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Jiangsu Skyray Instrument Co., Ltd.
Shenzhen Skyray Instrument Co., Ltd.

TEL86 136 1622 3382

hotline800-9993-818

addressNo. 1888, Zhonghuayuan West Road, Kunshan City, Jiangsu Province, 22/F, Taohuayuan Science and Technology Innovation Park, Furong East Road, Songgang, Bao'an District, Shenzhen, China

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Air Particles Heavy Metal Detection XRF Application Solution
Issuing Time:2018-03-20

Foreword


With the increasing demand for industry, energy, and transportation, the problem of atmospheric pollution has become increasingly prominent. Among them, heavy metals that enter the atmosphere in different forms become one of the most important pollutants in the air. It is estimated that more than 9,000 tons of five kinds of lead, mercury, cadmium, chromium, and arsenic in the air will be emitted in the country in one year. Non-ferrous metal smelting, lead storage batteries, recycled lead, coal-fired power plants, cement, iron and steel smelting, Chemicals production and other industries are the major sources of heavy metal pollution. Among them, non-ferrous metal smelting enterprises and coal-fired power plants are the major sources of mercury emissions. In addition, tail gas, tire friction, and brake friction are also important sources of pollution. Atmospheric heavy metals are present in suspended particles, and the dynamic diameter of particles is from 0.1 μm to 100 μm. Usually suspended particles of 50 μm or more settle in the atmosphere in minutes or hours. However, suspended particles less than 10 μm, especially less than 2.5 μm, do not easily settle. They can float in the atmosphere for days or even years, and can migrate hundreds or even thousands of kilometers.


Heavy metal pollutants in the air damage buildings, form soils, and cross-contamination of surface water systems through wind, rain, and snow. Heavy metals that enter the water body undergo a series of physical and chemical reactions such as oxidation, dissolution, desorption, complexation, and bio-methylation that produce water-soluble metal salts that diffuse with the flow of water. When the physical and chemical conditions of the basin change, these metal salts may be reduced, precipitated, adsorbed, and precipitated in the soil. Respiratory organs of different diameter particles are: 10 ~ 100 μm, nasal cavity; 2.5 ~ 10 μm, nasopharyngeal area; 0.1 ~ 2.5 μm, bronchus and lungs; 0.1 μm or less, heavy metal elements have strong migration, Enrichment and concealment, through the air, water, food chain and other ways into the human body, significant biological toxicity, easy to cause chronic poisoning, with carcinogenic, teratogenic and mutagenic effects on the immune system has a certain impact, a serious threat to human health.


At present, the Ministry of Environmental Protection has officially issued the relevant standards for the determination of inorganic elements in ambient air particles - energy dispersive X-ray fluorescence spectrometry, which shows that energy dispersive X-ray fluorescence spectrometers can easily, quickly and accurately analyze atmospheric particulate matter in samples. The heavy metal content.


Energy Dispersion X Fluorescence Spectrometer Analysis Principle

When the primary X-rays generated by the X-ray tube are irradiated to the surface of a uniform and uniform particle, the atoms of the test element contained in the sample are excited to emit characteristic X-rays. After being received by the detector, the light signal is converted into an analog electrical signal. The analog-to-digital converter converts the analog electrical signal into a digital signal and sends it to a computer for processing. The X-ray intensity of the element feature is obtained by dedicated software, and the content of the element to be measured is calculated according to the corresponding mathematical model of the spectral peak intensity and content of the element feature.


 


EDX4500H Energy Dispersion X Fluorescence Spectrometer Introduction


EDX 4500H X Energy Dispersive Fluorescence Spectrometer utilizes XRF detection principle to achieve fast, accurate and non-destructive analysis of various elemental components. The main feature of this instrument is the use of intelligent vacuum system, which can have good excitation effect on light elements such as Si, P, S, Al, Mg, etc. The XRF technology can be used to accurately analyze the heavy elements of atmospheric particulate matter enrichment in atmospheric filtration. The analysis of membrane enrichment content has the characteristics of non-destructiveness, rapidness, accuracy, etc., effectively improving the detection time and work efficiency.





