# US 12,181,452 B2 · Use of vapor deposition coated flow paths for improved chromatography of metal interacting analytes

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- Number: US 12,181,452 B2
- Document ID: US12181452B2
- Status: Granted
- Kind: B2
- Application number: 17/204,021
- Filed: 2021-03-17
- Published: 2021-07-22
- Granted: 2024-12-31
- Earliest claimed: 2017-09-18
- Assignees: Waters Technologies Corporation
- Applicants: Waters Technologies Corporation
- Inventors: Stephen J. Shiner; Cheryl Boissel; Matthew A. Lauber; Kevin Wyndham; Michael O. Fogwill
- Web page: https://patentgrep.com/patent/US12181452B2

## CPC

- G01N 30/56: Packing methods or coating methods
- G01N 30/603: {retaining the stationary phase, e.g. Frits}
- B01D 15/22: relating to the construction of the column
- B05D 1/60: {Deposition of organic layers from vapour phase (vapour phase deposition in general C23C14/00, C23C16/00)}
- B05D 7/14: to metal, e.g. car bodies (involving a chemical reaction between the metal and the coating C23)
- C23C 16/045: {Coating cavities or hollow spaces, e.g. interior of tubes; Infiltration of porous substrates}
- C23C 16/30: Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- G01N 30/6052: {body}
- B05D 2518/10: Silicon-containing polymers
- G01N 30/7266: {by electric field, e.g. electrospray}
- G01N 2030/027: {Liquid chromatography}
- G01N 2030/567: {coating}
- G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q)
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)
- B05D: PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL (conveying articles or workpieces through baths of liquid B65G, e.g. B65G49/02)
- C23C: COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL (making metal-coated products by extrusion B21C23/22; covering with metal by connecting pre-existing layers to articles, see the relevant places, e.g. B21D39/00, B23K; metallising of glass C03C; metallising mortars, concrete, artificial stone, ceramics or natural stone C04B41/00; enamelling of, or applying a vitreous layer to, metals C23D; treating metal surfaces or coating of metals by electrolysis or electrophoresis C25D; single-crystal film growth C30B; by metallising textiles D06M11/83; decorating textiles by locally metallising D06Q1/04)

## Abstract

A chromatographic device including a coated metallic frit is disclosed. The coating is provided over the fluid exposed surfaces of the frit, thereby covering metallic surfaces to prevent interaction with an analyte in the flowstream. This technology relates to the use of a vapor deposition coated frit together with an uncoated frit in a liquid flow path for improved chromatography. More specifically, this technology relates to liquid chromatographic devices for separating analytes in a sample having a single coated frit within an uncoated metallic fluidic flow path (i.e., the column tube or channel is formed of stainless steel, titanium (pure or alloyed), or some mixture of stainless steel and titanium) and does not include the coating applied to the frit.

## Claims

### Claim 1

A chromatographic column, comprising:
an uncoated tube comprising stainless steel or titanium or both; and
a coated frit comprising a coating, wherein a vapor reagent used to form the coating is bis(trichlorosilyl)ethane or bis(trimethoxysilyl)ethane and the coated frit is disposed proximate to an end of the uncoated tube;
wherein the uncoated tube does not have the coating, and
during a separation of sample components in the chromatography column, the coating reduces binding of one or more sample components to the coated frit relative to binding of the one or more sample components to the uncoated tube.

### Claim 2 (depends on 1)

The chromatography column of claim 1, wherein the chromatography column is a preparative liquid chromatography column.

### Claim 3 (depends on 1)

The chromatographic column of claim 1, wherein the coated frit is a tube outlet frit.

### Claim 4 (depends on 1)

The chromatographic column of claim 1, wherein the coated frit is a tube inlet frit.

### Claim 5 (depends on 1)

The chromatographic column of claim 1, wherein the coated frit includes an underlying substrate of titanium.

### Claim 6 (depends on 1)

The chromatographic column of claim 1, wherein the uncoated tube has a length to diameter ratio of between 40 and 4.

### Claim 7 (depends on 1)

The chromatographic column of claim 1, wherein the coating has a thickness of at least 100 Å.

### Claim 8 (depends on 1)

The chromatographic column of claim 1, wherein the coating comprises a primer layer and a top layer.

### Claim 9 (depends on 8)

The chromatographic column of claim 8, wherein the primer layer is an alkylsilyl formed using a vapor reagent selected from the group consisting of bis(trichlorosilyl)ethane or bis(trimethoxysilyl)ethane.

### Claim 10 (depends on 8)

The chromatographic column of claim 8, wherein a vapor reagent used to form the top layer is (3-glycidyloxypropyl) trimethoxysilane, n-decyltrichlorosilane, trimethylchlorosilane, trimethyldimethyaminosilane, methoxy-polyethyleneoxy(1-10) propyl trichlorosilane, or methoxy-polyethyleneoxy(1-10) propyl trimethoxysilane.

### Claim 11 (depends on 8)

The chromatographic column of claim 8, wherein a vapor reagent used to form the top layer comprises (3-glycidyloxypropyl) trimethoxysilane after hydrolysis.

### Claim 12 (depends on 8)

The chromatographic column of claim 8, wherein a vapor reagent used to form the primer layer is bis(trichlorosilyl)ethane or bis(trimethoxysilyl)ethane and a second vapor reagent used to form the top layer is (3-glycidyloxypropyl)trimethoxysilane.

### Claim 13 (depends on 8)

The chromatographic column of claim 8, wherein a vapor reagent used to form the primer layer is bis(trichlorosilyl)ethane or bis(trimethoxysilyl)ethane and a second vapor reagent used to form the top layer is (3-glycidyloxypropyl)trimethoxysilane after hydrolysis.

### Claim 14 (depends on 8)

The chromatographic column of claim 8, wherein a vapor reagent used to form the primer layer is bis(trichlorosilyl)ethane or bis(trimethoxysilyl)ethane and a second vapor reagent used to form the top layer is n-decyltrichlorosilane.

### Claim 15 (depends on 8)

The chromatographic column of claim 8, wherein a vapor reagent used to form the primer layer is bis(trichlorosilyl)ethane or bis(trimethoxysilyl)ethane and a second vapor reagent used to form the top layer is trimethylchlorosilane or trimethyldimethyaminosilane.

### Claim 16 (depends on 8)

The chromatographic column of claim 8, wherein a vapor reagent used to form the primer layer is bis(trichlorosilyl)ethane or bis(trimethoxysilyl)ethane and a second vapor reagent used to form the top layer is methoxy-polyethyleneoxy(3)silane.

### Claim 17 (depends on 8)

The chromatographic column of claim 8, wherein a vapor reagent used to form the top layer is bis(trichlorosilyl)ethane or bis(trimethoxysilyl)ethane.

### Claim 18 (depends on 8)

The chromatographic column of claim 8, wherein a vapor reagent used to form the primer layer is bis(trichlorosilyl)ethane or bis(trimethoxysilyl)ethane and a second vapor reagent used to form the top layer is bis(trichlorosilyl)ethane or bis(trimethoxysilyl)ethane.