Changzhou Quarantine Bureau Develops APEO Technology To Provide Green Textile New Technology Path

< p > 2003/371/EC is a new standard stipulated in the EU regulation < a target= "_blank" href= "//www.sjfzxm.com/" > textile > /a > product ecological label (Eco-Label). It prohibits 7 kinds of surfactants including APEO, and the waste water which is made from them.

Jiangsu Changzhou inspection and Quarantine Bureau adopted the advanced technology of HPLC, hydrophilic interaction chromatography, and applied it in the field of inspection and quarantine. A new method of APEO detection was successfully developed, providing a new technology path < a href= "http:// www.sjfzxm.com/news/index_c.asp" > Green Textile < /a >.

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< p > < strong > small amount of hazards is huge, < /strong > /p >

< p > alkylphenol polyoxyethylene ether is an important nonionic surfactant. Among them, nonylphenol polyoxyethylene ether (NPEO) is the most abundant, accounting for more than 80%, followed by octyl phenol polyoxyethylene ether (OPEO), accounting for more than 15%, twelve alkyl polyoxyethylene ether (DPEO) and two nonylphenol polyoxyethylene ether (DNPEO) account for about 1%.

Alkylphenol polyoxyethylene ether has good wetting, permeating, emulsifying, dispersing, solubilizing and washing effects. It is widely used in many industries, especially in detergent industry, followed by textile auxiliaries.

In order to improve the penetration of enzyme products into fiber, there is also a certain amount of APEO in enzyme products.

For the same reason, APEO is often used in dyeing and printing process recipes.

It is not difficult to see that APEO is widely used in the textile industry.

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< p > the biodegradability of alkylphenol polyoxyethylene ether (APEO) has always been a concern.

In many parts of the United States, the removal rates and residues of APEO have been measured. The biodegradability of APEO is generally over 90%, up to 92.5% to 99.8%.

OP, NP, NP1EO and NP2EO produced in the process of biodegradation are recognized as environmental hormone chemicals, which can damage the normal secretion of human hormones. It can lead to the reduction of sperm count, abnormal reproductive organs, and the decline of the reproductive capacity of organisms.

In view of this, there have been regulations on prohibition or restriction of APEOs since 1980s, and the most effective law is the 2003/53/EC regulation of the European Union.

The regulations stipulate that since January 17, 2005, the use of APEO has been strictly restricted except for specific situations, such as adhesives used for pigment printing. For those who enter the EU countries, < a href= "//www.sjfzxm.com/news/" > textile > /a > and a target= "_blank" href= "//www.sjfzxm.com/" > clothing < /a > all require effective proof of the test of the //www.sjfzxm.com/, and stipulate that the allowable limit of "0.1%" for textiles and "clothing" shall be limited.

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< p > < strong > in-depth research and development ideas < /strong > /p >

< p > at present, there is no international standard related to APEOs detection in < a href= "//www.sjfzxm.com/news/" > textile > /a >.

China's national standards for textile APEOs detection methods are: GB/T23322-2009 "textile surfactant determination - alkylphenol polyoxyethylene ether".

China's entry exit inspection and quarantine industry standard has three methods for the detection of APEOs in textiles, namely: SN/T 1850.1-2006. Determination of alkylphenol and alkylphenol polyoxyethylene ether in textiles. First parts: high performance liquid chromatography, SN/T1850.2-2006 "determination of alkylphenol and alkylphenol polyoxyethylene ether in textiles. Second part: high performance liquid chromatography-mass spectrometry" and SN/T1850.1-2010 < < a href= > //www.sjfzxm.com > > textile > /a > Product Determination of alkylphenol and alkylphenol polyoxyethylene ether third part: normal phase high performance liquid chromatography and liquid chromatography tandem mass spectrometry.

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< p > these methods use Soxhlet extraction to put APEOs in textiles, then separate them by high performance liquid chromatography, and then conduct qualitative and quantitative analysis by fluorescence detector or mass spectrometric detector. The difference between various methods is mainly due to different chromatographic separation techniques.

Among them, the C18 liquid chromatography (RPLC) separation technology is the most widely used.

