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GASMET傅立叶红外仪器说明书

GASMET傅立叶红外仪器说明书
GASMET傅立叶红外仪器说明书

GASMET TM DX-4010 FT-IR Gas Analyzer

ON-SITE Series

Instruction & Operating

Manual

2002-03-15

WARRANTY STATEMENT

This warranty applies to the GASMET TM brand name products sold with this warranty statement. This warranty is applicable in all countries and may be enforced in any country where Temet Instruments Oy or its authorised service providers offer warranty service subject to the terms and conditions set forth in this warranty statement.

Temet Instruments Oy shall not be liable for technical or editorial errors or omissions contained herein. The information in this document is provided “as is” without warranty of any kind and is subject to change without notice. Should you find any error, we would appreciate if you notified us.

Temet Instruments Oy quarantees that all products manufactured and sold by it are free of defects in materials and workmanship under normal use during the warranty period.

Temet Instruments’ products are manufactured using new materials or new and used materials equivalent to new in performance and reliability. Spare parts may be new or equivalent to new.

Temet Instruments Oy agrees to either replace or repair free of charge (Ex Works Helsinki, Incoterms 2000), any such defective product or part, that is returned to its repair facility within one (1) year of the delivery date. All parts or products removed under this warranty become the property of Temet Instruments Oy. The replacement product or part takes on the warranty status of the removed product or part.

The warranty does not extend to any product from which the serial number has been removed or that has been damaged or rendered defective (a) as a result of accident, misuse, abuse, normal wear of components or other external causes; (b) by operation outside the usage parameters stated in the user documentation that is provided with the product; (c) by the use of parts not manufactured by Temet Instruments Oy; or (d) by modification or service by anyone other than Temet Instruments Oy.

Temet Instruments Oy is not liable for any damages caused by the product or the failure of the product to perform, including any loss of profits or savings, incidental damages, or consequential damages.

GASMET TM and CALCMET TM are trademarks of Temet Instruments Oy

CONTENTS

1INTRODUCTION (8)

2PRINCIPLE OF MEASUREMENT (8)

2.1P RINCIPLES OF I NFRARED S PECTROSCOPY (9)

2.2C OMPONENTS OF A F OURIER T RANSFORM I NFRARED S PECTROMETER (11)

2.3Q UANTITATIVE A NALYSIS OF FT-IR S PECTRA (13)

2.4M ULTICOMPONENT A NALYSIS (14)

2.5R ESOLUTION OF FT-IR A NALYSIS (15)

2.6D ESCRIPTION OF THE GASMET TM DX-4010 (16)

2.6.1 Applications of the GASMET TM DX-4010 Analyzer (16)

2.6.2 The GASMET TM DX-4010 Analyzer Performance (17)

2.6.3 Structure of the GASMET TM DX-4010 Analyzer (17)

2.7GASMET TM DX-4010 T ECHNICAL D ATA (18)

2.7.1 General Parameters (18)

2.7.2 Spectrometer (18)

2.7.3 Sample Cell (18)

2.7.4 Measuring parameters (19)

2.7.5 Electrical connectors (19)

2.7.6 Gas Inlet and Outlet Conditions (19)

2.7.7 Computer and Electronics (19)

2.7.8 Enclosure (19)

3INSTALLATION (21)

3.1S UPPLY S CHEDULE (21)

3.1.1 Package (21)

3.1.2 Contents of the GASMET TM Package (21)

3.1.3 Settings (21)

3.2A MBIENT C ONDITIONS (22)

3.2.1 Storing and Transporting the GASMET TM (22)

3.2.2 Installation location (22)

3.2.3 Explosion Protection (22)

3.3S AMPLE G AS S UPPLY (23)

3.4G AS C ONNECTORS (24)

3.5O N-B OARD S AMPLE P UMP (25)

3.6P OWER C ONNECTION (25)

3.6.1 Power Supply (25)

3.6.2 Fuses (25)

3.7S IGNAL C ONNECTIONS (26)

3.7.1 Optional Analog Output Signals (26)

3.7.2 RS232C-Interface (26)

3.7.3 Sample sequencing control (26)

3.7.3.1Valve Dry Contact (27)

3.7.3.2Pump Dry Contact (27)

4MAINTENANCE (28)

4.1S AFETY P RECAUTIONS (28)

4.2M AINTENANCE P LAN (28)

4.3V ISUAL I NSPECTION (29)

4.4S AMPLE C ELL I NSPECTION (29)

4.5R EPLACEMENT OF O PTOELECTRONIC C OMPONENTS (29)

5START-UP (30)

5.1C ONNECTIONS (30)

5.2I NSTALLING THE SOFTWARE (30)

5.2.1 Installing Calibration Files (30)

5.3S WITCHING THE ANALYZER’S POWER ON (31)

5.4O PERATION (31)

5.4.1 Using the CALCMET Software (31)

5.4.2 Setting the Measuring Times (34)

5.4.3 Zero Calibration (34)

5.4.4 Measuring the Sample Spectrum (35)

5.4.4.1Single Measurement (35)

5.4.4.2Continuous Measurement (36)

5.4.5 Checking the Hardware (37)

5.4.6 Analyzing the Sample Spectrum (37)

5.5S AMPLE CALCMET SESSION (37)

