A method for detecting the arsenic content in red phosphorus

Abstract

The present invention discloses a method for detecting the arsenic content in red phosphorus. In the present invention, first, 130-150 parts of red phosphorus raw material and 400-500 parts of concentrated sulfuric acid are weighed and pickled; after mixing 130-150 parts of the weighed red phosphorus and 400-500 parts of concentrated sulfuric acid, vigorous stirring is started; after clarification for 50 min, after the mixture cools down to 40 °C; after pickling, chlorination → rectification are carried out in sequence; then the obtained substance is treated with chemical reagents, and then arsenic spot colorimetry is carried out and calculated to obtain the arsenic content; by detecting the impurity content, the product purity is improved to solve the problem of too high impurity content in the product; through impurity detection, the arsenic impurity content of each batch of products can be known, and the cost required for cooperation with third-party detection can be reduced; potential safety hazards brought during the production process are eliminated, thereby improving the safety of the entire production and preparation process and ensuring personal safety.

Description

Technical Field

[0001] The present invention belongs to the technical field of arsenic content detection, and specifically relates to a method for detecting the arsenic content in red phosphorus. Background Art

[0002] Red phosphorus, also known as red phosphorus, is a purple-red amorphous powder, shiny and non-toxic. When heated under high pressure to 590 °C, it begins to melt. If not pressurized, it sublimes without melting, and white phosphorus is obtained after condensation of the vaporization. Red phosphorus forms a chain or ring high-polymer structure with single bonds of P4 tetrahedrons, has high stability, is insoluble in water and carbon disulfide, slightly soluble in absolute ethanol, and soluble in alkaline solutions. It reacts with nitric acid to form phosphoric acid and forms chlorides when heated in chlorine. Yellow phosphorus gradually converts to red phosphorus when heated in a vacuum at normal pressure to 250 °C for several days. Red phosphorus can be used as a diffusion source in the semiconductor industry, for organic synthesis and match manufacturing, and also as an insecticide, rodenticide, fireworks and smoke bombs, etc. When red phosphorus is produced and used, it is necessary to detect the arsenic element content inside to determine the purity of red phosphorus.

[0003] In the prior art when detecting the arsenic content, after digesting yellow phosphorus and red phosphorus samples, certain chemical reagents are added to form arsenic spots, which are compared with standard arsenic spots.

[0004] However, when using this type of detection method, the following problems exist:

[0005] 1: The detection time of arsenic is too long. When there is an error, the retest takes too long;

[0006] 2: The sample treatment of arsenic needs to be carried out at high temperature, which has potential safety hazards;

[0007] 3: The detection efficiency of arsenic is low. Summary of the Invention

[0008] The purpose of the present invention is to provide a method for detecting the arsenic content in red phosphorus in order to solve the above-mentioned problems.

[0009] The technical solution adopted by the present invention is as follows: A method for detecting the arsenic content in red phosphorus, the method for detecting the arsenic content in red phosphorus includes the following steps:

[0010] S1: First, weigh 130 - 150 parts of red phosphorus raw material and 400 - 500 parts of concentrated sulfuric acid, and perform pickling;

[0011] S2: After mixing 130 - 150 parts of the red phosphorus and 400 - 500 parts of concentrated sulfuric acid weighed in step S1, start to stir it vigorously;

[0012] S3: After clarification for 50 min, wait until the mixture cools down to 40 °C;

[0013] S4: After pickling, perform chlorination → rectification in sequence;

[0014] S5: Then, the obtained substance is treated with chemical reagents, and then compared with arsenic spots for colorimetry and calculation to obtain the arsenic content.

[0015] In a preferred embodiment, in the step S2, the stirring speed is 1000 r / min, and the stirring time is 30 - 45 min.

[0016] In a preferred embodiment, in the step S3, during the cooling process, it is stirred, and the stirring speed is 200 r / min.

[0017] In a preferred embodiment, in the step S4, the sample is treated by reflux condensation during the rectification process.

[0018] In a preferred embodiment, in the step S5, the detection environment temperature is lower than the sample temperature.

[0019] In a preferred embodiment, in the step S4, the process of chlorination → rectification is carried out in a fume hood.

[0020] In summary, due to the adoption of the above technical solutions, the beneficial effects of the present invention are as follows:

[0021] In the present invention, by detecting the impurity content, the product purity is improved to solve the problem of excessive impurity content in the product; through impurity detection, the arsenic impurity content of each batch of products can be known, reducing the cost required for cooperation with third - party detection; eliminating potential safety hazards brought during the production process, thereby improving the safety of the entire production and preparation process and ensuring personal safety. Specific Embodiments

[0022] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Apparently, the described embodiments are some, but not all, of the embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

[0023] Example 1:

[0024] A method for detecting the arsenic content in red phosphorus, the method for detecting the arsenic content in red phosphorus includes the following steps:

[0025] S1: First, weigh 130 parts of red phosphorus raw material and 400 parts of concentrated sulfuric acid, and perform pickling;

[0026] S2: After mixing 130 parts of red phosphorus and 400 parts of concentrated sulfuric acid weighed in step S1, start to stir it vigorously; in step S2, the stirring speed is 1000 r / min, and the stirring time is 30 - 45 min;

[0027] S3: After clarification for 50 min, wait until the mixture cools down to 40 °C; in step S3, stir it during the cooling process, and the stirring speed is 200 r / min;

[0028] S4: After pickling, carry out chlorination → rectification in sequence; in step S4, use reflux condensation to treat the sample during the rectification process; in step S4, the chlorination → rectification process is carried out in a fume hood;

[0029] S5: Then treat the obtained substance with chemical reagents, and then compare with arsenic spot colorimetry and calculate to obtain the arsenic content. In step S5, the detection ambient temperature is lower than the sample temperature.

