CN110824036A - Method for determining octabromo S ether in daily consumer product - Google Patents
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Abstract
The invention discloses a method for determining octabromoS ether in a daily consumable product, which comprises the following steps: sampling; pretreating and detecting the content of octabromoS ether in a pretreated target object, wherein the pretreatment step comprises the following steps: mixing a sample with a first extractant to form a first mixed solution, and performing ultrasonic treatment at a first specified temperature for a first specified time; mixing the first mixed solution with a second extractant to form a second mixed solution, and performing ultrasonic treatment at a second specified temperature for a second specified time. Various reagents are reduced, so that the method is more environment-friendly and healthier for human bodies; the detection limit is low, the method is simple to operate and strong in popularization, and the HPLC-DAD analyzer is easy to obtain and use by a testing instrument, and has high sensitivity and strong anti-interference capability.
Description
Technical Field
The invention relates to the field of detection, in particular to a method for determining octabromo S ether in a daily consumer product.
Background
Most of the light industrial materials such as plastics, rubber, fiber, etc. can be combustible. In particular, in order to apply the plastic to transportation, construction, electrical equipment, aviation, space flight and the like, the problem of combustion resistance is urgently needed to be solved. The addition of flame retardants in plastic articles is the best solution at present. Generally, organic flame retardant has good affinity, and in plastics, brominated flame retardant has absolute advantage in organic flame retardant systems, and although the brominated flame retardant is more "unquestionable" in terms of environmental protection, other flame retardant systems are difficult to replace. In recent years, the production and consumption situation of the flame retardant in China are both good, and the annual average consumption is kept at a speed of 15 percent and is continuously increased. With the strengthening of national requirements on flame-retardant technology and the establishment and perfection of various flame-retardant rules, the flame retardant in China will be developed and developed in a hot round.
The flame retardant scientific technology is developed for meeting the requirements of safe production and life of the society, preventing fire from happening and protecting lives and properties of people. The flame retardant is an application of a flame retardant technology in actual life, is a special chemical auxiliary agent for improving the combustion performance of combustible and combustible materials, and is widely applied to flame retardant processing of various decoration materials. Flame retardants have become an integral part of modern life. The fire retardant industry is a law-promoting industry, and related laws and regulations at home and abroad are successively released and gradually improved. The varieties and consumption of domestic flame retardants are mainly organic flame retardants, and although the most common halogen flame retardants have incomparable high efficiency compared with other flame retardant series, the harm to the environment and people is not negligible. The use of flame retardants must be limited, thereby prompting the detection of flame retardants. Although the use limit and the detection standard of the flame retardant have been provided by related standards in China, octabromoS-ether (octabromospiro-S) serving as a substitute product of the traditional octabromoS-ether flame retardant is originally disclosed in the flame retardant industry, but an effective detection means is lacked, and is not limited in the regulation, and the related mature detection standard is not provided for reference. Therefore, the research of the related detection method can more standardize the use of the octabromoS ether, avoid risks for social production and assist related industries to accelerate the solution of international admission processes.
Disclosure of Invention
The invention mainly aims to provide a method for determining octabromoS ether in a daily consumer product, so as to solve at least one technical problem pointed out in the background technology.
The invention provides a method for determining octabromo S ether in a daily consumer product, which comprises the following steps: sampling; pretreating and detecting the content of octabromoS ether in a pretreated target object, wherein the pretreatment step comprises the following steps:
mixing a sample with a first extractant to form a first mixed solution, and performing ultrasonic treatment at a first specified temperature for a first specified time;
mixing the first mixed solution with a second extractant to form a second mixed solution, and performing ultrasonic treatment at a second specified temperature for a second specified time.
Further, still include:
and filtering the second mixed solution after ultrasonic treatment to obtain filtrate.
Further, the step of detecting the content of octabromos ether in the pretreated target comprises:
the content of octabromoS ether in the pretreated sample solution was measured using an HPLC-DAD analyzer.
Further, the collection wavelength of the HPLC-DAD analyzer is 200nm-280nm, and the flow rate is 500 μ L/min.