5.5.1 Step 1: Select the Components that will be analyzed (37)

5.5.2 Step 2: Measure Background (37)

5.5.3 Step 3: Measure and Analyze the Sample (38)

5.5.4 Step 4: Verify the Results (38)

6ANALYZER INSPECTION (39)

6.1GASMET FT-IR G AS A NALYZER I NSPECTION S HEET (40)

FIGURES

Figure 1 Normal modes of vibration of carbon dioxide CO2 (9)

Figure 2 An absorbance spectrum of Sulfur dioxide SO2 (11)

Figure 3 Basic components of a FT-IR spectrometer (11)

Figure 4 Michelson interferometer (12)

Figure 5 A typical intereferogram (12)

Figure 6 An example of spectra for multicomponent analysis (15)

Figure 7 A basic structure of GASMET TM DX-4010 analyzer (17)

Figure 8 Dimensionnal Drawing of the Analyzer Enclosure (20)

Figure 9 Gas Connectors of the GASMET DX-4010 (24)

Figure 10 Flow schematics of the on-board sample pump package (25)

Figure 11 GASMET TM DX-4010 Connector unit (26)

Figure 11 Welcome to Calcmet dialog (32)

Figure 12 A typical background spectrum (35)

TABLES

Table 1 GASMET fuses. Physical size of each fuse is 5*20 mm (26)

Table 2 Maintenance plan (29)

Table 3 Welcome to Calcmet system parameters (33)

Table 4 Commands for setting measuring times (34)

Table 5 Zero Calibration measurement commands (34)

Table 6 Single measurement commands (36)

Table 7 Continuous measurement commands (36)

Table 8 Commands for checking hardware status (37)

PREFACE

Thank you for choosing GASMET TM, the state-of-the-art FT-IR gas analyzer manufactured by Temet Instruments. The GASMET TM is a high-tech product made of high quality components.

Temet Instruments’ substantial investment in R&D is targeted at innovative, customer-driven solutions. Working closely with customers and global distribution network, the company offers extensive technical applications support services. Along with high reliability, Temet products offer easy operation and consistent and accurate results, together with competitive pricing.

To develop the powerful technology of FT-IR has required uncompromising commitment and expertise in several fields of high technology. As a result, Temet products are not only superior in performance, but simple to operate and maintain. Temet Instruments’ continuing philosophy is to provide reliable measurements in a variety of industrial applications now and in the future. Whatever your applications are, we hope you will find the GASMET TM gas analyzer fast, accurate, reliable, and easy to use.

1 INTRODUCTION

This instructions manual provides information of the GASMET TM DX-SERIES Fourier Transform Infrared (FT-IR) Gas Analyzer. Please read this manual carefully prior to using the analyzer. Improper use of the analyzer may damage the equipment.

Chapter 2, "Error! Not a valid bookmark self-reference.", discusses theoretical aspects of infrared spectroscopy. These fundamentals help understand the physical principles the GASMET TM system is based on. “Description of the Gas Analyzer” provides information about the GASMET TM DX-SERIES hardware and technical specifications.

Chapter 3, “Installation”, provides information of installing the GASMET TM DX-SERIES Gas Analyzer. Use this paragraph to check the contents of the GASMET TM package and to get the GASMET TM from storage into operational condition.

Chapter 4, “Maintenance”, describes the maintenance operations that may be necessary in the long run.

Chapter 5, "Start-Up", provides some basic information of the operation of the GASMET TM DX-SERIES. This chapter is recommended to read, before any operation.

Chapter 6, “Error! Reference source not found.”, describes what shloud be done when the analyzer is used first time. This chapter includes inspection sheet, what should be filled within 30 days from the date of delivery, in order that the warranty is in full valid.

To learn how to operate the GASMET TM analyzer with the CALCMET TM controlling and analyzing software, refer to the CALCMET User’s Guide.

This instructions manual is copyrighted 2001 by Temet Instruments. All rights reserved. No part of this manual may be reproduced in whole or in part in any form without the prior permission of Temet Instruments Oy.

2 PRINCIPLE OF MEASUREMENT

2.1 Principles of Infrared Spectroscopy

When infrared radiation is passed through a sample of gaseous molecules, it can be observed that certain wavelengths of the infrared radiation are not transmitted through the gas very well. That is, the gas absorbs some specific wavelengths of the infrared radiation. What happens is that the infrared radiation interacts with the gas molecules. The gas molecules get energy from the infrared radiation and start to vibrate or rotate with increasing amplitude. This energy transfer from the infrared radiation to the gas molecules can be seen as decreased intensity of some wavelengths of the transmitted infrared radiation. If the infrared source sends a broad band of wavelengths of infrared radiation through the sample, some of the wavelengths will be partly absorbed by the gas sample.

Figure 1shows how a gas molecule may behave when it interacts with infrared radiation. All different vibrations, rotations, and their combinations result in absorption of specific wavelengths

of the infrared radiation.

CONTRACT

STRETCH

STRETCH

STRETCH C O

O C O

O C

O

O

O

O υ1

υ2

υ3

4

Figure 1

Normal modes of vibration of carbon dioxide CO 2.

