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Method for measuring metal element content in polycarbonate

A technology of metal element content and metal element, which is applied in the field of determination of metal element content in polycarbonate, can solve the problems of long cooling and acid removal treatment, volatilization and dissipation of metal elements, inaccurate measurement results, etc., so as to save processing time , improve the accuracy, the effect of simple operation

Active Publication Date: 2015-09-02
LUXI CHEM GRP
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  • Application Information

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Problems solved by technology

However, the pretreatment of polycarbonate by this method takes 4 hours, which is too long; during the dry ashing pretreatment, the metal elements are easily volatilized and dissipated due to the high temperature; the crucible may react with the metal elements and has a certain effect on the metal elements Occlusion, resulting in the loss of metal elements, resulting in inaccurate determination results
[0003] Although Chinese patent 201210376219.2 discloses a method for determining the content of metal elements in polymer resins, its pretreatment uses microwave digestion (closed high-pressure digestion), and the disadvantage is that microwave digestion uses a closed high-temperature and high-pressure digestion method. Pressure will cause the digestion tank to explode, which poses a great safety hazard; although the microwave digestion process only takes 10-30 minutes to complete, the subsequent cooling and acid removal treatment takes too long

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  • Method for measuring metal element content in polycarbonate
  • Method for measuring metal element content in polycarbonate
  • Method for measuring metal element content in polycarbonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Preparation of sample solution: Accurately weigh 0.3914g polycarbonate sample and put it into a Kjeldahl nitrogen flask, add 10ml of concentrated sulfuric acid solution (the mass fraction of sulfuric acid in the sulfuric acid solution is 98.5%), and place it on a closed electric furnace (120°C ) and heat until the solution turns black, then switch to (65°C) and add 10ml of hydrogen peroxide solution dropwise (the mass fraction of hydrogen peroxide in the hydrogen peroxide solution is 27%) and heat until the solution turns from black to a colorless transparent solution, and continue heating until the solution has no bubbles produce. Afterwards, the solution was cooled to room temperature, transferred to a 100ml volumetric flask, and made up to the mark with ultrapure water to prepare a sample solution.

[0036] Prepare a blank solution: add 10 ml of concentrated sulfuric acid solution (the mass fraction of sulfuric acid in the sulfuric acid solution is 98.5%) to a Kjelda...

Embodiment 2

[0054] The only difference from Example 1 is that the volume ratio of the added concentrated sulfuric acid solution to the hydrogen peroxide solution is 1:0.5, and the solution becomes a light yellow transparent solution after the hydrogen peroxide solution is added dropwise.

[0055] Other experimental conditions are with embodiment 1, prepare blank solution and 3 parts of parallel sample solutions, measure the absorbance of iron, chromium, manganese and nickel element in blank solution and sample solution respectively by means of flame atomic absorption spectrometer, calculate this respectively according to linear fitting equation The content of iron, chromium, manganese and nickel element in 3 parts of sample solution, then according to formula C=(C i -C 0 )×V / 1000M to calculate the metal element content in the polycarbonate sample, and take the average value. The obtained values ​​are shown in Table 2.

[0056] Table 2

[0057] metal element

[0058] Relative...

Embodiment 3

[0060] The only difference from Example 1 is that the volume ratio of the added concentrated sulfuric acid solution to the hydrogen peroxide solution is 1:1.5, and the solution becomes a colorless and transparent solution after the hydrogen peroxide solution is added dropwise.

[0061] Other experimental conditions are with embodiment 1, prepare blank solution and 3 parts of parallel sample solutions, measure the absorbance of iron, chromium, manganese and nickel element in blank solution and sample solution respectively by means of flame atomic absorption spectrometer, calculate this respectively according to linear fitting equation The content of iron, chromium, manganese and nickel element in 3 parts of sample solution, then according to formula C=(C i -C 0 )×V / 1000M to calculate the metal element content in the polycarbonate sample, and take the average value. The obtained values ​​are shown in Table 3.

[0062] table 3

[0063] metal element

[0064] Relativ...

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Abstract

The invention discloses a method for measuring metal element content in polycarbonate. The method mainly comprises the following steps: (1) wet digestion treatment of a sample, namely adding a sulfuric acid solution to a polycarbonate sample to be detected, and then performing heating of the first stage, when the solution turns to black, performing heating of the second stage, and meanwhile, adding hydrogen peroxide solution, and after the solution turns to a colorless and transparent solution from black, continuing heating until no bubble is generated in the solution, and then cooling the solution to room temperature for later use; (2) preparation of a sample solution; (3) preparation of a blank solution; (4) preparation of a standard solution; (5) drawing of a standard curve; (6) measurement of the metal element content. The method has the advantages of simple operation, safety, speediness, good repeatability, high accuracy and the like, and is suitable for measuring metal elements in similar substances.

Description

technical field [0001] The invention relates to a method for measuring the content of metal elements in polycarbonate, in particular to a method for measuring the content of metal elements in polycarbonate by wet digestion-flame atomic absorption spectrometry. Background technique [0002] At present, the method for determining the content of metal elements in polycarbonate has spectrophotometry, which firstly adopts the method of carbonizing polycarbonate in a porcelain crucible on an electric heating plate, and then burning the carbonized residue in a muffle furnace. The sample was pretreated by dry ashing, and then the burning residue was dissolved with nitric acid, and the metal element content was measured with a 721 visible spectrophotometer. However, the pretreatment of polycarbonate by this method takes 4 hours, which is too long; during the dry ashing pretreatment, the metal elements are easily volatilized and dissipated due to the high temperature; the crucible may...

Claims

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Application Information

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IPC IPC(8): G01N21/72
Inventor 张金成张文陈运锋毕静利李娥
Owner LUXI CHEM GRP
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