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首页> 外文会议>SMTA international conference >DETERMINATION OF TOTAL HALOGEN CONTENT IN HALOGEN-FREE FLUXES BY INDUCTIVELY COUPLED PLASMA AND SOME LIMITATIONS OF ION CHROMATOGRAPHY
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DETERMINATION OF TOTAL HALOGEN CONTENT IN HALOGEN-FREE FLUXES BY INDUCTIVELY COUPLED PLASMA AND SOME LIMITATIONS OF ION CHROMATOGRAPHY

机译：电感耦合等离子体法测定无卤离子通量中的总卤离子含量及离子色谱法的某些局限性

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Brominated flame retardants (BFRs) are coming under heavy scrutiny due to increasing evidence of the risks they pose to the environment and human health. Therefore, it is important for industrial quality laboratories to follow robust methods to assure commercial products meet the safety requirements established by the governing bodies of the world. Currently, the most common method to determine halogen content is oxygen combustion, followed by ion chromatography. The oxygen combustion test is widely established in environmental as well as in industrial laboratories. One current accepted test method, EN14582, may under-report bromine and chlorine content by as much as 65%. The use of inductively coupled plasma (ICP) methods of detection appears to resolve this discrepancy. Flux marketed as "zero intentionally-added halogens" was combusted in a bomb calorimeter vessel under 30atm of high-purity oxygen in the presence of 25ml of water. The resultant solution was analyzed using both ion chromatography (IC) and ICP. The flux was found to contain ＜10ppm of each element using both techniques. Samples were then spiked using a common flux additive containing chlorine and bromine, combusted in the same manner, and analyzed. At a low concentration (15ppm Br, 6ppm Cl), the average %recovery of Br was 60.7% by IC and 100.8% by ICP; the %recovery of Cl was 109.5% by IC and 84.8% by ICP. At a moderate concentration (150ppm Br, 65ppm Cl), the %recovery of Br was 25.5% by IC and 86.9% by ICP; the %recovery of Cl was 81.8% by IC and 104.2% by ICP. The effect of pH and buffering capacity of the absorbing solution was explored by ICP in an attempt to optimize the sequestration of Cl and Br in the solution as stable oxyanions; however, the results of hypothetically optimal solutions were no more accurate than those using analytical water as the absorbing solution. Additionally, thirty samples of flux containing 275ppm intentionally-added organic bromine were combusted and analyzed using the techniques described. The average %recovery of bromine by IC was 64.3% and 105.1% by ICP.
机译：由于越来越多的证据表明溴化阻燃剂（BFR）对环境和人类健康构成风险，因此对其进行了严格的审查。因此，对于工业质量实验室而言，遵循可靠的方法以确保商业产品满足世界理事机构制定的安全要求非常重要。当前，最常见的确定卤素含量的方法是氧气燃烧，然后再进行离子色谱分析。氧气燃烧测试已在环境实验室和工业实验室中广泛建立。一种当前公认的测试方法EN14582可能会低报溴和氯含量多达65％。使用感应耦合等离子体（ICP）检测方法似乎可以解决这种差异。在25毫升水的存在下，在30atm高纯度氧气下，在炸弹量热计容器中燃烧以“零故意添加的卤素”销售的助焊剂。使用离子色谱法（IC）和ICP对所得溶液进行分析。使用这两种技术，发现助焊剂的每种元素含量均＜10ppm。然后使用含有氯和溴的普通助焊剂添加样品，以相同的方式燃烧并进行分析。在低浓度（15ppm Br，6ppm Cl）的情况下，IC的平均溴回收率为60.7％，ICP的平均回收率为100.8％; IC的Cl回收率为109.5％，ICP的Cl回收率为84.8％。在中等浓度（150ppm Br，65ppm Cl）下，IC的Br回收率为25.5％，ICP的Br的回收率为86.9％。 IC的Cl回收率为81.8％，ICP的Cl回收率为104.2％。 ICP探讨了pH值和吸收溶液缓冲能力的影响，试图优化溶液中Cl和Br的螯合形式，使其成为稳定的氧阴离子。但是，假设的最佳解决方案的结果并不比使用分析水作为吸收解决方案的结果更准确。另外，使用所描述的技术燃烧并分析了含有275ppm有意添加的有机溴的助焊剂样品。 IC的平均溴回收率分别为ICP的64.3％和105.1％。

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