Name: chemical analysis of water-accommodated fractions of crude oil spills using tims-ft-icr ms
Uploaded: 2017-03-03T14:00:00
Description: Watch this Scientific Journal Video about Chemical Analysis of Water-accommodated Fractions of Crude Oil Spills Using TIMS-FT-ICR MS at JoVE.com

이 작품은 국립 보건 연구소 (FFL을 부여 제 R00GM106414)에 의해 지원되었다. 우리는 그들의 지원을 위해 플로리다 국제 대학의 고급 질량 분석 시설을 인정하고 싶습니다.

낮은 에너지 물 수용 분수 1. 준비 (LEWAF) <ol><li> 잠재적 인 오염 물질을 제거하기 위해 염화 메틸렌으로 병을 세정하여 클린 2 L 흡인기 병. </li><li> 염화 메틸렌 50 mL로 병을 채울을 닫고 30 초 동안 교반한다. 적절한 폐기물 용기로를 배출합니다. 세 세척의 총 반복합니다. </li><li> 조사 노광 및 대조 샘플과 같은 다른 병 한 흡입기를 사용하여 병 (각 가능한 경우 중복 세트를 수행). </li><li> 33 부품 당...

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프로토콜 내에서 중요한 단계 LEWAFs의 화학적 복잡성은 정확하게 자연적으로 발생하는 것을 반영하기 위해 실험실 실험 위해서는 정확한 준비가 필요합니다. 유효한 데이터 평가는 세 가지 조건에 달려있다 : 처리 샘플에 걸쳐 인공물의 도입을 최소화하는 (예를 들면, 분석 용 시료의 LEWAF 샘플링, 추출 및 제제의 제조), 실험 프로토콜을 검증 (즉, 어두운 컨트롤을 ...

자연적인 원인에서 인위적 노출 모두 원유에 대한 환경 노출의 다양한 원인이있다. 환경으로 배출되면, 특히 해양에서 원유의 표면에 유막을 형성, 대기에 휘발성 성분의 손실 및 침전으로 분할을 겪을 수있다. 그러나, 고전 용해하지 않은 난 용성 오일 발생 않는 물이 혼합물의 낮은 에너지 혼합은 저에너지 물 - 수용 부분 (LEWAF)이라 무엇 형성한다. 물 속에서 오일 성분의 용해는 일반적으로 태양 방사 오일 - 물 계면의 노광시 향상된다. 바다에서 원유의이 사진 가용화 인해 효소 분해 1, 2 태양 복사 및 / 또는 인해 노출에 중요한 화학적 변화를 겪을 수 있습니다. 이러한 화학적 변화를 이해하고<html> 그들은 대량 행렬 (즉, 원유)의 존재하에 발생하는 노광 방법이 환경에 미치는 영향을 완화하는 기본이다. 이전 연구 원유 산소, 미생물을 입히거나 생체 축적을 거쳐 오염의 맹독성 소스를 나타내는, 특히 다환 방향족 탄화수소 류 (PAHs에)를 거쳐, 그리고 생물 3, 5, 6 인 것으로 나타났다. 그들은 단지 벌크 매트릭스의 존재 하에서 발생할 수 있기 때문에 다른 산소화 공정의 제품을 이해 도전. 따라서, 하나의 표준 분석은 자연에서 발생하는 변동을 반영하지 않을 수 있습니다. LEWAF의 제조는 환경 설정에서 일어나는 자연적인 과정을 복제해야합니다. 특히 관심 태양 복사로 인해 발생의 PAHs의 산소입니다. t &quot;&gt; 물 수용 분획의 연구에서 두 번째 과제는 샘플의 다른 화학적 성분의 분자 식별한다. 인해 높은 질량 및 산소의 정도에 의한 시료의 복잡성 때문에, 산소 제품은 일반적으로 기존의 분석에 적합하지가 MS 분석 (7, 8)과 결합 된 기체 크로마토 그래피로 수행 하였다. 대안적인 접근 방법은 (예를 들어, FT-ICR MS를 초고 질량 분석 MS 기술을 이용하여 샘플의 화학식의 변화를 특성화하는 ).이 MS 도메인에서 등압 분리 외에도, FT-ICR MS에 TIMS 결합함으로써, 이온 이동도 분광 (IMS) 치수는 샘플 9, 10, 11에 존재하는 다른 이성체에 대한 분리 및 특성 정보를 제공한다. 대기압 레이저와 결합이온화 (APLI) 자료는 분석의 PAHs가 될 겪는다 변경 정확하게 13 12 특징 있도록 샘플에서 발견 된 공역 분자에 선택적 일 수있다. 본 연구에서, 우리는 오일 성분의 변환 과정을 연구하기 위해서 광 조사에 노출 LEWAFs의 준비를위한 프로토콜을 설명한다. 또한 광 조사에 의해 발생하는 변화뿐만 아니라, 샘플 추출하기위한 절차를 도시한다. 또한 광에 대한 노출의 함수로서 LEWAF에서의 PAHs를 특성화하는 FT-ICR MS 결합 TIMS와 APLI의 사용을 제시한다.