An absorption spectrum shows graphically to what extent the different wavelengths of the infrared radiation are absorbed by the sample gas. The spectrum shows the transmission of the infrared radiation through the gas as a function of wavelength. For each wavelength, the

transmittance T is the intensity of the infrared radiation that has passed through the sample gas, divided by the intensity of the infrared radiation that has entered the sample gas. When there is no absorption, the value of transmittance T is 1 (or 100 %), which indicates that 100 % of the infrared radiation at that wavelength goes through the sample gas. If the intensity of the radiation entering the sample is I 0 and the intensity of the radiation that has passed through the sample is I, the transmittance T can be expressed as:

T I I =/0

T transmittance

I =intensity entering the sample I =intensity that has passed through the sample

0=

Besides using transmittance T, the absorption of the infrared radiation can be presented using the absorbance scale. Absorbance A is given by the logarithm of the transmittance reciprocal: A T =log 10(/)1

A absorbance T transmittance ==

The advantage of using the absorbance scale is that the value of absorbance is directly

proportional to the thickness of the sample gas (absorption path length), and the concentration of the sample gas.

The infrared absorption spectrum is unique to all different gas molecules. It is possible to identify any gas component from the spectrum of the sample. An example of infrared absorbance spectrum is shown in Figure 2.

Figure 2 An absorbance spectrum of Sulfur dioxide SO2.

2.2 Components of a Fourier Transform Infrared Spectrometer

There are some basic parts that are typical for all FT-IR spectrometers. First of all, there is an infrared source that emits a broad band of different wavelengths of infrared radiation. The infrared radiation goes through an interferometer that modulates the infrared radiation. The interferometer performs an optical inverse Fourier transform on the infrared radiation entering the interferometer. The modulated infrared beam passes through the gas sample. Finally, the intensity of the infrared beam is detected by a detector. The detected signal is digitized and Fourier transformed by the computer to get the IR-spectrum of the sample gas.

Figure 3 Basic components of a FT-IR spectrometer.

The unique part of a FT-IR spectrometer is the interferometer. A Michelson type plane mirror interferometer is displayed in Figure 4. Infrared radiation from the source is collected and collimated before it strikes the beamsplitter. The beamsplitter ideally transmits one half of the radiation, and reflects the other half. Both transmitted and reflected beams strike mirrors, which reflect the two beams back to the beamsplitter. Thus, one half of the infrared radiation that finally

then back to the beamsplitter. The other half of the infrared radiation going to the sample has first gone through the beamsplitter and then reflected from the fixed mirror back to the beamsplitter. When these two optical paths are reunited, interference occurs at the beamsplitter because of the optical path difference caused by the scanning of the moving mirror.

Radiation to the sample gas and detector Moving mirror

Fixed mirror

Figure 4 Michelson interferometer.

The optical path length difference between the two optical paths of a Michelson interferometer is two times the displacement of the moving mirror. The interference signal measured by the detector as a function of the optical path length difference is called the interferogram. A typical interferogram produced by the interferometer is shown in Figure 5. The graph shows the intensity of the infrared radiation as a function of the displacement of the moving mirror. At the peak position, the optical path length is exactly the same for the radiation that comes from the moving mirror as it is for the radiation that comes from the fixed mirror.

Figure 5 A typical intereferogram.

The spectrum can be computed from the interferogram by performing a Fourier transform. The Fourier transform is performed by the same computer that ultimately performs the quantitative analysis of the spectrum.

2.3 Quantitative Analysis of FT-IR Spectra

The basic law for spectroscopic quantitative analysis is Beer's law. Beer's law shows how the concentration of the sample gas is related to the measured absorbance of the sample spectrum. Beer's law is commonly expressed as:

log(/)log(/)I I T A abc 01===

I =intensity entering the sample

I =intensity that has passed

through the sample

A absorbance T transmittance

a a()absorptivity

b optical path length

c =sample concentration

0=====v

The absorptivity a is a constant that characterizes the capacity of the molecule to absorb infrared radiation. The value of a varies from one molecule to another and one wavelength to another, but is constant for a given molecule at a given wavelength. The quantity b is the optical path length, that is, the distance the infrared radiation beam traverses in the gas sample. The quantity c

indicates the concentration of the sample gas molecules in the sample. If the optical path length is held constant, Beer's law states that the absorbance is directly proportional to the concentration of the sample gas at a given wavelength. Since Beer's law is additive, absorbance A is equal to the sum of the values of the a , b , and c for each gas component.

Two conditions are implied in the derivation of Beer's law. The radiation being measured is monochromatic, and the sample absorptivity does not vary with concentration. If the sample concentration range is wide, the change in the sample environment can cause absorptivity

changes and deviations from Beer's law. For narrow concentration ranges and for low absorbance values a plot of concentration versus absorbance is nearly linear.

The changes in the gas pressure may cause broadening in the absorption line shape of the sample gas. The rotational fine structure of gas-phase bands are broadened by collisions between the molecules of the component being measured. All IR-bands are broadened.

