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Decabromodiphenyl Oxide CAS 1163-19-5

Molecular Formula: C12Br10O

Formula Weight: 959.17

ZSpharmac: Decabromodiphenyl Oxide Supplement

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Product Name: Decabromodiphenyl Oxide
CAS No: 1163-19-5
Purity: 99%

Basic Info

Product Name:Decabromodiphenyl Oxide
Other Names:Decabromodiphenyl Ether, 99%
CAS:1163-19-5
Place of Origin:Shandong, China
Brand Name:ZSpharmac
Type:Organic Chemical Raw Materials
Appearance:White Powder
EINECS No.:214-604-9
Storage:2-8°C
Provide:Decabromodiphenyl Oxide MSDS;
Decabromodiphenyl Oxide COA

Decabromodiphenyl Oxide Background Technology

Plastic materials in electrical and electronic products need to be added with flame retardants due to their special requirements for fire resistance.In 2006, the global demand for Decabromodiphenyl Oxide was 56,000 tons, of which more than 7,500 tons were imported by EU countries. An important reason for the current huge demand for Decabromodiphenyl Oxide is that Decabromodiphenyl Oxide is safer for the environment than its less brominated counterparts. On July 1, 2006, the European Union has begun to ban the use of polybrominated diphenyl ethers other than Decabromodiphenyl Oxide as plastic additives.

The research on the bioaccumulation properties and photoreactive activity of Decabromodiphenyl Oxide has triggered a big discussion on the potential risks of using Decabromodiphenyl Oxide. Techniques for the rapid detection of Decabromodiphenyl Oxide content in plastics are needed. Several authoritative laboratories around the world have participated in the evaluation of detection methods for PBDEs (all congeners including Decabromodiphenyl Oxide), and the results show that the quantitative analysis of Decabromodiphenyl Oxide is very difficult. For this reason, in recent years, many analytical methods for Decabromodiphenyl Oxide have been developed, including three steps of pre-separation, extraction and detection. In these three steps, the detection process determines the way and method of pre-separation and extraction, so the detection technology of Decabromodiphenyl Oxide is the key to the whole analysis process. Current detection techniques can generally be divided into two categories: gas chromatography and liquid chromatography. Gas chromatography is a recommended method by the U.S. Environmental Protection Agency (EPA method 1614) and is considered the standard analytical method for polybrominated diphenyl ethers. However, this method evolved from the trace analysis of PCB-based persistent organic pollutants, but the high molecular weight and boiling point of Decabromodiphenyl Oxide require higher processing temperatures. Therefore, the application of gas chromatography to detect Decabromodiphenyl Oxide requires heating the sample to 320 degrees Celsius in the chromatographic column. However, the decomposition temperature of Decabromodiphenyl Oxide is only 300 degrees Celsius (in some cases, decomposition occurs when it exceeds 200 degrees Celsius), so the possible decomposition loss during the analysis process makes the application of gas chromatography controversial; The shortcomings of gas chromatography have attracted much attention. my country’s Quality and Inspection and Quarantine Bureau also recommends the use of liquid chromatography as the standard method for PBDEs (SN/T2005.1-2005).

The main process of existing liquid chromatography is to adopt high performance liquid chromatography (HPLC) to analyze and detect after first solvent extraction. Because Decabromodiphenyl Oxide is dispersed in plastic solids, Soxhlet extraction is traditionally used to extract Decabromodiphenyl Oxide from plastic solids, but due to the unsatisfactory extraction effect, supercritical fluid extraction, Methods such as pressure extraction, ultrasonic-assisted extraction and microwave-assisted extraction. The extracted Decabromodiphenyl Oxide can be analyzed and detected by conventional HPLC conditions. For example, in the recommended standard SN/T 2005.1-2005, C18 bonded phase is used as stationary phase, methanol and phosphate buffer solution are used as mobile phase, After gradient elution, UV light with a wavelength of 226 nm was used for detection.

The biggest disadvantage of the existing liquid chromatography is that the solvent extraction time is long (at least two hours), and if the enhanced extraction methods such as supercritical fluid extraction are used, expensive equipment is required, and the quality of the HPLC analysis results is poor and it is difficult to be accurate. Quantitative. The Chinese invention patent whose patent application number is 200910050956.1 discloses a method for analyzing and measuring brominated flame retardants in the plastic parts of waste household appliances. The biggest difference between this method and the recommended standard SN/T 2005.1-2005 is that a new sample preparation method is adopted, the solvent of Soxhlet extraction is changed to isopropanol, and acetonitrile and water are used as the mobile phase of HPLC. The essence of this method is to shorten the liquid-solid mass transfer distance, reduce the mass transfer resistance and thus reduce the extraction time to 1 hour, and the quality of the HPLC chromatogram is also greatly improved.