Figure 1 EDX4500H Energy Dispersive X-ray Fluorescence Spectrometer

Performance characteristics



High-efficiency, ultra-thin window X-ray tube, the indicators have reached the international advanced level

Using digital multi-channel technology, it can achieve ultra-high count rate, improve test efficiency and accuracy

SDD silicon drift detector, good energy linearity, energy resolution, peak-to-back ratio and energy spectrum characteristics

Low-energy X-rays excite the test element and have good excitation effect on light elements such as Si and P

Intelligent vacuum pumping system shields the influence of air and greatly expands the scope of testing

Automatic spectrum stabilization device ensures the consistency of instrument work

High signal-to-noise ratio electronic circuit unit

Automatically switch collimators and filters for different samples, eliminating the need for manual operations

Decompose spectrum to decompose spectral peaks so that the measured results of the measured elements have equal analytical accuracy

Multi-parameter linear regression method to significantly suppress absorption and enhancement effects between elements

The LCD screen shows the important parameters of the instrument (tube pressure, tube flow, vacuum degree) at a glance


Technical Parameters


Product Model:EDX 4500H

Product Name: Energy Dispersive X Fluorescence Spectrometer

Measurement element range: from sodium (Na) to uranium (U)

Element content analysis range: ppm-99.99% (different elements, different analysis range)

Simultaneous analysis of elements: one-time measurement of dozens of elements

Measurement time: 30 seconds - 200 seconds

Detector energy resolution: 145±5 eV

Tube pressure: 5KV-50KV

Tube flow: 50μA-1000μA

Measurement object status: powder, solid, liquid

Input voltage: AC 110V/220V

Ambient temperature: 15°C-30°C

Humidity: 35%-70%

Sample chamber volume: 320mm×100mm

Dimensions: 660mm×510mm×350mm

Weight: 65Kg



 


Standard configuration


High-efficiency thin window X-ray tube

SDD silicon drift detector

Digital multi-channel technology

Optical path enhancement system

High signal to noise ratio electronic circuit unit

Built-in high-definition camera

Automatic Switching Collimators and Filters

Automatic spectrum stabilization device

Triple security protection model

Reliable overall steel structure

90mm × 70mm status display LCD screen

Vacuum pump


 


Atmospheric particulate collection and preparation

 Ambient air particulate sampling point settings should meet the relevant requirements of HJ664. The sampling process should be performed according to the particle sampling requirements in HJ/T194. When the target element content is low or PM10 (PM2.5) samples are collected, the sampling volume can be increased appropriately. Unorganized emission particulate sample collection Set monitoring points according to the relevant requirements in HJ/T55. Others are consistent with the collection requirements for ambient air samples. The collection of two types of particulate samples should meet the requirements of the relevant standards issued by the Ministry of Environmental Protection.


The heavy metal detection process in atmospheric particles is shown in Figure 2. First, the air and the carried particulate matter are pumped into the cutter by a flow control pump. The particulate collection mainly depends on the cutting head of the sampler, and the PM10 sampler cut point is 10 μm. The capture efficiency of 10 μm particles is more than 50%, and then the particles are captured by a certain size of sampling filter. Commonly used sampling membranes are quartz filter, PTFE filter, polycarbonate filter (PC ) Etc. After a period of time, the sample was collected and collected. After the sampling was completed, the filter was removed with a tweezers and stored in a dry, clean, numbered sample box.


Figure 2 Atmospheric heavy metal collection and detection process

In this experiment, a quartz filter membrane was used. The diameter of the filter membrane (0.4-0.8 μm) was 47 mm, the particle cutter (PM10), and the gas flow rate was controlled at 1 m3/h, and the sample was sampled for 24 hours. The numbers are 1#, 2#, ... 7#. The collected samples were stored dry for testing.


 


Formulation and Analysis of Heavy Metal Curves of Atmospheric Particulates


 


     Set the appropriate measurement conditions, use EDX4500H energy dispersive X-ray fluorescence spectrometer to scan the standard filter material, establish the calibration working curve of the content and intensity of the test element, and then measure the unknown sample of the atmospheric particulate filter.


Fig. 3 Pb element working curve of atmospheric particles in EDX4500H

 

Fig. 4 Fluorescence analysis of an enriched filter X by an atmospheric particle of EDX4500H

 

Table 1 Analytical results of atmospheric heavy metal membrane EDX4500H in a certain area Unit: μg/m3

