Determination Of The Content Of Ortho Phenyl Phenol In Textiles By Standard Curve Method

< p > ortho phenyl phenol (OPP) is mainly used for bactericides of < a href= "http://www.91se91.com/news/index_c.asp" > fiber > /a > a href= "http://www.91se91.com/news/index_c.asp" > Leather > /a > wood, fruits and vegetables. As textile auxiliaries, it can be used as dyeing carrier for polyester fibers and increase dyeing ability of polyester fibers.

OPP has certain biological toxicity, and OPP in textile and clothing will cause some harm to human health. Therefore, OPP is an important monitoring item [1] for textile ecological performance. For this reason, the state issued the national standard of GB/T 20386 - 2006 "determination of adjacent phenylene phenol in textiles".

In this standard, there are two methods for the extraction of O - phenyl phenol, one is direct extraction, that is, after extraction by methanol, after spin concentration, the content of O - phenyl phenol is determined directly by acetone constant volume. The second is acetylation after methanol extraction, followed by spin evaporation, and finally the content of O - phenyl phenol is determined by [2].

The first test process is simple and easy to operate, but the recovery rate is low. The tedious acetylation process in the second test processes is not easy to control, and it is easy to cause acetylation.

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< p > in view of the shortcomings of the two test methods, the gradient concentration method is used to make a blank addition curve for the standard product of ortho phenyl phenol, so as to accurately quantify the < a href= "http://www.91se91.com/news/index_c.asp" > ortho phenyl phenol < /a > content in textiles.

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< p > < strong > 1 reagent and instrument < /strong > < /p >

< p > 1.1 reagent < /p >

< p > the reagents used in the experiment are analytically pure, methanol, acetone, hexane, acetic anhydride, anhydrous potassium carbonate, anhydrous sodium sulfate (burning at 4H at 650 degrees C, stored in desiccator after cooling), 0.1mol/L potassium carbonate solution, 20g/L sodium sulfate solution, and ortho phenyl phenol standard (purity > 98%).

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< p > 1.2 instruments and test parameters < /p >

< p > TRACE ISQ, ultrasonic generator (40kHz), centrifuge (4000 R / m i n), rotary evaporator < /p >

< p > instrument [can control temperature at (40 + 2) C], anhydrous sodium sulfate column, 100mL plug cone bottle.

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< p > 1.3 chromatographic condition < /p >

< p > 1.4, sample < /p >

< p > Sample#12162 and Sample#12163 are all cotton knitwear, provided by Holland IIS international laboratory.

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< p > < strong > 2 test method < /strong > < /p >

< p > 2.1 direct extraction method < /p >

< p > the standard product of ortho phenyl phenol with a concentration of 20 1mL g/mL was placed in 100mL plug cone bottle [3], added 50mL methanol, and 20min was extracted from ultrasonic generator.

The extraction solution was filtered, the residue was extracted by 30mL methanol, and the 5min was extracted by ultrasonic. After being dehydrated by anhydrous sodium sulfate column, the residue was collected in a 100mL concentrated bottle. The water evaporator was evaporated at 40 degrees, concentrated near dry, dissolved in acetone and fixed to 5.0mL, and the content of phenylephenol in the sample was tested by gas chromatography-mass spectrometry TRACE ISQ.

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< p > 2.2 acetylation method < /p >

< p > the standard product of ortho phenyl phenol with a concentration of 20 1mL g/mL was placed in a 100mL plug cone bottle. The extraction process was concentrated near dry with the direct extraction method, filtrate 40 degree water bath evaporator, and then dissolved in 8mL potassium carbonate solution and pferred to the 15mL centrifuge tube.

Add 1mL acetic anhydride, shake 2min, add 5.0mL hexane accurately, shake 2min and centrifuge 3min by 4000r/min.

The lower water phase is extracted by a sharp nozzle.

Add 10mL sodium sulfate solution, shake 1min, centrifuge 4000r/min and 3min.

The content of N-phenyl phenol in the sample solution was determined by gas chromatography mass spectrometry TRACE ISQ.

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< p > 2.3 standard curve method < /p >

< p > the standard solution of concentration of 100 phenylene phenol was diluted to 20 g/mL g/L and 50 g/L standard solution by acetone.