<table border="0" cellpadding="0" cellspacing="0" width="915">
	<tbody>
		<tr height="20">
			<td height="20" style="height:20px;width:228px;">Reagents</td>
			<td style="width:156px;"></td>
			<td style="width:156px;"></td>
			<td style="width:375px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">methylene chloride</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">methanol</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">toluene</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Na2SO4</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Crude oil</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Instant Ocean&#174;</td>
			<td>Aquarium Systems</td>
			<td></td>
			<td>33 ppt salinity with 0.45 &#956;m pore filtration&#160;</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Name&#160;</td>
			<td>Company</td>
			<td>Catalog Number</td>
			<td>Comments</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Equipment</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Suntext XLS+</td>
			<td>Atlas Chicalo Ill, USA</td>
			<td></td>
			<td>1500 w xeon arc lamp, light intensity of 765 W/m2&#160;</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Atmospheric Pressure Laser Ionization</td>
			<td>Bruker Daltonics Inc, MA</td>
			<td></td>
			<td>Note a 266 nm laser is used</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">TIMS-FT-ICR MS Instrument</td>
			<td>Bruker Daltonics Inc, MA</td>
			<td></td>
			<td>The set up we had consisted of a 7T magnet with an infinity cell</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Name&#160;</td>
			<td>Company</td>
			<td>Catalog Number</td>
			<td>Comments</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Software</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">DataAnalysis 4.2</td>
			<td>Bruker Daltonics Inc, MA</td>
			<td></td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Python 2.7</td>
			<td></td>
			<td></td>
			<td>Requires Numpy, Scipy, Pandas, glob, oct2py, and os</td>
		</tr>
		<tr height="20">
			<td height="20" style="height:20px;">Octave 4.0</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
	</tbody>
</table>

chemical analysis of water-accommodated fractions of crude oil spills using tims-ft-icr ms