According to the existing extraction technology, the Decabromodiphenyl Oxide dissolved in the solvent is separated from the plastic body by osmosis, and its separation efficiency is subject to the mass transfer resistance of the solvent system in the plastic solid. Various existing extraction techniques, such as pressure extraction, ultrasonic extraction and microwave extraction, are all aimed at reducing the mass transfer resistance between liquid and solid. Obviously, the mass transfer resistance between liquid and solid is far greater than the mass transfer resistance between liquid and liquid. For this reason, the present invention proposes to completely dissolve Decabromodiphenyl Oxide together with solid plastic, and convert the large mass transfer resistance between solid and liquid into the interior of the liquid phase. The small mass transfer resistance, thereby greatly reducing the analysis processing time.

Decabromodiphenyl Oxide Properties:

Melting point >300 °C(lit.)
Boiling point 425°C
density 3 g/cm3
refractive index 1.5000 (estimate)
Fp -12 °C
storage temp. 2-8°C
solubility <0.0001mg/l
Water Solubility <0.1 g/100 mL at 20 ºC

 

Decabromodiphenyl Oxide Uses

  1. Decabromodiphenyl Oxide items are made use of as fire resistants in polyethylene, polypropylene and also polybutylene terephthalate. Its physical and cost-effective properties are much better. The drawback is poor weather resistance.
  2. Decabromodiphenyl Oxide is a high-efficiency additive flame resistant, which has exceptional fire retardant impact on HIPS, ABDOMINAL MUSCLE, LDPE, rubber, PBT, and so on. It can additionally be utilized for nylon fibers and polyester-cotton fabrics.
  3. Decabromodiphenyl Oxide products are primarily made use of as additive fire retardants, with huge bromine content, good thermal stability, high fire retardant performance, and a wide range of uses, appropriate for polyethylene, polypropylene, ABS material, epoxy resin, PBT resin, silicone rubber, EPDM, polyester fiber, cotton fiber and other fire retardants.
  4. Decabromodiphenyl ether combined with antimony trioxide has better flame retardant effect and is a non-polluting flame retardant. As a flame retardant, the product is better in both physical properties and economy. But its disadvantage is poor weather resistance and yellowing of the resin. The addition amount for high impact polystyrene is 12%-15%.

Decabromodiphenyl Oxide Invention

The object of the invention is to overcome the defect of the prior art, a kind of method of liquid chromatographic determination of decabromodiphenyl ether content in plastic is provided. The present invention proposes that decabromodiphenyl ether is completely dissolved together with solid plastics, and the large mass transfer resistance between solid and liquid is converted into the small mass transfer resistance inside the liquid phase, thereby greatly reducing the time of analysis and treatment. The invention can realize the rapid analysis of the decabromodiphenyl ether flame retardant content in the plastics of various electronic and electrical products. These electronic and electrical products include televisions, computers, mobile phones, etc. The main components of their plastics are polystyrene, high-impact polystyrene and ABS resin.

The method for determining the content of decabromodiphenyl ether in plastics by liquid chromatography includes the following steps: dissolving the plastics in tetrahydrofuran to form a solution, and after the solution is centrifuged; taking the supernatant for microfiltration, and the filtrate is a solution to be tested by chromatography; The content of decabromodiphenyl ether in the solution to be tested was determined by high performance liquid chromatography.

A method for determining the content of decabromodiphenyl ether in plastics by liquid chromatography, which specifically includes the following steps

(1) collect plastic solids, pulverize; get solid 0.5-1.0g after pulverization, add 50-150mL tetrahydrofuran, stir to make solid dissolve, obtain solution;

(2) get solution 2-10mL, centrifuge more than 3 minutes, draw supernatant after microfiltration, and filtrate is solution to be tested;

(3) Determining the decabromodiphenyl ether content in the solution to be tested by high performance liquid chromatography.

The plastic content in the solution was below 10 mg/mL.

The dissolution time is 10-30 minutes, and it is completely dissolved.

The microfiltration is carried out by using a tetrahydrofuran-resistant filter membrane with a pore size of less than 0.46 μm.

The assay was performed by high performance liquid chromatography with external standard method.