The changes in the gas temperature may cause 'hot bands' in the spectrum of the sample gas. As the temperature increases, the distribution of the molecules in different energy levels changes. The changes in the temperature cause changes in the absorption line shape of the sample gas. To analyze the concentration of a gas compound, the GASMET TM calculates the number of gas molecules in the sample cell. The number of the gas molecules in the sample cell depends linearly on both the gas pressure and the volume of the sample cell, and reciprocally on the gas temperature:

pV nRT =

p=pressure

V=volume

n=number of the gas molecules

T=temperature

R=Ideal gas constant

Any changes in sample gas temperature or pressure in the sample cell directly affect on the measured gas compound concentration. In addition, gas pressure or temperature changes may effect the line shape of the measured absorbance spectrum, and thus the accuracy of the analysis results.

2.4 Multicomponent Analysis

The degree of absorption of infrared radiation at each wavelength is quantitatively related to the number of absorbing molecules in the sample gas. Since there is a linear relationship between the absorbance and the number of absorbing molecules, multicomponent quantitative analysis of gas mixtures is feasible.

To perform multicomponent analysis we start with the sample spectrum. In addition, we need reference spectra of all the gas components that may exist in the sample, if these components are to be analyzed. A reference spectrum is a spectrum of one single gas component of specific concentration. In multicomponent analysis we try to combine these reference spectra with appropriate multipliers in order to get a spectrum that is as close as possible to the sample spectrum. If we succeed in forming a spectrum similar to the sample spectrum, we get the concentration of each gas component in the sample gas using the multipliers of the reference spectra, provided that we know the concentrations of the reference gases.

For example, suppose we have a sample spectrum and reference spectra like those shown in Figure 6. In this case, we know that the sample gas consists of gases Reference 1 and Reference 2. We have the reference spectra available and we know that these reference spectra represent concentrations of 10 ppm and 8 ppm respectively. To find out the concentration of each component in the sample gas, we try to form the measured sample spectrum using a linear combination of the reference spectra. We find out that if we multiply the spectrum Reference 1 by 5 and the spectrum Reference 2 by 2, and combine these two spectra, we get a spectrum that is similar to the sample spectrum. Accordingly, the sample gas contains reference gas 1 at five times the amount in the reference spectrum 1, and reference gas 2 at two times the amount in the reference spectrum 2. The analysis indicates that the sample indeed consists of these two reference gases. The concentration of the reference gas 1 in the sample is found to be 50 ppm, and the concentration of the reference gas 2 in the sample is 16 ppm.

increases and makes the analysis less precise.

Furthermore, the information content of the measurement is not maximized by using as high a resolution as possible. Scientific research1 has proved that when the resolution is reduced by the some factor 1/k, signal-to-noise-ratio can be increased by a factor of k3/2 in the same registration time. This makes the use of low resolution quite worthwhile. To achieve precise quantitative analysis results, a low resolution measurement should be used provided that the spectral overlap problem can be taken care of.

There are two reasons for the increase of the signal-to-noise ratio:

? In an FT-IR spectrometer, the length of the measured interferogram determines the resolution. The longer the interferogram, the more data points, and the higher the resolution.

In a high resolution study the time required by a single measurement is also high, so that we are able to co-add less measurements in a fixed time, leading to higher noise level. As a result, the longer the measured interferogram is, the lower signal-to-noise-ratio results.

? High resolution requires narrow slit or a small aperture to prevent a phenomenon called aperture broadening. Narrow slit, in turn, reduces the signal and thus signal-to-noise-ratio ratio.

1 See for example, P Saarinen & J Kauppinen. 1991. Multicomponent Analysis of FT-IR Spectra. Applied Spectroscopy. Volume 45, Number 6. Pages 953 - 963.

2.6 Description of the GASMET TM DX-4010

GASMET TM ON-SITE SERIES includes portable and transportable multicomponent gas analyzers for demanding applications. The GASMET TM DX-4010 incorporates a Fourier Transform Infrared, FT-IR spectrometer. The analyzer offers versatility and high performance for all users.

The GASMET TM DX-4010 in designed for on site measurements. It is an ideal tool to environmental applications. Sample cell absorption path length is 9.6 m and the temperature 50 °C.

The GASMET TM DX-4010 incorporates advanced hardware and software to provide a portable high-speed gas analysis system. The GASMET TM DX-4010 brings analytical laboratory performance in non-laboratory conditions. The GASMET TM DX-4010 eliminates the equipment, calibration, and service costs associated with multiple, single component gas analyzers. GASMET TM DX-4010 allows simple calibration using only single component calibration gases, the user can easily configure the analyzer for a new set of compounds.

The software of GASMET TM is based on the powerful multicomponent analysis method CALCMET TM. The CALCMET TM analysis method is used to compute the concentrations and error limits of the different components present in the sample gas. The reference spectra needed in the analysis are stored on the fixed disk of computer and are simply loaded from the library when used in the analysis of an unknown sample. CALCMET for Windows software is described in the “CALCMET for Windows Software Manual”

2.6.1 Applications of the GASMET TM DX-4010 Analyzer

The GASMET TM DX-4010 enables identification and quantification of multiple gaseous compounds simultaneously and accurately, with results available in seconds.

The GASMET TM DX-4010 is a versatile gas analyzer that can be used in several applications. The GASMET TM DX-4010 is specially designed for:

? Environmental emissions monitoring

? Quality control

? Workplace air monitoring

2.6.2 The GASMET TM DX-4010 Analyzer Performance

? Lowest detectable concentrations: 0.2-2 ppm (depends on the application).