여러 화학 공정은 또한 초과 발생하는 화학 반응을 해수에 통합되는 방법 원유 제어한다. 이 시스템을 공부하는 것은 정확하게 자연에서 발생하는 물 수용 분수의 자연 형성을 복제하기 위해 샘플의 신중한 준비가 필요합니다. 저에너지 물 수용 분획 (LEWAF)을주의 깊게 설정된 비율 원유 및 물을 혼합하여 제조된다. 흡입기는 병을 조사하고, 설정 한 시점에서, 물은 샘플링 된 표준 기술을 이용하여 추출 하였다. 두 번째 문제는 고려 사항으로 시간이 지남에 따라 발생하는 화학적 변화를 취해야합니다 샘플의 대표적인 특성이다. LEWAF의 방향족 분획의 표적 분석은 맞춤형 트랩 이온 이동도 분광 퓨리에 변환 이온 사이클로트론 공진 질량 분석계를 (TIMS-FT 결합 대기압 레이저 이온화 원을 사용하여 수행 될 수있다-ICR MS). TIMS-FT-ICR MS 분석은 또한 자신의 충돌 단면 (CCS) 및하기 화학식 이성체 성분의 식별을 허용 고해상도 이온의 이동성과 초 - 해상도 MS 분석을 제공한다. 결과는 오일 - 물 혼합물을 빛에 노출 될 때, 물에 대한 표면의 오일 중요한 광 가용화가 있다는 것을 보여준다. 시간이 지남에 따라 용해 된 분자의 화학적 변형은 일반적으로베이스 오일에서 관찰 된 것보다 더 많은 산소 함량과 그 대신에 질소 및 황 - 함유 종의 동정의 수의 감소와 함께 이루어진다.

m / z 및 TIMS 랩핑 전압에 기초하여 이차원 스펙트럼 TIMS FT-ICR-MS에 의한 결과 LEWAF 분석. 화학식의 분포 및 IMS (도 1 참조)에 의해 식별 이성질체 기여하여 관찰 상이한 시점에서 촬영 한 각 샘플은 따라서 변화하는 화학 성분에 기초하여 특성화 될 수있다. 일반적으로, m / z 정보 분석 피크 원소 수식을 할당하는데 이용 될 수있다. APLI의 사용은 분자 ...

Watch this Scientific Journal Video about Chemical Analysis of Water-accommodated Fractions of Crude Oil Spills Using TIMS-FT-ICR MS at JoVE.com

Chemical Analysis of Water-accommodated Fractions of Crude Oil Spills Using TIMS-FT-ICR MS

원유 저에너지 물 - 수용 부분 (LEWAF)는 시간이 지남에 따라,이 복합체는 화학적 변형을 거치게되므로 분석하기 어려운 방식이다. 이 프로토콜은 LEWAF 시료의 제조 및 포획 이온 이동도 분광 FT-ICR-MS에 의해 광 조사 및 화학 분석을 수행하는 방법을 도시한다.

원유의 물 수용 분수의 화학 분석은 TIMS-FT-ICR MS를 사용하여 유출

Multiple chemical processes control how crude oil is incorporated into seawater and also the chemical reactions that occur overtime. Studying this system ...