滤膜

1#

2#

3#

4#

5#

6#

7#

Ti

0.000

0.000

0.000

0.018

0.000

0.000

0.000

V

0.000

0.000

0.000

0.000

0.000

0.000

0.000

Cr

0.002

0.001

0.000

0.007

0.003

0.002

0.001

Mn

0.000

0.000

0.000

0.023

0.022

0.026

0.000

Fe

0.237

0.131

0.156

1.062

0.264

0.541

0.153

Co

0.000

0.000

0.000

0.000

0.000

0.000

0.000

Cu

0.001

0.001

0.001

0.162

0.007

0.008

0.001

Zn

0.021

0.011

0.015

0.346

0.119

0.140

0.014

As

0.000

0.000

0.000

0.063

0.000

0.000

0.000

Se

0.000

0.000

0.000

0.000

0.000

0.000

0.000

Cd

0.000

0.000

0.000

0.063

0.000

0.000

0.000

Ba

0.000

0.000

0.000

0.027

0.001

0.027

0.000

Pb

0.006

0.004

0.009

2.955

0.076

0.095

0.011

At present, the “Ambient Air Quality Standard” GB3095-2012 stipulates that the annual average concentration limit of Pb element is 0.5 μg/m3. Because Pb belongs to the more toxic metal, its concentration limit is lower among various heavy metals. The instrument detected that the content of Pb in the sample #4 exceeded the standard, up to 2.955 μg/m3, and the Fe element content was also high, reaching 1.062 μg/m3. In addition, Fe and Zn, the most common heavy metal contaminants in the atmosphere, were detected in each sample.


The results show that the particulates in the atmosphere can be collected by the quartz filter and the standard calibration curve can be used to directly analyze the content of atmospheric heavy metals in the unknown sample. This method does not require digestion, and the measurement time of each sample only takes a few minutes. The instrument satisfies the requirements of the relevant standards for the "Determination of inorganic elements in ambient air particles - energy dispersive X-ray fluorescence spectrometry" implemented by the Ministry of Environmental Protection on July 1, 2017.


 


Accessories: Installation and Operating Environment of the Instrument


First, the overall design of the laboratory:


According to the characteristics of sample testing and sample preparation, each sub-compartment shall be established. Sample testing rooms and sample preparation rooms shall be established. Scientific equipment shall be arranged and placed, power lines shall be arranged, and reasonable lighting, natural ventilation and lighting shall be provided.


Schematic diagram: The sample testing room is as follows. For specific requirements, see the instrument installation conditions below.


Second, the working environment requirements


2.1 Ambient temperature: 10°C-35°C


2.2 Relative humidity: less than 70%


2.3 Power supply: AC 220V (If the power grid fluctuates ≥ 10%, a special AC voltage regulator (1kw or more) is required.


2.4 Room: No corrosive gas, no mechanical vibration, no electromagnetic field interference.


Why select Skyray Instruments?

Air Particles Heavy Metal Detection XRF Application Solution

    First, the industry leader:

    Listed on Shenzhen Stock Exchange in 2011(Code:300165)
    Analytical instrument industry leader in the field

    Skyray Instrument, as a leader in the domestic chemical analysis industry, specializes in the production of high-end analytical instruments such as spectrometers, chromatographs, and mass spectrometers. Mainly used in environmental protection and safety (electronics, electricity, toys and other consumer products industries, food safety, air, soil, water quality pollution detection, etc.), industrial production quality control (metallurgy, building materials, petroleum, chemical, precious metals, medical equipment, etc. ), minerals and resources (geology, mining), commodity inspections, quality inspections, and even human trace element testing and many other areas.The core patent technology is the first in the industry; the sales volume is the first in the industry; the product category is the first in the industry;

Air Particles Heavy Metal Detection XRF Application Solution

    Second, the standard makers:

    Skyray Instrument participated in drafting and formulating 18 national standards, Industry standards, confident in the right to speak in the industry.

    GBT 28020-2011 Ornaments Determination of harmful elements X-ray fluorescence spectroscopy
    GBT 31364-2015 Energy dispersive X-ray fluorescence spectrometer main performance test method
    GBT 33352-2016 General requirements for screening of restricted substances in electrical and electronic products X-ray fluorescence spectroscopy
    GB/T 25934.1-2010 High-Purity Gold Chemical Analysis Method Ethyl Acetate Extraction Separation ICP-AES Spectrometry Determination of Impurity Elements
    GB/T 27730-2011 Determination of dimethyl fumarate in toy products Gas chromatography-mass spectrometry GC-MS method
    GB/T 28020-2011 articles - Determination of harmful elements - X-ray fluorescence spectrometry
    GBT 22788-2008 Determination of Total Lead in Coatings on Toys
    GB/T 30419-2013 Determination of migrating elements in gallium arsenic, cadmium, chromium, lead, mercury selenium in toy materials Inductively coupled plasma atomic emission spectrometry
    GB/T 31364-2015 Energy dispersive X-ray fluorescence spectrometer main performance test method
    JBT 12962.1-2016 Energy Dispersive X-Ray Fluorescence Spectrometer Part 1: General Techniques
    JBT 12962.2-2016 Energy Dispersive X-Ray Fluorescence Spectrometer Part 2: Elemental Analyzers
    JBT 12962.3-2016 Energy dispersive X-ray fluorescence spectrometer Part 3: Coating thickness analyzer
    LS_T 6115-2016.4672 LST6115-2016 "Fastness determination of cadmium in rice by X-ray fluorescence spectrometry" standard
    (Unfinished……)

