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The solid wastes are of three types namely: Municipal

namely: Municipal Solid Waste, Hazardous Waste, and Hospital Waste. Waste. If
these solid wastes are not disposed of properly and safely, they can cause major health concerns and an
unpleasant living environment. They can also serve as a breeding ground for disease-carrying insects, pests,
snakes, and animals, increasing the risk of disease transmission. It has the potential to pollute water supplies as
well as the environment. This article will explain to you about the types of solid waste which will be helpful in
preparing the Environment syllabus for the UPSC Civil service exam.
Table of Contents
1. Solid Waste
2. Types of Solid Waste
3. Solid Waste Management
4. Solid Waste Management Rules, 2016
5. Conclusion
6. FAQs
7. MCQs
What does Solid Waste mean?

Solid wastes are materials that have been thrown (or are considered waste-like) or discarded.
https://prepp.in/news/e-492-types-of-solid-waste-environment-notes 1/10
Any garbage, refuse, sludge from a wastewater treatment plant or an air pollution control facility, and other
discarded materials, including solid, liquid, semi-solid, or contained gaseous material, resulting from industrial,
commercial, mining, and agricultural operations, as well as community activities, are considered solid waste.
Solid or dissolved materials in domestic sewage, as well as solid or dissolved pollutants in irrigation return
flows or industrial discharges, are not included.
Other Relevant Links
Municipal solid waste Hazardous waste
Hospital waste Solid Waste
E–Waste Plastic Waste
Effects of solid waste Disposal of solid waste
Treatment of solid waste Radioactive wastes
Types of Solid Waste

Municipal Solid Waste
Municipal solid waste includes household waste, construction and demolition debris, sanitation residue, and
waste from roadways.
The volume of municipal solid waste has been quickly increasing and its composition is altering as a result of
rising urbanisation and changes in lifestyle and eating habits.
In 1947, India's cities and towns created an estimated 6 million tonnes of solid waste; by 1997, that number
had risen to almost 48 million tonnes.
More than a quarter of municipal solid waste is never collected.
70% of Indian cities lack the necessary transportation capacity, and there are no sanitary landfills to dispose
of the waste.
Existing landfills are not well prepared nor appropriately lined to prevent soil and groundwater from
contamination.
The consumer market has risen quickly in recent years, resulting in products being packaged in cans,
aluminum foils, plastics, and other nonbiodegradable materials that damage the environment infinitely.
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Hazardous wastes are toxic, extremely flammable, or explosive, and can be very harmful to humans, animals,
and plants.
Every year, India produces around 7 million tonnes of hazardous waste, with the majority of it concentrated in
four states: Andhra Pradesh, Bihar, Uttar Pradesh, and Tamil Nadu.
Old batteries, shoe polish, paint tins, old pharmaceuticals, and medicine bottles are examples of household
waste that might be classified as hazardous waste.
Metal, chemical, paper, pesticide, dye, refining, and rubber goods sectors are important sources of hazardous
waste in the industrial sector.
Direct contact with hazardous waste compounds such as mercury and cyanide can be lethal.
Composition of Household Hazardous Waste
*For detailed notes of this topic, check this link Hazardous Waste
Biomedical / Hospital Waste

Hospital waste is generated during the diagnosis, treatment, or immunisation of humans or animals, as well
as during research, biological production, and testing.
Soiled waste, disposables, anatomical waste, cultures, abandoned pharmaceuticals, chemical wastes,
disposable syringes, swabs, bandages, body fluids, human excreta, and other wastes may be included under
this category.
These are highly infectious and can pose a major hazard to human health if not handled scientifically and
selectively.
According to surveys conducted by several organizations, India's healthcare facilities are not paying enough
attention to waste management.
Following the publication of the Bio-medical Waste (Handling and Management) Rules, 1998, these
facilities are gradually streamlining the waste segregation, collection, treatment, and disposal processes.
Composition of Hospital Waste
*For detailed notes of this topic, check this link Hospital Waste
Solid Waste Management

The process of collecting and treating solid waste is referred to as solid waste management.
It also provides recycling options for items that do not belong in garbage or trash.
Garbage or solid waste has been a problem for as long as people have lived in settlements and residential
areas. Waste management is concerned with the transformation of solid waste into a valuable resource.
Every household, including business owners, should embrace solid waste management around the world.
Solid waste management is a critical component of urban area management.
Improper municipal solid waste disposal can lead to unsanitary conditions, which can lead to pollution and the
spread of vector-borne disease.
The task of solid waste management is fraught with technical difficulties. They also present a number of
economic, administrative, and social issues that require immediate attention.
Solid Waste Management
Solid Waste Management Rules, 2016

These laws, which replace the Municipal Solid Wastes (Management and Handling) Rules of 2000, now
apply to urban agglomerations, census towns, notified industrial townships, and other locations outside of
municipal jurisdiction.
They emphasize waste separation at the source, the manufacturer's obligation for sanitary and packaging
waste disposal, and user fees for bulk generator collection, disposal, and processing.
It has also been recommended that biodegradable waste be processed, treated, and disposed of within the
premises as much as possible by composting or bio-methanation, with the remainder garbage being handed
to the waste collectors or agency as ordered by the local authorities.
The guidelines encourage the use of compost, the conversion of waste into energy, and the adjustment of
landfill location and capacity parameters.
The government has also established a Central Monitoring Committee, chaired by the Secretary of the
Ministry of Environment, Food and Climate Change, to oversee the overall implementation of the laws.
All open dumpsites and existing operating dumpsites in India must use bio-remediation and bio-mining,
according to the Rules for the Safe Treatment of Legacy Waste.
Conclusion
The collected waste piles up and creates a problem for both the environment and the population as a result of poor
solid waste disposal, notably by waste management agencies. According to surveys conducted by several
organizations, India's healthcare facilities are not paying enough attention to waste management. Following the
publication of the Bio-medical Waste (Handling and Management) Rules, 1998, these facilities are gradually
streamlining the waste segregation, collection, treatment, and disposal processes.
Environment Notes Environmental Pollution
Causes of pollution Classifications of Pollutants
Plastic Pollution Bioremediation
Radioactive Pollution Air Pollution
Noise Pollution Soil Pollution
Water Pollution Thermal Pollution
FAQs
Question: What is solid waste management? ➕
Question: What do you mean by biomedical or hospital waste? ➕
Question: What is solid waste? What are its types? ➕
MCQs
Question: Consider the following statements on the types of solid wastes:
1. Solid waste includes all non-liquid wastes, including solid and semi-solid wastes.
2. It also includes human and animal excreta.
Which of the statement(s) given above is/are correct?
(a) 1 only
(b) 2 only
(c) Both 1 and 2
(d) Neither 1 nor 2
Answer: (a) See the Explanation ➕
Question: Which of the following is not a type of solid waste?
(a) Municipal solid waste
(b) Industrial Solid Waste
(c) Hospital waste
(d) Hazardous Waste
Answer: (b) See the Explanation ➕
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Internal Security Notes Ethics Notes
Disaster Management Notes World History
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CSAT Notes Government Scheme Notes
*The article might have information for the previous academic years, please refer the official
website of the exam.
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About Us Contact Us Terms & Conditions Privacy Policy Prepp © 2022
ISSN: 2320-5407 Int. J. Adv. Res. 7(4), 160-164
Journal Homepage: -www.journalijar.com
Article DOI:10.21474/IJAR01/8802
DOI URL: http://dx.doi.org/10.21474/IJAR01/8802
RESEARCH ARTICLE
SOLID WASTE MANAGEMENT: ITS SOURCES, COLLECTION, TRANSPORTATION AND

RECYCLING.
V. Nathiya1 and Dr. V. Thandapani2.

1. Research Scholar, Department of Economics, Thiru.Vi.Ka.Govt. Arts College, Tiruvarur.
2. Assistant Professor, Department Of Economics, Presidency College, Chennai.
……………………………………………………………………………………………………....
Manuscript Info Abstract
……………………. ………………………………………………………………
Manuscript History Solid wastes may be defined as useless, unused, unwanted, or discarded
Received: 03 February 2019 material available in solid form. Semisolid food wastes and municipal
Final Accepted: 05 March 2019 sludge may also be included in municipal solid waste. The subject of
Published: April 2019 solid wastes came to the national limelight after the passage of the solid
waste disposal act of 1965. Today, solid waste is accepted as a major
Key words:-
Community, density, generation, problem of our society. In the United States over 180 million tons of
landfills, population, solid waste. municipal solid waste (MSW) was generated in 1988. At this
generation quantity, the average resident of an urban community is
responsible for more than 1.8 kg (4.0 lbs.) of solid waste per day. This
quantity does not include industrial, mining, agricultural, and animal
wastes generated in the country each year. If these quantities are added,
the solid waste production rate reaches 45 kg per capita per day (100 lb.
/c.d.). To introduce the reader to the solid waste management field, an
overview of municipal solid waste problems, sources, collection,
resource recovery, and disposal methods are presented in this paper.
Greater emphasis has been given to the design and operation of
municipal sanitary landfills, regulations governing land disposal, and
leachate generation, containment and treatment methods.
Copy Right, IJAR, 2019,. All rights reserved.

……………………………………………………………………………………………………....
Introduction:-
Municipal solid waste (MSW) includes wastes such as durable goods, nondurable goods, containers and packaging,
food wastes yard wastes, and miscellaneous inorganic wastes from residential, commercial, institutional, and
industrial sources. Example of waste from these categories include appliances, newspapers, clothing, food scarps,
boxes, disposable tableware, office and classroom paper, wood pallets, and cafeteria wastes. MSW does not include
wastes from sources such as municipal sludge, combustion ash, and industrial non-hazardous process wastes that
might also be disposed of in municipal waste landfills or incinerators. Determining actual MSW generation rates is
difficult. Different studies report a wide variation as they use different components. Many times industrial and
demolition wastes are included in municipal solid wastes. It is estimated that, without source reduction, MSW
generation will increase to 200 million tons or 1.9 kg/c.d (4.2 lb. /c.d) by the year 1995, and 216 million tons or 2.0
kg/c.d (4.4 lb. /c.d) by the year 2000. Based on current trends and information, EPA projects that 20 to 28 percent of
MSW will be recovered annually by 1995. A successful solid waste management system utilizes many functional
elements associated with generation, on-site storage, collection, transfer, transport, characterization and processing,
resource recovery and final disposal. All these elements are interrelated, and must be studied and evaluated carefully
Corresponding Author:-V. nathiya.

160
Address:-Research Scholar, Department of Economics, Thiru.Vi.Ka.Govt. Arts College, Tiruvarur.
ISSN: 2320-5407 Int. J. Adv. Res. 7(4), 160-164
before any solid waste management system can be adapted. It is a multidisciplinary activity involving engineering
principles, economics, and urban and regional planning.
Sources And Characteristics

Municipal solid waste (MSW) or urban solid waste is normally comprised of food wastes, rubbish, demolition and
construction wastes, street sweepings, garden wastes, abandoned vehicles and appliances, and treatment plant
residues. Quantity and composition of MSW vary greatly for different municipalities and time of the year. Factors
influencing the characteristics of MSW are climate, social customs, per capita income, and degree of urbanization
and industrialization. The composition of MSW as collected may vary greatly depending upon geographical region
and season. The typical moisture content of MSW may vary from 15 to 40 percent depending upon the composition
of the waste and the climatic conditions. The density of MSW depends upon the composition and degree of
compaction. The uncompacted density of MSW is around “150 kg/m3 (250 lb. /yd3 ).” The density of collected
solid waste is “235-350 kg/m3 .” The energy content of MSW as collected is “9,890 kJ/kg (4,260 BTU/lb.)”.
Information of chemical composition of the organic portion of MSW is important for many processes such as
incineration, composting, biodegradability, leachate generation, and others. The ultimate analysis of the organic
fraction of MSW is in terms of the constituents carbon, hydrogen, oxygen, nitrogen, sulfur and ash.
Collection And Transport

Solid waste collection and transport involves storage at the generation and pick-up points, pick up by the crew,
trucks driving around the neighborhood, and truck transport to a transfer station or disposal point. The collection is
difficult, complex and costly. Collection of solid waste typically consumes 60-80 percent of the total solid waste
budget of a community. Therefore, any improvement in the collection system can reduce overall cost significantly.
Onsite Storage and Handling

In single family residential areas solid waste storage is handled by residents and tenants. Commonly used containers
are plastic or galvanized metal containers, and disposable paper or plastic bags. The plastic or galvanized containers
are 75-150 liter size with tight covering. The single use paper or plastic bags are generally used when curb service is
provided and the homeowner is responsible for placing the bags along the curb. In high-rise buildings the waste is
picked up by the building maintenance personnel, or special vertical chutes are provided to deliver the waste to a
central location for storage, processing, or resource recovery. A recent development is to provide underground
pneumatic transport systems to move waste to a central location for onsite storage, processing, or resource recovery.
Apartment districts utilize stationary container systems into which the residents drop the solid wastes. Solid wastes
from commercial buildings are collected in large containers that may be stationary or transportable.
Collection of Solid Waste

In residential areas, the most common collection methods are curb or alley, setout-setback, and backyard carry. In
curb or alley service, the residents carry the single-use plastic bags and containers to the curb or collection point, and
then return the empty container after pickup. Setout service utilizes a crew that carries the containers to the
collection point. A separate collection crew empties the containers and residents return the empty containers. In
setout-setback service, a third crew returns the empty containers. In backyard carry service, the collection crew
transfers the solid waste into a wheeled barrel, and then unloads it into the collection truck. The containers remain in
the backyard. Many communities have instituted regulations for separation of solid wastes at the source by residents.
Components such as newspapers and cardboard, aluminum, mixed glass, and food wastes from restaurants have
been separated at the source. Although the concept is good, the participation of the public drops quickly. Also, the
price of recycle material fluctuates greatly, and it is often more expensive to recycle waste material. All these factors
are considered for instituting a mandatory separation and recycling program. There is, however, much interest in
recycling these days due to mounting pressures of decreasing landfill sites, environmental concerns, economic
incentives, and political support. The usual vehicle for residential collection of solid wastes is the manually rear or
side-loaded compaction truck operating with a crew of two or three, including the driver. The typical truck is 14 to
18 m3 (15 to 20 yd3 ), and can carry 4 to 5 tons of wastes to the disposal site or transfer station. Large self-loading
compactor vehicles are equipped to centers, and then replace the empty ones for reuse at the site. Other container
trucks provide container exchange service. They are equipped to carry an empty storage container to a collection
point, pick up a full container and transport it to a central location or disposal site, then replace the empty container
at a new location. The frequency of solid waste collection in most communities is once or twice per week. The daily
truck routes are fixed and balanced to provide a fair day’s work. Several methods are used to optimize the route.
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ISSN: 2320-5407 Int. J. Adv. Res. 7(4), 160-164
Transfer Station And Transfer

