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Method for determining elemental sulfur in fertilizer

A determination method and technology of elemental sulfur, applied in the field of phosphorus chemical industry, can solve the problems of large limitations, hidden dangers of production safety cannot be effectively monitored and monitored, and time-consuming, etc., to achieve improved accuracy and precision, and long-term monitoring of hidden dangers of safety. , sensitive and selective effect

Active Publication Date: 2017-02-15
WENGFU DAZHOU CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But at present, there is no suitable detection method for elemental sulfur in diamine thiophosphate at home and abroad.
[0003] The domestic standard GB / T 19203 sample dissolution method uses concentrated nitric acid and perchloric acid, but this method is only applicable to the detection method of total sulfur in compound fertilizers. The previous compound fertilizer products did not add sulfur powder. Chloric acid is the most oxidizing acid among inorganic acids. Although it can react with sulfur, it is dangerous and prone to explosion under heating conditions. Therefore, this method is not suitable for adding diammonium phosphate total sulfur and elemental sulfur. Content detection
[0004] At present, the detection methods of sulfate mainly include turbidimetry, spectrophotometry, burning method and drying method. Although these methods require low detection conditions, they have large limitations. The first two methods are mainly suitable for low-content sulfuric acid. For the determination of salt, the results of the latter two methods are ideal for the detection of constants, but they take too long. It takes at least 4 hours from sample processing to the issuance of the results, and it is impossible to provide timely results of the sulfur content of the dust generated during the production of diammonium phosphate. , production safety hazards cannot be effectively monitored and monitored

Method used

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  • Method for determining elemental sulfur in fertilizer
  • Method for determining elemental sulfur in fertilizer
  • Method for determining elemental sulfur in fertilizer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] 1. Instruments: electronic balance, Prodigy XP inductively coupled plasma emission spectrometer (Leaman Corporation, USA)

[0062] 2. Reagents: potassium chlorate (analytical pure), concentrated nitric acid (analytical pure), (1+1) nitric acid, SO 4 Standard stock solution (1mg / mL)

[0063] 3 Analytical conditions: the parameter settings of the atomic emission spectrometer are shown in Table 1

[0064] Table 1 Test parameters of atomic emission spectrometer

[0065]

[0066] 4. Establish a working curve:

[0067] Take 0.00mg, 50mg, and 100mg standard stock solutions respectively and put them in a series of 500mL volumetric flasks, dilute to the mark with pure water, shake well, and detect the sulfate radical value on an atomic emission spectrometer. Take the quality mg of sulfate radical as the abscissa, and the corresponding atomic emission spectrometer value as the ordinate, draw the working curve with the detection value of the sulfate radical standard solution...

Embodiment 2

[0085] Precision experiment

[0086] Weigh 0.4012g and 0.4008g samples respectively and measure 10 sets of data according to the test method in Example 1, and the test results are shown in Table 3.

[0087] Table 3 precision measurement data

[0088] serial number 1 2 3 4 5 6 7 8 9 10 RSD% Total Sulfur % 7.25 7.43 7.55 7.33 7.38 7.50 7.38 7.43 7.46 7.40 1.15 Compound sulfur% 3.80 3.99 3.90 3.86 3.89 3.84 3.82 3.86 3.87 3.92 1.40 Elemental sulfur 3.45 3.44 3.65 3.47 3.49 3.66 3.56 3.57 3.59 3.48 0.02

[0089] It can be seen from Table 3 that the extreme difference of the results of 10 groups is less than or equal to 0.2%, the RSD is less than 2%, and the interference of the matrix is ​​small, indicating that the precision of the present invention is better.

Embodiment 3

[0091] Accuracy experiment

[0092] Three groups of samples were weighed, and a standard addition recovery experiment was carried out to measure the accuracy of the detection method of the present invention. The experimental data are shown in Table 4.

[0093] Table 4 horizontal atomic emission spectrometer plus diammonium thiophosphate standard recovery test data

[0094]

[0095]

[0096] It can be seen from Table 4 that the recovery rates of the samples were all above 96.8%, indicating that the detection method of the present invention has better accuracy.

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Abstract

The invention provides a method for determining elemental sulfur in fertilizer. The method comprises steps as follows: (1), determination of total sulfur content of the fertilizer: a fertilizer sample is taken, potassium chlorate is added and the components completely react under the heating and acidic conditions, then the sulfur content is determined by an atomic emission spectrometer, and total sulfur content is obtained; (2), determination of combined-state sulfur content of the fertilizer: a fertilizer sample with the same mass as the fertilizer sample in the step (1) is taken and completely dissolved with strong acid under the heating condition, then the sulfur content is determined by the atomic emission spectrometer, and combined-state sulfur content is obtained; (3), calculation of elemental sulfur content of the fertilizer: a difference value between the total sulfur content and the combined-state sulfur content is calculated, and the elemental sulfur content is obtained. According to the determination method, mass fraction of elemental sulfur in the sulfur-containing fertilizer can be detected accurately, and the detection time can be shortened, so that hidden dangers of long-periodic safety production of sulfurated diammonium phosphate are effectively monitored.

Description

technical field [0001] The invention relates to the technical field of phosphorus chemical industry, in particular to a method for determining elemental sulfur in sulfur-added ammonium phosphate fertilizers. Background technique [0002] Diammonium phosphate is a high-concentration quick-acting fertilizer, which is suitable for various crops and soils, especially for nitrogen-loving and phosphorus-demanding crops. It can be used as base fertilizer or top dressing, and it should be applied deeply. Sulfur is mixed into diammonium phosphate, and after it is applied to the soil, sulfur (elemental sulfur) is slowly converted into sulfate and absorbed by plants, which can increase the production of grain and so on. However, there is currently no suitable detection method for elemental sulfur in diamine thiophosphate at home and abroad. [0003] The domestic standard GB / T 19203 sample dissolution method uses concentrated nitric acid and perchloric acid, but this method is only app...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/73
CPCG01N21/73
Inventor 杨晓梅王剑杨胜平赵强伍庆先伍兴梅
Owner WENGFU DAZHOU CHEM CO LTD
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