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Method for determining tris (2,3-dibromopropyl) phosphate content of water

A technology of dibromopropyl and determination method, which is applied in the field of determination of phosphate triester content in water, can solve the problems of unsuitability of gas chromatography, difficulty in guaranteeing stability, inaccuracy of flame photometry, etc., and achieves accurate and credible results. The effect of improving instrument analysis rate and shortening instrument analysis time

Active Publication Date: 2013-02-27
NANJING UNIV
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  • Summary
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AI Technical Summary

Problems solved by technology

Due to the high boiling point of tris(2,3-dibromopropyl) phosphate, it is difficult to volatilize, and its stability is difficult to guarantee under high temperature conditions, so gas chromatography is not suitable, and the flame photometry is not accurate enough, and there are false positives. positive question
In addition, the long analysis time is also an important disadvantage of gas chromatography

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Adopt the assay method and condition in the technical scheme:

[0023] 1. Preparation of the standard curve sample: the standard sample of tris(2,3-dibromopropyl) phosphate was prepared with methanol into a standard sample stock solution with a concentration of 1mg / L, and the stock solution was used to prepare a gradient of 1-500ng / L L mixed standard liquid;

[0024] concentration area Relative error 1 2.34 -12.65% 2 4.95 -10.75% 5 12.22 -13.50% 10 29.22 2.63% 20 67.25 17.72% 50 139.38 -2.53% 100 281.55 -1.62% 200 575.38 0.50% 500 1475.50 3.07%

[0025] The obtained standard curve is: y = 2.8634x + 0.1611, the correlation coefficient R2 = 0.9995, the relative error of each concentration is less than 20%, and the linear range is wide. The resulting instrumental detection limit (defined as three times the signal-to-noise ratio) was 0.195 ug / L and the instrumental limit of quantitation was 1 ug / L.

Embodiment 2

[0027] 1. Take 6 parts of 1L tap water, add 50 μL of the standard sample of tris(2,3-dibromopropyl)phosphate with a concentration of 1 mg / L to 3 parts respectively, and then prepare tris(2,3-dibromopropyl)phosphate with a concentration of 50 ng / L (2,3-Dibromopropyl) ester tap water sample.

[0028] 2. Sample treatment: Carry out solid phase extraction with a pre-activated C18 cartridge at a flow rate of about 5 mL / min. During the whole process, pay attention to ensure that the cartridge is moist. After the water sample passes through, dry the SPE cartridge; after drying Elution was carried out according to the method in the summary of the invention. The two eluents were collected in the same collection bottle, and the volume of the eluent was reduced to below 1 mL by a rotary evaporator. After cleaning and transfer, blow slowly to nearly dry with high-purity nitrogen. The solvent was replaced with methanol, and the final volume was adjusted to 0.5 mL, transferred to a sample i...

Embodiment 3

[0031] 1. Take 6 parts of 1L mineral water, add 50 μL of the standard sample of tris(2,3-dibromopropyl) phosphate with a concentration of 1 mg / L to 3 parts respectively, and then make phosphoric acid with a concentration of 50 ng / L Tris(2,3-dibromopropyl) ester mineral water sample.

[0032] 2. Sample processing was carried out as in Example 1, and three blank samples were not detected, and the recoveries of the other three samples were all above 80%.

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Abstract

The invention provides a method for determining tris (2, 3-dibromopropyl) phosphate content of water, and belongs to the field of organic phosphate flame retardant. The method mainly comprises the following steps: (1) conducting solid-phase extraction on a sample; (2) eluting and collecting the extraction column; (3) concentrating the eluent obtained in the step (2) to a constant volume; and (4) determining the concentrated liquid with a high-performance liquid chromatograph-triple quadrupole mass spectrometer. The method provided by the invention improves determination method of tris (2,3-dibromopropyl) phosphate in water environment; and through ultra performance liquid chromatograph-triple quadrupole mass spectrometry combination, the method for detecting tris (2,3-dibromopropyl) phosphate method has more advantages than other methods. The present invention using ultra performance liquid chromatograph has larger separation speed than gas chromatograph and general high performance liquid chromatograp; triple quadrupole mass spectrometry for SRM scanning realizes higher selectivity, more accurate qualitative diagnosis, and improved sensitivity. Therefore, the method provided by the invention has obvious advantages compared with other gas-phase method and liquid mass chromatography method.

Description

technical field [0001] The invention belongs to the detection field of organic phosphate flame retardants, and in particular relates to a method for measuring the content of tris(2,3-dibromopropyl) phosphate in water. Background technique [0002] Tris (2,3-dibromopropyl) phosphate (tris (2,3-dibromopropyl) phosphate), referred to as TDBPP, is an excellent additive organic phosphate flame retardant, adding bromine to the organic phosphate, There is a good synergistic effect between the two, and it can play a flame-retardant role in the gas phase and the condensed phase respectively, and the flame-retardant effect is good. At present, it has been widely used in cellulose acetate, nitrocellulose, phenolic resin, polyvinyl chloride, Polyacrylate, polyurethane, etc., and the substance can also be used as a flame-retardant plasticizer. TDBPP is a light yellow transparent viscous liquid, relatively stable in water and not easy to degrade. This, combined with the fact that the su...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 韦斯李俊于红霞史薇于南洋李梅映胡梦阳
Owner NANJING UNIV
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