If the disposal site is too far from the city, the time spent by the crew of the pickup truck in unproductive travel
becomes excessive. As a result, it may be uneconomical to use collection trucks for travel to the disposal site.
Transfer stations are therefore established at convenient locations, and one-person trailer or large trucks, 27 to 46 m3
(35 to 60 yd3 ) or larger, are used to transfer wastes to the disposal site. Among the important considerations in
planning and designing a transfer station are location, type of station, access, and environmental effects. At the
transfer station, partial or complete solid waste processing such as sorting, shredding, compacting, baling, or
composting may be provided. The objective is to reduce the volume, alter the physical form, and recover usable
materials. It is important that the transfer station be located as near as possible to the generation center. Good access
roads as well as secondary or supplemental means of transportation are necessary. Also, the site must be
environmentally acceptable. If more than one transfer station and disposal sites are used, then optimum allocation of
wastes from each transfer station to each disposal site will be necessary. This is a classical problem in the field of
operations research. Several mathematical models can be used to achieve economical solid waste allocation to the
transfer stations and distribution to the disposal sites.
Resource Recovery And Recycling

Many components of municipal solid wastes can be reused as secondary material. Among these are papers,
cardboard, plastic, glass, ferrous metal, aluminum, and other nonferrous metals. These materials must be separated
from MSW before they can be recycled. In this section, material recycling, and separation methods are first briefly
presented, followed by bioconversion and refuse derived fuel (RDF) methods.
Material Recycling
The thrust of much state and local legislative action in mid-1980s was to encourage recycling of various components
of municipal solid waste. Many have been made in the area of recycling, but not have been very successful. There
are several reasons such as recycled material may contain increased levels of foreign materials that could interfere
with product quality, uncertainty of supply and price variation of secondary material, methods of quality control of
recycled material are not developed as for virgin materials. Many components of MSW are currently recycled.
Among these are paper and paper products. These products are recycled in manufacturing building materials such as
roofing felt, insulation and wallboard, and are also used to manufacture cartons and containers. Plastic is recycled to
produce insulating material, sheets, bags, and structural material. Energy is recovered from combustion of organic
wastes. Other components of MSW (1990) estimate that approximately 13% of MSW is currently recycled, and a 14
percent fraction is incinerated.
Separation Methods
The separation of material is performed by the users at the source, or separated from mixed refuse at a central
processing facility. Material separation at the source involves users separating the material into different
components, followed by transporting from the point of generation to a secondary material dealer. Unfortunately,
active household response for separation at the source has been very poor. As a result, effort has been directed
toward separation of MSW at a central facility. Handpicking is a long-used form of separation of a few components
of solid wastes. In this operation, a conveyor moves the solid waste pass by a group of workers who pick up the
designated components by hand. This method of separation is costly, and only a few bulky components, such as
bundled newspapers and cardboard, can be separated. A mechanized material recovery method provided by utilizes
shearers that break open the bags and liberate cans and bottles. Trammel screens separate cans, glass and other
inorganic material. The organic material is shredded and passed through air classifiers, which separate the
components desired for recovery of fibers for paper making or for producing refuse derived fuel. Magnetic and
electromechanical systems separate ferrous and nonferrous metals.
Bioconversion
Bioconversion of the organic fraction of municipal solid waste into a number of products including sugar, ethanol,
and protein compost, has been reported in the literature.
Sugar
The recovery of fibers from paper has cellulose as major constituent. The cellulose is hydrolyzed into sugars. The
hydrolysis of cellulose produces glucose and mixtures of other sugars. Hydrolysis of paper fibers is achieved under
low pH, or by enzymes.
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ISSN: 2320-5407 Int. J. Adv. Res. 7(4), 160-164
Ethanol and other fermentation products

Microorganisms can produce alcohols and short-chain organic acids. These products have commercial value in the
industrial chemical market.
Many researchers have investigated the production of commercial quantities of these products using paper fibers
recovered from municipal solid wastes. However, the cost of production and recovery of these products in a
relatively pure state from MSW is much greater than the cost of producing the raw materials.
Protein
Earlier research conducted by the Denver Research Institute suggested that fibers produced from waste paper can be
converted to protein using a fast-growing-hydrocarbon-cellulose digesting organism. The organism is Candia utilis
culture, commonly called Torula yeast. The protein thus produced is usable by livestock. This process is called
annelidic recycling. The organic component is converted into a rich fertilizer in the form of worm of worm castings,
the excess worms are dried into high-protein food supplement in animal food. Another similar concept is to breed
flies and recover larvae as a protein source for animal feed supplement.
Incineration And Energy Recovery

Incineration of MSW is practiced to reduce waste volume and recover energy. The batch-fed incinerators built in the
1930s and 1940s reduced the volume but were major contributors of air pollution problems. Most of these
incinerators have been shut down or replaced by newer designs. The newer incinerators utilize innovative
technology to produce steam more efficiently and reduce air pollutants to greater extent. The capital and operating
costs, however, are quite high. The unit cost of incinerators for smaller cities is even larger. The high cost of
installing the air pollution control equipment forced municipalities to seek cheaper methods such as sanitary landfills
for solid waste disposal. Due to stricter regulation on landfilling, and rapidly diminishing capacity, there is renewed
interest in incinerator design and construction. Today there are more than 100 facilities in operation, and over 100
more are in the planning and construction stages.
Refuse-Derived Fuel (Rdf)

Solid wastes may be burned directly in incinerators (a process called mass-burning) or converted to more efficient
refuse-derived fuel (RDF). The solid waste is processed by means of size reduction and material separation
techniques to obtain a product which has a substantial heat value. Physically, shredded and air classified organic
fraction of solid wastes are burned along with a fossil fuel such as coal. Many boilers need only minor modifications
to accept such fuel. Also, the shredded and air classified solid wastes can be made densely into cubes or pellets that
are suitable for many thermal conversion processes such as incineration, gasification, and pyrolysis. Many
communities have built refuse-to-energy plants that are fast replacing sanitary landfills. The steam is used for
heating and for driving turbines to produce electricity. Of these, 142 facilities are waste-to-energy combustors. The
total processing capacity exceeds 31.4 million tons of MSW per year. These facilities do not include RDF-
processing plants or simple incinerators. There are also approximately 49 waste-to-energy combustors planned or
under construction.
Disposal By Landfilling
The volume of municipal solid waste is greatly reduced by incineration, conversion processes or resource recovery.
In all cases, there is a residue that must be disposed of so that it no longer creates a nuisance or hazard to the society.
Engineering principles must be followed for site selection and design of ultimate-land disposal methods. An
acceptable land disposal method of MSW and residues utilizes sanitary landfills. Sanitary landfilling is the most
common method of solid waste disposal in the United States. It is economical, and applies to all components of
MSW. Proper site selection is perhaps the most difficult part of disposal by landfilling. The operation involves
compaction of solid wastes in layers, then covering with a layer of compacted soil at the end of each day’s
operation. In recent years, special care has been required in site selection, refuse compaction, cover application,
leachate collection and treatment, and site monitoring.
Conclusions:-
The quantity of MSW generated is increasing rapidly due to increasing population and change in lifestyle. The
current MSW crisis should be approached holistically; while planning for long term solutions, focus on the solving
the present problems should be maintained. The Government and local authorities should work with their partners to
promote source separation, achieve higher percentages of recycling and produce high quality compost from
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ISSN: 2320-5407 Int. J. Adv. Res. 7(4), 160-164
organics. While this is being achieved and recycling is increased, provisions should be made to handle the non-
recyclable wastes that are being generated and will continue to be generated in the future. Policy to include waste-
pickers in the private sector must be introduced to utilize their low cost public and environmental service and to
provide better working conditions to these marginalized populations.
References:-
1. U.S. Environmental Protection Agency, “Characterization of municipal solid waste in
the United States,” Solid Waste and Emergency Response, Washington D.C., 1990.
2. U.S. Environmental Protection Agency, “Characterization of municipal solid waste in
the United States,” Final Report Prepared by Franklin Associates, Inc, 1988.
3. P. A. Vesilind, J. J. Pierce, and R. F. Weiner, Environmental Engineering, 2nd ed. Boston, MA:
Butterworth's, 1988.
4. U.S. Environmental Protection Agency, “Decision-Makers guide in solid waste management,” SW-500,
Washington D.C.: U.S. Government Printing Office, 1976.
5. U.S. Congress, “Facing America's trash: What next for municipal solid waste,” OTA-0-424, Office of
Technology Assessment, Washington D.C.: U.S. Government Printing Office, 1989.
6. R. Woods, “Refuse vehicles of the „90s,” Waste Age, vol. 23, no. 5, 38-44, 1992.
7. K. A. Shuster and D. A. Schur, “Heuristic routing for solid waste collection vehicles,” SW-11, U.S.
Environmental Protection Agency, 1974.
8. Matrecon, “Lining of waste impoundment and disposal facilities,” SW-870, U.S. Environmental
Protection Agency, Cincinnati, OH, 1980.
9. M. L. Davis and D. A. Cornwell, Introduction to Environmental Engineering, 2nd ed. New York:
MacGraw-Hills, Inc, 1991.
10. G. Tchobanoglous, H. Theisen, and S. Vigil, “Integrated solid waste management,” Engineering
Principles and Management Issues, New York: McGraw Hill, 1993.
11. [11] D. C. Wilson, Waste Management: Planning, Evaluation Technologies, Oxford: Clarendon Press, 1981.
12. N. L. Drobny, H. E. Hull, and R. F. Testin, “Recovery and utilization of municipal solid waste,” EPA-
SW-10C-71, U.S. Environmental Protection Agency, Office of Solid Waste Management Program,
Washington D.C. (NTIS No. PB-204 922), 1971.
13. P. A. Vesilind and A. E. Rimer, Unit Operations in Response Recovery Engineering, Englewood Cliffs,
NJ: Prentice Hall, Inc, 1981.
14. J. V. L. Kiser, “Municipal waste combustion in North America,” Waste Age, vol. 23, no. 11, pp. 26-34,
1992.
164
8/29/22, 4:14 PM Scanning electron microscope - Wikipedia
Scanning electron microscope

A scanning electron microscope (SEM) is a type of electron
microscope that produces images of a sample by scanning the
surface with a focused beam of electrons. The electrons interact
with atoms in the sample, producing various signals that contain
information about the surface topography and composition of the
sample. The electron beam is scanned in a raster scan pattern, and
the position of the beam is combined with the intensity of the
detected signal to produce an image. In the most common SEM
mode, secondary electrons emitted by atoms excited by the
electron beam are detected using a secondary electron detector Image of pollen grains taken on a
(Everhart–Thornley detector). The number of secondary electrons SEM shows the characteristic depth
that can be detected, and thus the signal intensity, depends, of field of SEM micrographs
among other things, on specimen topography. Some SEMs can
achieve resolutions better than 1 nanometer.
Specimens are observed in high vacuum in a conventional SEM, or

in low vacuum or wet conditions in a variable pressure or
environmental SEM, and at a wide range of cryogenic or elevated
temperatures with specialized instruments.[1]
Contents
History
Principles and capacities
Sample preparation
Biological samples
Materials
Scanning process and image formation
Magnification M. von Ardenne's first SEM
Detection of secondary electrons

Detection of backscattered electrons
Beam-injection analysis of semiconductors
Cathodoluminescence
X-ray microanalysis
Resolution of the SEM
Environmental SEM Operating principle of a Scanning
Electron Microscope (SEM)
Transmission SEM
Color in SEM
https://en.wikipedia.org/wiki/Scanning_electron_microscope 1/26
False color using a single detector

SEM image coloring
Color built using multiple electron detectors
Analytical signals based on generated photons
3D in SEM
3D SEM reconstruction from a stereo pair
Photometric 3D SEM reconstruction from a four-quadrant
detector by "shape from shading"
Photometric 3D rendering from a single SEM image SEM with opened sample chamber
Other types of 3D SEM reconstruction
Applications of 3D SEM
Gallery of SEM images
See also
References
External links
History Analog type SEM
An account of the early history of scanning electron microscopy

has been presented by McMullan.[2][3] Although Max Knoll produced a photo with a 50 mm object-
field-width showing channeling contrast by the use of an electron beam scanner,[4] it was Manfred
von Ardenne who in 1937 invented[5] a microscope with high resolution by scanning a very small
raster with a demagnified and finely focused electron beam. Ardenne applied scanning of the electron
beam in an attempt to surpass the resolution of the transmission electron microscope (TEM), as well
as to mitigate substantial problems with chromatic aberration inherent to real imaging in the TEM.
He further discussed the various detection modes, possibilities and theory of SEM,[6] together with
the construction of the first high resolution SEM.[7] Further work was reported by Zworykin's
group,[8] followed by the Cambridge groups in the 1950s and early 1960s[9][10][11][12] headed by
Charles Oatley, all of which finally led to the marketing of the first commercial instrument by
Cambridge Scientific Instrument Company as the "Stereoscan" in 1965, which was delivered to
DuPont.
Principles and capacities

The signals used by a SEM to produce an image result from
interactions of the electron beam with atoms at various depths
within the sample. Various types of signals are produced including
secondary electrons (SE), reflected or back-scattered electrons
(BSE), characteristic X-rays and light (cathodoluminescence)
(CL), absorbed current (specimen current) and transmitted Schottky-emitter electron source
electrons. Secondary electron detectors are standard equipment in
all SEMs, but it is rare for a single machine to have detectors for
all other possible signals.
Secondary electrons have very low energies on the order of 50 eV,

which limits their mean free path in solid matter. Consequently,
SEs can only escape from the top few nanometers of the surface of
a sample. The signal from secondary electrons tends to be highly
localized at the point of impact of the primary electron beam,
making it possible to collect images of the sample surface with a
resolution of below 1 nm. Back-scattered electrons (BSE) are beam
electrons that are reflected from the sample by elastic scattering.
Since they have much higher energy than SEs, they emerge from
deeper locations within the specimen and, consequently, the
resolution of BSE images is less than SE images. However, BSE
are often used in analytical SEM, along with the spectra made Electron–matter interaction volume
from the characteristic X-rays, because the intensity of the BSE and types of signal generated
signal is strongly related to the atomic number (Z) of the
specimen. BSE images can provide information about the
distribution, but not the identity, of different elements in the sample. In samples predominantly
composed of light elements, such as biological specimens, BSE imaging can image colloidal gold
immuno-labels of 5 or 10 nm diameter, which would otherwise be difficult or impossible to detect in
secondary electron images.[13] Characteristic X-rays are emitted when the electron beam removes an
inner shell electron from the sample, causing a higher-energy electron to fill the shell and release
energy. The energy or wavelength of these characteristic X-rays can be measured by Energy-
dispersive X-ray spectroscopy or Wavelength-dispersive X-ray spectroscopy and used to identify and
measure the abundance of elements in the sample and map their distribution.
Due to the very narrow electron beam, SEM micrographs have a large depth of field yielding a
characteristic three-dimensional appearance useful for understanding the surface structure of a
sample.[14] This is exemplified by the micrograph of pollen shown above. A wide range of
magnifications is possible, from about 10 times (about equivalent to that of a powerful hand-lens) to
more than 500,000 times, about 250 times the magnification limit of the best light microscopes.
Sample preparation
SEM samples have to be small enough to fit on the specimen
stage, and may need special preparation to increase their electrical
conductivity and to stabilize them, so that they can withstand the
high vacuum conditions and the high energy beam of electrons.
Samples are generally mounted rigidly on a specimen holder or
stub using a conductive adhesive. SEM is used extensively for
defect analysis of semiconductor wafers, and manufacturers make
instruments that can examine any part of a 300 mm
semiconductor wafer. Many instruments have chambers that can
tilt an object of that size to 45° and provide continuous 360° A spider sputter-coated in gold,
rotation. having been prepared for viewing
with an SEM
Nonconductive specimens collect charge when scanned by the
electron beam, and especially in secondary electron imaging
mode, this causes scanning faults and other image artifacts. For conventional imaging in the SEM,
specimens must be electrically conductive, at least at the surface, and electrically grounded to prevent
the accumulation of electrostatic charge. Metal objects require little special preparation for SEM
except for cleaning and conductively mounting to a specimen stub. Non-conducting materials are
usually coated with an ultrathin coating of electrically conducting