The standard solution 1mL of 20 mu g/mL, 50 g/mL and 100 g/mL g/mL was used for blank label test. The test method was carried out according to the direct extraction method.

The three points of 20 axis g/mL, 50 g/mL and 100 g/mL g/mL were selected as the X axis. The standard curve was obtained from the three points of the Y axis corresponding to the peak area of the corresponding blank addition test, and the concentration equation y = 227134.7837x + 995303.5918 was obtained.

The standard curve is shown in Figure 1.

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The R value of < p > standard curve is 0.9998 or 0.995, which is close to 1. The standard curve is ideal [5], which can be used for concentration calculation. 2

The R value is close to 1, indicating that the recovery rate of ortho phenyl phenol is stable during the test. This test method is feasible.

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< p > < --EndFragment-- > strong > 3 results and analysis < /strong > /p >

< p > 3.1 recovery rate < /p >

< p > the quantitative reference material was added to the blank sample matrix without the substance being tested. According to the sample processing steps, the ratio of the obtained result to the theoretical value was the blank plus standard recovery rate of [4].

In the direct extraction method, the peak area of the standard product of 20 - g/mL - O - phenyl phenol is 79785381, the standard area of 20 - g/mL - ortho phenyl phenol is 5452311, the blank recovery rate of the direct extraction method is 34.17%, and the recovery rate of the blank standard addition is low, which can not meet the test requirements.

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< p > standard curve method, the peak area of the sample is substituted into the concentration equation, and the concentration is calculated.

In this experiment, the concentration of the standard area is taken as reference. The concentration obtained from the concentration equation is the true concentration of the sample, and the recovery rate is not needed to avoid the problem of low standard recovery rate.

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< p > 3.2 acetylation degree < /p >

< p > the spectrum of direct extraction and acetylation is shown in Figure 2 (a) and (b).

Two there is a peak of 9.28min at the retention time of B, but there is also a peak of 9.97min at the retention time, which indicates that the acetylation process is incomplete.

Acetylation does not completely cause the peak of two ortho phenyl phenol, and it can not calculate the recovery rate of ortho phenyl phenol blank, nor can it accurately quantify the content of ortho phenyl phenol in the sample.

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< p > the standard curve method is the same as the direct extraction method. The operation process is simple and quick, avoiding the complicated and complicated acetylation process, and there is no problem of acetylation incomplete.

The standard curve method combines the advantages of direct extraction and simple and quick operation. Its C shows the peak area of o-phenyl phenol simply and intuitively, and is convenient for the analysis and calculation of the results.

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< p > 3.3 accuracy comparison < /p >

< p > Sample#12162 and Sample#12163 are the test samples uniformly distributed by the Holland IIS international laboratory proficiency testing institution. The laboratory tests the uniformity of the samples, and the peak area of the ortho phenyl phenol is calculated by external standard method in the direct extraction method of GB/T 20386 - 2006.

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The relative deviation of the concentration of Sample#12162 and Sample#12163 ortho phenyl phenol measured by the direct extraction method and the concentration measured in Holland IIS international laboratory is greater than 30%, which does not meet the test requirements. The relative deviation between the concentration of ortho phenyl phenol measured by the standard curve method and the concentration measured in Holland IIS international laboratory is less than 3%, so the standard curve method can be used to test the accuracy of the content of ortho phenyl phenol in cotton textiles.

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< p > < strong > 4 Conclusion < /strong > < /p >

< p > this paper summarizes the shortcomings of the two extraction methods of direct extraction and acetylation in GB/T 20386 - 2006, and proposes that the standard curve R value of ortho phenol phenol standard should be close to 1, indicating that the recovery rate of ortho phenol is stable. The standard curve can be used in the experiment. The content of ortho phenyl phenol in the samples is tested by the direct extraction method and the standard curve method. The relative deviation between the direct extraction method and the results of the IIS International Laboratory in Holland is more than 30%, and the test results are not accurate. The relative deviation of the standard curve method and that of Holland IIS international laboratory is less than 3%, and the test results are accurate and reliable.

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< p > standard curve method combines the advantages of the direct extraction method, avoids the shortcomings of acetylation method, and accurately determines the content of the adjacent phenyl phenol in the sample, which makes the detection of the sample more accurate and simple, and is a scientific and reliable test method.

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