adding 8ml of hydrazine sulfate and 2ml of sodium molybdate sulfuric acid solution into 5 standard solutions, and heating in a boiling hot water bath for 10 minutes;
s1.3, adjusting the wavelength to be zero by using a spectrophotometer at 650nm and a 5cm cuvette with water, and respectively measuring the absorbance of the 5 standard solutions heated in the step S1.2;
and S1.4, drawing a standard curve by taking the absorbance as a vertical coordinate and the phosphorus amount as a horizontal coordinate according to the measurement result in the step S1.3.
As an embodiment of the present invention, in step S2, the sample pretreatment specifically includes the following steps:
s2.1, adding 0.2-0.3 g of carbonization-assisting catalyst into a sample, uniformly mixing, and placing in a ceramic crucible;
s2.2, placing the ceramic crucible on a temperature-adjusting electric furnace padded with an asbestos gauze, slowly heating, shaking up the content of the crucible, heating until the content is completely carbonized, and taking down the crucible;
s2.3, transferring the porcelain crucible processed in the step S2.2 into a high-temperature furnace, burning and ashing at 600-700 ℃ for 1.5-2 hours, taking out the crucible, and cooling;
s2.4, placing the porcelain crucible processed in the step S2.3 on an electric furnace, adding 3-5 ml of HCI, heating and stirring until the content is clear, slightly boiling for 1-2 minutes, cooling, transferring the test solution into a 100ml volumetric flask, and uniformly shaking to a constant volume with water.
As an embodiment of the present invention, in step 3, the color development of the test solution comprises the following steps:
s3.1, sucking 10ml of the test solution pretreated in the step S2, injecting the test solution into a 50ml volumetric flask, adding 8ml of hydrazine sulfate solution, adding 2ml of sodium molybdate dilute sulfuric acid solution, and shaking up;
and S3.2, placing the test solution processed in the step S3.1 in a boiling water bath, heating for 10 minutes, taking out, cooling to room temperature, fixing the volume with water, and fully shaking up.
As an embodiment of the present invention, in step S4, the absorbance of the sample obtained after the color development treatment in step S3 is measured with a spectrophotometer at a wavelength of 650nm in a 2cm cuvette with reference to water.
The invention mainly comprises the following contents:
1. drawing a standard curve for measuring phosphorus
5 volumetric flasks with phosphorus contents of 0.01, 0.02, 0.04, 0.06 and 0.08 respectively are prepared by taking 5 volumetric flasks, 8ml of hydrazine sulfate and 2ml of sodium molybdate sulfuric acid solution are added, and the 5 volumetric flasks are placed in a boiling hot water bath for heating for 10 minutes. The absorbance was measured with a spectrophotometer at a wavelength of 650nm, using a 5cm cuvette, and adjusted to zero with water. And drawing a standard curve by taking the absorbance as an ordinate and the phosphorus amount as an abscissa.
2. Sample pretreatment
2.1 weighing a sample and a carbonization-assisting catalyst, placing the sample and the carbonization-assisting catalyst in a ceramic crucible, placing the crucible on a temperature-adjusting electric furnace padded with an asbestos screen, slowly heating, shaking up the crucible content, heating until the content is completely carbonized, taking down and transferring the crucible to a high-temperature furnace, and burning and ashing for 1.5 to 2 hours at the temperature of 600 to 700 ℃. Taking out the crucible and cooling.
2.2 placing the crucible on an electric furnace, adding 3-5 ml of HCI (HCI: H)2O1: 1) is heated and stirred until the content is clear, slightly boiled for 1-2 minutes, cooled, transferred to a 100ml volumetric flask (filtered if residue is available), and shaken uniformly with water to a constant volume.
3 color development of the test solution
Sucking 10ml of test solution, injecting into a 50ml volumetric flask, adding 8ml of hydrazine sulfate solution, adding 2ml of sodium molybdate dilute sulfuric acid solution, shaking up, heating in a boiling water bath for 10 minutes, taking out, cooling to room temperature, metering volume with water, and fully shaking up.