[0030] In the present invention, by detecting the impurity content, the product purity is improved to solve the problem of excessive impurity content in the product; through impurity detection, the arsenic impurity content of each batch of products can be known, and the cost required for cooperation with third - party detection can be reduced; eliminate the potential safety hazards brought during the production process, thereby improving the safety of the entire production and preparation process and ensuring personal safety.

[0031] Example 2:

[0032] A method for detecting the arsenic content in red phosphorus, the method for detecting the arsenic content in red phosphorus includes the following steps:

[0033] S1: First, weigh 140 parts of red phosphorus raw material and 400 parts of concentrated sulfuric acid, and carry out pickling;

[0034] S2: After mixing 140 parts of red phosphorus and 400 parts of concentrated sulfuric acid weighed in step S1, start to stir it vigorously; in step S2, the stirring speed is 1000 r / min, and the stirring time is 30 - 45 min;

[0035] S3: After clarification for 50 min, wait until the mixture cools down to 40 °C; in step S3, stir it during the cooling process, and the stirring speed is 200 r / min;

[0036] S4: After pickling, carry out chlorination → rectification in sequence; in step S4, use reflux condensation to treat the sample during the rectification process; in step S4, the chlorination → rectification process is carried out in a fume hood;

[0037] S5: After treating the obtained substance with chemical reagents, then compare with the arsenic spot colorimetry and calculate to obtain the arsenic content. In step S5, the detection ambient temperature is lower than the sample temperature.

[0038] In the present invention, by detecting the impurity content, the product purity is improved to solve the problem of excessive impurity content in the product; through impurity detection, the arsenic impurity content of each batch of products can be known, reducing the cost required for cooperation with third-party detection; eliminating potential safety hazards brought during the production process, thereby improving the safety of the entire production and preparation process and ensuring personal safety.

[0039] Example 3:

[0040] A method for detecting the arsenic content in red phosphorus, the method for detecting the arsenic content in red phosphorus includes the following steps:

[0041] S1: First weigh 130 parts of red phosphorus raw material and 450 parts of concentrated sulfuric acid, and perform pickling.

[0042] S2: After mixing the 130 parts of red phosphorus and 450 parts of concentrated sulfuric acid weighed in step S1, start to stir it vigorously; in step S2, the stirring speed is 1000 r / min, and the stirring time is 30 - 45 min.

[0043] S3: After clarification for 50 min, wait until the mixture cools down to 40 °C; in step S3, stir it during the cooling process, and the stirring speed is 200 r / min.

[0044] S4: After pickling, carry out chlorination → rectification in sequence; in step S4, the sample is treated with reflux condensation during the rectification process; in step S4, the chlorination → rectification process is carried out in a fume hood.

[0045] S5: After treating the obtained substance with chemical reagents, then compare with the arsenic spot colorimetry and calculate to obtain the arsenic content. In step S5, the detection ambient temperature is lower than the sample temperature.

[0046] In the present invention, by detecting the impurity content, the product purity is improved to solve the problem of excessive impurity content in the product; through impurity detection, the arsenic impurity content of each batch of products can be known, reducing the cost required for cooperation with third-party detection; eliminating potential safety hazards brought during the production process, thereby improving the safety of the entire production and preparation process and ensuring personal safety.

[0047] Example 4:

[0048] A method for detecting the arsenic content in red phosphorus, the method for detecting the arsenic content in red phosphorus includes the following steps:

[0049] S1: First, weigh 150 parts of red phosphorus raw material and 400 parts of concentrated sulfuric acid, and perform pickling;

[0050] S2: After mixing the 150 parts of red phosphorus and 400 parts of concentrated sulfuric acid weighed in step S1, start to stir it vigorously; in step S2, the stirring speed is 1000 r / min, and the stirring time is 30 - 45 min;

[0051] S3: After clarification for 50 min, wait until the mixture cools down to 40 °C; in step S3, stir it during the cooling process, and the stirring speed is 200 r / min;

[0052] S4: After pickling, carry out chlorination → rectification in sequence; in step S4, reflux condensation is used to treat the sample during the rectification process; in step S4, the chlorination → rectification process is carried out in a fume hood;

[0053] S5: Then treat the obtained substance with chemical reagents, and then compare and calculate with arsenic spot colorimetry to obtain the arsenic content. In step S5, the detection environmental temperature is lower than the sample temperature.

