# US 10,481,135 B1 · Separation devices and sensors including two dimensional materials that change properties when exposed to components separated from a sample

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- Number: US 10,481,135 B1
- Document ID: US10481135B1
- Status: Granted
- Kind: B1
- Application number: 15/067,881
- Filed: 2016-03-11
- Granted: 2019-11-19
- Earliest claimed: 2015-03-13
- Assignees: Howard University
- Applicants: Joshua Halpern
- Inventors: Joshua Halpern
- Web page: https://patentgrep.com/patent/US10481135B1

## CPC

- G01N 30/10: using a splitter
- G01N 30/64: Electrical detectors
- G01N 30/66: Thermal conductivity detectors
- G01N 30/76: Acoustical detectors {(measurement of mechanical vibrations or ultrasonic, sonic or infrasonic waves G01H)}
- G01N 30/6095: {Micromachined or nanomachined, e.g. micro- or nanosize}
- 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)

## Abstract

A device and method for the separation, detection, and identification of multiple individual components in a sample where the separation device is gas chromatograph or a microchip separation device. The chromatograph or microchip separation and detection device has a detector including a two dimensional or substantially two dimensional sensor material sensitive to and has a property change (such as a change in resistance) when the surface of the two dimensional or substantially two dimensional sensor material is exposed to a component of a sample in amounts as low as 10−21 grams of component.

## Claims

### Claim 1

A detection and separation device configured to separate and detect multiple individual components in a sample, the device comprising:
a separation device having at least one inlet configured to receive the sample and at least one outlet configured to permit outflow of the multiple individual components of the sample from the separation device; and
at least one detector comprising at least one sensor configured to detect volatilized components of the sample when the sensor is exposed to an individual component received from the separation device, the sensor including at least one material selected from the group consisting of a two dimensional material, a substantially two dimensional material, and combinations thereof, the sensor having one or more channels formed in the at least one material, the sensor configured to sense a property which changes at least 3% when the at least one material is exposed to a component forming not more than about one pico gram of the sample, and the sensor configured to sense a property which changes at least 3% when the at least one material is exposed to a component forming not more than about 3 ppb of the sample.

### Claim 2 (depends on 1)

The detection and separation device recited in claim 1, wherein the sensor is configured to detect multiple ones of the multiple individual components of the sample and to detect at least one of the individual components which forms not more than about one picoliter of the sample.

### Claim 3 (depends on 1)

The detection and separation device recited in claim 1, wherein the sensor is configured to detect multiple ones of the multiple individual components of the sample and to detect at least one of the individual components which forms not more than about 10−21 grams of the sample.

### Claim 4 (depends on 1)

The detection and separation device recited in claim 1, wherein the material is selected from the group consisting of two dimensional or substantially two dimensional graphene, two dimensional or substantially two dimensional graphene oxide, two dimensional or substantially two dimensional boron nitride, two dimensional or substantially two dimensional molybdenum disulfide, and combinations thereof.

### Claim 5 (depends on 1)

The detection and separation device recited in claim 1, wherein the material is two dimensional graphene, substantially two dimensional graphene, or a combination thereof.

### Claim 6 (depends on 1)

The detection and separation device recited in claim 1, comprising a gas chromatograph comprising at least one heated chamber configured to volatize the sample to provide a volatilized sample; and at least one column downstream the inlet, wherein the column is configured to hold a stationary phase material through which the volatilized sample is moved with a carrier gas, the column including at least one outlet downstream the inlet, the outlet configured to provide egress from the at least one column for at least a portion of the volatilized sample, the detector being downstream from the inlet.

### Claim 7 (depends on 1)

The detection and separation device in claim 1, wherein the detection and separation device comprises a channel which comprises a stationary phase including at least one of the two dimensional or substantially two dimensional material between the inlet and the outlet, and wherein the sensor is downstream of the inlet.

### Claim 8 (depends on 1)

The detection and separation device in claim 1, wherein the device is in the configuration of a microchip and the sensor has a surface area of about 10 μm2 to about 100 μm2.

### Claim 9 (depends on 8)

The detection and separation device in claim 8 wherein the microchip is not larger than about one square millimeter.