? Accuracy: 2 % of the measurement range (depends on the application)

? Precision: 0.01 % of the measurement range (depends on the application)

? Diatomic homonuclear gases (i.e. N2, O2, H2, Cl2) and noble gases (i.e. He, Ne, Ar, Kr) do not absorb infrared radiation. They are the only gases that cannot be measured by the GASMET TM

2.6.3 Structure of the GASMET TM DX-4010 Analyzer

Figure 7 outlines a complete gas analysis system. The IR source produces broad band IR radiation which is modulated in the interferometer. The interferometer actually performs an optical inverse Fourier transform. The modulated IR radiation passes through the sample cell where sample gas absorbs certain wavelengths of the IR radiation. The detector detects the transmitted IR radiation. The signal is digitized by A/D converter. The computer performs a mathematical Fourier transform on the digitized modulated signal, and a spectrum is obtained. The GASMET TM uses a Fast Fourier Transform to compute the spectrum from the interferogram. The transmittance spectrum is computed as a ratio of the sample spectrum to the background spectrum. The absorbance spectrum is computed from the transmittance spectrum. The GASMET TM uses the CALCMET TM software to compute the concentrations of the components present in the sample gas from the absorbance spectrum.

Figure 7 A basic structure of GASMET TM DX-4010 analyzer.

The data and signal processing electronics control the operation of the GASMET. An external PC compatible computer controls the GASMETTM DX-4010.

A unique part of the GASMET is the Temet Carousel interferometer. The Carousel interferometer is rugged and withstands the demanding environmental conditions of non-laboratory environment. The Carousel interferometer modulates the infrared radiation coming from the infrared source, as discussed previously.

The modulated light passes through the temperature controlled sample cell. The gas sample is introduced into the gas cell through standard gas line connectors. The transmitted infrared radiation is finally detected by a thermoelectrically cooled detector.

2.7 GASMET TM DX-4010 Technical Data

2.7.1 General Parameters

Measurement principle:FT-IR (Fourier Transform Infrared)

Performance: Simultaneous analysis of up to 50 gas compuonds

Response time: <120 s, depending on the gas flow and measurements time

Operating temperature: 20 ± 20°C, optimum 15 - 25°C non condensing

Storage temperature: -20 - 60°C, non condensing

Power supply: 12 VDC or 100-240 VAC / 50 - 60 Hz

2.7.2 Spectrometer

Interferometer: Temet? Carousel Interferometer

Resolution: recommended 8 cm-1 or 4 cm-1

Scan frequency: 10 spectra/s

Aperture: 1’’

Detector: Thermo-electrically cooled MCT or DTGS

IR-source Ceramic, SiC, 1550 K temperature

Beamsplitter: ZnSe

Window material: ZnSe

Wavenumber range: 700 – 4200 cm-1

2.7.3 Sample Cell

Structure: Multi pass, fixed path length 1.2m, 2.5m, 5.0m, or 9.8m

Material: 100 % Gold coater aluminium

Mirrors: fixed, protected gold coating

Volume: 1.07 l

Connectors: Swagelok 6 mm or 1/4"

Gaskets: Teflon? coated Viton? or Kaltrez? O-rings

Temperature: 50 °C, maximum

Maximum sample gas pressure: 2 bars

Flow rate 1-5 l/min

Response time: <60 s

Sample condition: non condensing

2.7.4 Measuring parameters

Zero point calibration: 24 hours calibration with nitrogen (4.0 or higher N2 rekomended)

Zero point drift: 2 % of smallest measuring range per zero point calibration interval Sensitivity drift: none

Linear derivation: 2 % of smallest measuring range

Temperature drift: 2 % of smallest measuring range per 10 °C temperature change

Pressure influence: 1 % change of measuring value for 1 % sample pressure change

2.7.5 Electrical connectors

Digital interface: RS-232 C, 9-pole D-Connectors. CR4000/2000/1000 is connected to an

external computer via RS-232 C cable. The external computer controls the

GASMET.

Power connection: Standard plug CEE-22

Relay connection: External PC

Analog input/output External PC

2.7.6 Gas Inlet and Outlet Conditions

Gas temperature: non-condensing, the sample gas temperature should be the same as the sample

cell temperature

Sample pump: Internal

Flow rate: 120-160 l per hour

Gas filtration: filtration of particulates (2μ) required

Sample gas pressure: ambient

2.7.7 Computer and Electronics

A/D converter: dynamic range 95 dB

Signal Processor: 32-bit floating point DSP 120 MFLOPS speed

Computer: External, not included

Operating system: Windows 95 or 98

Analysis software: CALCMET for windows 95/98

2.7.8 Enclosure

Material: Aluminum

Dimensions (mm): 433 ? 185 ? 425

Weight: 16 kg

CE label: according to EMI guideline 89/336/EC

CE mark indicates compliance with directive 89/336/EEC for electromagnetic Compability. The CE marked GASMET models are certified by the manufacturer as follows:

Immunity: EN 50082-2 (March1995) table 1:1.1, 1.2 and 1.4, and table 5 for immunity conducted disturbances induced by radio-frequency fields, electrostatic discharge and electrical fast transients/burst.

Emission: EN 55022 (1987) class A for radiated and conducted emissions.

Figure 8 Dimensionnal Drawing of the Analyzer Enclosure.

