公开(公告)号：US08309361B2

公开(公告)日：2012-11-13

申请号：US12623846

申请日：2009-11-23

Applicant: Lisa Edith Helberg ,  Jane Ramsey Marsh ,  Craig Steven Westphal

Inventor： Lisa Edith Helberg ,  Jane Ramsey Marsh ,  Craig Steven Westphal

IPC: H01J49/26 ,  C09K3/00

CPC classification number: C01G23/024 ,  B01J8/1809 ,  C01G19/04

Abstract: This disclosure relates to a method for detecting at least one analyte in a tetrachloride sample comprising titanium, tin or silicon tetrachloride; comprising, (a) adding a mixture of water and acid, typically hydrochloric acid, to the sample under conditions effective for forming an aqueous solution of the sample; (b) introducing the aqueous solution of the sample into an inductively coupled mass spectrometer having a cell selected from the group of a reactive cell and a collision cell or both and producing an analyte ion comprising an interfering species; (c) contacting the analyte ion with a gas to produce a product which is substantially free from the interfering species; and (d) detecting and measuring at least one signal from the analyte in the solution. This disclosure further relates to a method for making an aqueous titanium, tin or silicon tetrachloride sample suitable for analysis in using inductively coupled plasma mass spectroscopy.

Abstract translation: 本公开涉及用于检测包含钛，锡或四氯化硅的四氯化物样品中的至少一种分析物的方法; 包括：（a）在有效形成样品水溶液的条件下，向样品中加入水和酸（通常为盐酸）的混合物; （b）将样品的水溶液引入具有选自反应性细胞和碰撞细胞或两者的细胞的电感耦合质谱仪，并产生包含干扰物质的分析物离子; （c）使分析物离子与气体接触以产生基本上不含干扰物质的产物; 和（d）检测和测量来自溶液中的分析物的至少一种信号。 本公开还涉及一种制备适用于使用电感耦合等离子体质谱法分析的钛，锡或四氯化硅水溶液的方法。

公开(公告)号：US08889094B2

公开(公告)日：2014-11-18

申请号：US13980582

申请日：2012-02-22

Applicant: Lisa Edith Helberg

Inventor： Lisa Edith Helberg

IPC: C01G23/00 ,  C22B34/12 ,  C01G23/02

CPC classification number: C22B34/1259 ,  C01G23/024 ,  C01P2006/80

Abstract: The present disclosure relates to reacting tin metal with crude TiCl4 containing arsenic to produce pure TiCl4, SnCl4, and an arsenic solid co-product. In some embodiments, the contaminant vanadium is removed as well. In another embodiment, the vanadium is removed separately through a commercial process and the resulting arsenic containing commercial grade of purified TiCl4 is reacted with elemental tin, sulfur and ferric chloride to substantially reduce the arsenic. The reaction is preferably done in a continuous fashion in two stages for maximum through-put and utility at an elevated temperature. Distillation can be used to purify the TiCl4 produced and simultaneously yield a purified SnCl4 product. The synthesis of SnCl4 in this method utilizes waste chloride to save virgin chlorine which would otherwise be used.

Abstract translation: 本公开涉及使锡金属与含有砷的粗TiCl 4反应以产生纯TiCl 4，SnCl 4和砷固体共产物。 在一些实施方案中，还除去污染物钒。 在另一个实施方案中，通过商业方法分开除去钒，并将得到的含有砷的商业级纯化的TiCl 4与元素锡，硫和氯化铁反应，以显着降低砷。 反应优选以两个阶段的连续方式进行，以实现最大的通过和在高温下的应用。 蒸馏可用于纯化所生产的TiCl4并同时产生纯化的SnCl4产物。 该方法中SnCl4的合成利用废氯化合物来保存原来的氯，否则将使用氯。

公开(公告)号：US20100065736A1

公开(公告)日：2010-03-18

申请号：US12623846

申请日：2009-11-23

Applicant: Lisa Edith Helberg ,  Jane Ramsey Marsh ,  Craig Steven Westphal

Inventor： Lisa Edith Helberg ,  Jane Ramsey Marsh ,  Craig Steven Westphal

IPC: H01J49/26 ,  C09K3/00

CPC classification number: C01G23/024 ,  B01J8/1809 ,  C01G19/04

Abstract: This disclosure relates to a method for detecting at least one analyte in a tetrachloride sample comprising titanium, tin or silicon tetrachloride; comprising, (a) adding a mixture of water and acid, typically hydrochloric acid, to the sample under conditions effective for forming an aqueous solution of the sample; (b) introducing the aqueous solution of the sample into an inductively coupled mass spectrometer having a cell selected from the group of a reactive cell and a collision cell or both and producing an analyte ion comprising an interfering species; (c) contacting the analyte ion with a gas to produce a product which is substantially free from the interfering species; and (d) detecting and measuring at least one signal from the analyte in the solution. This disclosure further relates to a method for making an aqueous titanium, tin or silicon tetrachloride sample suitable for analysis in using inductively coupled plasma mass spectroscopy.

Abstract translation: 本公开涉及用于检测包含钛，锡或四氯化硅的四氯化物样品中的至少一种分析物的方法; 包括：（a）在有效形成样品水溶液的条件下，向样品中加入水和酸（通常为盐酸）的混合物; （b）将样品的水溶液引入具有选自反应性细胞和碰撞细胞或两者的细胞的电感耦合质谱仪，并产生包含干扰物质的分析物离子; （c）使分析物离子与气体接触以产生基本上不含干扰物质的产物; 和（d）检测和测量来自溶液中的分析物的至少一种信号。 本公开还涉及一种制备适用于使用电感耦合等离子体质谱法分析的钛，锡或四氯化硅水溶液的方法。