Citation: WANG Hui, XUE Qiuhong, TAO Lin, YE Xiwen, LIANG Shengkang, LI Yanqiu, NIU Zengyuan. Determination of hexabromocyclododecane in coatings by gas chromatography-mass spectrometry[J]. Chinese Journal of Chromatography, ;2013, 31(8): 791-794. doi: 10.3724/SP.J.1123.2013.01014 shu

Determination of hexabromocyclododecane in coatings by gas chromatography-mass spectrometry

WANG Hui ^1,2 ,
XUE Qiuhong ^2,, ,
TAO Lin ³ ,
YE Xiwen ² ,
LIANG Shengkang ¹ ,
LI Yanqiu ² ,
NIU Zengyuan ²

1.
1. College of Chemistry and Chemical Engineering, Ocean University of China, Qingdao 266003, China;

Corresponding author: XUE Qiuhong,
Received Date: 7 January 2013
Available Online: 11 February 2013
Fund Project: 出入境检验检疫行业标准项目(2011B052) (2011B052)质检总局科研项目(2011IK039). (2011IK039)

A method has been developed for the determination of hexabromocyclododecane (HBCD) in fire proof coatings by gas chromatography-mass spectrometry (GC-MS). The sample was extracted with dichloromethane and purified through an organic membrane before analysis with GC-MS. The characteristic fragments (m/z 157, 239, 319, 401) and the quantitative ion (m/z 239) were selected. With the optimized conditions, the good linear relationship was obtained between the peak area and the mass concentration of HBCD in the range of 5 to 100 mg/L with the correlation coefficient more than 0.999. The spiked recoveries in the coatings of acrylic and epoxy resins were 92.9%-116.3% with the RSDs not more than 8%. The LOD (S/N≥3) of HBCD was 30 μg/g, and the LOQ (S/N≥10) was 100 μg/g, which were much lower than the international maximum residue limit. The method is simple, quick, accurate and precise, which can meet the requirements of the European Commission Regulation (EC) No. 1907/2006 and Norway PoHS instruction (Prohibition on Certain Hazardous Substances in Consumer Products) for the determination of HBCD. It is suitable for the analysis of HBCD in fire proof coatings.
- gas chromatography-mass spectrometry (GC-MS),
- hexabromocyclododecane,
- brominated flame retardants,
- coatings
1. [1]
  [1] Du W. Environmental Chemistry (杜伟. 环境化学), 2011, 30(10): 1833
2. [2]
  [2] Li Y D, Yun X, Na G S, et al. Journal of Environment and Health (李永东, 云霞, 那广水, 等. 环境与健康杂志), 2010, 27(10): 933
3. [3]
  [3] Ueno D, Isobe T, Ramu K, et al. Chemosphere, 2010, 78: 1213
4. [4]
  [4] Ramu K, Kajiwara N, Isobe T, et al. Environ Pollut, 2007, 148: 562
5. [5]
  [5] Ramu K, Isobe T, Takahashi S, et al. Chemosphere, 2010, 79: 713
6. [6]
  [6] Li Y N, Zhou Q X, Wang Y Y, et al. Chemosphere, 2011, 82: 204
7. [7]
  [7] Wang T, Han S L, Ruan T, et al. Chemosphere, 2013, 90: 182
8. [8]
  [8] Darnerud P O. Environ Int, 2003, 29: 841
9. [9]
  [9] Ilyas M, Sudaryanto A, Setiawan I E, et al. Mar Pollut Bull, 2011, 62: 89
10. [10]
  [10] Covaci A, Gerecke A C, Law R J, et al. Environ Sci Technol, 2006, 40(12): 3679
11. [11]
  [11] Asante K A, Adu-Kumi S, Nakahiro K, et al. Environ Int, 2011, 37: 921
12. [12]
  [12] Yue Q. Guangdong Agricultural Sciences (岳强. 广东农业科学), 2010(6): 217
13. [13]
  [13] Liang Y Y. Electronic Quality (梁元媛. 电子质量), 2008(4): 78
14. [14]
  [14] Ma Q, Bai H, Wang C, et al. Chemical Journal of Chinese Universities (马强, 白桦, 王超, 等. 高等学校化学学报), 2010, 31(3): 473
