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Method for detecting haloalkylphosphate by liquid phase chromatograph

A halogenated alkyl phosphate ester and detection method technology, applied in instruments, measuring devices, scientific instruments, etc., can solve problems such as decomposition, achieve high recovery rate, simple pretreatment method, and less loss

Inactive Publication Date: 2008-11-26
CENT TESTING INT GRP CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The current method for detecting haloalkyl phosphates is mainly through gas chromatography-mass spectrometry (GC-MS). However, most of the haloalkyl phosphate flame retardants have high boiling points, and some may even decompose before reaching the boiling point. , For example, the boiling point of tris(2-chloroethyl) phosphate is as high as 300°C, and tris(2,3-dibromopropyl)phosphate decomposes at 200°C. These are gas chromatography-mass spectrometry (GC- MS) testing contraindicated

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  • Method for detecting haloalkylphosphate by liquid phase chromatograph
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  • Method for detecting haloalkylphosphate by liquid phase chromatograph

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Experimental program
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Effect test

Embodiment 1

[0028] Using acetonitrile as a solvent, a series of standard solutions of tris(2,3-dibromopropyl) phosphate were prepared, and analyzed and detected by high performance liquid chromatography and diode array detector coupled with HPLC-DAD according to the experimental conditions. figure 1 It is a chromatogram of tris(2,3-dibromopropyl)phosphate, and the retention time of the target is at 8.386 minutes. Concentration plotting with total target peak area, according to 3 parallel measurement results of standard solution, set up the standard curve of three (2,3-dibromopropyl) phosphate, as figure 2 Shown, the abscissa represents the concentration of three (2,3-dibromopropyl) phosphate standard solutions, and the ordinate represents the liquid chromatography peak area response value, and the functional relation of the gained standard curve is y=1.8396x+1.6445, wherein y represents the liquid chromatography peak area response value, x represents the concentration of three (2,3-dibro...

Embodiment 2

[0030] Accurately weigh 2g of shredded PVC sample, wrap it carefully, place it in a Soxhlet extractor, add an appropriate amount of acetonitrile into the round bottom flask, place it on the heater, arrange the Soxhlet extractor and condensing device, and turn on Heat source, the solvent was heated to reflux, and the sample was extracted for 7h. After the extraction, remove the condensing device and the Soxhlet extractor, concentrate the sample solution in the round bottom flask, and dilute it to a 25ml volumetric flask with acetonitrile, take 10ml, filter, and take the mother liquor for HPLC-DAD testing. Three parallel samples were made to the PVC sample, the test tube numbers were A-1, A-2 and A-3 respectively, the analysis results are shown in Table 1, and the first parallel sample (test tube number A-1) was measured 5 times , and the analysis results are shown in Table 2. Known from Table 1, the relative standard deviation of parallel samples is 2.68%. Known from Table 2,...

Embodiment 3

[0036] Add quantitative tris(2,3-dibromopropyl) phosphate standard solution into the PVC sample, and carry out the experiment according to the above-mentioned sample pretreatment method and instrumental analysis and detection method. Two spiked levels were made, and the average value was measured 3 times for each sample with the spiked amount. According to the actual added amount and the measured results, the spiked recoveries of various samples were calculated. The experimental results are shown in Table 3. It can be seen from Table 3 that the standard addition recovery rate of the sample is above 85%.

[0037] The recovery rate of standard addition of table 3 sample

[0038]

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Abstract

The invention relates to a detection method of halogenated alkyl phosphate and includes the following steps: samples are pre-treated with a Soxhlet extraction method or a supersonic extraction method; a high-performance liquid phase color spectrometer which connects diode array detectors is used for detecting the halogenated alkyl phosphate, and the proportions of the organic flow phases of the spectrometer are set from 50 to 100 percent, and the proportions of the inorganic flow phases are set from 0 to 50 percent, and the flow rates are set from 0.5 to 1.0ml per minute and the injection volume is set from 10 to 40ul and an anti-phase chromatographic column is selected as the chromatographic column; the samples pre-treated are brought into the chromatographic column by the flow phases of the high performance liquid phase color spectrometer, and the temperature of a column temperature box is set from 20 to 40 DEG C and components of the samples are separated from the chromatographic column; the components of the samples separated by the chromatographic column enter the diode array detectors to be detected. The detection method of the invention can prevent the samples from decomposing and is accurate and secure in analysis method.

Description

【Technical field】 [0001] The invention relates to a method for detecting halogenated alkyl phosphates, in particular to a method for detecting halogenated alkyl phosphates by using a high-performance liquid chromatography technology connected with a diode array detector. 【Background technique】 [0002] Halogenated alkyl phosphate is a kind of additive organic flame retardant widely used in polyurethane foam plastics and has remarkable effect. It has high thermal stability, high flame retardant efficiency, and has a certain plasticizing effect. Because its structure contains halogen and phosphorus elements at the same time, this kind of flame retardant works in the gas phase and condensation phase, and the flame retardant effect is very ideal. In addition, halogenated alkyl phosphates have low volatility, colorless, bromine-free, hydrolysis resistance, etc., and are widely used in plastics, synthetic rubber, synthetic fibers, wood, paper, coatings and other fields. Common ha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/89
Inventor 刘蔷薇杨果王鑫何树悠梁圆圆郭冰
Owner CENT TESTING INT GRP CO LTD
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