The overall goal of these experiments is to illustrate the analytical advantages of enabling emerging technologies based on TIMS-FT-ICR MS for the molecular characterization of complex mixtures, such as water-accommodated fractions for crude oils. The TIMS-FT-ICR MS coupling combines two of the most comprehensive orthogonal and alluvial techniques for the analysis of complex mixtures. TIMS-FT-ICR MS coupling permits in a single analysis the characterization of thousands of molecular components with mobility resolving powers of over 150, mass resolution of 500, 000, and sub-ppm mass accuracy.TIMS-FT-ICR MS enables the separation, identification, and quantitation at the molecular level of complex mixtures, based on differences in size, charge and mass with minimal sample appropriation. To begin the LEGAF preparation, add 50 milliliters of dicholomethane to a two liter glass aspirator bottle. Close the bottle and agitate the bottle for 30 seconds.Discard the dichloromethane wash, and repeat this process two more times. Wash one more two liter aspirator bottle in this way, then add about 1.6 liters of filtered artificial seawater with a salinity of 33 parts per thousand to each bottle. Add a stir bar, and then use a gas-tight syringe to add sufficient crude oil sample to each bottle to achieve a final concentration of one gram per liter of oil and seawater.Wrap the bottles in aluminum foil to exclude light, and stir the mixtures at approximately 100 RPM for 24 hours to finish preparing the LEWAF. It's important that care is used when first mixing the oil and water to avoid over-mixing the solution. Next, unwrap one of the LEWAF bottles in aluminum foil, leaving one as the dark control.Place the bottles in the solar irradiator with the temperature set to maintain the samples at 25 degrees Celsius. Irradiate the mixtures continuously for the desired experiment length. At set intervals during the experiment, obtain 150 milliliter fractions from each bottle by uncorking the bottle and opening the drain valve.Extract each sample aliquot using 50 milliliters of dichloromethane three times using a separatory funnel. Shake the funnel for two minutes each time, remembering to regularly vent the funnel to avoid pressure buildup. Drain the sample into a flat-bottom flask through a funnel containing sulfate and rinse the sodium sulfate with additional DCM.Concentrate the extract to 15 milliliters using a hot water bath set at 58 degrees Celsius. Transfer the concentrate into a concentration tube, rinsing the flask with DCM. Concentrate each sample to one milliliter under a gentle stream of nitrogen gas.For each concentrated sample, using a glass positive displacement micropipette, add 990 microliters of a one to one by volume mixture of methanol and toluene to a glass vial. Then mix in 10 microliters of the sample. To begin the FTR-ICR MS analysis, set the instrument to Operate mode.Draw a sample into a sample syringe. Set the infusion rate to 200 microliters per hour, the nebulizer pressure to two bar, and the vaporizer temperature to 300 degrees Celsius. Set the dry gas rate to 1.2 liters per minute and the temperature to 220 degrees Celsius.Then set the instrument to Tune mode. Based on the resulting spectrum adjust the instrument parameters and recalibrate the mass spectrometer to improve the ion transmission and detection for the desired range of mass to charge ratios. Once the instrument parameters have been optimized, exit Tune mode.Set the desired number of scans to be average per mass spectrum, and then acquire the spectrum. To begin the trapped ion mobility spectrometry analysis turn on the external breaker to the TIMS instrument to engage TIMS mode. Set the FT-ICR instrument to chromatography mode.Turn on the supplementary roughing pump and set the inlet and outlet pressures to the desired values using the TIMS control valve. Allow the pump to warm up for at least three hours, then perform a fast sweep over a wide voltage range at a low IMS and MS resolution to identify the needed voltage range for the analysis. Once the range has been identified, set the voltage per frame to 0.1 volts.Set the number of frames to cover the entirety of the DeltaV ramp and run the analysis. After performing the analyses, process the data with the appropriate software and scripts to determine the chemical composition and mobility values of identified peaks. After sunlight irradiation of an LEWAF of a crude oil sample, changes in the chemical complexity are observed as a function of exposure time.This complexity was detected and visualized in a 2D spectrum based on mass to charge ratio and ion mobility. The use of APLI resulted in greater analytical sensitivity to molecules with double bonds. Four molecular classes were identified in the sample.Distribution plots of double bond equivalents as a function of the number of carbons were used to monitor changes in the molecular composition over time. Two-dimensional plots of inverse mobility versus carbon number were created, with the double bond equivalents represented as the color of each point. Linear trends were observed for each of the four common molecular classes.After watching this video you should have a good understanding of the basic steps and unique advantages of APLI-TIMS-FT-ICR MS for the analysis of LEWAF samples as well as other complex mixtures. While attempting this procedure it's important to remember that sample integrity, such as reducing sources of contamination, is fundamental for accurate results. The characterization at the molecular level of the water-accommodated fractions of crude oils, the transformation products, and their fate during exposure to sunlight in the ocean is of the utmost environmental importance.Compared to other separation techniques such as liquid chromatography and gas chromatography, TIMS separation occurs in a shorter time scale, and is timing dependent, which permits better coupling with ultra high resolution MS analyzers while providing collision cross sections and chemical formulas in a single analysis. The generation of new comprehensive analytical tools for the analysis of complex mixtures at molecular level, such as TIMS-FT-ICR MS has great implications for our understanding of the chemical transformations and fate of crude oil in the ocean.

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