15. [15]
  [15] Ding Y C, Cao X Z, Qian K, et al. Dyeing & Finishing (丁友超, 曹锡忠, 钱凯, 等. 印染), 2010(9): 36
16. [16]
  [16] Gerecke A C, Kohler M, Zennegg M, et al. Organohalogen Compd, 2003, 61: 155
17. [17]
  [17] Tang C M. J Chromatogr B, 2010, 878: 3317
18. [18]
  [18] Feng J Y, Wang Y W, Ruan T, et al. Talanta, 2010, 82: 1929
19. [19]
  [19] Morris S, Bersuder P, Allchin C R, et al. Trends Anal Chem, 2006, 25(4): 343
20. [20]
  [20] Guerra P, Eljarrat E, Barcelo D. Trends Anal Chem, 2011, 30(6): 842
21. [21]
  [21] Pan H F, Hui Y, Wang J, et al. Journal of Analytical Science (潘荷芳, 惠阳, 王静, 等. 分析科学学报), 2008, 24(4): 414
22. [22]
  [22] Yu Z Q, Peng P A, Sheng G Y, et al. J Chromatogr A, 2008, 1190: 74
23. [23]
  [23] Vilaplana F, Karlsson P, Greus A R, et al. J Chromatogr A, 2008, 1196: 139
24. [24]
  [24] Shi Z X, Feng J F, Li J G, et al. Chinese Journal of Chromatography (施致雄, 封锦芳, 李敬光, 等. 色谱), 2008, 26(1): 1
25. [25]
  [25] Tang Z K, Chen Q, Li D, et al. Physical Testing and Chemical Analysis Part B: Chemical Analysis (唐志锟, 陈强, 李丹, 等. 理化检验-化学分册), 2012, 48(7): 807
1. [1]
  Yanhui Zhong , Ran Wang , Zian Lin . Analysis of Halogenated Quinone Compounds in Environmental Water by Dispersive Solid-Phase Extraction with Liquid Chromatography-Triple Quadrupole Mass Spectrometry. University Chemistry, 2024, 39(11): 296-303. doi: 10.12461/PKU.DXHX202402017
2. [2]
  Zunxiang Zeng , Yuling Hu , Yufei Hu , Hua Xiao . Analysis of Plant Essential Oils by Supercritical CO₂Extraction with Gas Chromatography-Mass Spectrometry: An Instrumental Analysis Comprehensive Experiment Teaching Reform. University Chemistry, 2024, 39(3): 274-282. doi: 10.3866/PKU.DXHX202309069
3. [3]
  Xiaowu Zhang , Pai Liu , Qishen Huang , Shufeng Pang , Zhiming Gao , Yunhong Zhang . Acid-Base Dissociation Equilibrium in Multiphase System: Effect of Gas. University Chemistry, 2024, 39(4): 387-394. doi: 10.3866/PKU.DXHX202310021
4. [4]
  Jiao CHEN , Yi LI , Yi XIE , Dandan DIAO , Qiang XIAO . Vapor-phase transport of MFI nanosheets for the fabrication of ultrathin b-axis oriented zeolite membranes. Chinese Journal of Inorganic Chemistry, 2024, 40(3): 507-514. doi: 10.11862/CJIC.20230403
5. [5]
  Jinyao Du , Xingchao Zang , Ningning Xu , Yongjun Liu , Weisi Guo . Electrochemical Thiocyanation of 4-Bromoethylbenzene. University Chemistry, 2024, 39(6): 312-317. doi: 10.3866/PKU.DXHX202310039
6. [6]
  Xiaoling LUO , Pintian ZOU , Xiaoyan WANG , Zheng LIU , Xiangfei KONG , Qun TANG , Sheng WANG . Synthesis, crystal structures, and properties of lanthanide metal-organic frameworks based on 2, 5-dibromoterephthalic acid ligand. Chinese Journal of Inorganic Chemistry, 2024, 40(6): 1143-1150. doi: 10.11862/CJIC.20230271
7. [7]
  Yinwu Su , Xuanwen Zheng , Jianghui Du , Boda Li , Tao Wang , Zhiyan Huang . Green Synthesis of 1,3-Dibromoacetone Using Halogen Exchange Method: Recommending a Basic Organic Synthesis Teaching Experiment. University Chemistry, 2024, 39(5): 307-314. doi: 10.3866/PKU.DXHX202311092
8. [8]
  Xueli Mu , Lingli Han , Tao Liu . Quantum Chemical Calculation Study on the E2 Elimination Reaction of Halohydrocarbon: Designing a Computational Chemistry Experiment. University Chemistry, 2025, 40(3): 68-75. doi: 10.12461/PKU.DXHX202404057