4 measuring the absorbance of the sample
The absorbance was measured with a spectrophotometer at a wavelength of 650nm using a 2cm cuvette with a water reference.
5 calculation of results
According to the absorbance of the detected liquid, the phosphorus content (P) is found from the standard curve, and the phosphorus content in the sample is calculated according to the following formula:
in the formula:
p is the phosphorus amount found by a standard curve, mg;
V2-volume of sample diluted after ashing, ml;
V1the volume of the test solution, ml, taken during the development;
w-sample mass, g.
The specific detection method comprises the following steps:
weighing about 10 samples and 0.2g of carbonization-assisting catalyst, placing the samples in a porcelain crucible, placing the crucible on a temperature-adjusting electric furnace padded with an asbestos screen, slowly heating, shaking up the content in the crucible, heating until the content is completely carbonized, taking down and transferring the content to a high-temperature furnace, and burning and ashing for 1.5-2 hours at 600-700 ℃. Taking out the crucible and cooling.
Placing the crucible on an electric furnace, adding 3-5 ml of HCI (HCI: H)2O1: 1) is heated and stirred until the content is clear, slightly boiled for 1-2 minutes, cooled, transferred to a 100ml volumetric flask (filtered if residue is available), and shaken uniformly with water to a constant volume.
Sucking 10ml of test solution, injecting into a 50ml volumetric flask, adding 8ml of hydrazine sulfate solution, adding 2ml of sodium molybdate dilute sulfuric acid solution, shaking up, heating in a boiling water bath for 10 minutes, taking out, cooling to room temperature, metering volume with water, and fully shaking up.
The absorbance was measured with a spectrophotometer at a wavelength of 650nm using a 2cm cuvette with a water reference. According to the absorbance of the detected liquid, the phosphorus content (P) is found from the standard curve, and the phosphorus content in the sample is calculated according to the following formula:
in the formula:
p is the phosphorus amount found by a standard curve, mg;
V2-volume of sample diluted after ashing, ml;
V1the volume of the test solution, ml, taken during the development;
w-sample mass, g.
A total of 5 batches of dimer acid were tested in actual operation, and the data are shown in the following table:
| batch number | Phosphorus content PPm |
| 20101008 | 15.0 |
| 20101010 | 13.0 |
| 20101012 | 10.0 |
| 20101015 | 12.0 |
| 20101018 | 12.5 |
The invention provides a method for accurately and efficiently detecting the content of phosphorus in dimer acid, which has the advantages of low cost and simple and convenient operation.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.
Claims (5)
1. A method for detecting the content of phosphorus in dimer acid is characterized by comprising the following steps:
s1, drawing a standard curve for measuring phosphorus: preparing a plurality of bottles of phosphorus-containing standard solution, and drawing a standard curve by taking the absorbance as a vertical coordinate and the phosphorus amount as a horizontal coordinate;
s2, sample pretreatment: adding a catalyst into a sample to be detected for carbonization pretreatment;
s3, color development of the test solution: adding a color developing agent into the sample pretreated in the step S2 for color development;
s4, measuring the absorbance of the sample: measuring the absorbance of the sample obtained after the color development treatment in the step S3 by using a spectrophotometer;
s5, calculating the result: comparing the absorbance obtained in step S4 with the standard curve in step S1, calculating the phosphorus content in the sample according to formula 1),
in the formula:
p-amount of phosphorus found on the standard curve, unit: mg;
V2-volume of sample diluted after ashing, unit: ml;
V1the volume of the test solution taken during color development, unit: ml;
w-sample mass, unit: g.
