CN1081331C - 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(V/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∶V)，其余同实施例6，检测结果见图7。
实施例8
阻燃剂为三(2，3一二溴丙基)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，检测器为紫外多波长检测器、示差检测器，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V∶V为10∶90～90∶10配成移动相，流量为1毫升/分-3毫升/分；
(4).将阻燃剂溶于四氢呋喃中，配成重量百分比为0.5％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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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 97123374 CN1081331C (zh) | 1997-12-04 | 1997-12-04 | 高效液相色谱分析有机阻燃剂的方法 |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 97123374 CN1081331C (zh) | 1997-12-04 | 1997-12-04 | 高效液相色谱分析有机阻燃剂的方法 |
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| CN1218905A CN1218905A (zh) | 1999-06-09 |
| CN1081331C true CN1081331C (zh) | 2002-03-20 |
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| 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 |
| 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 |
| 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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