material, deposited on the sample either by low-vacuum sputter
coating or by high-vacuum evaporation. Conductive materials in
current use for specimen coating include gold, gold/palladium
alloy, platinum, iridium, tungsten, chromium, osmium,[13] and
graphite. Coating with heavy metals may increase signal/noise
ratio for samples of low atomic number (Z). The improvement
arises because secondary electron emission for high-Z materials is
enhanced.
Low-voltage micrograph (300 V) of
An alternative to coating for some biological samples is to increase distribution of adhesive droplets on
the bulk conductivity of the material by impregnation with a Post-it note. No conductive
osmium using variants of the OTO staining method (O-osmium coating was applied: such a coating
tetroxide, T-thiocarbohydrazide, O-osmium).[15][16] would alter this fragile specimen.
Nonconducting specimens may be imaged without coating using

an environmental SEM (ESEM) or low-voltage mode of SEM operation. In ESEM instruments the
specimen is placed in a relatively high-pressure chamber and the electron optical column is
differentially pumped to keep vacuum adequately low at the electron gun. The high-pressure region
around the sample in the ESEM neutralizes charge and provides an amplification of the secondary
electron signal. Low-voltage SEM is typically conducted in an instrument with a field emission guns
(FEG) which is capable of producing high primary electron brightness and small spot size even at low
accelerating potentials. To prevent charging of non-conductive specimens, operating conditions must
be adjusted such that the incoming beam current is equal to sum of outgoing secondary and
backscattered electron currents, a condition that is most often met at accelerating voltages of 0.3–4
kV.
Embedding in a resin with further polishing to a mirror-like finish can be used for both biological and
materials specimens when imaging in backscattered electrons or when doing quantitative X-ray
microanalysis.
The main preparation techniques are not required in the environmental SEM outlined below, but
some biological specimens can benefit from fixation.
Biological samples
For SEM, a specimen is normally required to be completely dry, since the specimen chamber is at
high vacuum. Hard, dry materials such as wood, bone, feathers, dried insects, or shells (including egg
shells[17]) can be examined with little further treatment, but living cells and tissues and whole, soft-
bodied organisms require chemical fixation to preserve and stabilize their structure.
Fixation is usually performed by incubation in a solution of a buffered chemical fixative, such as

glutaraldehyde, sometimes in combination with formaldehyde[18][19][20] and other fixatives,[21] and
optionally followed by postfixation with osmium tetroxide.[18] The fixed tissue is then dehydrated.
Because air-drying causes collapse and shrinkage, this is commonly achieved by replacement of water
in the cells with organic solvents such as ethanol or acetone, and replacement of these solvents in turn
with a transitional fluid such as liquid carbon dioxide by critical point drying.[22] The carbon dioxide
is finally removed while in a supercritical state, so that no gas–liquid interface is present within the
sample during drying.
The dry specimen is usually mounted on a specimen stub using an adhesive such as epoxy resin or
electrically conductive double-sided adhesive tape, and sputter-coated with gold or gold/palladium
alloy before examination in the microscope. Samples may be sectioned (with a microtome) if
information about the organism's internal ultrastructure is to be exposed for imaging.
If the SEM is equipped with a cold stage for cryo microscopy, cryofixation may be used and low-
temperature scanning electron microscopy performed on the cryogenically fixed specimens.[18] Cryo-
fixed specimens may be cryo-fractured under vacuum in a special apparatus to reveal internal
structure, sputter-coated and transferred onto the SEM cryo-stage while still frozen.[23] Low-
temperature scanning electron microscopy (LT-SEM) is also applicable to the imaging of
temperature-sensitive materials such as ice[24][25] and fats.[26]
Freeze-fracturing, freeze-etch or freeze-and-break is a preparation method particularly useful for

examining lipid membranes and their incorporated proteins in "face on" view. The preparation
method reveals the proteins embedded in the lipid bilayer.
Materials
Back-scattered electron imaging, quantitative X-ray analysis, and X-ray mapping of specimens often
requires grinding and polishing the surfaces to an ultra-smooth surface. Specimens that undergo
WDS or EDS analysis are often carbon-coated. In general, metals are not coated prior to imaging in
the SEM because they are conductive and provide their own pathway to ground.
Fractography is the study of fractured surfaces that can be done on a light microscope or, commonly,
on an SEM. The fractured surface is cut to a suitable size, cleaned of any organic residues, and
mounted on a specimen holder for viewing in the SEM.
Integrated circuits may be cut with a focused ion beam (FIB) or other ion beam milling instrument for
viewing in the SEM. The SEM in the first case may be incorporated into the FIB, enabling high-
resolution imaging of the result of the process.
Metals, geological specimens, and integrated circuits all may also be chemically polished for viewing
in the SEM.
Special high-resolution coating techniques are required for high-magnification imaging of inorganic
thin films.
Scanning process and image formation

In a typical SEM, an electron beam is thermionically emitted from an electron gun fitted with a
tungsten filament cathode. Tungsten is normally used in thermionic electron guns because it has the
highest melting point and lowest vapor pressure of all metals, thereby allowing it to be electrically
heated for electron emission, and because of its low cost. Other types of electron emitters include
lanthanum hexaboride (LaB
6) cathodes, which can be used in a standard tungsten filament SEM if the
vacuum system is upgraded or field emission guns (FEG), which may be of the cold-cathode type
using tungsten single crystal emitters or the thermally assisted Schottky type, that use emitters of
tungsten single crystals coated in zirconium oxide.
The electron beam, which typically has an

energy ranging from 0.2 keV to 40 keV, is
focused by one or two condenser lenses to a
spot about 0.4 nm to 5 nm in diameter. The
beam passes through pairs of scanning coils or
pairs of deflector plates in the electron column,
typically in the final lens, which deflect the
beam in the x and y axes so that it scans in a
raster fashion over a rectangular area of the
sample surface.
When the primary electron beam interacts with

the sample, the electrons lose energy by
repeated random scattering and absorption
within a teardrop-shaped volume of the Schematic of an SEM
specimen known as the interaction volume,
which extends from less than 100 nm to
approximately 5 µm into the surface. The size of the interaction
volume depends on the electron's landing energy, the atomic
number of the specimen and the specimen's density. The energy
exchange between the electron beam and the sample results in the
reflection of high-energy electrons by elastic scattering, emission
of secondary electrons by inelastic scattering and the emission of
electromagnetic radiation, each of which can be detected by
specialized detectors. The beam current absorbed by the specimen
can also be detected and used to create images of the distribution
of specimen current. Electronic amplifiers of various types are
used to amplify the signals, which are displayed as variations in
brightness on a computer monitor (or, for vintage models, on a
cathode-ray tube). Each pixel of computer video memory is
synchronized with the position of the beam on the specimen in the
microscope, and the resulting image is, therefore, a distribution
Mechanisms of emission of
map of the intensity of the signal being emitted from the scanned
secondary electrons, backscattered
area of the specimen. Older microscopes captured images on film,
electrons, and characteristic X-rays
but most modern instrument collect digital images.
from atoms of the sample
Magnification
Magnification in an SEM can be controlled over a range of about 6 orders of magnitude from about 10
to 3,000,000 times.[27] Unlike optical and transmission electron microscopes, image magnification in
an SEM is not a function of the power of the objective lens. SEMs may have condenser and objective
lenses, but their function is to focus the beam to a spot, and not to image the specimen. Provided the
electron gun can generate a beam with sufficiently small diameter, a SEM could in principle work
entirely without condenser or objective lenses, although it might not be very versatile or achieve very
high resolution. In an SEM, as in scanning probe microscopy, magnification results from the ratio of
the raster on the display device and dimensions of the raster on the specimen. Assuming that the
display screen has a fixed size, higher magnification results from reducing the size of the raster on the
specimen, and vice versa. Magnification is therefore controlled by the current supplied to the x, y
scanning coils, or the voltage supplied to the x, y deflector plates, and not by objective lens power.
Detection of secondary electrons

The most common imaging mode collects low-energy (<50 eV) secondary
electrons that are ejected from conduction or valence bands of the
specimen atoms by inelastic scattering interactions with beam electrons.
Due to their low energy, these electrons originate from within a few
nanometers below the sample surface.[14] The electrons are detected by
an Everhart–Thornley detector,[28] which is a type of collector-
scintillator-photomultiplier system. The secondary electrons are first
collected by attracting them towards an electrically biased grid at about
+400 V, and then further accelerated towards a phosphor or scintillator
positively biased to about +2,000 V. The accelerated secondary electrons
are now sufficiently energetic to cause the scintillator to emit flashes of
light (cathodoluminescence), which are conducted to a photomultiplier
outside the SEM column via a light pipe and a window in the wall of the
specimen chamber. The amplified electrical signal output by the
photomultiplier is displayed as a two-dimensional intensity distribution
that can be viewed and photographed on an analogue video display, or
subjected to analog-to-digital conversion and displayed and saved as a
digital image. This process relies on a raster-scanned primary beam. The
brightness of the signal depends on the number of secondary electrons
reaching the detector. If the beam enters the sample perpendicular to the
surface, then the activated region is uniform about the axis of the beam
and a certain number of electrons "escape" from within the sample. As
the angle of incidence increases, the interaction volume increases and the
"escape" distance of one side of the beam decreases, resulting in more
secondary electrons being emitted from the sample. Thus steep surfaces
and edges tend to be brighter than flat surfaces, which results in images
with a well-defined, three-dimensional appearance. Using the signal of
secondary electrons image resolution less than 0.5 nm is possible.
Detection of backscattered electrons

Backscattered electrons (BSE) consist
of high-energy electrons originating
in the electron beam, that are
reflected or back-scattered out of the
specimen interaction volume by
elastic scattering interactions with
Low-temperature SEM
specimen atoms. Since heavy
magnification series for a
elements (high atomic number)
snow crystal. The crystals
backscatter electrons more strongly Comparison of SEM techniques:
are captured, stored, and

than light elements (low atomic Top: backscattered electron
sputter-coated with analysis – composition
platinum at cryogenic
number), and thus appear brighter in
the image, BSEs are used to detect Bottom: secondary electron
temperatures for imaging.
contrast between areas with different analysis – topography
chemical compositions.[14] The
Everhart–Thornley detector, which is normally positioned to one
side of the specimen, is inefficient for the detection of backscattered electrons because few such
electrons are emitted in the solid angle subtended by the detector, and because the positively biased
detection grid has little ability to attract the higher energy BSE. Dedicated backscattered electron
detectors are positioned above the sample in a "doughnut" type arrangement, concentric with the
electron beam, maximizing the solid angle of collection. BSE detectors are usually either of scintillator
or of semiconductor types. When all parts of the detector are used to collect electrons symmetrically
about the beam, atomic number contrast is produced. However, strong topographic contrast is
produced by collecting back-scattered electrons from one side above the specimen using an
asymmetrical, directional BSE detector; the resulting contrast appears as illumination of the
topography from that side. Semiconductor detectors can be made in radial segments that can be
switched in or out to control the type of contrast produced and its directionality.
Backscattered electrons can also be used to form an electron backscatter diffraction (EBSD) image
that can be used to determine the crystallographic structure of the specimen.
Beam-injection analysis of semiconductors

The nature of the SEM's probe, energetic electrons, makes it uniquely suited to examining the optical
and electronic properties of semiconductor materials. The high-energy electrons from the SEM beam
will inject charge carriers into the semiconductor. Thus, beam electrons lose energy by promoting
electrons from the valence band into the conduction band, leaving behind holes.
In a direct bandgap material, recombination of these electron-hole pairs will result in

cathodoluminescence; if the sample contains an internal electric field, such as is present at a p-n
junction, the SEM beam injection of carriers will cause electron beam induced current (EBIC) to flow.
Cathodoluminescence and EBIC are referred to as "beam-injection" techniques, and are very powerful
probes of the optoelectronic behavior of semiconductors, in particular for studying nanoscale features
and defects.
Cathodoluminescence
Cathodoluminescence, the emission of light when atoms excited
by high-energy electrons return to their ground state, is analogous
to UV-induced fluorescence, and some materials such as zinc
sulfide and some fluorescent dyes, exhibit both phenomena. Over
the last decades, cathodoluminescence was most commonly
experienced as the light emission from the inner surface of the
cathode-ray tube in television sets and computer CRT monitors.
In the SEM, CL detectors either collect all light emitted by the
specimen or can analyse the wavelengths emitted by the specimen Color cathodoluminescence overlay
and display an emission spectrum or an image of the distribution on SEM image of an InGaN
of cathodoluminescence emitted by the specimen in real color. polycrystal. The blue and green
channels represent real colors, the
X-ray microanalysis red channel corresponds to UV
emission.
Characteristic X-rays that are produced by the interaction of

electrons with the sample may also be detected in an SEM equipped for energy-dispersive X-ray
spectroscopy or wavelength dispersive X-ray spectroscopy. Analysis of the x-ray signals may be used
to map the distribution and estimate the abundance of elements in the sample.
Resolution of the SEM