### Claim 10 (depends on 1)

The detection and separation device in claim 1, wherein the detector comprises at least one measuring device which measures conductivity, which is a surface acoustical wave measuring device or a nano-mechanical resonator measuring device.

### Claim 11

A microchip detection and separation device configured to separate and detect multiple individual components in a sample, the microchip comprising:
a separation device having at least one inlet configured to receive the sample and at least one outlet configured to permit the outflow of the multiple individual components of the sample, and channels between the inlet and the outlet, the channels having at least one diameter in the range of from about one micron to about one millimeter; and
at least one sensor configured to detect at least one of the multiple individual components of the sample when at least one of the individual multiple components is volatilized or is a liquid, the sensor including at least one channel formed in at least one material selected from the group consisting of a two dimensional material, a substantially two dimensional material and combinations thereof, the sensor having a sensing property which changes at least 3% when the material is exposed to a component forming not more than about one pico gram of the sample, and the material is configured to detect multiple individual components of the sample and is capable of detecting at least one of the individual components which form not more than about 1 pico gram of the sample.

### Claim 12 (depends on 11)

The microchip detection and separation device of claim 11 wherein the material is selected from the group consisting of two dimensional or substantially two dimensional graphene, two dimensional or substantially two dimensional graphene oxide, two dimensional or substantially two dimensional boron nitride, two dimensional or substantially two dimensional molybdenum disulfide, and combinations thereof.

### Claim 13 (depends on 11)

The microchip detection and separation device recited in claim 11, wherein the material is two dimensional graphene, substantially two dimensional graphene, or a combination thereof.

### Claim 14 (depends on 11)

The microchip detection and separation device recited in claim 11, wherein the sensor has a surface area of about 10 μm2 to about 100 μm2.

### Claim 15 (depends on 11)

The microchip detection and separation device recited in claim 11, wherein the microchip is not larger than one square millimeter.

### Claim 16 (depends on 11)

The microchip detection and separation device recited in claim 11, wherein the sensor is included in a detector further comprising at least one conductivity measuring device.

### Claim 17 (depends on 16)

The microchip detection and separation device recited in claim 16, wherein the conductivity measuring device is a surface acoustical wave measuring device.

### Claim 18 (depends on 16)

The microchip detection and separation device recited in claim 16, wherein the conductivity measuring device is a nano-mechanical resonator measuring device.

### Claim 19

A method for detecting and separating components of a sample having multiple individual components, the method comprising:
transporting a sample through a separation device having at least one inlet configured to receive the sample and at least one outlet configured to permit outflow of the multiple individual components of the sample from the separation device;
impinging the multiple individual components of the sample onto at least one sensor configured to detect individual components of the sample, the at least one sensor including at least one channel formed in at least one material selected from the group consisting of a two dimensional material, a substantially two dimensional material, and combinations thereof;
the sensor sensing a property which changes at least 3% when the material is exposed to a component forming not more than about one pico gram of the sample; and
the sensor sensing a property which will change at least 3% when the material is exposed to a component forming not more than about 3 ppb of the sample.

### Claim 20 (depends on 19)

The method of claim 19 wherein individual components which are detected and separated do not form more than about 10−21 gram of the sample.

### Claim 21 (depends on 19)

The method of claim 19, wherein the separation device is a microchip and wherein the method comprises transporting the multiple individual components to a detector which includes the sensor, the detector including one or both of a conductivity measuring device or a nano-mechanical resonator measuring device.

### Claim 22 (depends on 19)

The method of claim 19, wherein the material is selected from the group consisting of two dimensional or substantially two dimensional graphene, two dimensional or substantially two dimensional graphene oxide, two dimensional or substantially two dimensional boron nitride, two dimensional or substantially two dimensional molybdenum disulfide, and combinations thereof.

### Claim 23 (depends on 19)

The method of claim 19, wherein the transporting the sample through the separation device comprises transporting the sample through sensor having a surface area of about 10 μm2 to about 100 μm2.

### Claim 24 (depends on 19)

The method of claim 19, further comprising the sensor detecting multiple ones of the multiple individual components of the sample and detecting at least one of the individual components which forms not more than about 10−21 grams of an individual component of the sample.
