CN1218905A - 高效液相色谱分析有机阻燃剂的方法 - Google Patents
高效液相色谱分析有机阻燃剂的方法 Download PDFInfo
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Abstract
一种高效液相色谱分析有机阻燃剂的方法,采用高效液相色谱仪,紫外多波长检测器单独或与示差检测器串联使用,紫外波长为210-350nm,HSG-10分析柱,移动相为C1-C3醇与四氢呋喃的混合物,流量为1.0-3.0ml/分,进样量为5-20μl。本发明具有组份峰呈现性好,分辨率高,重复性好,可表征各种类型的阻燃剂的组成,结构特征的优点。
Description
本发明属于一种分析方法,具体地说涉及一种高效液相色谱分析有机阻燃剂的方法。
目前,对阻燃剂的检测只是进行一般的化学法测定卤素总含量,挥发份含量测定,以及酸值的测定。由于阻燃剂在色谱移动相中的溶解性与组份峰的呈现性、分辨率的矛盾、相互制约性极大,用高效液相色谱法分析其它有机化合物的原有色谱体系,如一般的正相色谱体系,反相色谱体系,凝胶渗透色谱体系,离子色谱体系是难以分离分析阻燃剂的组份。经文献检索,用高效液相色谱法分离分析阻燃剂未见文献报道。
本发明的发明目的是提供一种高效液相色谱分析有机阻燃剂的方法。
本发明的分析方法如下:
1.使用高效液相色谱分析仪,检测器为紫外(UV)多波长检测器,示差检测器(RID),紫外检测器单独使用或与示差检测器串联使用,紫外波长为210nm-350nm;
2.采用HSG-10分析柱,柱温为室温;
3.把C1-C3醇与四氢呋喃按10∶90~90∶10(V/V)配成移动相,流量为1ml/分-3ml/分;
4.将阻燃剂溶于四氢呋喃配成0.1-10%(重量百分比)待分析溶液;
5.将待分析溶液以5-20μl进样,检测器进行检测,记录器图示谱图。
本发明的分析方法可适用于溴系有机阻燃剂、氯系有机阻燃剂、磷系有机阻燃剂。包括三嗪系列阻燃剂、中间体产品、阻燃增塑剂等各种阻燃剂。
本发明与现有技术相比具有如下优点:
(1)分析方法使用现代仪器,实施目前化学法所不能进行的组份分离分析。
(2)可表征比较各种类型的阻燃剂组成、结构特征。
(3)可测定阻燃剂的纯度,各组份含量。
(4)组份谱峰呈现性好。
(5)色谱分辨率高。
(6)检测结果重复性好。
实施例1
(1)采用LC-3A高效液相色谱仪,检测器为紫外(UV)多波长检测器,紫外波长固定为230nm;(2)分析柱为HSG-10,柱温为室温;(3)移动相配比为甲醇∶四氢呋喃=20∶80(V∶V),流速为2.0ml/分;(4)将待分析的B-MAP(密胺三聚氰胺)阻燃剂配成0.5%的四氢呋喃溶液,以10μl进样,检测结果见图1。
实施例2
阻燃剂为TBC,即三(2,3二溴丙基)异氰尿酸酯,学名:1,3,5-三(2,3-二溴丙基)-1,3,5-三嗪-2,4,6酮,紫外波长固定在270nm,移动相为甲醇∶四氢呋喃=50∶50(V∶V),移动相流速为1.8ml/分,进样量为15μl,其余同实施例1,检测结果见图2。
实施例3
阻燃剂为PZ-747(含氯多磷酸酯,分子量为747)。紫外波长固定在310nm。移动相为甲醇∶四氢呋喃=30∶70(V∶V),移动相流速为2.5ml/分,进样量为15μl,其余同实施例1,检测结果见图3。
实施例4
阻燃剂为BBP,即双(2,3二溴丙基)二氯丙基磷酸酯,检测器为紫外(UV)多波长检测器与示差检测器串联使用,紫外波固定在260nm,移动相为甲醇∶四氢呋喃=10∶30(U/V)其余同实施例1。检测结果见图4。
实施例5
阻燃剂为TBP,即三(2,3二溴丙基磷酸酯,其余同实施例4,检测结果见图5。
实施例6
阻燃剂为亚磷酸三苯酯,紫外波固定在254nm,移动相为甲醇∶四氢呋喃=90∶10(V∶V),进样量为20μl,其余同实施例4,检测结果见图6。
实施例7
阻燃剂为阻燃增塑剂FR-15,移动相为甲醇∶四氢呋喃=60∶40(V∶U),其余同实施例6,检测结果见图7。
实施例8
阻燃剂为三(2,3-二溴丙基)硼酸酯,紫外波长为280nm,进样量为10ml/次,其余同实施例6,检测结果见图8。
实施例9
阻燃剂为八溴二苯醚,其余同实施例4,检测结果见图9。
Claims (1)
1.一种高效液相色谱分析有机阻燃剂的方法,其分析方法如下:
(1).使用高效液相色谱分析仪,检测器为紫外(UV)多波长检测器,示差检测器(RID),紫外检测器单独使用或于示差检测器串联使用,紫外波长为210nm-350nm;
(2).采用HSG-10分析柱,柱温为室温;
(3).把C1-C3醇与四氢呋喃按10∶90~90∶10(V/V)配成移动相,流量为1ml/分-3ml/分;
(4).将阻燃剂溶于四氢呋喃配成0.1-10%(重量百分比)待分析溶液;
(5).将待分析溶液以5-20μl进样,检测器进行检测,记录器图示谱图。
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101216467B (zh) * | 2008-01-14 | 2010-12-15 | 谱尼测试科技(北京)有限公司 | 一种电子材料中六溴环十二烷含量的测定方法 |
CN106501400A (zh) * | 2016-10-21 | 2017-03-15 | 广东环境保护工程职业学院 | 一种液相色谱测定水样中tcep的检测方法 |
CN113125625A (zh) * | 2021-06-21 | 2021-07-16 | 天地恒一制药股份有限公司 | 一种富马酸丙酚替诺福韦中基因毒性杂质的检测方法 |
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1997
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101216467B (zh) * | 2008-01-14 | 2010-12-15 | 谱尼测试科技(北京)有限公司 | 一种电子材料中六溴环十二烷含量的测定方法 |
CN106501400A (zh) * | 2016-10-21 | 2017-03-15 | 广东环境保护工程职业学院 | 一种液相色谱测定水样中tcep的检测方法 |
CN106501400B (zh) * | 2016-10-21 | 2017-10-24 | 广东环境保护工程职业学院 | 一种液相色谱测定水样中tcep的检测方法 |
CN113125625A (zh) * | 2021-06-21 | 2021-07-16 | 天地恒一制药股份有限公司 | 一种富马酸丙酚替诺福韦中基因毒性杂质的检测方法 |
CN113125625B (zh) * | 2021-06-21 | 2021-09-03 | 天地恒一制药股份有限公司 | 一种富马酸丙酚替诺福韦中基因毒性杂质的检测方法 |
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