Article citation info:

FABER, J., BRODZIK, K., NYCZ, M. Understanding technical cleanliness: importance, assessment, maintenance. Combustion Engines.
2021, 186(3), 41-50. https://doi.org/10.19206/CE-140531

Joanna FABER
Krzysztof BRODZIK
Marta NYCZ
Polish Scientific Society of Combustion Engines

Understanding technical cleanliness: importance, assessment, maintenance

ARTICLE INFO Development of the automotive industry, including so-called dowsizing and rightsizing, entails the need to
ensure, and hence to verify, the stringent cleanliness levels of an increasing number of car components. The
assurance of proper cleanliness level requires knowledge of the entire production process and precise
information on the contaminants that will allow to identify their sources. Obtaining reliable cleanliness
information requires establishing of many different factors, i. a. selection of proper contamination extraction
and collection technique, proper parameters of extraction, validation of extraction procedure, methods of
Received: 15 July 2021 particles analysis. Analytical techniques which are implemented include gravimetric, optical microscopy and
Revised: 26 July 2021 advanced techniques like scanning electron microscopy. This work present’s actual state of knowledge
Accepted: 26 July 2021 regarding technical cleanliness analysis of components. Important aspects of QA&QC in technical cleanliness
Available online: 27 July 2021 assessment are also discussed.

Key words: technical cleanliness, component cleanliness code, contaminations, particles, optical microscopy, SEM

This is an open access article under the CC BY license (http://creativecommons.org/licenses/BY/4.0/)

1. Introduction to technical cleanliness According to [3], modern automotive components and

The automotive industry, one of the biggest industries in systems are sensitive to presence of single or a few critical-
the world, is still developing, which is rather a need than ly sized particles. The presence of foreign particles is espe-
a wish. This development includes works not only on com- cially crucial in case of any flow system in vehicle, pressur-
pact engines and gearboxes without decreasing their power ized or not, and with extreme importance in all injections
(so-called downsizing), but also on new light materials, i.e. systems. Particles such as sand, metals, machining chips or
lightweight metals, what entails necessity of using different abrasive residues may have negative impact on proper
materials processing [1]. Global trends in environmental component or assembly functioning, i.e. by its damaging
protections, which result in introducing restrictive regula- effect, increased wear or rapid corrosion occurrence [5, 6].
tions, also force the need of improvement and development. As a standard, particles ranged from 15 µm to 1000 µm are
Therefore, when talking about downsizing, the need of under control [2], but, in some cases, the presence of parti-
ensuring and verifying the stringent cleanliness levels of an cles as small as 5 µm may result in components damage [7].
increasing number of car components is necessary. In fact, the function of the component in vehicle deter-
Technical cleanliness can be defined as: mines the level of permissible particle types and sizes.
– a present state of components cleanliness, that means However, as the internal cleanliness of the components has
the presence of different contaminations on internal or huge effect on whole car performance, operation and safety
external area, or on both areas, of the driver and passengers, its importance declines fast
– a process of ensuring cleanliness of components from after the vehicle is put to the service. After successful start
their manufacturing, storage, packing to transportation of operation, the importance of cleanliness is reoriented to
to end user [2], external sources such as fuels and oils [8–10]. The level of
– a process of components cleaning in order to check their contaminations in these fluids, as the most frequently re-
cleanliness level. filled or exchanged in the vehicle, is well established, de-
Confirmation of the importance of technical cleanliness scribed and understood, as it needs to fulfill and excel all
topic is the fact, that international standard ISO 16232, cars technical limitations. The importance of these fluids’
dedicated to automotive industry, was developed [3] which cleanliness is of great interest, and remains an attractive
is very similar to VDA 19.1 standard [4] developed by research topic [11–13]
German Association of the Automotive Industry. The aim The assurance of proper cleanliness level of any product
of both standards is to establish comparative methods for requires knowledge of the entire production process and
cleanliness assessment, including extraction procedure, test precise information on the contaminants, that will allow to
fluid, cleaning parameters settings, and analytical instru- identify their sources. Avoiding product contamination
ments, and to establish universal Component Cleanliness requires awareness of all operations in process that influ-
Code (CCC) [3, 4]. Moreover, car producers and compo- ence the product’s cleanliness level. This leads to stringent
nent producers, also have their own, internal standards or productions regimes, including assembly operations to be
technical specifications, which precise and expand cleaning performed in clean areas, separated from production lines,
processes, but first of all, which define cleanliness level or even in cleanrooms. However, the requirements are
requirements. ISO standard is more worldwide used, for based on engineering needs and technical premises, the
that reason this standard will be cited in present work as the product should be as good (in this case – clean) as required,
basis.