SEM is not a camera and the detector is not continuously image-
forming like a CCD array or film. Unlike in an optical system, the
resolution is not limited by the diffraction limit, fineness of lenses
or mirrors or detector array resolution. The focusing optics can be
large and coarse, and the SE detector is fist-sized and simply
detects current. Instead, the spatial resolution of the SEM
depends on the size of the electron spot, which in turn depends on
both the wavelength of the electrons and the electron-optical A video illustrating a typical practical
magnification range of a scanning
system that produces the scanning beam. The resolution is also
electron microscope designed for
limited by the size of the interaction volume, the volume of
biological specimens. The video
specimen material that interacts with the electron beam. The spot
starts at 25×, about 6 mm across
size and the interaction volume are both large compared to the
the whole field of view, and zooms
distances between atoms, so the resolution of the SEM is not high
in to 12000×, about 12 μm across
enough to image individual atoms, as is possible with a
the whole field of view. The
transmission electron microscope (TEM). The SEM has spherical objects are glass beads
compensating advantages, though, including the ability to image a with a diameter of 10 μm, similar in
comparatively large area of the specimen; the ability to image bulk diameter to a red blood cell.
materials (not just thin films or foils); and the variety of analytical
modes available for measuring the composition and properties of
the specimen. Depending on the instrument, the resolution can fall somewhere between less than
1 nm and 20 nm. As of 2009, The world's highest resolution conventional (≤30 kV) SEM can reach a
point resolution of 0.4 nm using a secondary electron detector.[29]
Environmental SEM
Conventional SEM requires samples to be imaged under vacuum, because a gas atmosphere rapidly
spreads and attenuates electron beams. As a consequence, samples that produce a significant amount
of vapour, e.g. wet biological samples or oil-bearing rock, must be either dried or cryogenically frozen.
Processes involving phase transitions, such as the drying of adhesives or melting of alloys, liquid
transport, chemical reactions, and solid-air-gas systems, in general cannot be observed with
conventional high-vacuum SEM. In environmental SEM (ESEM), the chamber is evacuated of air, but
water vapor is retained near its saturation pressure, and the residual pressure remains relatively high.
This allows the analysis of samples containing water or other volatile substances. With ESEM,
observations of living insects have been possible.[30]
The first commercial development of the ESEM in the late 1980s[31][32] allowed samples to be
observed in low-pressure gaseous environments (e.g. 1–50 Torr or 0.1–6.7 kPa) and high relative
humidity (up to 100%). This was made possible by the development of a secondary-electron
detector[33][34] capable of operating in the presence of water vapour and by the use of pressure-
limiting apertures with differential pumping in the path of the electron beam to separate the vacuum
region (around the gun and lenses) from the sample chamber. The first commercial ESEMs were
produced by the ElectroScan Corporation in USA in 1988. ElectroScan was taken over by Philips (who
later sold their electron-optics division to FEI Company) in 1996.[35]
ESEM is especially useful for non-metallic and biological materials because coating with carbon or
gold is unnecessary. Uncoated plastics and elastomers can be routinely examined, as can uncoated
biological samples. This is useful because coating can be difficult to reverse, may conceal small
features on the surface of the sample and may reduce the value of the results obtained. X-ray analysis
is difficult with a coating of a heavy metal, so carbon coatings are routinely used in conventional
SEMs, but ESEM makes it possible to perform X-ray microanalysis on uncoated non-conductive
specimens; however some specific for ESEM artifacts are introduced in X-ray analysis. ESEM may be
the preferred for electron microscopy of unique samples from criminal or civil actions, where forensic
analysis may need to be repeated by several different experts. It is possible to study specimens in
liquid with ESEM or with other liquid-phase electron microscopy methods.[36]
Transmission SEM
The SEM can also be used in transmission mode by simply incorporating an appropriate detector
below a thin specimen section.[37] Detectors are available for bright field, dark field, as well as
segmented detectors for mid-field to high angle annular dark-field. Despite the difference in
instrumentation, this technique is still commonly referred to as scanning transmission electron
microscopy (STEM).
Color in SEM
Electron microscopes do not naturally produce color images, as an SEM produces a single value per
pixel; this value corresponds to the number of electrons received by the detector during a small period
of time of the scanning when the beam is targeted to the (x, y) pixel position.
This single number is usually represented, for each pixel, by a grey level, forming a monochrome
image.[38] However, several ways have been used to get color electron microscopy images.[39]
False color using a single detector

On compositional images of flat surfaces (typically BSE):
The easiest way to get color is to associate to this single number an arbitrary color, using a color look-
up table (i.e. each grey level is replaced by a chosen color). This method is known as false color. On a
BSE image, false color may be performed to better distinguish the various phases of the sample.[40]
On textured-surface images:
As an alternative to simply replacing each grey level by a color, a sample observed by an oblique beam
allows researchers to create an approximative topography image (see further section "Photometric 3D
rendering from a single SEM image"). Such topography can then be processed by 3D-rendering
algorithms for a more natural rendering of the surface texture
Surface of a kidney stone The same after re-processing of

the color from the estimated
topography
SEM image of a diagenetically The same image after similar

altered discoaster colorization
SEM image coloring
Very often, published SEM images are artificially colored.[40] This may be done for aesthetic effect, to
clarify structure or to add a realistic appearance to the sample and generally does not add information
about the specimen.[41]
Coloring may be performed manually with photo-editing software, or semi-automatically with

dedicated software using feature-detection or object-oriented segmentation.[42]
SEM image of Cobaea scandens The same after semi-automatic

pollen coloring. Arbitrary colors help
identifying the various elements of
the structure
Colored SEM image of Colored SEM image of native gold

Tradescantia pollen and stamens and arsenopyrite crystal
intergrowth
Color built using multiple electron detectors
In some configurations more information is gathered per pixel, often by the use of multiple
detectors.[43]
As a common example, secondary electron and backscattered electron detectors are superimposed
and a color is assigned to each of the images captured by each detector,[44][45] with an end result of a
combined color image where colors are related to the density of the components. This method is
known as density-dependent color SEM (DDC-SEM). Micrographs produced by DDC-SEM retain
topographical information, which is better captured by the secondary electrons detector and combine
it to the information about density, obtained by the backscattered electron detector.[46][47]
DDC-SEM of calcified particle in Signal 2 : BSE

cardiac tissue - Signal 1 : SE
Colorized image obtained from the Same work with a larger view, part
two previous. Density-dependent of a study on human
color scanning electron cardiovascular tissue calcification
micrograph SEM (DDC-SEM) of
cardiovascular calcification,
showing in orange a calcium
phosphate spherical particle
(denser material) and, in green,
the extracellular matrix (less
dense material)
Analytical signals based on generated photons
Measurement of the energy of photons emitted from the specimen is a common method to get
analytical capabilities. Examples are the energy-dispersive X-ray spectroscopy (EDS) detectors used
in elemental analysis and cathodoluminescence microscope (CL) systems that analyse the intensity
and spectrum of electron-induced luminescence in (for example) geological specimens. In SEM
systems using these detectors it is common to color code these extra signals and superimpose them in
a single color image, so that differences in the distribution of the various components of the specimen
can be seen clearly and compared. Optionally, the standard secondary electron image can be merged
with the one or more compositional channels, so that the specimen's structure and composition can
be compared. Such images can be made while maintaining the full integrity of the original signal data,
which is not modified in any way.
3D in SEM
SEMs do not naturally provide 3D images contrary to SPMs. However 3D data can be obtained using
an SEM with different methods as follows.
3D SEM reconstruction from a stereo pair

photogrammetry is the most metrologically accurate method to bring the third dimension to SEM
images.[40] Contrary to photometric methods (next paragraph), photogrammetry calculates
absolute heights using triangulation methods. The drawbacks are that it works only if there is a
minimum texture, and it requires two images to be acquired from two different angles, which
implies the use of a tilt stage. (Photogrammetry is a software operation that calculates the shift (or
"disparity") for each pixel, between the left image and the right image of the same pair. Such
disparity reflects the local height).
An SEM stereo pair of microfossils of less than

1 mm in size (Ostracoda) produced by tilting along
the longitudinal axis.
From this pair of SEM images, the third dimension

has been reconstructed by photogrammetry (using
MountainsSEM software, see next image) ; then a
series of 3D representations with different angles
have been made and assembled into a GIF file to
produce this animation.
3D surface reconstruction of a (Ra = 3 µm)

roughness calibration sample (as used to calibrate
profilometers), from 2 scanning electron
microscope images tilted by 15° (top left). The
calculation of the 3D model (bottom right) takes
about 1.5 second[48] and the error on the Ra
roughness value calculated is less than 0.5%.
Photometric 3D SEM reconstruction from a four-quadrant detector by "shape

from shading"
This method typically uses a four-quadrant BSE detector (alternatively for one manufacturer, a 3-
segment detector). The microscope produces four images of the same specimen at the same time, so
no tilt of the sample is required. The method gives metrological 3D dimensions as far as the slope of
the specimen remains reasonable.[40] Most SEM manufacturers now (2018) offer such a built-in or
optional four-quadrant BSE detector, together with proprietary software to calculate a 3D image in
real time.[49]
Other approaches use more sophisticated (and sometimes GPU-intensive) methods like the optimal
estimation algorithm and offer much better results[50] at the cost of high demands on computing
power.
In all instances, this approach works by integration of the slope, so vertical slopes and overhangs are
ignored; for instance, if an entire sphere lies on a flat, little more than the upper hemisphere is seen
emerging above the flat, resulting in wrong altitude of the sphere apex. The prominence of this effect
depends on the angle of the BSE detectors with respect to the sample, but these detectors are usually
situated around (and close to) the electron beam, so this effect is very common.
Photometric 3D rendering from a single SEM image
This method requires an SEM image obtained in oblique low angle lighting. The grey-level is then
interpreted as the slope, and the slope integrated to restore the specimen topography. This method is
interesting for visual enhancement and the detection of the shape and position of objects ; however
the vertical heights cannot usually be calibrated, contrary to other methods such as
photogrammetry.[40]
SEM image of a house fly Detail of the previous image.

compound eye surface at 450×
magnification.
SEM 3D reconstruction from the Same as the previous, but with

previous using shape from lighting homogenized before
shading algorithms. applying the shape from shading
algorithms
Other types of 3D SEM reconstruction

Inverse reconstruction using electron-material interactive models[51][52]
Multi-Resolution reconstruction using single 2D File: High-quality 3D imaging may be an ultimate
solution for revealing the complexities of any porous media, but acquiring them is costly and time-
consuming. High-quality 2D SEM images, on the other hand, are widely available. Recently, a
novel three-step, multiscale, multiresolution reconstruction method is presented that directly uses
2D images in order to develop 3D models. This method, based on a Shannon Entropy and
conditional simulation, can be used for most of the available stationary materials and can build
various stochastic 3D models just using a few thin sections.[53][54][55]
Ion-abrasion SEM (IA-SEM) is a method of nanoscale 3D imaging that uses a focused beam of
gallium to repeatedly abrade the specimen surface 20 nanometres at a time. Each exposed
surface is then scanned to compile a 3D image.[56][57]
Applications of 3D SEM
One possible application is measuring the roughness of ice crystals. This method can combine
variable-pressure environmental SEM and the 3D capabilities of the SEM to measure roughness on
individual ice crystal facets, convert it into a computer model and run further statistical analysis on
the model.[58] Other measurements include fractal dimension, examining fracture surface of metals,
characterization of materials, corrosion measurement, and dimensional measurements at the nano
scale (step height, volume, angle, flatness, bearing ratio, coplanarity, etc.).
SEM is also used by art conservationists to discern threats to paintings' surface stability due to aging,
such as the formations of complexes of zinc ions with fatty acids.[59] Forensic scientists use SEM to
detect art forgeries.
Gallery of SEM images

The following are examples of images taken using an SEM.
Colored SEM image of Compound eye of Ommatidia of Antarctic

soybean cyst nematode Antarctic krill Euphausia krill eye, a higher
and egg. The artificial superba. Arthropod eyes magnification of the krill's
coloring makes the image are a common subject in eye. SEMs cover a range
easier for non-specialists SEM micrographs due to from light microscopy up
to view and understand the depth of focus that an to the magnifications
the structures and SEM image can capture. available with a TEM.
surfaces revealed in Colored picture. Colored picture.
micrographs.
SEM image of normal SEM image of a Backscattered electron

circulating human blood. hederelloid from the (BSE) image of an
This is an older and noisy Devonian of Michigan antimony-rich region in a
micrograph of a common (largest tube diameter is fragment of ancient glass.
subject for SEM 0.75 mm). The SEM is Museums use SEMs for
micrographs: red blood used extensively for studying valuable artifacts
cells. capturing detailed images in a nondestructive
of micro and macro manner.
fossils.
SEM image of the SEM image of a SEM image of the surface

corrosion layer on the photoresist layer used in of a kidney stone showing
surface of an ancient semiconductor tetragonal crystals of
glass fragment; note the manufacturing taken on a Weddellite (calcium
laminar structure of the field emission SEM. oxalate dihydrate)
corrosion layer. These SEMs are emerging from the
important in the amorphous central part of
semiconductor industry the stone. Horizontal
for their high-resolution length of the picture
capabilities. represents 0.5 mm of the
figured original.
Two images of the same Epidermal cells from the SEM image of stomata on
depth hoar snow crystal, inner surface of an onion the lower surface of a
viewed through a light flake. Beneath the leaf.
microscope (left) and as shagreen-like cell walls
an SEM image (right). one can see nuclei and
Note how the SEM image small organelles floating
allows for clear perception in the cytoplasm. This
of the fine structure BSE-image of a
details which are hard to lanthanoid-stained sample
fully make out in the light was taken without prior
microscope image. fixation, nor dehydration,
nor sputtering.
See also
Applications for electron microscopy
Electron microscopy
Energy-dispersive X-ray spectroscopy
Cathodoluminescence microscope
Forensic engineering
Forensic science
List of surface analysis methods
Microscopy
Teeny Ted from Turnip Town (World's smallest book requires a scanning electron microscope to
read).
Transmission electron microscopy (TEM)
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External links
General
HowStuffWorks – How Scanning Electron Microscopes Work (http://www.howstuffworks.com/scan

ning-electron-microscope.htm)
Learn to use an SEM (https://myscope.training/#/SEMlevel_3_1) – An online learning environment
for people wanting to use an SEM. Provided by Microscopy Australia
Virtual SEM – sparkler (http://www.ammrf.org.au/myscope/sem/practice/virtualsem/sparkler.php) –
an interactive simulation of a scanning electron microscope (SEM)
Multichannel color SEM imaging (http://www.danilatos.com/colorESEM/colrESEM317.html) – and

with BSE (http://www.danilatos.com/scancol/scancol09.html)
DDC-SEM image examples (https://twitter.com/sbertazz)
Video on the scanning electron microscope (https://www.youtube.com/watch?v=GY9lfO-tVfE),
Karlsruhe University of Applied Sciences
Animations and explanations on various types of microscopes including electron microscopes (htt
p://toutestquantique.fr/en/microscopy/) (Université Paris Sud)
History
Environmental Scanning Electron Microscope (ESEM) history (http://www.danilatos.com)
Images
Rippel Electron Microscope Facility (http://remf.dartmouth.edu/imagesindex.html) Many dozens of

(mostly biological) SEM images from Dartmouth College.
Lanthanoid staining (http://bioree.ru/?lang=en) SEM images from Research Institute of Eye
Diseases, Moscow.
Retrieved from "https://en.wikipedia.org/w/index.php?title=Scanning_electron_microscope&oldid=1100146463"
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8/29/22, 4:13 PM Fourier-transform infrared spectroscopy - Wikipedia
Fourier-transform infrared spectroscopy

