Red Phosphorus Resin Standard Sample Preparation
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Solution Overview
Problem
The challenge in accurately preparing standard samples for quantitative determination of red phosphorus in resins using pyrolysis-GC/MS lies in ensuring uniform dispersion of red phosphorus in small amounts, as existing methods face contamination issues and difficulty in achieving uniform dispersibility due to the small sample size and solid nature of the samples.
Innovation Solution
A method involving kneading red phosphorus into a resin to create a red-phosphorus-containing compound, followed by fine pulverization to achieve uniform dispersion, ensuring the particles are predominantly less than 5 µm in diameter, and weighing the compound in amounts ranging from 0.05 to 10 mg to guarantee accurate calibration curves.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Object-affected harmful factors
If the amount of solid sample is reduced to 10 mg or less for pyrolysis-GC/MS analysis, then detector contamination is reduced, but uniform dispersibility of red phosphorus becomes difficult to ensure
Solution Approach 1:
The patent applies preliminary action by thoroughly mixing red phosphorus with resin powder before pulverization to create a homogeneous red-phosphorus-containing compound. This preliminary uniform distribution ensures that even when the final sample amount is reduced to 10 mg or less, the red phosphorus remains uniformly dispersed throughout the sample, solving both the detector contamination issue and maintaining manufacturing precision
Solution Approach 2:
The patent changes the physical state and size parameters by pulverizing the red-phosphorus-containing compound to obtain fine particles with a maximum diameter of 5 μm or less. This particle size reduction improves dispersibility in the minimal sample amount while preventing aggregation that would cause non-uniform distribution, thereby maintaining manufacturing precision even at reduced sample sizes
2Ease of manufacture
If red phosphorus is directly analyzed without blending into resin, then analysis simplicity is maintained, but uniform dispersion cannot be achieved in small sample amounts
Solution Approach 1:
The patent creates a composite material by blending red phosphorus with resin powder to form a red-phosphorus-containing compound. This composite structure ensures uniform dispersion of red phosphorus throughout the sample matrix, solving the uniform dispersion problem while maintaining analytical simplicity through the integrated nature of the composite sample
3Ease of manufacture
If existing kneading technologies are used for solid samples, then mixing is achieved, but uniform dispersibility cannot be guaranteed in very small sample amounts of 0.05 to 10 mg
Solution Approach 1:
The patent applies preliminary action by performing thorough mixing of red phosphorus with resin powder before pulverization to create a homogeneous red-phosphorus-containing compound. This preliminary uniform distribution ensures that even when the final sample amount is reduced to 0.05 to 10 mg, the red phosphorus remains uniformly dispersed throughout the sample, solving both the detector contamination issue and maintaining manufacturing precision
Solution Approach 2:
The patent changes the physical state and size parameters by pulverizing the red-phosphorus-containing compound to obtain fine particles with a maximum diameter of 5 μm or less. This particle size reduction improves dispersibility in the minimal sample amount while preventing aggregation that would cause non-uniform distribution, thereby maintaining manufacturing precision even at reduced sample sizes
Applied Scientific Principles
This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.
Function Achieved in This Case
This method allows for the production of standard samples with uniform red phosphorus dispersion, enabling accurate quantitative determination of red phosphorus in resins, reducing contamination risks and improving the reliability of calibration curves.
Implementation Method 1
a method in which a sample is gasified with a pyrolysis-gas chromatograph
Data Source
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AI summary
Provided are a method for preparing a standard sample in which a uniform dispersion of a predetermined concentration of red phosphorus is guaranteed even in a very small amount, and an analytical method for quantitatively determining red phosphorus contained in a resin by pyrolysis-GC/MS, in which the standard sample is used. The method for producing a standard sample for quantitatively determining red phosphorus contained in a resin includes the steps of preparing a red-phosphorus-containing compound by weighing a predetermined amount of red phosphorus and uniformly mixing the red phosphorus in a resin; decreasing the number of particles having a maximum diameter of 5 µm or more to 1/20 or less of the number of particles having a maximum diameter of 1 µm or more and less than 5 µm by pulverizing the red-phosphorus-containing compound; and obtaining a standard sample by weighing about 0.05 to 10 mg, preferably about 0.1 to 0.5 mg of the pulverized red-phosphorus-containing compound. The analytical method is a method for quantitatively determining red phosphorus contained in a resin by pyrolysis-GC/MS, in which the standard sample is used.