Air Particles Heavy Metal Detection XRF Application Solution

    Third, technology pioneers:

    252 utility patents to fill domestic gaps and break the import monopoly

    As of the end of 2017, Tianrui Instrument Company and its subsidiaries have obtained 252 patents authorized by the State Intellectual Property Office.
    "Computer Software Copyright Registration Certificate" 91 items;
    Of which 115 are invention patents,
    80 utility model patents,
    Appearance patent 57 items.

Air Particles Heavy Metal Detection XRF Application Solution

    Fourth, service practitioners:

    Do not forget the initial heart, with the customer with the fate, a total of growth.

    Skyray customers include the General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China and the National Museum of China,
    China National Center for Geoanalysis and Experiments, Chinese Academy of Geological Sciences, Changchun Institute of Opto-Mechanical Engineering, China Taier Laboratory,
    Other government departments and well-known testing agencies,
    And PetroChina, Sinopec, Huawei, Haier, Skyworth, Fanta, Meiling, Lite-On, TCL, LG, Midea, Samsung, China Test (CTI), Avionics, etc.

研发实力:

Air Particles Heavy Metal Detection XRF Application Solution

    Analytical Testing Instrument Research Institute

    Skyray Analytical Testing Instrument Research Institute has three centers, namely "analysis instrument research and development center", "physiochemical analysis and testing center" and "analysis and testing technology application development center."Tianrui Analytical Instruments Co., Ltd. recently formed a staff of 1 academician, 11 Ph.D., 13 senior engineers, 17 masters, and 50 undergraduate R&D personnel from famous universities.

Air Particles Heavy Metal Detection XRF Application Solution

    Dr. Liu Zhaogui, specialist in special allowance of the State Council

    Mr. Liu Zhaogui: graduate student in nuclear physics from Tsinghua University. It has been appraised as the outstanding entrepreneur of Jiangsu Province, the young and middle-aged experts who have outstanding contribution in Jiangsu Province, the first science and Technology Minister of Kunshan, and the national science and technology ministry "scientific and technological innovation and entrepreneurial talent". With the approval of the State Council, the special allowance of the State Council is enjoyed.

Air Particles Heavy Metal Detection XRF Application Solution

    Dr. Yaodong Dong, Expert in X-Ray Fluorescence Spectroscopy

    Dr. Yao graduated from the Department of Engineering Physics of Tsinghua University with a Ph.D. in nuclear electronics. He has been engaged in the development of analytical instruments for 26 years. He is mainly engaged in the research of X-ray fluorescence analysis technology and application technology, and he participated in the "Thirteenth Five-Year Plan" national key instrument technology research and development. Patent of "Spectrometer Grating 2D" patent, "X-ray fluorescence double crystal fixed element track spectrometer" patent and "X-ray fluorescence spectrum analyzer pyrolytic graphite crystal beam splitter" patent, and participated in the drafting of a number of national standards industry The standard is an authoritative expert in the X-ray fluorescence spectrometer industry in China.

Eight technical advantages:

Air Particles Heavy Metal Detection XRF Application Solution

    First, FP basic parameter method

    The FP (Basic Parameters) algorithm is an effective method for X-ray fluorescence spectrometry analysis. It can perform qualitative and quantitative analysis of the elemental components of the sample with little or no standard sample, and can also analyze the thickness of the coating or coating.It is well known that the biggest problem with X-ray fluorescence analysis is that elemental fluorescence intensity is affected by coexisting elements (matrix absorption and enhancement effects) and is not usually linear with content. The basic parameter method has already taken into account the matrix effect in the calculation of the spectrum, and the linear relationship between the calculated content and the known content can be obtained. Using a few known sample calibration algorithms to eliminate systematic errors can achieve accurate quantitative results.