2. the method for detecting the content of phosphorus in dimer acid according to claim 1, wherein the method comprises the following steps: in step S1, the drawing of the standard curve includes the steps of:
s1.1, taking 5 volumetric flasks, and preparing 5 standard solutions with phosphorus contents of 0.01mg, 0.02mg, 0.04mg, 0.06mg and 0.08mg respectively;
s1.2, adding 8ml of hydrazine sulfate and 2ml of sodium molybdate sulfuric acid solution into 5 standard solutions, and heating in a boiling hot water bath for 10 minutes;
s1.3, adjusting the wavelength to be zero by using a spectrophotometer at 650nm and a 5cm cuvette with water, and respectively measuring the absorbance of the 5 standard solutions heated in the step S1.2;
and S1.4, drawing a standard curve by taking the absorbance as a vertical coordinate and the phosphorus amount as a horizontal coordinate according to the measurement result in the step S1.3.
3. The method for detecting the content of phosphorus in dimer acid according to claim 1, wherein the method comprises the following steps: in step S2, the sample pretreatment specifically includes the following steps:
s2.1, adding 0.2-0.3 g of carbonization-assisting catalyst into a sample, uniformly mixing, and placing in a ceramic crucible;
s2.2, placing the ceramic crucible on a temperature-adjusting electric furnace padded with an asbestos gauze, slowly heating, shaking up the content of the crucible, heating until the content is completely carbonized, and taking down the crucible;
s2.3, transferring the porcelain crucible processed in the step S2.2 into a high-temperature furnace, burning and ashing at 600-700 ℃ for 1.5-2 hours, taking out the crucible, and cooling;
s2.4, placing the porcelain crucible processed in the step S2.3 on an electric furnace, adding 3-5 ml of HCI, heating and stirring until the content is clear, slightly boiling for 1-2 minutes, cooling, transferring the test solution into a 100ml volumetric flask, and uniformly shaking to a constant volume with water.
4. The method for detecting the content of phosphorus in dimer acid according to claim 1, wherein the method comprises the following steps: in step 3, the development of the test solution comprises the following steps:
s3.1, sucking 10ml of the test solution pretreated in the step S2, injecting the test solution into a 50ml volumetric flask, adding 8ml of hydrazine sulfate solution, adding 2ml of sodium molybdate dilute sulfuric acid solution, and shaking up;
and S3.2, placing the test solution processed in the step S3.1 in a boiling water bath, heating for 10 minutes, taking out, cooling to room temperature, fixing the volume with water, and fully shaking up.
5. The method for detecting the content of phosphorus in dimer acid according to claim 1, wherein the method comprises the following steps: in step S4, the absorbance of the sample obtained after the color development treatment in step S3 is measured with a spectrophotometer at a wavelength of 650nm using a 2cm cuvette with a water reference.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4843015A (en) * | 1987-11-05 | 1989-06-27 | Westvaco Corporation | Method for determining volatile phosphorus in carbon |
| CN105092496A (en) * | 2015-08-14 | 2015-11-25 | 武钢集团昆明钢铁股份有限公司 | Method for detecting content of phosphorus in nitrification intensifier |
| CN105300975A (en) * | 2015-11-11 | 2016-02-03 | 武钢集团昆明钢铁股份有限公司 | Detecting method for phosphorus content in vanadium slag |
-
2021
- 2021-03-31 CN CN202110345206.8A patent/CN112858199A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4843015A (en) * | 1987-11-05 | 1989-06-27 | Westvaco Corporation | Method for determining volatile phosphorus in carbon |
| CN105092496A (en) * | 2015-08-14 | 2015-11-25 | 武钢集团昆明钢铁股份有限公司 | Method for detecting content of phosphorus in nitrification intensifier |
| CN105300975A (en) * | 2015-11-11 | 2016-02-03 | 武钢集团昆明钢铁股份有限公司 | Detecting method for phosphorus content in vanadium slag |
Non-Patent Citations (1)
| Title |
|---|
| 陈勇: "植物油磷含量快速检测方法探讨", 中国油脂, vol. 34, no. 05, pages 69 - 70 * |
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