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Understanding technical cleanliness: importance, assessment, maintenance

and not necessarily better because every change and every fications definitions of particles are different. Moreover,
new operation carries additional costs. also division of particles and requirements regarding their
In order to get knowledge about cleanliness level of allowable sizes are different. For that reason, for technical
component, laboratory tests in special cleanrooms are re- cleanliness assurance and assessment all parameters, that
quired. Obtaining reliable information requires establishing mean target values, are needed:
of many different factors, i.a.:  type of particles: metallic, non-metallic, fibers, hard
 selection of proper contamination extraction and collec- particles, soft particles,
tion technique (i.e. pressure rinsing, ultrasound-assisted  allowable sizes (minimum size of particle),
extraction, flushing, shaking, and others),  allowable number of particles,
 proper parameters of extraction,  additional requirements for particles (chemical compo-
 validation of extraction procedure (declining perfor- sition, hardness, height, area etc.).
mance), Examples of different definitions of particle (contami-
 methods of particles analysis. nant) are presented in Table 1 with some photographic
Analytical techniques which are implemented include [14]: documentation, from optical microscope, of different parti-
 gravimetric analysis (total amount of all particles col- cles with division into hard and soft, found during BOS-
lected from component, expressed in mg/component, MAL laboratory practice is presented in Figs 2–4. As can
mg/cm2 or mg/cm3), be seen, it is possible to differentiate particles on the basis
 optical microscopy (granulometry, that means determi- of their microscopic appearance.
nation of number, sizes and types of particles, including
division into metallic, non-metallic and fibrous parti-
cles),
 advanced techniques, like scanning electron microscopy
(SEM, allowing for determination of elemental compo-
sition and hardness of particles).
The aim of present work is to present actual state of
knowledge regarding technical cleanliness of components,
required analytical techniques to perform cleanliness test in
laboratory in order to check the compliance with specific
customer’s requirements. Important aspects of QC&QA in
technical cleanliness assessment will also be discussed.
2. Technical cleanliness inspection
Cleanliness inspection starts as soon as component
leave production line, but proper cleanliness level should be
ensured just during production process. Each next step in
component life has to be taken into account in order to Fig. 1. BOSMAL’s ISO 6 class cleanroom equipped with pressure rinsing
obtain reliable results. In the end it will help to verify the equipment, ultrasonic bath, analytical balance, temperature chamber and
effectiveness of actions taken for assuring the required filtration equipment
cleanliness level.
Before transfer of component to laboratory, it has to be Despite multiplicity of extraction methods, types and
properly protected and packed. It is especially important step, meshes of filters used for particles collection, and then
because it should be ensured that none of the particle may be analytical methods involved, laboratory cleaning procedure
lost and in reverse: no foreign particles can contaminate the may be described in few general steps (Fig. 5). The main
component. Awareness of the matter and sources of potential steps are: equipment and filters preparation, blank value
foreign contaminations is required to conclude about whole check, cleaning procedure, gravimetric analysis, microscop-
process state and improvement. Therefore, also laboratory ic analysis, test report preparation.
room in which inspection will be carried out need to assure Technical cleanliness inspection is a kind of indirect test
proper cleanliness level in order to avoid cross-contamination as it requires transport of particles from analyzed surface
of tested object and filters with foreign particles. Such la- onto the filter on which detailed analysis is performed. This
boratories are called cleanrooms and may be also used on transport is necessary as the visual inspection of the com-
production lines if very strict requirements regarding the ponent inner surface is usually difficult due to object’s
cleanliness level of produced part apply. These areas are geometry, base material, visual similarities component with
governed by the need of avoiding foreign contaminations contaminations, surface roughness etc. [3]. Choosing proper
presence and according to ISO 14644-1 [15] are coded from extraction method is crucial in order to get reliable infor-
ISO 1 class (the most stringent requirements) to ISO 9 class mation regarding the cleanliness level. Extraction method
(the least stringent) cleanroom. Example of BOSMAL’s ISO should ensure transport of all particles from the tested sur-
6 class cleanroom is presented in Fig. 1. face to the filter. Even though that in real life not all parti-
First of all, even during project of component and pro- cles will be deposited on filter, and some of them may re-
duction line, cleanliness requirements need to be known. main on tested object, in extraction equipment or will be
Both in ISO/VDA standards, and in different OEMs speci- too small to be stopped by the filter mesh, extraction is