Further, the step of detecting the content of octabromoS ether in the pretreated sample solution by using an HPLC-DAD analyzer comprises:
after the sample was placed in the HPLC-DAD analyzer, the ratio of mobile phase a to mobile phase B was maintained at 2: 8;
gradually changing the ratio of mobile phase A to mobile phase B to 1: 9;
gradually changing the ratio of mobile phase a to mobile phase B to 0 in 3-6 minutes: 10;
maintaining the ratio of mobile phase A to mobile phase B at 0: 10;
gradually changing the ratio of mobile phase a to mobile phase B to 2: 8;
maintaining the ratio of mobile phase A to mobile phase B at 2: 8.
further, the mobile phase a and the mobile phase B of the HPLC-DAD analyzer respectively comprise: water, methanol and a methanol-tetrahydrofuran mixture.
Further, the ratio of the sample to the first extractant is 0.45g to 0.55 g: 5mL, wherein the volume ratio of the first extractant to the second extractant is 1: 0.5-2.
Further, the first extractant and the second extractant are respectively one of acetonitrile, dichloromethane, trichloromethane, tetrachloromethane, dichloroethane, chloroethane, chloropropane, chlorobutane, methanol and tetrahydrofuran in volume ratio.
Further, the first specified temperature and the second specified temperature comprise 60 ℃ to 120 ℃.
Further, the first designated time and the second designated time comprise 20min to 50 min.
Compared with the prior art, the method for determining the octabromoS ether in the daily consumer product has the beneficial effects that: comprises the following steps: sampling; pretreating and detecting the content of octabromoS ether in a pretreated target object, wherein the pretreatment step comprises the following steps: mixing a sample with a first extractant to form a first mixed solution, and performing ultrasonic treatment at a first specified temperature for a first specified time; mixing the first mixed solution with a second extractant to form a second mixed solution, and performing ultrasonic treatment at a second specified temperature for a second specified time. Various reagents are reduced, so that the method is more environment-friendly and healthier for human bodies; the detection limit is low, the method is simple to operate and strong in popularization, and the HPLC-DAD (high performance liquid chromatography-diode array detector) analyzer is easy to obtain and use by a testing instrument, and is high in sensitivity and strong in anti-interference capability.
Drawings
FIG. 1 is a schematic flow chart of a method for determining octabromoS-ether in a consumable product according to one embodiment of the present invention;
FIG. 2 is a schematic representation of the linear dependence of octabromoS ether in the method of determination of octabromoS ether in a consumer product according to one embodiment of the present invention;
fig. 3 is a liquid chromatogram of a sample treatment solution in the method for measuring octabromos-ether in a consumable product for daily use according to an embodiment of the present invention.
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In addition, the descriptions related to "first", "second", etc. in the present invention are for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In addition, the technical solutions of the respective embodiments may be combined with each other, but must be realized by those skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.
Referring to fig. 1, in an embodiment of the present invention, the present invention provides a method for measuring octabromo S-ether in a consumer product for daily use, comprising: s1, sampling; s2, preprocessing and S3, detecting the content of octabromoS ether in the preprocessed target object,
wherein the pretreatment step comprises: s21, mixing the sample with a first extractant to form a first mixed solution, and carrying out ultrasonic treatment at a first specified temperature for a first specified time; s22, the first mixed solution and the second extractant are mixed to form a second mixed solution, and the ultrasonic treatment is performed at a second specified temperature for a second specified time.
As shown in step S1, the sampling is generally one of the important steps for extracting a small amount of target substance from the target substance for detection, and has one of the effective ways to obtain each item of data from the target substance for testing without affecting the main properties of the target substance, the extraction amount of the target substance is sufficient for 3-5 times of testing, the sampling process requires randomness for the selection process of the sampling area of the target substance, and subjective selection cannot be mixed in the selection process, in the embodiment of the present invention, the sampling weight is generally 0.4g-1g, and preferably 0.45, 0.5 or 0.55 g.