傅立叶转换红外光谱仪FT-IR

傅立叶转换红外光谱仪(FT-IR) 一、红外光谱的基本原理:当一束红外光照射物质时,被照射物质的分子将吸收一部分相应的光能,转变为分子的振动和转动能量,使分子固有的振动和转动能级跃迁到较高的能级,光谱上即出现吸收谱带。通常以波长(μm)或波数(cm-1)为横坐标,吸光度(A)或百分透过率(T%)为纵坐标,将这种吸收情况以吸收曲线的形式记录下来,得到该物质的红外吸收光谱,简称红外光谱。 二、红外光谱在结构解析中的作用: 1.利用基团特征频率确定分子中的官能团,区分化合物的类别。 2.提供未知物的精细结构,确定化合物是否相同。 三、红外光谱仪的主要附件: 1.衰减全反射 (ATR) 附件:ATR附件主要用于固体、凝胶、橡胶等材料表面的研究。测量表面厚度需在1μm以上,也可用于溶液分析(蛋白水溶液)。2.漫反射附件:漫反射附件主要用于测量颗粒表面,或不平整的表面,适用于表面厚度约在10μm左右的材料。 3.固定角度镜面反射附件:镜面反射附件主要借助反射吸收分析坚硬平整表面的涂层,也可以测量光亮的样品表面,适用于表面厚度>10μm。 4.万能采样器:适用于各种液体、固体等样品。 5.变温红外附件:测定不同温度下样品的红外光谱。 四、红外光谱仪操作规程和注意事项 红外光谱仪由专人负责维护,所有操作人员均应经过培训方可使用。具体操作规

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本人郑重声明: 所呈交的毕业设计(论文)是本人在指导教师指导下进行的研究工作及取得的研究成果。其中除加以标注和致谢的地方外,不包含其他人已经发表或撰写并以某种方式公开过的研究成果,也不包含为获得其他教育机构的学位或证书而作的材料。其他同志对本研究所做的任何贡献均已在文中作了明确的说明并表示谢意。 本毕业设计(论文)成果是本人在江西师范大学读书期间在指导教师指导下取得的,成果归江西师范大学所有。 特此声明。 声明人(毕业设计(论文)作者)学号:06 声明人(毕业设计(论文)作者)签名:

摘要 红外光谱仪是鉴别物质和分析物质结构的有效手段,其中傅立叶变换红外光谱仪(FT-IR)是七十年代发展起来的第三代红外光谱仪的典型代表。它是根据光的相干性原理设计的,是一种干涉型光谱仪,具有优良的特性,完善的功能,并且应用范围极其广泛,同样也有着广泛的发展前景。本文就傅立叶变换红外光谱仪的基本原理作扼要的介绍,总结了傅立叶变换红外光谱法的主要特点,综述了其在各个方面的应用,并对傅立叶变换红外光谱仪的发展方向提出了一些基本观点。 关键词:傅立叶变换红外光谱仪;基本原理;应用;发展

(完整版)浅谈原位漫反射傅立叶变换红外光谱

浅谈原位漫反射傅立叶变换红外光谱 漫反射傅立叶变换红外光谱(DRIFTS)是近年来发展起来的一项原位(in situ)技术,通过对催化剂上现场反应吸附态的跟踪表征以获得一些很有价值的表面反应信息,进而对反应机理进行剖析,已在催化表征中日益受到重视。该表征技术适合于固体粉末样品的直接测定以及材料的表面分析。将漫反射方法,红外光谱与原位红外技术结合,试样处理简单,无需压片,并且不改变样品原有形态,所以较之其他原位红外方法更容易实现在各种温度,压力和气氛下的原位分析。 1实验原理与装置 原位漫反射红外光谱的实验系统一般由漫反射附件、原位池、真空系统、气源、净化与压力装置,加热与温度控制装置、FTIR光谱仪组成。 在红外光谱仪样品室加装一个漫反射装置,将装好样品的原位池置于其中,调整漫反射装置,使样品上的漫反射光与主机的光路匹配,以实现漫反射测量。原位池可在高温、高压,高真空状态下工作。图1所示为漫反射红外装置的光路图。光谱仪光源发出的红外辐射光束经一椭圆镜会聚在样品表面并在内部进行折射、散射、反射和吸收,当这部分辐射再次穿出样品表面时,即是被样品吸收所衰减了的漫反射光。如图2所示。图3为漫反射原位池结构示意图,图4为热电公司红外的漫反射附件实物图 图1 图2 图3