42 COMBUSTION ENGINES, 2021, 186(3)

 Understanding technical cleanliness: importance, assessment, maintenance

Table 1. Different definitions of contaminants

Standard/
Particles Fibers Ref.
OEM
ISO 16232/ tiny structure made from solid organic or inorganic matter long, thin structure, stretched
VDA 19.1 length to maximum inner circle
[3, 4]
diameter ratio is ≥ 20; the width
≤ 50 µm
VW Hard particles: metallic particles (incl. shiny Soft particles: non-metallic, Fibers: cotton fibers, metallic
and non-shiny: corroded, oxidized); non-metallic non-abrasive fibers, glass fibers
[16]
abrasive (sand, blasting and grinding particles,
other abrasive particles)
BMW Hard particles – mineral (H1): of mineral, ceramic nature (corundum Al2O3, silicon
carbide SiC, boron nitride BN, Diamond C, sand SiO2, further nitrides, oxides,
carbides, further minerals and ceramics, glass, glass fibers, mineral fibers [17]
Hard particles – metallic (H2): steel, hard coating materials (wear resistance coat-
ings)
Mercedes- Residual dirt: machining chips, sand, blasting shot residues, metals, abrasive resi-
[18]
Daimler dues, lint, paint, plastic particles
GM Burrs and loose chips resulting from machining operations, casting processes etc. [19]
Volvo Solid matter Soft particles: i.e. textile, lint, Particle with length/diameter
Hard particles: harder than soft particles paper, plastics, foil, hair ratio: ≥ 20:1, minimum length: [20]
500 µm
Scania Hard particles: machining chips, general metallic Soft particles: coating/paint Single elongated, soft particles,
particles, blasting shot media, foundry residue, particles, oxide flakes, plastics, with the Feret max:Feret min
sand, ceramics, hard oxides, abrasive residues, wood particles, agglomerated ratio of ≥ 20:1 [21]
hard coating materials, amorphous glass particles fibers, chemical residues

Type Exemplary pictures

Machining chips

General
Particle with metallic appearance

metallic particles

Blasting shot media

Foundry residua/sand
(silicates)

Fig. 2. Examples of hard (H) particles

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Understanding technical cleanliness: importance, assessment, maintenance

Type Exemplary pictures

Coating/paint particles

Oxides flakes
(thin & brittle)
Particle with non-metallic appearance

Plastic particles

Wood particles

Agglomerated fibers
(lint/fluff)

