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Mono-methyl halogenated diphenyl methane detection method

A monomethyl halide diphenyl, detection method technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problem of no corresponding test standards and related documents, etc., achieve small interference, accurate analysis method, quantitative results accurate effect

Active Publication Date: 2010-08-04
宁波市华测检测技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although the directive has restrictions on PCB, PCT, Ugilec 141, Ugilec 121 and DBBT, there are currently only standard methods for testing PCB and PCT at home and abroad, and there are no corresponding testing standards and related testing methods for Ugilec 141, Ugilec 121 and DBBT. literature

Method used

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  • Mono-methyl halogenated diphenyl methane detection method

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Using toluene as solvent, prepare monomethyltetrachlorodiphenylmethane (Ugilec 141) series standard solutions, carry out gas chromatography-mass spectrometry GC-MS analysis and detection according to the above experimental conditions, wherein the gas chromatography-mass spectrometry The inlet temperature was set at 260°C; the interface temperature was set at 260°C; helium was used as the carrier gas, and the flow rate was 1 ml / min; The temperature was raised to 200°C at a rate of 20°C / min, and then raised to 300°C at a rate of 10°C / min, and kept for 2 minutes; the ion source for mass spectrometry detection was an electron bombardment source (EI source), and the ion source bombardment energy was 70ev. The ion source temperature is 250°C; the injection volume is 1 microliter. Figure 1a It is the chromatogram of the monomethyltetrachlorodiphenylmethane (Ugilec 141) detected in Example 1 of the present invention, the ordinate in the chromatogram represents the intensity of ...

Embodiment 2

[0028] Accurately weigh 2 g (accurate to 0.1 g) of shredded plastic samples, place them in filter paper, wrap them carefully, place them in a Soxhlet extractor, add an appropriate amount of toluene into a round bottom flask, place them on a heater, and Install the Soxhlet extractor and condensing device, turn on the heat source, heat the solvent to reflux, and extract the sample for 4 hours. 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 toluene, take an appropriate amount, filter, and take the mother liquor for GC-MS testing. Three parallel samples were made on the plastic sample, the test numbers were A-1, A-2 and A-3 respectively, the analysis results are shown in Table 1, and the first parallel sample (test number A-1) was repeatedly measured 6 times , and the analysis results are shown in Table 2. Known from Table 1, the relative standar...

Embodiment 3

[0034]The standard solution in Example 1 was added to the plastic sample in Example 2, and the experiment was carried out according to the above-mentioned sample pretreatment method and instrumental analysis and detection method. Do four spiked levels to the sample, and perform 3 parallel measurements to get the average value for each sample with the spiked content, and calculate the spiked recovery rate of the sample according to the actual amount added and the measured results. The experimental results are shown in Table 3. It can be seen from Table 3 that the recovery rate of the samples was between 95% and 105%.

[0035] Table 3 The recovery of standard addition of this sample

[0036]

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Abstract

The invention relates to a detection method of mono-methyl halide diphenylmethane and includes the following steps: pre-treating the detected samples with a Soxhlet extraction method or a supersonic extraction method; detecting the mono-methyl halide diphenylmethane by adopting the gas chromatography-tandem mass spectrometry, setting the injection port temperature of the gas chromatograph-mass spectrometer of 180 to 300 DEG C, the flow rate of 0.5 to 2.0 ml per minute, selecting a non-polar or weak polar column as the chromatographic column and the interface temperature of 200 to 300 DEG C; the samples pre-treated enter the chromatographic column through a sample inlet of the gas chromatograph-tandem mass spectrometer for temperature programmed beginning from 40 to 120 DEG C to 250 to 320DEG C; isomers of the samples are separated from the chromatographic column. The method is characterized by cheap and secure detection instrument, accurate and fast analysis method, small interference, etc.

Description

【Technical field】 [0001] The invention relates to a detection method for monomethyl halide diphenylmethane, in particular to a method for detecting monomethyl halide diphenylmethane by means of gas chromatography-mass spectrometry technology. 【Background technique】 [0002] At present, the monomethylhalogenated diphenylmethane mentioned in the market mainly refers to monomethyltetrachlorodiphenylmethane (Ugilec 141), monomethyldichlorodiphenylmethane (Ugilec 121) restricted by EU directives and monomethyldibromodiphenylmethane (DBBT), both of which are revisions of EU Directive 76 / 769 / EEC 85 / 467 / EEC restricting polychlorinated biphenyls (PCBs) and polychlorinated terphenyls (PCTs) Finally, the compounds that appeared on the market in the 1980s were originally developed as substitutes for PCBs and PCTs, mainly used as dielectric fluids in capacitors and transformers, and used as hydraulic machine fluids in underground coal pit engineering. . [0003] Studies have found that...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 王鑫杨果刘蔷薇何树悠梁圆圆郭冰
Owner 宁波市华测检测技术有限公司
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