图4 目前原位红外漫反射方面国内做的最好是大连化物所的辛勤老师,自行设计出一套漫反射红外装置。利用该装置在催化反应机理推导方面研究出很多有意义的结果。 2.实验操作 开机前需要更换干燥剂,装好液氮先对检测器冷却,依次打开电脑、仪器、软件并检查各项参数是否在指定范围内,根据需要设置扫描次数、分辨率、纵坐标。对于智能型有的参数一般是不需要更改设置的。调节样品池高度使探测器接收到的能量最大(粗调),然后将所测固体粉末样品装入样品池中,刮平样品表面,装上窗体,再调节样品池高度(细调),保证光正好打在样品上。样品颗粒越细越好,这样得出的谱图会更精细。对于深色样品不利于测样可以掺入溴化钾稀释。一般样品,比如我们制的的催化剂要进行预处理,即在惰性气体氛围中高温加热一两个小时,一来可以除去催化剂上的水分和二氧化碳气体,二来也是对催化剂的活化。注意,气速不能开的太大否则会吹散样品粉末堵塞气体管路对后续实验造成影响或是把样品表面吹不平整也会影响谱图质量。如果做探针分子的选择化学吸附,一般步骤是降温并在设定的温度段采集背景,然后在特定的温度下关闭惰性气体通入探针气体直到达到吸附饱和再改吹惰性气体吹扫,不断采集样品信息,然后升温,在开始采集背景时设定的温度段继续采样,背景和采样温度应一致。如果特定需要还可以抽真空或加到一定压力。我们所测的固体催化剂样品一般分辨率都选择4cm-1,扫描次数则常选择32、64。对于漫反射最好选择设置纵坐标以Kubelka-Munk表示,以便可以在需要定量时使用。 实验气路则是根据实验需要自行设计,没有一定的模式,切不同设计方法气路也有所不同。现举一例我们实验室常用来测样品酸性的气路图5如下 图5 1气体干燥装置,2气速控制装置,3阀门,4探针,5原位池 3.在催化中的应用 红外光谱法用于催化研究领域已有几十年的历史。1964年,Delfs等最先尝试用漫反射

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后变成两束光。其中一束被反射到可动镜头M1后又被M1反射回分束器,并在分束器上再次分城反射光和透射光,透射光部分照在举聚光镜M4上,然后到到达探测器,另一束光透过分束器,射在固定镜M2上,并被M2反射回分束器,在分束器上再次发生反射和透射,反射部分照在聚光镜M4上,最后也到达探测器。因而这两束到达探测器的光油了光程差,成了相干光,移动可动镜M1可改变两束光程差。在连续改变光程差的同时,记录下中央干涉条纹的光强变化,及得到干涉图。如果在复合的相干光路中放有样品,就得到样品的干涉图。需要通过计算机进行傅里叶变换后才能得到红外光谱图。 主要特点 1、信噪比高 傅里叶变换红外光谱仪所用的光学元件少,没有光栅或棱镜分光器,降低了光的损耗,而且通过干涉进一步增加了光的信号,因此到达检测器的辐射强度大,信噪比高。 2、重现性好 傅里叶变换红外光谱仪采用的傅里叶变换对光的信号进行处理,避免了电机驱动光栅分光时带来的误差,所以重现性比较好。 3、扫描速度快 傅里叶变换红外光谱仪是按照全波段进行数据采集的,得到的光谱是对多次数据采集平均后的结果,而且完成一次完整的数据采集只需要一至数秒,而色散型仪器则需要在任一瞬间只测试很窄的频率范围,一次完整的数据采集需要十分钟至二十分钟。 FTIR 的吸收强度和表示方法 红外吸收光谱分析对于同一类型的化学键,偶极矩的变化与结构的对称性有关。例如C =

傅立叶红外光谱仪测试样品的方法及注意事项-红外压片模具

傅立叶红外光谱仪测试样品的方法及注意事项 要获得一张高质量红外光谱图,除了仪器本身的因素外,还必须有合适的样品制备方法。 一、红外光谱法对试样的要求 红外光谱的试样可以是液体、固体或气体,一般应要求: 1. 试样应该是单一组份的纯物质,纯度应>98%或符合商业规格,才便于与纯物质的标准光谱进行对照。多组份试样应在测定前尽量预先用分馏、萃取、重结晶或色谱法进行分离提纯,否则各组份光谱相互重叠,难于判断。 2. 试样中不应含有游离水。水本身有红外吸收,会严重干扰样品谱,而且会侵蚀吸收池的盐窗。 3. 试样的浓度和测试厚度应选择适当,以使光谱图中的大多数吸收峰的透射比处于10%~80%范围内。 二、制样的方法 1. 气体样品 气态样品可在玻璃气槽内进行测定,它的两端粘有红外透光的NaCl或KBr窗片。先将气槽抽真空,再将试样注入。 2. 液体和溶液试样 (1)液体池法 沸点较低,挥发性较大的试样,可注入封闭液体池中,液层厚度一般为0.01~1mm。 (2)液膜法 沸点较高的试样,直接滴在两片盐片之间,形成液膜。对于一些吸收很强的液体,当用调整厚度的方法仍然得不到满意的谱图时,可用适当的溶剂配成稀溶液进行测定。一些固体也可以溶液的形式进行测定。常用的红外光谱溶剂应在所测光谱区内本身没有强烈的吸收,不侵蚀盐窗,对试样没有强烈的溶剂化效应等。 3. 固体试样