Fourier-transform infrared spectroscopy (FTIR)[1] is a technique used to obtain an infrared
spectrum of absorption or emission of a solid, liquid, or gas. An FTIR spectrometer simultaneously
collects high-resolution spectral data over a wide spectral range. This confers a significant advantage
over a dispersive spectrometer, which measures intensity over a narrow range of wavelengths at a
time.
The term Fourier-transform infrared spectroscopy originates from the fact that a Fourier transform
(a mathematical process) is required to convert the raw data into the actual spectrum.
Contents
Conceptual introduction
History
Michelson interferometer
Measuring and processing the interferogram
Advantages
An example of an FTIR
Resolution
spectrometer with an attenuated
Motivation total reflectance (ATR) attachment
Components
IR sources
Detectors
Beam splitter
Attenuated total reflectance
Fourier transform
Spectral range
Far-infrared
Mid-infrared
Near-infrared
Applications
Nano and biological materials
Microscopy and imaging
Nanoscale and spectroscopy below the diffraction limit
FTIR as detector in chromatography
TG-IR (thermogravimetric analysis-infrared spectrometry)
Water content determination in plastics and composites
See also
References
External links
https://en.wikipedia.org/wiki/Fourier-transform_infrared_spectroscopy 1/11
Conceptual introduction
The goal of absorption spectroscopy techniques (FTIR, ultraviolet-
visible ("UV-vis") spectroscopy, etc.) is to measure how much light
a sample absorbs at each wavelength. The most straightforward
way to do this, the "dispersive spectroscopy" technique, is to shine
a monochromatic light beam at a sample, measure how much of
the light is absorbed, and repeat for each different wavelength.
(This is how some UV–vis spectrometers work, for example.)
Fourier transform spectroscopy is a less intuitive way to obtain the

same information. Rather than shining a monochromatic beam of An FTIR interferogram. The central
light (a beam composed of only a single wavelength) at the peak is at the ZPD position ("zero
sample, this technique shines a beam containing many path difference" or zero retardation),
frequencies of light at once and measures how much of that beam where the maximal amount of light
passes through the interferometer to
is absorbed by the sample. Next, the beam is modified to contain a
the detector.
different combination of frequencies, giving a second data point.
This process is rapidly repeated many times over a short time
span. Afterwards, a computer takes all this data and works
backward to infer what the absorption is at each wavelength.
The beam described above is generated by starting with a broadband light source—one containing the
full spectrum of wavelengths to be measured. The light shines into a Michelson interferometer—a
certain configuration of mirrors, one of which is moved by a motor. As this mirror moves, each
wavelength of light in the beam is periodically blocked, transmitted, blocked, transmitted, by the
interferometer, due to wave interference. Different wavelengths are modulated at different rates, so
that at each moment or mirror position the beam coming out of the interferometer has a different
spectrum.
As mentioned, computer processing is required to turn the raw data (light absorption for each mirror
position) into the desired result (light absorption for each wavelength). The processing required turns
out to be a common algorithm called the Fourier transform. The Fourier transform converts one
domain (in this case displacement of the mirror in cm) into its inverse domain (wavenumbers in
cm−1). The raw data is called an "interferogram".
History
The first low-cost spectrophotometer capable of recording an infrared spectrum was the Perkin-Elmer
Infracord produced in 1957.[2] This instrument covered the wavelength range from 2.5 μm to 15 μm
(wavenumber range 4,000 cm−1 to 660 cm−1). The lower wavelength limit was chosen to encompass
the highest known vibration frequency due to a fundamental molecular vibration. The upper limit was
imposed by the fact that the dispersing element was a prism made from a single crystal of rock-salt
(sodium chloride), which becomes opaque at wavelengths longer than about 15 μm; this spectral
region became known as the rock-salt region. Later instruments used potassium bromide prisms to
extend the range to 25 μm (400 cm−1) and caesium iodide 50 μm (200 cm−1). The region beyond 50
μm (200 cm−1) became known as the far-infrared region; at very long wavelengths it merges into the
microwave region. Measurements in the far infrared needed the development of accurately ruled
diffraction gratings to replace the prisms as dispersing elements, since salt crystals are opaque in this
region. More sensitive detectors than the bolometer were required because of the low energy of the
radiation. One such was the Golay detector. An additional issue is the need to exclude atmospheric
water vapour because water vapour has an intense pure rotational spectrum in this region. Far-
infrared spectrophotometers were cumbersome, slow and expensive. The advantages of the Michelson
interferometer were well-known, but considerable technical difficulties had to be overcome before a
commercial instrument could be built. Also an electronic computer was needed to perform the
required Fourier transform, and this only became practicable with the advent of minicomputers, such
as the PDP-8, which became available in 1965. Digilab pioneered the world's first commercial FTIR
spectrometer (Model FTS-14) in 1969[1] (Digilab FTIRs are now a part of Agilent technologies's
molecular product line after it acquired spectroscopy business from Varian).[3][4]
Michelson interferometer
In a Michelson interferometer adapted for FTIR, light
from the polychromatic infrared source, approximately a
black-body radiator, is collimated and directed to a beam
splitter. Ideally 50% of the light is refracted towards the
fixed mirror and 50% is transmitted towards the moving
mirror. Light is reflected from the two mirrors back to the
beam splitter and some fraction of the original light
passes into the sample compartment. There, the light is
focused on the sample. On leaving the sample
compartment the light is refocused on to the detector.
The difference in optical path length between the two
arms to the interferometer is known as the retardation or
optical path difference (OPD). An interferogram is
obtained by varying the retardation and recording the
signal from the detector for various values of the Schematic diagram of a Michelson
retardation. The form of the interferogram when no interferometer, configured for FTIR
sample is present depends on factors such as the variation
of source intensity and splitter efficiency with wavelength.
This results in a maximum at zero retardation, when there is constructive interference at all
wavelengths, followed by series of "wiggles". The position of zero retardation is determined accurately
by finding the point of maximum intensity in the interferogram. When a sample is present the
background interferogram is modulated by the presence of absorption bands in the sample.
Commercial spectrometers use Michelson interferometers with a variety of scanning mechanisms to

generate the path difference. Common to all these arrangements is the need to ensure that the two
beams recombine exactly as the system scans. The simplest systems have a plane mirror that moves
linearly to vary the path of one beam. In this arrangement the moving mirror must not tilt or wobble
as this would affect how the beams overlap as they recombine. Some systems incorporate a
compensating mechanism that automatically adjusts the orientation of one mirror to maintain the
alignment. Arrangements that avoid this problem include using cube corner reflectors instead of
plane mirrors as these have the property of returning any incident beam in a parallel direction
regardless of orientation.
Systems where the path difference is generated by a rotary movement have proved very successful.
One common system incorporates a pair of parallel mirrors in one beam that can be rotated to vary
the path without displacing the returning beam. Another is the double pendulum design where the
path in one arm of the interferometer increases as the path in the other decreases.
A quite different approach involves moving a wedge of an IR-

transparent material such as KBr into one of the beams.
Increasing the thickness of KBr in the beam increases the optical
path because the refractive index is higher than that of air. One
limitation of this approach is that the variation of refractive index
over the wavelength range limits the accuracy of the wavelength
calibration. Interferometer schematics where
the path difference is generated by
a rotary motion.
Measuring and processing the
interferogram
The interferogram has to be measured from zero path difference to a maximum length that depends
on the resolution required. In practice the scan can be on either side of zero resulting in a double-
sided interferogram. Mechanical design limitations may mean that for the highest resolution the scan
runs to the maximum OPD on one side of zero only.
The interferogram is converted to a spectrum by Fourier transformation. This requires it to be stored

in digital form as a series of values at equal intervals of the path difference between the two beams. To
measure the path difference a laser beam is sent through the interferometer, generating a sinusoidal
signal where the separation between successive maxima is equal to the wavelength of the laser
(typically a 633 nm HeNe laser is used). This can trigger an analog-to-digital converter to measure the
IR signal each time the laser signal passes through zero. Alternatively, the laser and IR signals can be
measured synchronously at smaller intervals with the IR signal at points corresponding to the laser
signal zero crossing being determined by interpolation.[5] This approach allows the use of analog-to-
digital converters that are more accurate and precise than converters that can be triggered, resulting
in lower noise.
The result of Fourier transformation is a spectrum of

the signal at a series of discrete wavelengths. The range
of wavelengths that can be used in the calculation is
limited by the separation of the data points in the
interferogram. The shortest wavelength that can be
recognized is twice the separation between these data
points. For example, with one point per wavelength of
a HeNe reference laser at 0.633 μm (15 800 cm−1) the
shortest wavelength would be 1.266 μm (7900 cm−1).
Because of aliasing any energy at shorter wavelengths
would be interpreted as coming from longer
wavelengths and so has to be minimized optically or Values of the interferogram at times
electronically. The spectral resolution, i.e. the corresponding to zero crossings of the laser
separation between wavelengths that can be signal are found by interpolation.
distinguished, is determined by the maximum OPD.
The wavelengths used in calculating the Fourier
transform are such that an exact number of wavelengths fit into the length of the interferogram from
zero to the maximum OPD as this makes their contributions orthogonal. This results in a spectrum
with points separated by equal frequency intervals.
For a maximum path difference d adjacent wavelengths λ1 and λ2 will have n and (n+1) cycles,
respectively, in the interferogram. The corresponding frequencies are ν1 and ν2:
d = nλ1 and d = (n+1)λ2

λ1 = d/n and λ2 =d/(n+1)
ν1 = 1/λ1 and ν2 = 1/λ2
ν1 = n/d and ν2 = (n+1)/d
ν2 − ν1 = 1/d
The separation is the inverse of the maximum OPD. For example, a maximum OPD of 2 cm results in
a separation of 0.5 cm−1. This is the spectral resolution in the sense that the value at one point is
independent of the values at adjacent points. Most instruments can be operated at different
resolutions by choosing different OPD's. Instruments for routine analyses typically have a best
resolution of around 0.5 cm−1, while spectrometers have been built with resolutions as high as
0.001 cm−1, corresponding to a maximum OPD of 10 m. The point in the interferogram corresponding
to zero path difference has to be identified, commonly by assuming it is where the maximum signal
occurs. This so-called centerburst is not always symmetrical in real world spectrometers so a phase
correction may have to be calculated. The interferogram signal decays as the path difference
increases, the rate of decay being inversely related to the width of features in the spectrum. If the OPD
is not large enough to allow the interferogram signal to decay to a negligible level there will be
unwanted oscillations or sidelobes associated with the features in the resulting spectrum. To reduce
these sidelobes the interferogram is usually multiplied by a function that approaches zero at the
maximum OPD. This so-called apodization reduces the amplitude of any sidelobes and also the noise
level at the expense some reduction in resolution.
For rapid calculation the number of points in the interferogram has to equal a power of two. A string
of zeroes may be added to the measured interferogram to achieve this. More zeroes may be added in a
process called zero filling to improve the appearance of the final spectrum although there is no
improvement in resolution. Alternatively, interpolation after the Fourier transform gives a similar
result.
Advantages
There are three principal advantages for an FT spectrometer compared to a scanning (dispersive)
spectrometer.[1]
1. The multiplex or Fellgett's advantage. This arises from the fact that information from all
wavelengths is collected simultaneously. It results in a higher signal-to-noise ratio for a given
scan-time for observations limited by a fixed detector noise contribution (typically in the thermal
infrared spectral region where a photodetector is limited by generation-recombination noise). For
a spectrum with m resolution elements, this increase is equal to the square root of m.
Alternatively, it allows a shorter scan-time for a given resolution. In practice multiple scans are
often averaged, increasing the signal-to-noise ratio by the square root of the number of scans.
2. The throughput or Jacquinot's advantage. This results from the fact that in a dispersive
instrument, the monochromator has entrance and exit slits which restrict the amount of light that
passes through it. The interferometer throughput is determined only by the diameter of the
collimated beam coming from the source. Although no slits are needed, FTIR spectrometers do
require an aperture to restrict the convergence of the collimated beam in the interferometer. This
is because convergent rays are modulated at different frequencies as the path difference is
varied. Such an aperture is called a Jacquinot stop.[1] For a given resolution and wavelength this
circular aperture allows more light through than a slit, resulting in a higher signal-to-noise ratio.
3. The wavelength accuracy or Connes' advantage. The wavelength scale is calibrated by a laser
beam of known wavelength that passes through the interferometer. This is much more stable and
accurate than in dispersive instruments where the scale depends on the mechanical movement of
diffraction gratings. In practice, the accuracy is limited by the divergence of the beam in the
interferometer which depends on the resolution.
Another minor advantage is less sensitivity to stray light, that is radiation of one wavelength
appearing at another wavelength in the spectrum. In dispersive instruments, this is the result of
imperfections in the diffraction gratings and accidental reflections. In FT instruments there is no
direct equivalent as the apparent wavelength is determined by the modulation frequency in the
interferometer.
Resolution
The interferogram belongs in the length dimension. Fourier transform (FT) inverts the dimension, so
the FT of the interferogram belongs in the reciprocal length dimension([L−1]), that is the dimension
of wavenumber. The spectral resolution in cm−1 is equal to the reciprocal of the maximal retardation
in cm. Thus a 4 cm−1 resolution will be obtained if the maximal retardation is 0.25 cm; this is typical
of the cheaper FTIR instruments. Much higher resolution can be obtained by increasing the maximal
retardation. This is not easy, as the moving mirror must travel in a near-perfect straight line. The use
of corner-cube mirrors in place of the flat mirrors is helpful, as an outgoing ray from a corner-cube
mirror is parallel to the incoming ray, regardless of the orientation of the mirror about axes
perpendicular to the axis of the light beam. In 1966 Connes measured the temperature of the
atmosphere of Venus by recording the vibration-rotation spectrum of Venusian CO2 at 0.1 cm−1
resolution.[6] Michelson himself attempted to resolve the hydrogen Hα emission band in the spectrum
of a hydrogen atom into its two components by using his interferometer.[1] p25 A spectrometer with
0.001 cm−1 resolution is now available commercially. The throughput advantage is important for
high-resolution FTIR, as the monochromator in a dispersive instrument with the same resolution
would have very narrow entrance and exit slits.
Motivation
FTIR is a method of measuring infrared absorption and emission spectra. For a discussion of why
people measure infrared absorption and emission spectra, i.e. why and how substances absorb and
emit infrared light, see the article: Infrared spectroscopy.
Components
IR sources
FTIR spectrometers are mostly used for measurements in the mid and near IR regions. For the mid-
IR region, 2−25 μm (5,000–400 cm−1), the most common source is a silicon carbide (SiC) element
heated to about 1,200 K (930 °C; 1,700 °F) (Globar). The output is similar to a blackbody. Shorter
wavelengths of the near-IR, 1−2.5 μm (10,000–4,000 cm−1), require a higher temperature source,
typically a tungsten-halogen lamp. The long wavelength output of these is limited to about 5 μm
(2,000 cm−1) by the absorption of the quartz envelope. For the far-IR, especially at wavelengths
beyond 50 μm (200 cm−1) a mercury discharge lamp gives higher output than a thermal source.[7]
Detectors
Near-IR spectrometers commonly use pyroelectric

detectors that respond to changes in temperature as the
intensity of IR radiation falling on them varies. The
sensitive elements in these detectors are either deuterated
triglycine sulfate (DTGS) or lithium tantalate (LiTaO3).
These detectors operate at ambient temperatures and
provide adequate sensitivity for most routine
applications. To achieve the best sensitivity the time for a
scan is typically a few seconds. Cooled photoelectric
detectors are employed for situations requiring higher
sensitivity or faster response. Liquid nitrogen cooled
mercury cadmium telluride (MCT) detectors are the most
widely used in the mid-IR. With these detectors an FTIR setup. The sample is placed right before
interferogram can be measured in as little as 10 the detector.
milliseconds. Uncooled indium gallium arsenide
photodiodes or DTGS are the usual choices in near-IR
systems. Very sensitive liquid-helium-cooled silicon or germanium bolometers are used in the far-IR
where both sources and beamsplitters are inefficient.
Beam splitter
An ideal beam-splitter transmits and reflects 50% of the