[0054] In the present invention, by detecting the impurity content, the product purity is improved to solve the problem of too high impurity content in the product; through impurity detection, the arsenic impurity content of each batch of products can be known, and the cost required for cooperation with third - party detection can be reduced; the potential safety hazards brought during the production process are eliminated, thereby improving the safety of the entire production and preparation process and ensuring personal safety.

[0055] Example Five:

[0056] A method for detecting the arsenic content in red phosphorus, the method for detecting the arsenic content in red phosphorus includes the following steps:

[0057] S1: First, weigh 150 parts of red phosphorus raw material and 450 parts of concentrated sulfuric acid, and perform pickling;

[0058] S2: After mixing the 150 parts of red phosphorus and 450 parts of concentrated sulfuric acid weighed in step S1, start to stir it vigorously; in step S2, the stirring speed is 1000 r / min, and the stirring time is 30 - 45 min;

[0059] S3: After clarification for 50 min, wait until the mixture cools down to 40 °C; in step S3, stir it during the cooling process, and the stirring speed is 200 r / min;

[0060] S4: After pickling, carry out chlorination → rectification in sequence; in step S4, reflux condensation is used to treat the sample during the rectification process; in step S4, the chlorination → rectification process is carried out in a fume hood;

[0061] S5: Then, the obtained substance is treated with chemical reagents, and then colorimetric comparison is carried out with arsenic spots and calculations are made to obtain the arsenic content. In step S5, the detection ambient temperature is lower than the sample temperature.

[0062] In the present invention, by detecting the impurity content, the product purity is improved to solve the problem of excessive impurity content in the product; through impurity detection, the arsenic impurity content of each batch of products can be known, reducing the cost required for cooperation with third-party detection; eliminating potential safety hazards in the production process, thereby improving the safety of the entire production and preparation process and ensuring personal safety.

[0063] Example Six:

[0064] A method for detecting the arsenic content in red phosphorus, the method for detecting the arsenic content in red phosphorus includes the following steps:

[0065] S1: First, weigh 150 parts of red phosphorus raw material and 500 parts of concentrated sulfuric acid, and perform pickling.

[0066] S2: After mixing 150 parts of the red phosphorus and 500 parts of concentrated sulfuric acid weighed in step S1, start to stir it vigorously; in step S2, the stirring speed is 1000 r / min, and the stirring time is 30 - 45 min.

[0067] S3: After clarification for 50 min, wait until the mixture cools down to 40 °C; in step S3, stir it during the cooling process, and the stirring speed is 200 r / min.

[0068] S4: After pickling, perform chlorination → rectification in sequence; in step S4, the sample is treated with reflux condensation during the rectification process; in step S4, the chlorination → rectification process is carried out in a fume hood.

[0069] S5: Then, the obtained substance is treated with chemical reagents, and then colorimetric comparison is carried out with arsenic spots and calculations are made to obtain the arsenic content. In step S5, the detection ambient temperature is lower than the sample temperature.

[0070] In the present invention, by detecting the impurity content, the product purity is improved to solve the problem of excessive impurity content in the product; through impurity detection, the arsenic impurity content of each batch of products can be known, reducing the cost required for cooperation with third-party detection; eliminating potential safety hazards in the production process, thereby improving the safety of the entire production and preparation process and ensuring personal safety.

[0071] It should be noted that in this text, relational terms such as "first" and "second" are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any actual relationship or order between these entities or operations. Moreover, the term "comprising", "including" or any other variant thereof is intended to cover non-exclusive inclusion, so that a process, method, article or device comprising a series of elements not only includes those elements, but also includes other elements not expressly listed, or also includes elements inherent to such process, method, article or device. Without further limitation, an element defined by the statement "comprising one..." does not exclude the existence of additional identical elements in the process, method, article or device comprising the said element.

[0072] The above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that they can still modify the technical solutions recorded in the foregoing embodiments, or perform equivalent replacements for some of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A method for detecting the arsenic content in red phosphorus, characterized in that: The detection method for the arsenic content in red phosphorus comprises the following steps: S1: Weigh 130 - 150 parts of red phosphorus raw material and 400 - 500 parts of concentrated sulfuric acid first, and conduct pickling; S2: After mixing 130 - 150 parts of the red phosphorus and 400 - 500 parts of concentrated sulfuric acid weighed in step S1, start to stir it vigorously; S3: After clarification for 50 min, wait until the mixture cools down to 40 °C; S4: After pickling, conduct chlorination → rectification in sequence; S5: Then treat the obtained substance with chemical reagents, and then compare with an arsenic spot for colorimetry and calculate to obtain the arsenic content; In step S2, the stirring speed is 1000 r / min, and the stirring time is 30 - 45 min; In step S3, stir it during the cooling process, and the stirring speed is 200 r / min.

2. The detection method of arsenic content in red phosphorus according to claim 1, characterized in that: In step S4, the sample is treated with reflux condensation during the rectification process.

3. The method for detecting the arsenic content in red phosphorus according to claim 1, characterized in that: In step S5, the detection environmental temperature is lower than the sample temperature.

4. The detection method of arsenic content in red phosphorus according to claim 1, wherein: In step S4, the chlorination → rectification process is carried out in a fume hood.