The mobile phase of described high performance liquid chromatography adopts the mixed solvent of tetrahydrofuran and methanol in a volume ratio of 90:10.

The high performance liquid chromatography adopts an ultraviolet detector with a wavelength of 300 nm.

The rotational speed of the centrifugation is greater than 1000 rpm.

(1) Since most of the plastics using decabromodiphenyl ether as flame retardant are polystyrene, and tetrahydrofuran has good solubility for such plastics, and tetrahydrofuran is also a good solvent for decabromodiphenyl ether, its solubility It is 10-20 times that of existing alcohol and ketone solvents (such as isopropanol and acetone) used in various solid-liquid extraction, thus ensuring the rapid dissolution of solid samples. In addition, since all solid substances are completely dissolved in the solvent, the yield problem caused by incomplete extraction of decabromodiphenyl ether in the existing extraction technology is also avoided. Thus, adopting the technology that the tetrahydrofuran proposed by the present invention completely dissolves the solid sample can greatly shorten the sample processing time.

(2) Due to the complex composition of plastic samples, especially for a variety of electronic and electrical plastics, in addition to polystyrene plastics and decabromodiphenyl ether flame retardants, there are inorganic substances such as fillers and dyes. These substances Will interfere with and disrupt chromatographic analysis. For this reason, the present invention adopts the purification technology of first centrifugation and then microfiltration, which has the characteristics of low cost and high applicability.

(3) because the present invention adopts solid sample complete dissolving technology, so in the solution to be tested, in addition to containing the decabromodiphenyl ether that needs to detect, also contain a large amount of polystyrene. Existing HPLC methods for detecting polybrominated diphenyl ethers all use methanol or acetonitrile as the main mobile phase system, and obviously polystyrene has the problem of immiscibility in this mobile phase system, especially for the higher polystyrene content , resulting in a serious decline in the quality of the chromatogram. For this reason, the present invention re-optimizes the mobile phase conditions for chromatographic separation, considers the similarity of the mobile phase and the sample solvent syst

em and the feasibility of reverse-phase rinsing, and obtains a mobile phase system with a mixing ratio of tetrahydrofuran and methanol of 90: 10 through optimization. . Using this mobile phase system can greatly improve the quality of chromatograms and shorten the time of chromatographic analysis.

(4) The present invention adopts the most commonly used HPLC ultraviolet detection and analysis to measure the content of decabromodiphenyl ether. Since tetrahydrofuran is used as the main mobile phase system, and tetrahydrofuran has a high ultraviolet cut-off wavelength, the increase of the detection wavelength can reduce the interference caused by the background absorption of the mobile phase, but the response of decabromodiphenyl ether is also weakened at the same time. The invention comprehensively considers the measurement noise caused by the background absorption of the mobile phase and the signal response of the detection substance, and adopts an ultraviolet detector with a wavelength of 300 nm.

The Specific Embodiment of Decabromodiphenyl Oxide

As shown in Figure 1, the present invention is a process for determining the content of Decabromodiphenyl Oxide in high-impact polystyrene plastics. The solid sample was uniformly mixed by banburying using a high-impact polystyrene plastic masterbatch with a domestic brand of PS-I and an industrial product of Decabromodiphenyl Oxide, wherein the mass content of Decabromodiphenyl Oxide was 10.3%. After the above-mentioned solid sample was crushed into a solid powder with an average size of 0.5 mm with a blade solid crusher, 0.5821 g of the solid powder was weighed with an analytical balance and placed in a 150 mL conical flask, and then about 50 mL of analytically pure tetrahydrofuran was added. solvent. The above solvent and the solid sample powder were magnetically stirred for 10 minutes to completely dissolve the solid sample in the tetrahydrofuran solvent. The above liquid was transferred into a 100 mL volumetric flask, and the volume was adjusted with tetrahydrofuran to prepare a sample solution.

About 3 mL of the sample solution was taken and placed in a 5 mL glass centrifuge tube, and centrifuged at 2000 rpm for 10 minutes to separate the sample solution into a supernatant and a lower turbid. About 2 mL of the supernatant was carefully drawn with a 2.5 mL glass syringe syringe, and filtered with a 0.25 μm pore size polytetrafluoroethylene syringe filter to obtain the solution to be tested. The filtered solution to be tested was collected with a 1.5mL chromatographic injection bottle and prepared for HPLC analysis and determination.