Chemical residues

Fig. 3. Examples of soft (S) particles

Type Exemplary pictures

Fibers

Fig. 4. Examples of fibers

44 COMBUSTION ENGINES, 2021, 186(3)

 Understanding technical cleanliness: importance, assessment, maintenance

surface. In the same time the solvent should be pure and

volatile enough to allow its fast evaporation without any
residues remaining which could influence the results. Typi-
cal analytical methods which could follow liquid extraction
of such contamination is infrared spectroscopy (IR) or
chromatographic techniques like gas chromatography (GC),
high performance liquid chromatography (HPLC) or ionic
chromatography (IC).
2.1. Extraction methods
Pressure rinsing seems to be the most common extrac-
tion method as it can be easily applied for both external and
internal surface cleaning as long as surfaces are easily ac-
cessible. It can be also applied for multiple small compo-
nents testing in bulk as long as they are characterized by
simple geometries. Important factors influencing this meth-
od efficacy are:
 shape of pressure rinsing pistol nozzle (use of different
shapes may be useful for large/small areas components
or various geometries),
 test liquid characteristic (proper viscosity allowing fast
drainage and proper wetting of the surface) and flow
Fig. 5. Cleanliness inspection procedure
rate,
presumed sufficient while allows for removing of at least  angle and distance between nozzle and object surface,
90 percent of contaminations (see. p. 3).  time of extraction and number of repetitions per surface.
The factors need to be taken into account when choos- In case of pressure rinsing the detachment of particu-
ing the extraction method are, inter alia: lates is an effect of momentum transferred from the jet
 surface to be tested: external, internal or total, stream to particles. This technique is very flexible and al-
lows to extract the contaminations even from small cavities
 tested object’s size and geometry,
if other surfaces are properly secured. Moreover, it is very
 material and particles adhesion.
effective for cleaning of objects with multiple areas to be
Based on tested object characteristics (size, geometry)
evaluated separately from the same object.
basic extraction methods can be applied:
In case of ultrasonic technique particles are detaching
 liquid extraction methods: agitation, ultrasonics, pres- form the surface due to the high pressure peaks forming
sure rinsing, internal rinsing, when cavitation bubbles implode. This method seems to be
 air extraction methods: air jet, throughflow. dedicated to simple geometries, and is ideal when total area
Depending on the required cleanliness level removed of component need to be tested. However, more complicat-
particles can be analyzed by: ed objects with cavities could be subjected to this type of
 shortened analysis, with the use of liquid particle coun- cleaning when openings diameters and cavities volume are
ters or camera (seldom applied in laboratory), taken into account while selecting the extraction parame-
 standard analysis: gravimetry and light optical micro- ters. In general, it is advisable that tested object has clear-
scopic analysis, ances large enough to guarantee that detached particulates
 extended analysis, which can include such advanced will not remain on its surface due to any spherical barriers.
techniques as light scanning electron microscopy with This method could have unwanted effect on the surface of
energy-dispersive X-ray spectroscopy (SEM-EDX), la- object as improper parameters could lead to surface or ma-
ser induced breakdown spectroscopy (LIBS), Raman terial damage, especially in case of coated surfaces and
spectroscopy, infrared spectroscopy (IR) or X-ray to- sintered materials. The lower ultrasonic frequency the
mography. stronger forces affects the particles and the more efficient
Additional care needs to be taken when cleanliness cleaning become. That is why the most important factors
analysis is focused also on liquid or greasy contaminations for establishing efficient ultrasonic cleaning procedure are:
on the tested surface. Such cases are typical in many case  ultrasonic frequency and density,
studies which concentrate on indicating the failure causes  locations of ultrasonic oscillators in bath,
of various objects. In some cases presence of foreign liquid  orientation of tested object versus ultrasonic source,
is more dangerous for the component than foreign particu-  type and temperature of test liquid,
lates as it may lead for example to lowering the friction of
 extraction time.
mated parts or malfunction of electronic devices. The later
Internal rinsing is almost perfect choice for any auto-
is especially important while the latest technological devel-
motive component which is designed for conducting flow.
opments, including the increasing electrification of the
In this method component is filled with liquid at turbulent
powertrain is taken into account [1]. In this case the most
flow which allows proper particulates extraction. Relatively
important step is choosing the extraction liquid which
simple systems can be built in order to check cleanliness of
should be able to dissolve/remove the substance from the

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Understanding technical cleanliness: importance, assessment, maintenance