The separation of APEOs by reversed-phase chromatography is simple. The mobile phase is usually water, methanol or water, methanol and acetonitrile. OPEOs and NPEOs, OP and NPs all get stable baseline separation. The fluorescence detector has high sensitivity and accurate quantitative results.

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< p > but because of the different polarity and retention time of OPEOs or NPEOs with different degrees of polymerization, this method does not provide accurate qualitative results.

Because the mobile phase used by RPLC matches perfectly with the ESI ionization source, LC-MS or LC-MS/MS methods are commonly used in qualitative and quantitative analysis of APs and APEOs, GB/T 23322, SN/T 1850.2-2006 and SN/T 1850.3-2010 are all expressed.

But because APEOs is a mixture of oligomers with different degree of polymerization, the long chain APEOs containing more oxygen and ethylene groups is easier to ionize, and the short chain APEOs has ion inhibition. These effects are unknown and unstable, resulting in a large deviation in the actual detection results, and a variety of adducted ions are generated in the electrical ionization of APEOs, including hydrogenation, ammonium, sodium and potassium ions, and the proportion of various ions is not one of the uncertainty of the selection of ion quantitative analysis.

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< p > therefore, the normal phase liquid chromatography (NPLC) method is usually used as a supplement to RPLC, and APEOs is used for qualitative analysis.

In the standard NPLC method, n-hexane, isopropanol and water were used as mobile phase to separate APEOs with different polymerization degree.

Due to the large proportion of hydrophobic n-hexane used in the mobile phase, the HPLC system must carry out adequate cleaning between NPLC and RPLC, which will cost a lot of manpower and material resources.

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< p > aiming at various problems in APEOs detection, the comprehensive technology service center of Jiangsu Changzhou inspection and quarantine bureau adopts HPLC advanced technology, HILIC, to study its retention mechanism and apply it successfully to qualitative analysis of APEOs.

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< p > HILIC is a new type of chromatography technology which combines RPLC, NPLC and ion chromatography (IC) three. It uses the same mobile phase as RPLC and carries out the analysis of the same retention mechanism with NPLC. At the same time, bonding different stationary phases can also make IC have the ability to separate.

In order to realize the application of HILIC in the field of inspection and quarantine, a large number of theoretical studies and scientific experiments were carried out in the laboratory, and the mechanism of separation was explored and studied.

On the basis of theoretical research, the laboratory carried out experiments on HILIC separation of APEOs compounds with different degrees of polymerization.

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< p > the newly developed method in the laboratory adopts HILIC chromatographic column, acetonitrile and water as mobile phase, separating APEOs mixture into oligomer with single polymerization degree.

The whole analysis process takes only 10 minutes. The mobile phase matches the RPLC completely, which eliminates the complicated process of cleaning the HPLC system in the qualitative process of NPLC. The separation effect is the same as that of NPLC, which adds the confirmation of qualitative analysis for RPLC quantitative detection.

When the method is put into use, it ensures the accuracy of the test results, greatly shortens the detection time and saves a lot of manpower and material resources.

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< p > this research achievement has been attached great importance to by Cao Xizhong, deputy director of the Jiangsu industrial inspection and Quarantine Bureau. He has included this method in the < < a href= > //www.sjfzxm.com/news/ > > the international wool textile < /a > inspection standard (Determination of alkylphenols and alkylphenol and) (in the detection of wool and zinc), which provides technical guidance and standard service for the detection of the global and the wool.

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< p > can achieve technological breakthroughs in two aspects of basic theory and practical application. It embodies the research concept of integrating theory with practice, learning for practical purposes, and learning to use each other for a long time. At the same time, it also shows that a laboratory technician can continuously seek innovation and pursue breakthroughs in practical work, promote theoretical innovation on the basis of work, and further promote the progress of work with the theory as the cornerstone.

The head of the Changzhou Bureau said that it will continue to increase investment in scientific research, do well in scientific research projects, build up science and technology and strengthen science and technology inspection and Quarantine on the basis of scientific research capability and continuous output of scientific and technological achievements.

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