An imported high performance liquid chromatograph with an autosampler model of 1100 was used for HPLC analysis. The chromatographic column was a C18 column of the same brand as the instrument with a model of Hypersil 0DS and a specification of 250X4.6-5. The mobile phase was a domestically produced C18 column. Commercially available chromatographically pure tetrahydrofuran and methanol mixed solvent (volume ratio is 90:10). The injection volume was 5 μL, the isocratic elution flow rate was 1 mL/min, and the column temperature was set to 40 °C. The components in the sample were separated due to different retention factors in the chromatographic column, and the separated components were detected by an ultraviolet detector with a wavelength of 300 nm. Under the same chromatographic conditions, the Decabromodiphenyl Oxide standard solution of 0.1-1.0 mg/mL in concentration content was determined, and the Decabromodiphenyl Oxide content of the tested solution was determined by the peak area external standard method. By contrasting the chromatogram of standard solution, it can be determined that the retention time of Decabromodiphenyl Oxide under the above-mentioned chromatographic condition is 2.77min, and the Decabromodiphenyl Oxide content in the solution to be tested is 0.59±0.02mg/mL, which is equivalent to solid The content of the sample is 10.1±0.3%.

Adopt the Decabromodiphenyl Oxide chromatogram in the gained high-impact polystyrene of the inventive method as shown in accompanying drawing 3, wherein the Decabromodiphenyl Oxide peak time is 2.77 minutes, and the peak shape is sharp; In T 2005.1-2005 method gained chromatogram (as shown in accompanying drawing 2), the Decabromodiphenyl Oxide peak time is longer and the peak shape overlaps, which shows that the inventive method is obviously better than the existing method. The method of the present invention can complete the determination of the Decabromodiphenyl Oxide content in the high-impact polystyrene within 30 minutes, and the maximum relative deviation of the measurement is less than 5%.

About Us

The production base is located in Zhangqiu chemical industry park and Tai’an high-tech chemical industry park. laboratory and workshop in strict accordance with the GMP standard and the product fit national ISO9001 and ISO2000 standards.

“Zhishang” products are exported to Europe, North and South America, the Middle East, Asia Pacific and Africa area, so as to establish a long-term and stable cooperation relationship with customer in the world.

Company Info
  • Business Type: Manufacturer
  • Product Range: Additive , Chemical Auxiliary & Catalyst , Organic Chemicals
  • Products/Service: Organic Intermediate,Inorganic Chemistry, APIs, Dyestuffs And Pigments, Fragrance And Spices, Food Additives
  • Total Employees: 51~100
  • Capital (Million US $): 10000000RMB
  • Year Established: 2016
Production Capacity
  • No. of Production Lines : 8
  • No. of QC Staff : 5 -10 People
  • OEM Services Provided : yes
  • Factory Size (Sq.meters) : 3,000-5,000 square meters
  • Certificate: ISO9001 , CE , GMP , API , MSDS
  • Factory Location : Diao Town Industry Park, Zhangqiu City, Jinan City, Shandong Province, China.

Service

Pre-Sales Service

* Prompt reply and 24 hours online, professional team to provide best price and high quality product.

* Sample testing support.

* Every batch of products will be tested to ensureits quality.

*The packing also can be according the customers` requirment.

*Any inquiries will be replied within 24 hours.

*we provide Commerical Invoice, Packing List, Bill of loading, COA , Health certificate and Origin certificate. If your markets have any special requirements, let us know.

 

After-Sales Service

*The fact of logistics information monitoring.

* Any questions about the product can be consulted at any time.

*Product has any problem can return.

FAQ

Do you accept sample order?

We will make samples before mass production, and after sample approved, we’ll begin mass production. Doing 100% inspection during production, then do random inspection before packing.

 

HOW TO CONFIRM THE PRODUCT QUALITY BEFORE PLACING ORDERS?

You can get free samples for some products,you only need to pay the shipping cost or arrange a courier to us and take the samples. You can send us your product specifications and requests,we will manufacture the products according to your requests.

What’s your MOQ?

Our MOQ is 1kg. But usually we accept less quantity such as 100g on the condition that sample charge is 100% paid.

Do you supply product report?

Yes. We’ll give you product analysis report before shipping.

  Is there a discount?

Different quantity has different discount.

Shipping

1. ≤50kg, Express delivery recommended, usually called as DDU service;

2. ≤500kg, Air shipping recommended, usually called as FOB, CFR, or CIF service;

3. >500kg, sea shipping recommended, usually called as FOB, CFR, or CIF service;

4. For high value products, please select air shipping and express delivery for safe.

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