incident radiation. However, as any material has a limited
range of optical transmittance, several beam-splitters
may be used interchangeably to cover a wide spectral
range. For the mid-IR region the beamsplitter is usually
made of KBr with a germanium-based coating that makes
it semi-reflective. KBr absorbs strongly at wavelengths
beyond 25 μm (400 cm−1) so CsI or KRS-5 are sometimes
used to extend the range to about 50 μm (200 cm−1).
ZnSe is an alternative where moisture vapor can be a
Simple interferometer with a beam-splitter and
problem but is limited to about 20μm (500 cm−1). CaF2 is
compensator plate
the usual material for the near-IR, being both harder and
less sensitive to moisture than KBr but cannot be used
beyond about 8 μm (1,200 cm−1). In a simple Michelson interferometer one beam passes twice
through the beamsplitter but the other passes through only once. To correct for this an additional
compensator plate of equal thickness is incorporated. Far-IR beamsplitters are mostly based on
polymer films and cover a limited wavelength range.[8]
Attenuated total reflectance
Attenuated total reflectance (ATR) is one accessory of FTIR spectrophotometer to measure surface
properties of solid or thin film samples rather than their bulk properties. Generally, ATR has a
penetration depth of around 1 or 2 micrometers depending on sample conditions.
Fourier transform
The interferogram in practice consists of a set of intensities measured for discrete values of
retardation. The difference between successive retardation values is constant. Thus, a discrete Fourier
transform is needed. The fast Fourier transform (FFT) algorithm is used.
Spectral range
Far-infrared
The first FTIR spectrometers were developed for far-infrared range. The reason for this has to do with
the mechanical tolerance needed for good optical performance, which is related to the wavelength of
the light being used. For the relatively long wavelengths of the far infrared, ~10 μm tolerances are
adequate, whereas for the rock-salt region tolerances have to be better than 1 μm. A typical
instrument was the cube interferometer developed at the NPL[9] and marketed by Grubb Parsons. It
used a stepper motor to drive the moving mirror, recording the detector response after each step was
completed.
Mid-infrared
With the advent of cheap microcomputers it became possible to have a computer dedicated to
controlling the spectrometer, collecting the data, doing the Fourier transform and presenting the
spectrum. This provided the impetus for the development of FTIR spectrometers for the rock-salt
region. The problems of manufacturing ultra-high precision optical and mechanical components had
to be solved. A wide range of instruments are now available commercially. Although instrument
design has become more sophisticated, the basic principles remain the same. Nowadays, the moving
mirror of the interferometer moves at a constant velocity, and sampling of the interferogram is
triggered by finding zero-crossings in the fringes of a secondary interferometer lit by a helium–neon
laser. In modern FTIR systems the constant mirror velocity is not strictly required, as long as the laser
fringes and the original interferogram are recorded simultaneously with higher sampling rate and
then re-interpolated on a constant grid, as pioneered by James W. Brault. This confers very high
wavenumber accuracy on the resulting infrared spectrum and avoids wavenumber calibration errors.
Near-infrared
The near-infrared region spans the wavelength range between the rock-salt region and the start of the
visible region at about 750 nm. Overtones of fundamental vibrations can be observed in this region. It
is used mainly in industrial applications such as process control and chemical imaging.
Applications
FTIR can be used in all applications where a dispersive spectrometer was used in the past (see
external links). In addition, the improved sensitivity and speed have opened up new areas of
application. Spectra can be measured in situations where very little energy reaches the detector and
scan rates can exceed 50 spectra a second. Fourier transform infrared spectroscopy is used in geology,
chemistry, materials and biology research fields.
Nano and biological materials
FTIR is also used to investigate various nanomaterials and proteins in hydrophobic membrane
environments. Studies show the ability of FTIR to directly determine the polarity at a given site along
the backbone of a transmembrane protein.[10][11] The bond features involved with various organic and
inorganic nanomaterials and their quantitative analysis can be done with the help of FTIR.[12][13]
Microscopy and imaging
An infrared microscope allows samples to be observed and spectra measured from regions as small as
5 microns across. Images can be generated by combining a microscope with linear or 2-D array
detectors. The spatial resolution can approach 5 microns with tens of thousands of pixels. The images
contain a spectrum for each pixel and can be viewed as maps showing the intensity at any wavelength
or combination of wavelengths. This allows the distribution of different chemical species within the
sample to be seen. Typical studies include analysing tissue sections as an alternative to conventional
histopathology and examining the homogeneity of pharmaceutical tablets.
Nanoscale and spectroscopy below the diffraction limit
The spatial resolution of FTIR can be further improved below the micrometer scale by integrating it
into scanning near-field optical microscopy platform. The corresponding technique is called nano-
FTIR and allows for performing broadband spectroscopy on materials in ultra-small quantities (single
viruses and protein complexes) and with 10 to 20 nm spatial resolution.[14]
FTIR as detector in chromatography
The speed of FTIR allows spectra to be obtained from compounds as they are separated by a gas
chromatograph. However this technique is little used compared to GC-MS (gas chromatography-mass
spectrometry) which is more sensitive. The GC-IR method is particularly useful for identifying
isomers, which by their nature have identical masses. Liquid chromatography fractions are more
difficult because of the solvent present. One notable exception is to measure chain branching as a
function of molecular size in polyethylene using gel permeation chromatography, which is possible
using chlorinated solvents that have no absorption in the area in question.
TG-IR (thermogravimetric analysis-infrared spectrometry)
Measuring the gas evolved as a material is heated allows qualitative identification of the species to
complement the purely quantitative information provided by measuring the weight loss.
Water content determination in plastics and composites
FTIR analysis is used to determine water content in fairly thin plastic and composite parts, more
commonly in the laboratory setting. Such FTIR methods have long been used for plastics, and became
extended for composite materials in 2018, when the method was introduced by Krauklis, Gagani and
Echtermeyer.[15] FTIR method uses the maxima of the absorbance band at about 5,200 cm−1 which
correlates with the true water content in the material.
See also
Discrete Fourier transform – Type of Fourier transform in discrete mathematics − for computing
periodicity in evenly spaced data
Fourier transform – Mathematical transform that expresses a function of time as a function of
frequency
Fourier transform spectroscopy
Least-squares spectral analysis – Frequency-domain analysis method − for computing periodicity
in unevenly spaced data
References
1. Griffiths, P.; de Hasseth, J. A. (18 May 2007). Fourier Transform Infrared Spectrometry (https://bo
oks.google.com/books?id=C_c0GVe8MX0C) (2nd ed.). Wiley-Blackwell. ISBN 978-0-471-19404-
0.
2. "The Infracord double-beam spectrophotometer". Clinical Science. 16 (2). 1957.
3. "Archived copy" (https://web.archive.org/web/20200414155545/https://www.agilent.com/about/ne
wsroom/presrel/varian/2004/15sep-v04044.htm). Archived from the original (http://www.agilent.co
m/about/newsroom/presrel/varian/2004/15sep-v04044.htm) on 2020-04-14. Retrieved
2013-03-05.
4. "Agilent Technologies to Acquire Varian, Inc. for $1.5 Billion" (http://www.agilent.co.in/about/newsr
oom/presrel/2009/27jul-gp09016.html). Agilent. July 27, 2009.
5. Brault, James W. (1996). "New Approach to high-precision Fourier transform spectrometer
design". Applied Optics. 35 (16): 2891–2896. Bibcode:1996ApOpt..35.2891B (https://ui.adsabs.ha
rvard.edu/abs/1996ApOpt..35.2891B). doi:10.1364/AO.35.002891 (https://doi.org/10.1364%2FA
O.35.002891). PMID 21085438 (https://pubmed.ncbi.nlm.nih.gov/21085438).
6. Connes, J.; Connes, P. (1966). "Near-Infrared Planetary Spectra by Fourier Spectroscopy. I.
Instruments and Results". Journal of the Optical Society of America. 56 (7): 896–910.
doi:10.1364/JOSA.56.000896 (https://doi.org/10.1364%2FJOSA.56.000896).
7. Smith, D.R.; Morgan, R.L.; Loewenstein, E.V. (1968). "Comparison of the Radiance of Far-Infrared
Sources". J. Opt. Soc. Am. 58 (3): 433–434. doi:10.1364/JOSA.58.000433 (https://doi.org/10.136
4%2FJOSA.58.000433).
8. Griffiths, P.R.; Holmes, C (2002). Handbook of Vibrational Spectroscopy, Vol 1. Chichester: John
Wiley and Sons.
9. Chamberain, J.; Gibbs, J.E.; Gebbie, H.E. (1969). "The determination of refractive index spectra
by fourier spectrometry". Infrared Physics. 9 (4): 189–209. Bibcode:1969InfPh...9..185C (https://ui.
adsabs.harvard.edu/abs/1969InfPh...9..185C). doi:10.1016/0020-0891(69)90023-2 (https://doi.or
g/10.1016%2F0020-0891%2869%2990023-2).
10. Manor, Joshua; Feldblum, Esther S.; Arkin, Isaiah T. (2012). "Environment Polarity in Proteins
Mapped Noninvasively by FTIR Spectroscopy" (https://www.ncbi.nlm.nih.gov/pmc/articles/PMC33
41589). The Journal of Physical Chemistry Letters. 3 (7): 939–944. doi:10.1021/jz300150v (http
s://doi.org/10.1021%2Fjz300150v). PMC 3341589 (https://www.ncbi.nlm.nih.gov/pmc/articles/PM
C3341589). PMID 22563521 (https://pubmed.ncbi.nlm.nih.gov/22563521).
11. Brielle, Esther S.; Arkin, Isaiah T. (2018). "Site-Specific Hydrogen Exchange in a Membrane
Environment Analyzed by Infrared Spectroscopy". The Journal of Physical Chemistry Letters. 9
(14): 4059–4065. doi:10.1021/acs.jpclett.8b01675 (https://doi.org/10.1021%2Facs.jpclett.8b0167
5). PMID 29957958 (https://pubmed.ncbi.nlm.nih.gov/29957958). S2CID 49621115 (https://api.se
manticscholar.org/CorpusID:49621115).
12. "Structural, functional and magnetic ordering modifications in graphene oxide and graphite by 100
MeV gold ion irradiation". Vacuum. 182: 109700. 2020-12-01. doi:10.1016/j.vacuum.2020.109700
13. Deepty, M., Ch Srinivas, E. Ranjith Kumar, N. Krisha Mohan, C. L. Prajapat, TV Chandrasekhar
Rao, Sher Singh Meena, Amit Kumar Verma, and D. L. Sastry. "XRD, EDX, FTIR and ESR
spectroscopic studies of co-precipitated Mn–substituted Zn–ferrite nanoparticles." Ceramics
International 45, no. 6 (2019): 8037-8044.https://doi.org/10.1016/j.ceramint.2019.01.029
14. Amenabar, Iban; Poly, Simon; Nuansing, Wiwat; Hubrich, Elmar H.; Govyadinov, Alexander A.;
Huth, Florian; Krutokhvostov, Roman; Zhang, Lianbing; Knez, Mato (2013-12-04). "Structural
analysis and mapping of individual protein complexes by infrared nanospectroscopy" (https://www.
ncbi.nlm.nih.gov/pmc/articles/PMC3863900). Nature Communications. 4: 2890.
Bibcode:2013NatCo...4.2890A (https://ui.adsabs.harvard.edu/abs/2013NatCo...4.2890A).
doi:10.1038/ncomms3890 (https://doi.org/10.1038%2Fncomms3890). ISSN 2041-1723 (https://w
ww.worldcat.org/issn/2041-1723). PMC 3863900 (https://www.ncbi.nlm.nih.gov/pmc/articles/PMC
3863900). PMID 24301518 (https://pubmed.ncbi.nlm.nih.gov/24301518).
15. Krauklis, A. E.; Gagani, A. I.; Echtermeyer, A. T. (2018). "Near-Infrared Spectroscopic Method for
Monitoring Water Content in Epoxy Resins and Fiber-Reinforced Composites" (https://www.ncbi.nl
m.nih.gov/pmc/articles/PMC5951470). Materials. 11 (4): 586–599. Bibcode:2018Mate...11..586. (h
ttps://ui.adsabs.harvard.edu/abs/2018Mate...11..586.). doi:10.3390/ma11040586 (https://doi.org/1
0.3390%2Fma11040586). PMC 5951470 (https://www.ncbi.nlm.nih.gov/pmc/articles/PMC595147
0). PMID 29641451 (https://pubmed.ncbi.nlm.nih.gov/29641451).
External links
Infracord spectrometer (https://www.ncbi.nlm.nih.gov/pmc/articles/PMC441765/pdf/jcinvest00449-
0191.pdf) photograph
The Grubb-Parsons-NPL cube interferometer Spectroscopy, part 2 by Dudley Williams, page 81
(https://books.google.com/books?id=XTolQEkzSR0C&pg=PA81)
infrared materials (https://web.archive.org/web/20101114040356/http://infrared.als.lbl.gov/content/
web-links/58-irwindows) Properties of many salt crystals and useful links.
University FTIR lab example (http://www.bristol.ac.uk/earthsciences/research/petrology/facilities/fti
r-lab/) from University of Bristol
Retrieved from "https://en.wikipedia.org/w/index.php?title=Fourier-transform_infrared_spectroscopy&oldid=1100392184"
This page was last edited on 25 July 2022, at 17:47 (UTC).

8/29/22, 4:15 PM Powder diffraction - Wikipedia
Powder diffraction
Powder diffraction is a scientific technique using X-
ray, neutron, or electron diffraction on powder or
microcrystalline samples for structural
characterization of materials. [2] An instrument
dedicated to performing such powder measurements is
called a powder diffractometer.
Powder diffraction stands in contrast to single crystal

diffraction techniques, which work best with a single,
well-ordered crystal.
Contents
Explanation
Uses Electron powder pattern (red) of an Al film with an
Phase identification fcc spiral overlay (green) and a line of
Crystallinity intersections (blue) that determines lattice
parameter.[1]
Lattice parameters
Expansion tensors, bulk modulus
Phase transitions
Crystal structure refinement and determination
Size and strain broadening
Comparison of X-ray and neutron scattering
Aperiodically arranged clusters
Semi-quantitative analysis
Devices
Cameras
Diffractometers
Neutron diffraction
X-ray tubes
Other sources
Advantages and disadvantages
See also
X-ray powder diffraction of Y2Cu2O5 and Rietveld refinement with
References
two phases, showing 1% of yttrium oxide impurity (red tickers).
Further reading
External links
Explanation
https://en.wikipedia.org/wiki/Powder_diffraction 1/11
A diffractometer produces electromagnetic radiation (waves) with known wavelength and frequency,
which is determined by their source. The source is often x-rays, because they are the only kind of
energy with the optimal wavelength for inter-atomic-scale diffraction. However, electrons and
neutrons are also common sources, with their frequency determined by their de Broglie wavelength.
When these waves reach the sample, the incoming beam is either reflected off the surface, or can
enter the lattice and be diffracted by the atoms present in the sample. If the atoms are arranged
symmetrically with a separation distance d, these waves will interfere constructively only where the
path-length difference 2d sin θ is equal to an integer multiple of the wavelength, producing a
diffraction maximum in accordance with Bragg's law. These waves interfere destructively at points
between the intersections where the waves are out of phase, and do not lead to bright spots in the
diffraction pattern.[3] Because the sample itself is acting as the diffraction grating, this spacing is the
[atomic spacing].
The distinction between powder and single crystal diffraction is the degree of texturing in the sample.
Single crystals have maximal texturing, and are said to be anisotropic. In contrast, in powder
diffraction, every possible crystalline orientation is represented equally in a powdered sample, the
isotropic case. Powder X-ray diffraction (PXRD) operates under the assumption that the sample is
randomly arranged. Therefore, a statistically significant number of each plane of the crystal structure
will be in the proper orientation to diffract the X-rays. Therefore, each plane will be represented in the
signal. In practice, it is sometimes necessary to rotate the sample orientation to eliminate the effects
of texturing and achieve true randomness.
Mathematically, crystals can be described by a Bravais lattice with some regularity in the spacing
between atoms. Because of this regularity, we can describe this structure in a different way using the
reciprocal lattice, which is related to the original structure by a Fourier transform. This three-
dimensional space can be described with reciprocal axes x*, y*, and z* or alternatively in spherical
coordinates q, φ*, and χ*. In powder diffraction, intensity is homogeneous over φ* and χ*, and only q
remains as an important measurable quantity. This is because orientational averaging causes the
three-dimensional reciprocal space that is studied in single crystal diffraction to be projected onto a
single dimension.
When the scattered radiation is collected on a flat plate detector,