tubing, lines, filters or even heat exchangers. However, in are then immobilized on large surface membranes which
case of active components such as valves, injectors or can withstand high air flow rates. In order to be able to
pumps additional actions and functionalities may be re- perform analysis of contaminations, collected particulates
quired to perform the extraction from whole surface, which are transferred to final filter by means of pressure rinsing.
changes depending on the tested object status. In such case In both cases it is crucial to use clean, oil-free compressed
the extraction systems may be complicated and therefore air.
costly and usually are designed on purpose of selected
2.2. Filtration
object testing. As requirement for turbulent flow always
In order to perform analytical verification of particu-
need to be taken into account complex benches may suffer
lates, the particles need to be separated from the test liquid
from object geometry, large volumes and/or large diameters
in which they are suspended. This operation is based on
that may require large volumes of testing liquid as well as
vacuum filtration on various types of filters and their mesh-
additional equipment allowing to reach the required liquid
es. Its selection is depending on the required cleanliness
flow.
level – the ability to retain particles of interest, type of test
In case of this method care should be taken in selecting:
liquid used – chemical resistance and also optical characte-
 test liquid,
ristics.
 flow rate, Despite the chemical resistance to the extraction liquid,
 extraction time, the most important action is proper selection of the filter
 geometry of the component, porosity. The filter used should allow retaining the smallest
 connections used, particles which are in the area of interest. It needs to be
 pulsation frequency, taken into account that particles usually have irregular
 type and characteristics of the movement in case of shapes and their differentiation is based on the largest di-
active components. ameter. For that reason the actual filter porosity should be
It is worth to notice that in the case of internal rinsing significantly lower than diameter of the smallest particle of
procedure risk of falsifying the results with contaminations interest. For standard gravimetric and microscopic analysis,
from external surface is minimal. where contaminants greater than 50 µm are analyzed, the
In case of internal surface check of components with use of polyester (i.e. polyethylene terephthalate, PET) fil-
complex geometries and cavities, which are hard to reach ters with a porosity of 5 µm is recommended.
by pressure rinsing, ultrasonic or internal rinsing, simple In general, foamed membrane or mesh filters can be
yet effective method of agitation can be used. Agitation of used, both having its advantages and disadvantages. In case
partially filled with testing liquid and completely sealed of foamed membrane which, due to its smooth surface,
component allows the liquid to reach hard-to-reach zones significantly eases microscopic analysis these cons are:
and provide possibility of detaching contaminations’ parti-  good potential for absorbing pigment particles,
cles due to force acting from different directions and an-  lowering the contrast between its surface and particles,
gles. Detached particles are then suspended in test liquid  tendency for water absorption, what can influence grav-
until removed and filtered. Depending on the weight and imetric analysis.
volume of the object manual or automated agitation may be On the other hand, mesh filters do not suffer from these
used. This relatively simple method’s efficiency is related problems as they absorb much less water and have defined
to: test liquid used and its volume, time, duration, ampli- pore size. These allows avoiding of small pigment particles
tude and frequency of agitation and number of object fill- retaining, but, with high magnification, their structure may
ings with test liquid. It should be taken into account that cause reflections and artifacts. Moreover, some very thin
this method is not preferred in case of small diameter tubes particles may not be retained during filtration.
or narrow inner geometries. Basic types of filter materials with its chemical re-
In some types of components that are not intended for sistance are presented in Table 2, while exemplary view of
contact with liquids or may be damaged by such contact, air mesh membrane filter is in Fig. 6.
extraction should be applied. Two methods, similar to de-
scribed above internal rinsing and pressure rinsing, can be Table 2. Filters types and their compatibility with test liquids [3]
used. First one is called air jet extraction and may be ef- Test liquid
fectively used for cleaning electronic components or engine Filter material
Aq. Isopr. Eth. Aliph. Ket.
air intake tracts, from which particulates cannot be extract- Cellulose + – – – –
ed with liquid flow through method. The basics of this nitrate
method as well as factors influencing its efficiency are the Foamed
Cellulose + + – + –
membrane
same as in liquid pressure rinsing. The only change is in acetate
type of fluid which changed from liquid to air. This extrac- Polyamide + + + + +
tion procedure should be performed in hermetically closed Mesh
Polyester + + + + +
cabinet like glove-box. Contaminations detached from Polyamide + + + + +
tested surface are sticking to the wetted cabin’s walls and in + compatible , – incompatible
next step are rinsed and filtered with the test liquid. Second Aq. – aqueous neutral cleaner, Isopr. – isopropanol, Eth. – ethanol,
method of air extraction – air through-flow extraction is Aliph. – aliphatic hydrocarbons, Ket. – ketones (e.g. acetone)
similar to internal rinsing with liquid. Air flow is detaching
particulates from internal surface of the tested object which