As shown in step S2, the pretreatment step is generally a step for the purpose of impurity removal and purification before performing an effective process on the target object, and in some special experiments, the pretreatment step also includes the purpose of changing material properties, and in the embodiment of the present invention, the pretreatment step is preferably the steps S21-S22.
As shown in step S3, detecting the content of octabromos ether in the pretreated target, generally performing a specified experiment or detection step on the target after steps S1-S2, and generally obtaining direct data or indirect data, wherein the direct data is data of the target value or result directly detected by the data; the indirect data is data of a target value or result obtained only after corresponding calculation, replacement or comparison, the detection result generally has a deviation value according to the deviation of detection equipment, environment, preprocessing steps and auxiliary products, and after the difference between the preprocessing step and the auxiliary products is used for formulating a detection standard, the error amplitude caused by the preprocessing step and the auxiliary products can be correspondingly and effectively avoided.
As described in step S21, a sample is mixed with a first extractant to form a first mixed solution, and ultrasonic treatment is performed at a first predetermined temperature for a first predetermined time, wherein the sample and the first extractant are mixed together to such an extent that the sample and the first extractant are in contact with each other in the same reactor during step S21, and the first mixed solution is subjected to ultrasonic extraction after the sample and the first extractant are mixed, wherein the ultrasonic extraction is performed by using an ultrasonic extractor, wherein the temperature in the reaction apparatus is maintained at the first predetermined temperature during the ultrasonic extraction, wherein the first predetermined temperature is generally 60 ℃ to 120 ℃, and in the present embodiment, preferably 60 ℃, 70 ℃ or 120 ℃, during the ultrasonic extraction, the ultrasonic frequency provided by the ultrasonic extractor is generally 20kHz-80kHz, the preferred ultrasonic frequency is 20kHz, 50kHz or 80kHz, the ultrasonic power is generally 100W-800W, the preferred ultrasonic power is 100W, 500W or 800W, and the duration of the ultrasonic extraction process is generally 20-50min, preferably 25min, 30min or 50min for the first designated time.
In the step S22, a first mixed solution and a second extractant are mixed to form a second mixed solution, and ultrasonic treatment is performed for a second specified time at a second specified temperature, in the step S22, the first mixed solution and the second extractant are mixed to a degree that the first mixed solution and the second extractant are sufficiently mixed in the same reactor, generally, after the second extractant is added, the liquid in the container needs to be shaken for a certain time, generally, the shaking time may be 5min, and after the first mixed solution and the second extractant are mixed, the second mixed solution is subjected to ultrasonic extraction, generally, an ultrasonic extractor is used for performing the ultrasonic extraction, wherein the temperature in the reactor is required to be kept within the second specified temperature during the ultrasonic extraction, wherein the second designated temperature is generally 60 ℃ to 120 ℃, in the embodiment of the present invention, preferably 60 ℃, 70 ℃ or 120 ℃, wherein in the ultrasonic extraction process, the ultrasonic frequency provided by the ultrasonic extractor is generally 20kHz to 80kHz, the preferred ultrasonic frequency is 20kHz, 50kHz or 80kHz, the ultrasonic power is generally 100W to 800W, the preferred ultrasonic power is 100W, 500W or 800W, and the second designated time for the ultrasonic extraction process is generally 20min to 50min, preferably 25min, 30min or 50 min.
In this embodiment, the method for measuring octabromo S ether in a consumer product for daily use further comprises:
s23, filtering the second mixed solution after ultrasonic treatment to obtain filtrate.
And in step S23, filtering the second mixed solution after the ultrasonic treatment to obtain a filtrate, and filtering out sample residues in the second mixed solution to prevent solid particles remaining in the liquid phase from affecting the test and causing errors.
In this embodiment, the step of detecting the content of octabromos ether in the pretreated target includes:
and S31, detecting the content of the octabromoS ether in the pretreated sample solution by using an HPLC-DAD analyzer.