the rotational averaging leads to smooth diffraction rings around
the beam axis, rather than the discrete Laue spots observed in
single crystal diffraction. The angle between the beam axis and the
ring is called the scattering angle and in X-ray crystallography
always denoted as 2θ (in scattering of visible light the convention
is usually to call it θ). In accordance with Bragg's law, each ring
Two-dimensional powder diffraction
corresponds to a particular reciprocal lattice vector G in the
setup with flat plate detector.[4]
sample crystal. This leads to the definition of the scattering vector
as:
In this equation, G is the reciprocal lattice vector, q is the length of the reciprocal lattice vector, k is
the momentum transfer vector, θ is half of the scattering angle, and λ is the wavelength of the source.
Powder diffraction data are usually presented as a diffractogram in which the diffracted intensity, I, is
shown as a function either of the scattering angle 2θ or as a function of the scattering vector length q.
The latter variable has the advantage that the diffractogram no longer depends on the value of the
wavelength λ. The advent of synchrotron sources has widened the choice of wavelength considerably.
To facilitate comparability of data obtained with different wavelengths the use of q is therefore
recommended and gaining acceptability.
Uses
Relative to other methods of analysis, powder diffraction allows for rapid, non-destructive analysis of
multi-component mixtures without the need for extensive sample preparation.[5] This gives
laboratories around the world the ability to quickly analyze unknown materials and perform materials
characterization in such fields as metallurgy, mineralogy, chemistry, forensic science, archeology,
condensed matter physics, and the biological and pharmaceutical sciences. Identification is
performed by comparison of the diffraction pattern to a known standard or to a database such as the
International Centre for Diffraction Data's Powder Diffraction File (PDF) or the Cambridge Structural
Database (CSD). Advances in hardware and software, particularly improved optics and fast detectors,
have dramatically improved the analytical capability of the technique, especially relative to the speed
of the analysis. The fundamental physics upon which the technique is based provides high precision
and accuracy in the measurement of interplanar spacings, sometimes to fractions of an Ångström,
resulting in authoritative identification frequently used in patents, criminal cases and other areas of
law enforcement. The ability to analyze multiphase materials also allows analysis of how materials
interact in a particular matrix such as a pharmaceutical tablet, a circuit board, a mechanical weld, a
geologic core sampling, cement and concrete, or a pigment found in an historic painting. The method
has been historically used for the identification and classification of minerals, but it can be used for
nearly any material, even amorphous ones, so long as a suitable reference pattern is known or can be
constructed.
Phase identification
The most widespread use of powder diffraction is in the identification and characterization of
crystalline solids, each of which produces a distinctive diffraction pattern. Both the positions
(corresponding to lattice spacings) and the relative intensity of the lines in a diffraction pattern are
indicative of a particular phase and material, providing a "fingerprint" for comparison. A multi-phase
mixture, e.g. a soil sample, will show more than one pattern superposed, allowing for determination
of the relative concentrations of phases in the mixture.
J.D. Hanawalt, an analytical chemist who worked for Dow Chemical in the 1930s, was the first to
realize the analytical potential of creating a database. Today it is represented by the Powder
Diffraction File (PDF) of the International Centre for Diffraction Data (formerly Joint Committee for
Powder Diffraction Studies). This has been made searchable by computer through the work of global
software developers and equipment manufacturers. There are now over 1,047,661 reference materials
in the 2021 Powder Diffraction File Databases, and these databases are interfaced to a wide variety of
diffraction analysis software and distributed globally. The Powder Diffraction File contains many
subfiles, such as minerals, metals and alloys, pharmaceuticals, forensics, excipients, superconductors,
semiconductors, etc., with large collections of organic, organometallic and inorganic reference
materials.
Crystallinity
In contrast to a crystalline pattern consisting of a series of sharp peaks, amorphous materials (liquids,
glasses etc.) produce a broad background signal. Many polymers show semicrystalline behavior, i.e.
part of the material forms an ordered crystallite by folding of the molecule. A single polymer molecule
may well be folded into two different, adjacent crystallites and thus form a tie between the two. The
tie part is prevented from crystallizing. The result is that the crystallinity will never reach 100%.
Powder XRD can be used to determine the crystallinity by comparing the integrated intensity of the
background pattern to that of the sharp peaks. Values obtained from powder XRD are typically
comparable but not quite identical to those obtained from other methods such as DSC.
Lattice parameters
The position of a diffraction peak is independent of the atomic positions within the cell and entirely
determined by the size and shape of the unit cell of the crystalline phase. Each peak represents a
certain lattice plane and can therefore be characterized by a Miller index. If the symmetry is high, e.g.:
cubic or hexagonal it is usually not too hard to identify the index of each peak, even for an unknown
phase. This is particularly important in solid-state chemistry, where one is interested in finding and
identifying new materials. Once a pattern has been indexed, this characterizes the reaction product
and identifies it as a new solid phase. Indexing programs exist to deal with the harder cases, but if the
unit cell is very large and the symmetry low (triclinic) success is not always guaranteed.
Expansion tensors, bulk modulus
Cell parameters are somewhat temperature and

pressure dependent. Powder diffraction can be
combined with in situ temperature and pressure
control. As these thermodynamic variables are
changed, the observed diffraction peaks will migrate
continuously to indicate higher or lower lattice
spacings as the unit cell distorts. This allows for
measurement of such quantities as the thermal
expansion tensor and the isothermal bulk modulus, as
well determination of the full equation of state of the Thermal expansion of a sulfur powder
material.
Phase transitions
At some critical set of conditions, for example 0 °C for water at 1 atm, a new arrangement of atoms or
molecules may become stable, leading to a phase transition. At this point new diffraction peaks will
appear or old ones disappear according to the symmetry of the new phase. If the material melts to an
isotropic liquid, all sharp lines will disappear and be replaced by a broad amorphous pattern. If the
transition produces another crystalline phase, one set of lines will suddenly be replaced by another
set. In some cases however lines will split or coalesce, e.g. if the material undergoes a continuous,
second order phase transition. In such cases the symmetry may change because the existing structure
is distorted rather than replaced by a completely different one. For example, the diffraction peaks for
the lattice planes (100) and (001) can be found at two different values of q for a tetragonal phase, but
if the symmetry becomes cubic the two peaks will come to coincide.
Crystal structure refinement and determination
Crystal structure determination from powder diffraction data is extremely challenging due to the
overlap of reflections in a powder experiment. A number of different methods exist for structural
determination, such as simulated annealing and charge flipping. The crystal structures of known
materials can be refined, i.e. as a function of temperature or pressure, using the Rietveld method. The
Rietveld method is a so-called full pattern analysis technique. A crystal structure, together with
instrumental and microstructural information, is used to generate a theoretical diffraction pattern
that can be compared to the observed data. A least squares procedure is then used to minimize the
difference between the calculated pattern and each point of the observed pattern by adjusting model
parameters. Techniques to determine unknown structures from powder data do exist, but are
somewhat specialized.[6] A number of programs that can be used in structure determination are
TOPAS, Fox, DASH, GSAS-II, EXPO2004, and a few others.
Size and strain broadening
There are many factors that determine the width B of a diffraction peak. These include:
1. instrumental factors
2. the presence of defects to the perfect lattice
3. differences in strain in different grains
4. the size of the crystallites
It is often possible to separate the effects of size and strain. When size broadening is independent of q
(K=1/d), strain broadening increases with increasing q-values. In most cases there will be both size
and strain broadening. It is possible to separate these by combining the two equations in what is
known as the Hall–Williamson method:
Thus, when we plot vs. we get a straight line with slope and intercept .
The expression is a combination of the Scherrer equation for size broadening and the Stokes and
Wilson expression for strain broadening. The value of η is the strain in the crystallites, the value of D
represents the size of the crystallites. The constant k is typically close to unity and ranges from 0.8
to 1.39.
Comparison of X-ray and neutron scattering
X-ray photons scatter by interaction with the electron cloud of the material, neutrons are scattered by
the nuclei. This means that, in the presence of heavy atoms with many electrons, it may be difficult to
detect light atoms by X-ray diffraction. In contrast, the neutron scattering lengths of most atoms are
approximately equal in magnitude. Neutron diffraction techniques may therefore be used to detect
light elements such as oxygen or hydrogen in combination with heavy atoms. The neutron diffraction
technique therefore has obvious applications to problems such as determining oxygen displacements
in materials like high temperature superconductors and ferroelectrics, or to hydrogen bonding in
biological systems.
A further complication in the case of neutron scattering from hydrogenous materials is the strong
incoherent scattering of hydrogen (80.27(6) barn). This leads to a very high background in neutron
diffraction experiments, and may make structural investigations impossible. A common solution is
deuteration, i.e., replacing the 1-H atoms in the sample with deuterium (2-H). The incoherent
scattering length of deuterium is much smaller (2.05(3) barn) making structural investigations
significantly easier. However, in some systems, replacing hydrogen with deuterium may alter the
structural and dynamic properties of interest.
As neutrons also have a magnetic moment, they are additionally scattered by any magnetic moments
in a sample. In the case of long range magnetic order, this leads to the appearance of new Bragg
reflections. In most simple cases, powder diffraction may be used to determine the size of the
moments and their spatial orientation.
Aperiodically arranged clusters
Predicting the scattered intensity in powder diffraction patterns from gases, liquids, and randomly
distributed nano-clusters in the solid state[7] is (to first order) done rather elegantly with the Debye
scattering equation:[8]
where the magnitude of the scattering vector q is in reciprocal lattice distance units, N is the number
of atoms, fi(q) is the atomic scattering factor for atom i and scattering vector q, while rij is the distance
between atom i and atom j. One can also use this to predict the effect of nano-crystallite shape on
detected diffraction peaks, even if in some directions the cluster is only one atom thick.
Semi-quantitative analysis
Semi-quantitative analysis of polycristalline mixtures can be performed by using traditional single-

peaks methods such as the Relative Intensity Ratio (RIR) or whole-pattern methods using Rietveld
Refinement or PONCKS (Partial
Or No Known Crystal Structures) method. The use of each method
depends on the knowledge on the analyzed system, given that, for instance, Rietveld refinement needs
the solved crystal structure of each component of the mixture to be performed. In the last decades,
multivariate analysis begun spreading as an alternative method for phase quantification.[9][10]
Devices
Cameras
The simplest cameras for X-ray powder diffraction consist of a small capillary and either a flat plate
detector (originally a piece of X-ray film, now more and more a flat-plate detector or a CCD-camera)
or a cylindrical one (originally a piece of film in a cookie-jar, but increasingly bent position sensitive
detectors are used). The two types of cameras are known as the Laue and the Debye–Scherrer camera.
In order to ensure complete powder averaging, the capillary is usually spun around its axis.
For neutron diffraction vanadium cylinders are used as sample holders. Vanadium has a negligible
absorption and coherent scattering cross section for neutrons and is hence nearly invisible in a
powder diffraction experiment. Vanadium does however have a considerable incoherent scattering
cross section which may cause problems for more sensitive techniques such as neutron inelastic
scattering.
A later development in X-ray cameras is the Guinier camera. It is built around a focusing bent crystal
monochromator. The sample is usually placed in the focusing beam, e.g. as a dusting on a piece of
sticky tape. A cylindrical piece of film (or electronic multichannel detector) is put on the focusing
circle, but the incident beam prevented from reaching the detector to prevent damage from its high
intensity.
Cameras based on hybrid photon counting technology, such as the PILATUS detector, are widely used
in applications where high data acquisition speeds and increased data quality are required.[11]
Diffractometers
Diffractometers can be operated both in transmission and

reflection, but reflection is more common. The powder sample is
loaded in a small disc-like container and its surface carefully
flattened. The disc is put on one axis of the diffractometer and
tilted by an angle θ while a detector (scintillation counter) rotates
around it on an arm at twice this angle. This configuration is
known under the name Bragg–Brentano θ-2θ.
Another configuration is the Bragg–Brentano θ-θ configuration in

Hemisphere of diffraction showing
which the sample is stationary while the X-ray tube and the
the incoming and diffracted beams
detector are rotated around it. The angle formed between the x-
K0 and K that are inclined by an
ray source and the detector is 2θ. This configuration is most
angle θ with respect to the sample
convenient for loose powders.
surface.[12]
Diffractometer settings for different experiments can
schematically be illustrated by a hemisphere, in which the powder
sample resides in the origin. The case of recording a pattern in the Bragg-Brentano θ-θ mode is shown
in the figure, where K0 and K stand for the wave vectors of the incoming and diffracted beam that
both make up the scattering plane. Various other settings for texture or stress/strain measurements
can also be visualized with this graphical approach.[12]
Position-sensitive detectors (PSD) and area detectors, which allow collection from multiple angles at
once, are becoming more popular on currently supplied instrumentation.
Neutron diffraction
Sources that produce a neutron beam of suitable intensity and speed for diffraction are only available
at a small number of research reactors and spallation sources in the world. Angle dispersive (fixed
wavelength) instruments typically have a battery of individual detectors arranged in a cylindrical
fashion around the sample holder, and can therefore collect scattered intensity simultaneously on a
large 2θ range. Time of flight instruments normally have a small range of banks at different scattering
angles which collect data at varying resolutions.
X-ray tubes
Laboratory X-ray diffraction equipment relies on the use of an X-ray tube, which is used to produce
the X-rays. The most commonly used laboratory X-ray tube uses a copper anode, but cobalt and
molybdenum are also popular. The wavelength in nm varies for each source. The table below shows
these wavelengths, determined by Bearden[13] and quoted in the International Tables for X-ray
Crystallography (all values in nm):
Kα
Kα2
Kα1
Kβ
Element
(weight average) (strong) (very strong) (weak)
Cr 0.229100 0.229361 0.228970 0.208487
Fe 0.193736 0.193998 0.193604 0.175661
Co 0.179026 0.179285 0.178897 0.162079
Cu 0.154184 0.154439 0.154056 0.139222
Mo 0.071073 0.071359 0.070930 0.063229
According to the last re-examination of Hölzer et al. (1997),[14] these values are respectively:
Element Kα2 Kα1 Kβ

