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Preparation method of standard sample composed of more than ten elements (As, Se, P and the like) and multiple phthalates in polyvinyl chloride (PVC)

A technology of phthalates and standard samples, which is applied in the field of preparation of standard samples for analysis, can solve problems such as difficulty in ensuring uniform distribution of elements, digestion of substances that are difficult to add, and inability to implement processing and production, etc., to achieve the goal of manufacturing Uniform sample, easy operation, good reproducibility

Active Publication Date: 2017-05-10
KINGFA SCI & TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When there are many substances added, it is difficult to digest the added substances together by using the solvent method, and it is impossible to carry out processing and production
Another existing method is to use the direct processing method, but the direct processing method is difficult to ensure the smooth progress of the processing process and the uniformity of element distribution.

Method used

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  • Preparation method of standard sample composed of more than ten elements (As, Se, P and the like) and multiple phthalates in polyvinyl chloride (PVC)
  • Preparation method of standard sample composed of more than ten elements (As, Se, P and the like) and multiple phthalates in polyvinyl chloride (PVC)
  • Preparation method of standard sample composed of more than ten elements (As, Se, P and the like) and multiple phthalates in polyvinyl chloride (PVC)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0050] The standard samples that need to be prepared contain target elements, phthalates, and their concentrations as shown in Table 1:

[0051] Table 1

[0052]

[0053] S1, S2. According to the content in Table 1, select the substance in Table 2 as the source of the compound containing the target element, and perform concentration conversion to calculate its addition amount; the formula of the entire high-concentration masterbatch is shown in Table 2:

[0054] Table 2

[0055]

[0056] S3. Use a ball mill to grind the compounds in Table 2, pass through a 200-mesh sieve after grinding, and use a laser particle size analyzer to test the particle size and agglomeration of the compound after grinding to ensure that the compound after grinding will not agglomerate. From the results, it can be seen that the target added substances after grinding meet the production requirements, and no agglomeration occurs. The average particle size of the particles is between 30 and 50 μm...

Embodiment 2

[0064] The preparation method of the standard particle of embodiment 2 and embodiment 3, S1~S7 is identical with embodiment 1, and difference is, after the standard particle that S7 obtains, then according to the amount of table 3, adopt the standard particle that S7 obtains (as high Concentration masterbatch B) is mixed evenly with blank PVC again, and the fifth extrusion granulation is carried out.

[0065] S9. Carry out the sixth extrusion granulation to the particle of the fifth extrusion granulation; And according to the time required for the fifth extrusion granulation, carry out multiple interval sampling during the sixth extrusion granulation , to verify the uniformity between adjacent samples, and complete the preparation after the uniformity is qualified.

Embodiment 3

[0078] Table 7 Example 3 standard sample homogeneity verification

[0079]

[0080] Table 8 Verification of uniformity of prepared masterbatches in comparative examples

[0081]

[0082] It can be seen that if only one granulation is used, even if the uniformity of the small sample is verified during the preparation process, the concentration of the prepared masterbatch will fluctuate greatly between different batches, so this masterbatch is not suitable for standard samples preparation. However, the two-time granulation method of the present invention can well ensure the uniformity between batches.

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Abstract

The invention provides a preparation method of a standard sample composed of more than ten elements (As, Se, P and the like) and multiple phthalates in polyvinyl chloride (PVC). The method comprises the following steps: preparing a high-concentration master batch of which the concentration is several times of that of the standard sample, and mixing the high-concentration master batch with blank PVC to prepare the standard sample. In the high-concentration master batch preparation process and standard sample preparation process, two granulation processes are respectively performed. The target elements comprise Pb, Cd, Hg, Cr, Sb, Ba, Mg, Cu, Se and P. The phthalate substances comprise one or more of DBP (dibutyl phthalate), BBP (butyl benzyl phthalate), DEHP (di-2-ethylhexyl phthalate), DNOP (di-n-octyl phthalate), DIDP (diisodecyl phthalate) and DINP (diisononyl phthalate). The method can be used for obtaining the satisfactory standard sample, and the prepared sample has the advantages of high uniformity and favorable reproducibility.

Description

technical field [0001] The invention belongs to a preparation method of a standard sample for analysis, in particular to a preparation method of a polyvinyl chloride standard sample containing multiple heavy metal elements and multiple phthalates. Background technique [0002] Most of the existing technologies use the solution method to prepare standard samples. For example, the patent ZL200710047544.3 involves less heavy metal additives and does not contain o-benzene additives. When there are many substances added, it is difficult to digest the added substances together by using the solvent method, and it is impossible to implement processing and production. Another existing method is to adopt the direct processing method, but the direct processing method is difficult to guarantee the smooth progress of the processing process and the uniform distribution of elements. Contents of the invention [0003] The purpose of the present invention is to overcome the deficiencies i...

Claims

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Application Information

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IPC IPC(8): C08L27/06C08K13/02C08K5/12C08K3/22C08K3/30C08K3/38C08K3/16G01N1/28
CPCC08K3/16C08K3/22C08K3/2279C08K3/30C08K3/38C08K5/12C08K13/02C08K2003/2224C08K2003/2234C08K2003/2251C08K2003/3027C08K2201/014G01N1/28C08L27/06
Inventor 吴博李云巧胡金妮宋翠翠巢静波
Owner KINGFA SCI & TECH CO LTD
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