Detecting the content of the octabromoS ether in the pretreated sample solution by using an HPLC-DAD analyzer as described in the step S31, wherein the collection wavelength of the HPLC-DAD analyzer is 200nm-280nm, and the flow rate is 500 muL/min; after the sample was placed in the HPLC-DAD analyzer, the ratio of mobile phase a to mobile phase B was maintained at 2: 8; gradually changing the ratio of mobile phase A to mobile phase B to 1: 9; gradually changing the ratio of mobile phase a to mobile phase B to 0 in 3-6 minutes: 10; maintaining the ratio of mobile phase A to mobile phase B at 0: 10; gradually changing the ratio of mobile phase a to mobile phase B to 2: 8; maintaining the ratio of mobile phase A to mobile phase B at 2: 8; the mobile phase A and the mobile phase B of the HPLC-DAD analyzer respectively comprise: water, methanol and a methanol-tetrahydrofuran mixture.
In this embodiment, in the method for determining octabromo S ether in consumer goods, the ratio of the sample to the first extractant is 0.45g to 0.55 g: 5mL, preferably 0.45 g: 5mL, 0.5 g: 5mL or 0.55 g: 5mL, wherein the volume ratio of the first extractant to the second extractant is 1: 0.5-2, preferably 1: 1.
in this embodiment, in the method for measuring octabromos-ether in a consumer product, the first extractant and the second extractant are respectively one of acetonitrile, dichloromethane, trichloromethane, tetrachloromethane, dichloroethane, chloroethane, chloropropane, chlorobutane, methanol and tetrahydrofuran, wherein the first extractant is preferably tetrahydrofuran, and the second extractant is preferably acetonitrile.
In this embodiment, the first specified temperature and the second specified temperature include 60 ℃ to 120 ℃, and in the embodiment of the present invention, 60 ℃, 70 ℃ or 120 ℃ is preferred.
In this embodiment, in the method for measuring octabromos-ether in a consumer good for daily use, the first specified time and the second specified time include 20min to 50min, preferably 30 min.
Referring to FIGS. 2-3, in one embodiment, 0.5g of a homogeneous sample (sample types include: plastic, leather, textile) is weighed into a 50mL tube, 5mL tetrahydrofuran is added, ultrasonic extraction is performed at a constant temperature of 70 ℃ for 30 minutes, then 5mL acetonitrile is added, shaking is performed, ultrasonic extraction is performed again at a constant temperature of 70 ℃ for 30 minutes, filtration is performed, and qualitative and quantitative analysis is performed by using a high performance liquid chromatography combined diode array detector, wherein the analysis conditions of the instrument are as follows:
the instrument comprises the following steps: a high performance liquid chromatography-diode array detector;
column: c18(3.0 mm. times.3.5 μm. times.150 mm)
Collecting wavelength: 240nm
Sample introduction amount: 5 μ L
Gradient of the sample: (A is pure water, B is methanol)
| Time (min) | Flow rate (μ L/min) | A(％) | D(％) |
| 0 | 500 | 20 | 80 |
| 3 | 500 | 10 | 90 |
| 6 | 500 | 0 | 100 |
| 18 | 500 | 0 | 100 |
| 20 | 500 | 20 | 80 |
| 28 | 500 | 20 | 80 |
Standard recovery (%):
| material of | Plastic cement | Leather | Textile fabric |
| OBBPS recovery | 90.0 | 85.7 | 91.7 |
1. The linear range is (mg/L, solution concentration): 0.5; 1.0; 2.0; 5.0; 10
2. Minimum detection limit: 10mg/kg
3. The target substance includes: octabromo S-ether (octabromobishenol-S) CAS: 42757-55-1 abbreviation: OBBPS
4. The linear dependence of octabromos ether is graphically shown in figure 2.
Compared with the prior art, the method for determining the octabromoS ether in the daily consumer product has the beneficial effects that: comprises the following steps: sampling; pretreating and detecting the content of octabromoS ether in a pretreated target object, wherein the pretreatment step comprises the following steps: mixing a sample with a first extractant to form a first mixed solution, and performing ultrasonic treatment at a first specified temperature for a first specified time; mixing the first mixed solution with a second extractant to form a second mixed solution, and performing ultrasonic treatment at a second specified temperature for a second specified time. Various reagents are reduced, so that the method is more environment-friendly and healthier for human bodies; the detection limit is low, the method is simple to operate and strong in popularization, and the HPLC-DAD (high performance liquid chromatography-diode array detector) analyzer is easy to obtain and use by a testing instrument, and is high in sensitivity and strong in anti-interference capability.