Cr 0.2293663 0.2289760 0.2084920
Co 0.1792900 0.1789010 0.1620830
Cu 0.1544426 0.1540598 0.1392250
Mo 0.0713609 0.0709319 0.0632305
Other sources
In-house applications of X-ray diffraction has always been limited to the relatively few wavelengths
shown in the table above. The available choice was much needed because the combination of certain
wavelengths and certain elements present in a sample can lead to strong fluorescence which increases
the background in the diffraction pattern. A notorious example is the presence of iron in a sample
when using copper radiation. In general elements just below the anode element in the period system
need to be avoided.
Another limitation is that the intensity of traditional generators is relatively low, requiring lengthy
exposure times and precluding any time dependent measurement. The advent of synchrotron sources
has drastically changed this picture and caused powder diffraction methods to enter a whole new
phase of development. Not only is there a much wider choice of wavelengths available, the high
brilliance of the synchrotron radiation makes it possible to observe changes in the pattern during
chemical reactions, temperature ramps, changes in pressure and the like.
The tunability of the wavelength also makes it possible to observe anomalous scattering effects when
the wavelength is chosen close to the absorption edge of one of the elements of the sample.
Neutron diffraction has never been an in house technique because it requires the availability of an
intense neutron beam only available at a nuclear reactor or spallation source. Typically the available
neutron flux, and the weak interaction between neutrons and matter, require relative large samples.
Advantages and disadvantages

Although it is possible to solve crystal structures from powder X-ray data alone, its single crystal
analogue is a far more powerful technique for structure determination. This is directly related to the
fact that information is lost by the collapse of the 3D space onto a 1D axis. Nevertheless, powder X-ray
diffraction is a powerful and useful technique in its own right. It is mostly used to characterize and
identify phases, and to refine details of an already known structure, rather than solving unknown
structures.
Advantages of the technique are:
simplicity of sample preparation

rapidity of measurement
the ability to analyze mixed phases, e.g. soil samples
"in situ" structure determination
By contrast growth and mounting of large single crystals is notoriously difficult. In fact there are
many materials for which, despite many attempts, it has not proven possible to obtain single crystals.
Many materials are readily available with sufficient microcrystallinity for powder diffraction, or
samples may be easily ground from larger crystals. In the field of solid-state chemistry that often aims
at synthesizing new materials, single crystals thereof are typically not immediately available. Powder
diffraction is therefore one of the most powerful methods to identify and characterize new materials
in this field.
Particularly for neutron diffraction, which requires larger samples than X-ray diffraction due to a
relatively weak scattering cross section, the ability to use large samples can be critical, although newer
and more brilliant neutron sources are being built that may change this picture.
Since all possible crystal orientations are measured simultaneously, collection times can be quite
short even for small and weakly scattering samples. This is not merely convenient, but can be
essential for samples which are unstable either inherently or under X-ray or neutron bombardment,
or for time-resolved studies. For the latter it is desirable to have a strong radiation source. The advent
of synchrotron radiation and modern neutron sources has therefore done much to revitalize the
powder diffraction field because it is now possible to study temperature dependent changes, reaction
kinetics and so forth by means of time-resolved powder diffraction.
See also
Bragg diffraction Metallurgy
Condensed matter physics Neutron diffraction
Crystallographic database Pair distribution function
Crystallography Solid state chemistry
Diffractometer Texture (crystalline)
Electron crystallography Ultrafast x-ray
Electron diffraction X-ray crystallography
Materials science X-ray scattering techniques
References
1. P. Fraundorf & Shuhan Lin (2004). "Spiral powder overlays" (https://semanticscholar.org/paper/cb

13777780ee362765a91e1f029f00d7b7315229). Microscopy and Microanalysis. 10 (S02): 1356–
1357. Bibcode:2004MiMic..10S1356F (https://ui.adsabs.harvard.edu/abs/2004MiMic..10S1356F).
2. B.D. Cullity Elements of X-ray Diffraction Addison Wesley Mass. 1978 ISBN 0-201-01174-3
3. Klug, Harold; Alexander, Leroy (1954). X-ray diffraction Procedures (https://archive.org/details/xra
ydiffractionp00klug) (2nd ed.). Canada: John Wiley & Sons, Inc. p. 122 (https://archive.org/details/
xraydiffractionp00klug/page/122). ISBN 978-0-471-49369-3.
4. Liss, Klaus-Dieter; Bartels, Arno; Schreyer, Andreas; Clemens, Helmut (2003). "High-Energy X-
Rays: A tool for Advanced Bulk Investigations in Materials Science and Physics" (https://doi.org/1
0.1080%2F07303300310001634952). Textures and Microstructures. 35 (3–4): 219.
doi:10.1080/07303300310001634952 (https://doi.org/10.1080%2F07303300310001634952).
5. B.D. Cullity Elements of X-ray diffraction Addison–Wesley, 1978 ISBN 0-201-01174-3 Chapter 14
6. Structure determination form powder diffraction data IUCr Monographs on crystallography, Edt.
W.I.F. David, K. Shankland, L.B. McCusker and Ch. Baerlocher. 2002. Oxford Science
publications ISBN 0-19-850091-2
7. B. E. Warren (1969/1990) X-ray diffraction (https://books.google.com/books?id=wfLBhAbEYAsC&
printsec=frontcover) (Addison–Wesley, Reading MA/Dover, Mineola NY) ISBN 0-486-66317-5.
8. Debye, P. (1915). "Zerstreuung von Röntgenstrahlen" (https://zenodo.org/record/1447297).
Annalen der Physik. 351 (6): 809. Bibcode:1915AnP...351..809D (https://ui.adsabs.harvard.edu/ab
s/1915AnP...351..809D). doi:10.1002/andp.19153510606 (https://doi.org/10.1002%2Fandp.19153
510606).
9. Guccione, Pietro; Lopresti, Mattia; Milanesio, Marco; Caliandro, Rocco (December 2020).
"Multivariate Analysis Applications in X-ray Diffraction" (https://doi.org/10.3390%2Fcryst1101001
2). Crystals. 11 (1): 12. doi:10.3390/cryst11010012 (https://doi.org/10.3390%2Fcryst11010012).
10. Lopresti, M.; Mangolini, B.; Milanesio, M.; Caliandro, R.; Palin, L. (1 August 2022). "Multivariate
versus traditional quantitative phase analysis of X-ray powder diffraction and fluorescence data of
mixtures showing preferred orientation and microabsorption". Journal of Applied Crystallography.
55 (4). doi:10.1107/S1600576722004708 (https://doi.org/10.1107%2FS1600576722004708).
11. Šišak Jung, D; Donath, T; Magdysyuk, O; Bednarcik, J (2017). "High-energy X-ray applications:
Current status and new opportunities". Powder Diffraction, 32(S2). 32: 22–27.
12. M. Birkholz (2005). Thin Film Analysis by X-Ray Scattering (https://www.wiley.com/en-mx/Thin+Fil
m+Analysis+by+X+Ray+Scattering-p-9783527310524). Wiley-VCH. ISBN 978-3-527-31052-4.
13. Bearden, J. A. (1967). "X-Ray Wavelengths". Reviews of Modern Physics. 39 (1): 78–124.
Bibcode:1967RvMP...39...78B (https://ui.adsabs.harvard.edu/abs/1967RvMP...39...78B).
doi:10.1103/RevModPhys.39.78 (https://doi.org/10.1103%2FRevModPhys.39.78).
14. Hölzer, G.; Fritsch, M.; Deutsch, M.; Härtwig, J.; Förster, E. (1997-12-01). "Kα1,2 and Kβ1,3 x-ray
emission lines of the 3d transition metals". Physical Review A. 56 (6): 4554–4568.
doi:10.1103/PhysRevA.56.4554 (https://doi.org/10.1103%2FPhysRevA.56.4554).
Further reading
Gilmore, C.J.; Kaduk, J.A.; Schenk, H., eds. (2019). International Tables for Crystallography -
Volume H: Powder Diffraction (https://it.iucr.org/H/). Wiley. ISBN 978-1-118-41628-0.
External links
International Centre for Diffraction Data (http://www.icdd.com)

Powder Diffraction on the Web (http://pd.chem.ucl.ac.uk/pd/welcome.htm)
The Area DIffraction Machine – software to analyze powder diffraction data (https://web.archive.or
g/web/20080725022446/http://areadiffractionmachine.googlecode.com/)
Powder diffraction at ILL (http://www.ill.eu/instruments-support/instruments-groups/groups/dif/)
Retrieved from "https://en.wikipedia.org/w/index.php?title=Powder_diffraction&oldid=1103756588"
This page was last edited on 10 August 2022, at 22:48 (UTC).

8/29/22, 4:18 PM Solid Waste Volume Reduction | Encyclopedia.com
Solid Waste Volume Reduction
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Solid waste volume reduction

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used.
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Recycling diverts large volumes of materials from the waste stream to a manufacturing
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process. Glass, plastic, paper, cardboard, and other clean, source-separated materials are
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well-suited
tCB6rX4iX- for use in the manufacture of new products. As markets become more readily
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available, the volume of materials that end up in landfills will be reduced even more. Such
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troublesome wastes as tires, appliances and construction debris are targets of serious
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recycling
lQ- efforts because they are large-volume items, take up a lot of space in landfills, and
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not provide good fuel for waste-to-energy facilities in their discarded state. Once
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recyclables have been separated from the waste stream, solid waste can be further reduced
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inGet your through

volume FREE eGuide now!
several methods.
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It’s time to take a fresh look at risk
Compaction of waste materials after source separation is useful for two reasons.
management in new mobility to ensure tha…
Compaction prepares waste for efficient transport by truck, boat or rail car to landfills or other
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disposal facilities. Compacted waste takes up less space in a landfill, thereby extending
TL_CLICKTHROUGH=TRUE&REDIR=HTTP
the life of the landfill.
US- In some cases, compacted waste can be stored for later disposal. It must
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https://www.encyclopedia.com/environment/encyclopedias-almanacs-transcripts-and-maps/solid-waste-volume-reduction 1/8
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be understood that the compaction of waste should only be done after all recyclables have
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been removed since this process contaminates post-consumer materials and makes it almost
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impossible to recover them for a manufacturing process.
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Incineration has long been accepted as a waste volume reduction technique. The burning of
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solid waste can reduce the volume by 95%. In the early 1920s, incineration was used to
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reduce waste materials to what was thought of as a harmless ash. We now know that
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contaminants can become concentrated in the ash, qualifying it as a hazardous waste . It

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wasn't until the mid-1970s that waste-to-energy facilities using incineration were considered a
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TCB6RX4IX-
viable option, as a consequence of the added benefit of energy supply. Most states now
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require that the residual ash from burning municipal solid waste be landfilled in a monofill. A
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monofill is a landfill compartment that can only be used for incinerator ash.
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Composting is another volume reduction technique that can divert large volumes of waste
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material from the waste stream. Leaves, grass clippings and tree prunings can be reduced in
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NRMC0XGOMHOEMD6GRGGSJWWD8IJTP
volume through an active composting process both in the backyard and in municipal
composting yards. Individual homeowners can compost in their back yards by using simple
rounds of wire fencing placed in a shady, cool corner. The composting materials need to be
managed through the addition of moisture, temperature monitoring, and frequent turning, until
they become a rich soil for the garden. Municipal yards perform the same process on a much
larger scale and then use the resulting soil in city parks or give it back to the homeowners for
personal use. These solid waste volume reduction techniques for organics in the waste stream
are simple and low cost and can be very effective.
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Methods for encouraging solid waste volume reduction at the individual household level
consist of various incentive programs. The most common technique is a system of volume-
based user fees. With this method, homeowners are given free bags into which they can put
anything that is designated by the city as a recyclable material. Distinctly different bags are
sold at the local grocery store or city hall. These bags usually sell for somewhere between $2
and $5 a package and must be used for all materials destined for disposal. Homeowners who
want to reduce their garbage disposal costs would try to reduce the number of purchased
bags they need to use. They can do this through a concerted effort of solid waste volume
reduction. Careful decisions at the supermarket to reduce packaging and single-use items,
reuse of packaging and containers, careful source separation of recyclables, and composting
of all organically based materials can reduce the volume of solid waste considerably and
reduce the cost of garbage service. An even greater effort can be launched by dedicated
individuals by taking used clothing to consignment shops or donating it to organizations for
distribution to needy populations, taking clothes hangers back to cleaning establishments, and
requesting that junk mail no longer be sent to their households. Of course, there is also the
ongoing debate on using disposable diapers , which greatly add to the volume of the waste
stream.
Businesses that contribute to the reduction of solid waste are those that have been set up to
take back, repair, and reuse products and materials that would otherwise end up in the waste
stream. Small appliance repair shops can recondition appliances and resell them. Businesses
that repair wood pallets make a relatively new contribution to the effort to reduce the waste
volume. Tires are being chipped for fuel in waste-to-energy incinerators, and are also being
pulverized for use in soils for playing fields. All of these volume reduction techniques have a
significant effect on how we live and how we do business. The goal of solid waste volume
reduction is to view the waste stream as a resource to be "mined," leaving only those items
behind that have truly outlived their usefulness.
See also Solid waste incineration (/environment/encyclopedias-almanacs-transcripts-and-

maps/solid-waste-incineration); Yard waste (/environment/encyclopedias-almanacs-transcripts-
and-maps/yard-waste)
[Cynthia Fridgen ]
RESOURCES
BOOKS ×
Blumberg, L., and R. Gottlieb. War on Waste: Can America Win Its Battle With Garbage?
Covelo, CA: Island Press, 1989.
Kharbanda, O. P., and E. A. Stallworthy. Waste Management: Toward a Sustainable Society.

Westport, CT: Auburn House/Greenwood, 1990.
Noyes, R., ed. Pollution Prevention Technology Handbook. Park Ridge, NJ: Noyes Press,
1993.
PERIODICALS
Porter, J. W., and J. Z. Cannon. "Waste Minimization: Challenge for American Industry."
Business Horizons 35 (March-April 1992): 46–9.
Environmental Encyclopedia
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IAS Exam Latest Updates: Types of Solid Waste - Environment Notes

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8/29/22, 3:49 PM Types of Solid Waste - Environment Notes

Home > IAS Exam > News

Types of Solid Waste - Environment Notes

Neha Grover Aug 28, 2022

IAS Exam Latest Updates

The solid wastes are of three types namely: Municipal

What does Solid Waste mean?

Other Relevant Links

Municipal solid waste Hazardous waste

Hospital waste Solid Waste

E–Waste Plastic Waste

Effects of solid waste Disposal of solid waste

Treatment of solid waste Radioactive wastes

Types of Solid Waste

Composition of Household Hazardous Waste

Biomedical / Hospital Waste

Composition of Hospital Waste

Solid Waste Management

Solid Waste Management

Solid Waste Management Rules, 2016

Other Relevant Links

Environment Notes Environmental Pollution

Causes of pollution Classifications of Pollutants

Plastic Pollution Bioremediation

Radioactive Pollution Air Pollution

Noise Pollution Soil Pollution

Water Pollution Thermal Pollution

Question: What do you mean by biomedical or hospital waste? ➕

Question: What is solid waste? What are its types? ➕

Which of the statement(s) given above is/are correct?

(c) Both 1 and 2

(d) Neither 1 nor 2

Answer: (a) See the Explanation ➕

Question: Which of the following is not a type of solid waste?

(a) Municipal solid waste

(b) Industrial Solid Waste

(c) Hospital waste

(d) Hazardous Waste

Answer: (b) See the Explanation ➕

Other Relevant Links

Indian Polity Notes Indian Economy Notes

Art and Culture Notes Governance Notes

Ancient India History Notes Medieval India History Notes

Modern India History Notes Geography Notes

Science And Technology Notes Environment And Ecology Notes

Post Independence Notes Society Notes

Internal Security Notes Ethics Notes

Disaster Management Notes World History

International Relations Social Justice Notes

CSAT Notes Government Scheme Notes

Waste to Fertilizer in 1 Day Open

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