(1)压片法 将1~2mg试样与200mg纯KBr研细均匀,置于模具中,用(5~10)′107Pa压力在油压机上压成透明薄片,即可用于测定。试样和KBr都应经干燥处理,研磨到粒度小于2微米,以免散射光影响。 (2)石蜡糊法 将干燥处理后的试样研细,与液体石蜡或全氟代烃混合,调成糊状,夹在盐片中测定。 (3)薄膜法 主要用于高分子化合物的测定。可将它们直接加热熔融后涂制或压制成膜。也可将试样溶解在低沸点的易挥发溶剂中,涂在盐片上,待溶剂挥发后成膜测定。当样品量特别少或样品面积特别小时,采用光束聚光器,并配有微量液体池、微量固体池和微量气体池,采用全反射系统或用带有卤化碱透镜的反射系统进行测量。 仪器操作 1. 样品准备(固体样品) 取样品约0.5mg在红外灯下充分研磨,再加入干燥KBr粉末约50mg,继续研磨至混合均匀。 2. 模具准备 将干燥器中保存的简易模具取出,确认模具洁净。若其表面不洁净,可用棉花沾少许无水乙醇轻轻擦拭(绝对不可用力,以免模具表面被划伤),然后在红外灯下干燥。 3. 制片方法 将试样与纯KBr混合粉末置于模具中,用(5~10)′107Pa压力在油压机上压成透明薄片,即可用于测定。试样和KBr都应经干燥处理,研磨到粒度小于2微米,以免散射光影响。 样品测试过程中的注意事项

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一、傅里叶红外光谱仪 工作原理: FTIR是基于光相干性原理而设计的干涉型红外光谱仪。它不同于依据光的折射和衍射而设计的色散型红外光谱仪。与棱镜和光栅的红外光谱仪比较,称为第三代红外光谱仪。但由于干涉仪不能得到人们业已习惯并熟知的光源的光谱图,而是光源的干涉图。为此可根据数学上的傅立叶变换函数的特性,利用电子计算机将其光源的干涉图转换成光源的光谱图。亦即是将以光程差为函数的干涉图变换成以波长为函数的光谱图,故将这种干涉型红外光谱仪称为傅立叶变换红外光谱仪。 确切地说,即光源发出的红外辐射经干涉仪转变成干涉光,通过试样后得到含试样信息的干涉图,由电子计算机采集,并经过快速傅立叶变换,得到吸收强度或透光度随频率或波数变化的红外光谱图。其工作原理如

图所示: 操作步骤: 一、开机前准备 开机前检查实验室电源、温度和湿度等环境条件,当电压稳定,室温为21±5℃左右,湿度≤65%才能开机。 二.开机 开机时,首先打开仪器电源,稳定半小时,使得仪器能量达到最佳状态。开启电脑,并打开仪器操作平台OMNIC软件,运行Diagnostic菜单,检查仪器稳定性。 三.制样 根据样品特性以及状态,制定相应的制样方法并制样。 四.扫描和输出红外光谱图 测试红外光谱图时,先扫描空光路背景信号,再扫描样品文件信号,经傅立叶变换得到样品红外光谱图。根据需要,打印或者保存红外光谱图。 五.关机 1. 关机时,先关闭OMNIC软件,再关闭仪器电源,盖上仪器防尘罩。 2. 在记录本记录使用情况。 注意事项: 1、保持实验室电源、温度和湿度等环境条件,当电压稳定,室温为21±5℃左右,湿度≤65%。 2、保持实验室安静和整洁,不得在实验室内进行样品化学处理,实验完毕即取出样品室内的样品。 3、样品室窗门应轻开轻关,避免仪器振动受损 4、当测试完有异味样品时,须用氮气进行吹扫。 5、离开实验室前,须注意关灯,关空调,最后拉开总闸刀。

尼高力傅立叶红外光谱仪

Tel: (010) 5850 3588 ext. 236 Fax: (010) 6621 0845 Issued by: Wang Zheng TO: Date of Issue: 北京沃特瑞尔科技发展有限公司 Quotation No.: Payment:By Irrevocable L/C Delivery: 5 weeks after receipt of L/C Validity: Valid for 90 days ITEM PART NO. DESCRIPTION Q'TY FOB PRICE 2003-11-4WZsyxnw03-2001 960M0030 Nicolet IR200 FT-IR Spectrometer 1$29,458 IR200 傅立叶变换红外光谱仪主机System specifications include: ~ 60 degree Michelson, Cube Corner Interferometer Design 60o 迈克尔逊,立体角镜干涉仪 ~ Spectral Range of 7,800 to 375 cm -1 光谱范围:7,800 - 375 cm -1 ~ Spectral Resolution ranging from 16 to 1 cm -1 光谱分辨率:16 - 1cm -1 ~ Ge on KBr beamsplitter 镀锗溴化钾分束器 ~ Detector: DTGS DTGS 检测器 ~ Ceramic Source 陶瓷光源 ~ Sealed and Desiccated Optics 密封干燥光学仓 2699-075900 English Language Kit for Nicolet IR2001NO CHARGE 英文标识3860-006800DTGS Detector 1Included DTGS 检测器 4860-006900 1 cm -1 Resolution (1 cm -1 分辨率)1Included 5 833-011700 EZ OMNIC Plus Software 1 Included EZ OMNIC Plus 软件包 Includes the following: EZ OMNIC ~ Data Collection (数据采集软件) ~ Data Manipulation (数据处理软件) ~ QC Compare (QC 比较) ~ Ability to run macros and external programs 有能力运行宏程序和外部程序 ~ User Log-in (用户登录保护功能) TQ Analyst - EZ Edition Qualitative Tools ~ Measure Only Thermo Nicolet IR 200 FT-IR Spectrometer Thermo Nicolet IR 200傅立叶变换红外光谱仪

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