The above description is only a preferred embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by using the contents of the present specification and the accompanying drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (10)
1. A method for determining octabromo S ether in a daily consumer product comprises the following steps: sampling; pretreating and detecting the content of octabromoS ether in a pretreated target object, wherein the pretreatment step comprises the following steps:
mixing a sample with a first extractant to form a first mixed solution, and performing ultrasonic treatment at a first specified temperature for a first specified time;
mixing the first mixed solution with a second extractant to form a second mixed solution, and performing ultrasonic treatment at a second specified temperature for a second specified time.
2. The method of claim 1, further comprising:
and filtering the second mixed solution after ultrasonic treatment to obtain filtrate.
3. The method of claim 1, wherein the step of detecting the octabromos-ether content of the pretreated target comprises:
the content of octabromoS ether in the pretreated sample solution was measured using an HPLC-DAD analyzer.
4. The method of claim 3, wherein the HPLC-DAD analyzer has a collection wavelength of 200nm to 280nm and a flow rate of 500 μ L/min.
5. The method of claim 4, wherein the step of detecting the octabromos-ether content of the pre-treated sample solution using an HPLC-DAD analyzer comprises:
after the sample was placed in the HPLC-DAD analyzer, the ratio of mobile phase a to mobile phase B was maintained at 2: 8;
gradually changing the ratio of mobile phase A to mobile phase B to 1: 9;
gradually changing the ratio of mobile phase a to mobile phase B to 0 in 3-6 minutes: 10;
maintaining the ratio of mobile phase A to mobile phase B at 0: 10;
gradually changing the ratio of mobile phase a to mobile phase B to 2: 8;
maintaining the ratio of mobile phase A to mobile phase B at 2: 8.
6. the method of claim 5, wherein mobile phase a and mobile phase B of the HPLC-DAD analyzer respectively comprise: water, methanol and a methanol-tetrahydrofuran mixture.
7. The method of claim 1, wherein the ratio of the sample to the first extractant is from 0.45g to 0.55 g: 5mL, wherein the volume ratio of the first extractant to the second extractant is 1: 0.5-2.
8. The method of any one of claims 1-7, wherein the first and second extractants are each one of acetonitrile, dichloromethane, trichloromethane, tetrachloromethane, dichloroethane, chloroethane, chloropropane, chlorobutane, methanol, and tetrahydrofuran.
9. The method of any one of claims 1-7, wherein the first specified temperature and the second specified temperature comprise 60 ℃ -120 ℃.
10. The method of any of claims 1-7, wherein the first specified time and the second specified time comprise 20min to 50 min.
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| CN114414708A (en) * | 2021-12-16 | 2022-04-29 | 深圳天祥质量技术服务有限公司 | Method for detecting tetraethylene glycol dimethyl ether |
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| CN114113410A (en) * | 2021-12-15 | 2022-03-01 | 深圳天祥质量技术服务有限公司 | Method for detecting tribromoneopentanol and 2, 3-dibromopropanol |
| CN114113410B (en) * | 2021-12-15 | 2024-01-23 | 深圳天祥质量技术服务有限公司 | Method for detecting tribromoneopentyl alcohol and 2, 3-dibromopropanol |
| CN114414708A (en) * | 2021-12-16 | 2022-04-29 | 深圳天祥质量技术服务有限公司 | Method for detecting tetraethylene glycol dimethyl ether |
| CN114414708B (en) * | 2021-12-16 | 2024-01-23 | 深圳天祥质量技术服务有限公司 | Method for detecting tetraethylene glycol dimethyl ether |
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