9. [9]
  Ruolin CHENG , Haoran WANG , Jing REN , Yingying MA , Huagen LIANG . Efficient photocatalytic CO₂ cycloaddition over W₁₈O₄₉/NH₂-UiO-66 composite catalyst. Chinese Journal of Inorganic Chemistry, 2024, 40(3): 523-532. doi: 10.11862/CJIC.20230349
10. [10]
  Jiahui YU , Jixian DONG , Yutong ZHAO , Fuping ZHAO , Bo GE , Xipeng PU , Dafeng ZHANG . The morphology control and full-spectrum photodegradation tetracycline performance of microwave-hydrothermal synthesized BiVO₄:Yb³⁺,Er³⁺ photocatalyst. Journal of Fuel Chemistry and Technology, 2025, 53(3): 348-359. doi: 10.1016/S1872-5813(24)60514-1
11. [11]
  Gaoyan Chen , Chaoyue Wang , Juanjuan Gao , Junke Wang , Yingxiao Zong , Kin Shing Chan . Heart to Heart: Exploring Cardiac CT. University Chemistry, 2024, 39(9): 146-150. doi: 10.12461/PKU.DXHX202402011
12. [12]
  Yunxin Xu , Wenbo Zhang , Jing Yan , Wangchang Geng , Yi Yan . A Fascinating Saga of “Energetic Materials”. University Chemistry, 2024, 39(9): 266-272. doi: 10.3866/PKU.DXHX202307008
13. [13]
  Tingting Yu , Si Chen , Lianglong Sun , Tongtong Shi , Kai Sun , Xin Wang . Comprehensive Experimental Design for the Photochemical Synthesis, Analysis, and Characterization of Difluoropyrroles. University Chemistry, 2024, 39(11): 196-203. doi: 10.3866/PKU.DXHX202401022
14. [14]
  Jingming Li , Bowen Ding , Nan Li , Nurgul . Application of Comparative Teaching Method in Experimental Project Design of Instrumental Analysis Course: A Case Study in Chromatography Experiment Teaching. University Chemistry, 2024, 39(8): 263-269. doi: 10.3866/PKU.DXHX202312078
15. [15]
  Zhiwen HU , Weixia DONG , Qifu BAO , Ping LI . Low-temperature synthesis of tetragonal BaTiO₃ for piezocatalysis. Chinese Journal of Inorganic Chemistry, 2024, 40(5): 857-866. doi: 10.11862/CJIC.20230462
16. [16]
  Haiyang Zhang , Yanzhao Dong , Haojie Li , Ruili Guo , Zhicheng Zhang , Jiangjiexing Wu . Exploring the Integration of Chemical Engineering Principle Experiment with Cutting-Edge Research Achievements. University Chemistry, 2024, 39(10): 308-313. doi: 10.12461/PKU.DXHX202405035
17. [17]
  Jing Wang , Pingping Li , Yuehui Wang , Yifan Xiu , Bingqian Zhang , Shuwen Wang , Hongtao Gao . Treatment and Discharge Evaluation of Phosphorus-Containing Wastewater. University Chemistry, 2024, 39(5): 52-62. doi: 10.3866/PKU.DXHX202309097
18. [18]
  Linhan Tian , Changsheng Lu . Discussion on Sextuple Bonding in Diatomic Motifs of Chromium Family Elements. University Chemistry, 2024, 39(8): 395-402. doi: 10.3866/PKU.DXHX202401056
19. [19]
  Fang Niu , Rong Li , Qiaolan Zhang . Analysis of Gas-Solid Adsorption Behavior in Resistive Gas Sensing Process. University Chemistry, 2024, 39(8): 142-148. doi: 10.3866/PKU.DXHX202311102
20. [20]
  Jiahong ZHENG , Jingyun YANG . Preparation and electrochemical properties of hollow dodecahedral CoNi₂S₄ supported by MnO₂ nanowires. Chinese Journal of Inorganic Chemistry, 2024, 40(10): 1881-1891. doi: 10.11862/CJIC.20240170

Get Citation

PDF

XML

Metrics

PDF Downloads(0)
Abstract views(145)
HTML views(8)

通讯作者: 陈斌, bchen63@163.com

1.
沈阳化工大学材料科学与工程学院沈阳 110142