Air Particles Heavy Metal Detection XRF Application Solution

    Second, polarization secondary target excitation technology

    The polarization secondary target excitation technology can remove the scattering background to the maximum extent, improve the signal to noise ratio, and reduce the detection limit of the detector. Assuming that the x-ray generated by the anode of the x-ray tube is non-polarized and is incident on the target (scattering body) in the z-axis direction, the scattered beam propagating along the y-axis is linearly polarized light. The electric field vector vibrates in the v plane and the vibration direction is parallel to the X axis. The sample placed on the y-axis is excited by polarized light, producing unpolarized fluorescent x-rays. Since the sample and the sample support do not generate scattered radiation in the X-axis direction, placing the detector on the x-axis can fully utilize the polarization effect and reduce the background caused by the elastic and inelastic scattering of x-rays.

Air Particles Heavy Metal Detection XRF Application Solution

    Third, ultra-short optical design

    From the X-ray generator to the sample, the X-ray fluorescence emitted by the sample to the detector is called the light path. The shorter the distance traveled by the optical path is, the less interference will be caused. Skyray Instrument designed an ultra-short optical path technology to ensure the accuracy of light element detection results, and is particularly suitable for RoHS-compliant halogen-free instruction detection.

Air Particles Heavy Metal Detection XRF Application Solution

    Fourth, precision machinery design

    The micro-level positioning, micro-scanning analysis, the point-to-point centering of the spatial micro-sized spot and the determination of the spatial micro-focus spot position have been truly achieved. A translation and rotation switching position device realizes position rotation switching in a small space, avoids the large space required for the linear motion and the common rotation movement, because the problem of lengthening of the optical path caused by the inability to fit is eliminated.

Air Particles Heavy Metal Detection XRF Application Solution

    Five, no standard technology

    XRF test and analysis instruments are generally used for the comparison test of standard samples, which are subject to the quality of the standard samples during the test. Tianrui Instrument's original non-standard technology can carry out all-element analysis without standard samples, leading the development trend and trend of the industry.

Air Particles Heavy Metal Detection XRF Application Solution

    Sixth, secondary target excitation technology

    XRF test and analysis instruments are generally used for the comparison test of standard samples, which are subject to the quality of the standard samples during the test. Tianrui Instrument's original non-standard technology can carry out all-element analysis without standard samples, leading the development trend and trend of the industry.

Air Particles Heavy Metal Detection XRF Application Solution

    VII. Signal to Noise Enhancement Technology

    Skyray's unique SNR enhancement technology can effectively remove noise signal interference and minimize element detection limits.
    As shown in Figure SUPER XRF 1050, the determination of Pb in food can be as low as 0.59 ppm.

Air Particles Heavy Metal Detection XRF Application Solution

    VIII. XRF Core Technology (Intelligent Analysis Software)

    patented intelligent analysis software enables precise analysis of 80 elements, non-standard quantitative analysis, micro-analysis, thin film analysis, and advanced sub-spectral analysis.

Certificate of honor

The national Torch Program focuses on the high and new technology enterprises, the certification of heavy contract and credit enterprise, the confirmation certificate of measurement guarantee and the national high technology research and development plan (863 plan).:

国家火炬计划重点高新技术企业、重合同守信用企业认证、计量保证确认证书、国家高技术研究发展计划(863计划)-Jiangsu Skyray Instrument Co., Ltd.

ISO9001:2008 quality management system certification, ISO14001 environmental management system certificate, OHSAS 18001 occupational health and safety management health system, information security management system certification:

ISO9001:2008质量管理体系认证、ISO14001环境管理体系证书、OHSAS 18001 职业健康安全管理健康体系 、信息安全管理体系认证-Jiangsu Skyray Instrument Co., Ltd.

Practical patent certificate:

实用专利证书-Jiangsu Skyray Instrument Co., Ltd.

Standard formulation:

Jiangsu Skyray Instrument Co., Ltd.标准制定

Software copyright certificate:

软件著作权证书-Jiangsu Skyray Instrument Co., Ltd.

Other certificates:

Honor企业荣耀-Jiangsu Skyray Instrument Co., Ltd.
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Jiangsu Skyray Instrument Co., Ltd.
SHENZHEN Skyray Instrument Co., Ltd.

hotline:800-9993-818
TEL:86 136 1622 3382
Address: 1888 Zhonghuayuan West Road, Kunshan City, Jiangsu Province/
深圳宝安区松岗芙蓉东路桃花源科技创新园22层

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