46 COMBUSTION ENGINES, 2021, 186(3)

 Understanding technical cleanliness: importance, assessment, maintenance

as well as their overlapping do not allow obtaining reliable

results.
In case of light microscopic analysis simple differentia-
tion between solid metallic (shiny), non-metallic (non-
shiny) and fibrous particles is based only on microscopic
image and on pixels forming particle image. Metallic and
non-metallic particles are usually distinguished with the use
of two distinct images, e.g. polarized versus non-polarized,
of the same particle. This analytical method as the most
common has their disadvantages. Besides the ones de-
scribed above, these are: the need of use of automated mi-
croscopic systems with motorized stages, homogenous and
stable in time illumination of the whole filter surface during
the whole analysis. This method will also suffer from parti-
cles presence which color is similar to the filter material,
usually white. Some effort was made to overcome this issue
and yellow mesh filters were introduced making the analy-
sis of white contaminations much easier.
Even though automatic microscopic systems are re-
quired for image analysis and processing of results, well
Fig. 6. Mesh membrane filter (overall view, upper left) with metallic trained personnel is required as well. They role is very
(lower left), non-metallic (upper right) and fibrous (lower right) particles
important and includes set up proper analytical parameters,
2.3. Analytical methods like selecting the threshold, manual correction of some
Gravimetric analysis is the simplest approach in stand- common mistakes like dividing mat and shining particle
ard analysis to cleanliness inspection and can include both into two or more separate ones, or opposite – counting
particles and soluble contaminations assessment. The de- overlapped particles as one.
termination of total solid contaminations involves filtering Extended analysis of particulates may be performed
the extraction fluid through a filter and calculating their with light microscopic method in case of some additional
weight by the difference in filter mass before and after the requirements. For example, if particles height analysis is
filtration process. An analytical balance with a minimum needed differences between the focus position of the filter
precision of 0.1 mg is needed for accurate determination the and highest point of the particle are used. In some cases, for
differences in filter mass. What is very important, filters certain types of particles of interest additional measure-
must be properly prepared for the test: first dried in an oven ments need to be taken with the use of various illumination
at specified temperature, then cooled down to the room modes or double check in order to obtain requested infor-
temperature in desiccator. It is therefore important that mation.
temperature and humidity in the weighing room are both Another measurement technique is scanning electron
regulated and controlled. The filter drying temperature and microscopy (SEM) analysis, which allows particles’ count-
time should be determined by a pre-selected procedure, ing, and measuring conjugated with X-ray spectroscopy
taking into account the filter material and the type of ex- (EDX), which provides information about contaminations’
traction fluid used. Despite it’s simplicity, gravimetric elemental composition, and therefore its hardness. This
analysis gives information about overall component con- advanced method is advised when additional information
tamination. on particles composition is required in order to indicate
Determination of soluble contaminants, such as grease, more precisely their sources or to avoid presence of hard
oil or degreasing residue, consists of collecting the pre- particles which may lead to component malfunction. Appli-
filtered extraction fluid in appropriately dried and weighed cation of this technique allows verifying the presence of
beakers and calculating the difference in their mass as de- conductive particles which may interfere with electronic
scribed above. Similarly, as in case of filters care must be devices. As the SEM-EDX method counts particles on
taken in the preparation, drying and weighing of the beak- different contrast basis (material contrast) than light mi-
ers. Moreover, the inspection fluid has to be easily evapo- croscopy, results obtained by these two methods should not
rated and chemically clean to avoid cross-contamination be compared. However, it is possible to verify elemental
and interference with the results. composition of selected particles measured by means of
Light microscopic method is the basis of standard light microscopy if coordinates of these particles on the
cleanliness inspection. Its application allows obtaining filter can be transferred to SEM-EDX equipment. As this
information regarding the number, sizes/size ranges and method is more time consuming than light microscopy,
type of particles. All of this information is based on micro- additionally in case of high particle counts, only part of the
scopic image analysis which, in order to be reliable, should filter needs to be analyzed. If the filter occupancy is homo-
be taken with proper contrast – differentiation of particles geneous the corresponding results could be then extrapolat-
versus filter surface is based on grey scale. Filter for optical ed to the total filter area. Compromise between elemental
analysis should be properly prepared, and analyzed contam- composition results quality, the more X-ray impulses for
inations should be evenly distributed. Overload of particles

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Understanding technical cleanliness: importance, assessment, maintenance

each particle are counted the more reliable the results are, the filter in order to provide reliable results and is well
and total analysis time is needed. suited for analysis of particles not smaller than 15 μm.
It should be taken into consideration that classification In opposition to LIBS, which is sensitive for elemental
of particles to different materials groups are based only on composition, especially of pure metals and inorganic mate-
analyzed elemental composition which strongly depends on rials, Raman spectroscopy also based on laser excitation
EDX detector resolution. Moreover, SEM-EDX have their allows determination of organic and inorganic molecules
own limitations in case of organic/plastic particles analysis. but in this case pure metals do not generate signal. Identifi-
As the filters introduce the background containing a lot of cation of particles material is based on comparison of ob-
carbon, and X-ray spectroscopy in general is less sensitive tained spectra with database. Raman spectroscopy is well
for lighter elements like oxygen, carbon and nitrogen, only fitted for analysis of particles even as small as 0.5 µm but
specific plastic materials could be distinguished. Among the typical time for single contamination analysis ranges
them are those containing some other elements, like chlo- from 30 to 60 seconds. This means that cleanliness inspec-
rine (i.e. PVC), or fluorine (i.e. PTFE). The comparison of tion based on Raman spectroscopy will take similar time as
light microscopy and SEM-EDX analysis of the same parti- typical SEM-EDX analysis. However, this is the first meth-
cle is presented in Fig. 7. od from described above which allows identification plastic
materials, what could be necessary in some processes to
find source of component contamination.
Another method also using measurement of molecular
vibrations to identify the compounds is Fourier trans-
form infrared spectroscopy (FTIR). The disadvantage
of this method is that it does not allow analysis of such
small particles as Raman spectroscopy but is much more
common and relatively cheaper. FTIR is sensitive for
organic groups presence in tested molecules and particles,
allowing identification not only plastic particles material
but also solvents, greases, oils or even contaminated parti-
cles. This method is not well suited for analysis of inor-
ganic materials. In general two infrared techniques may be
used: transmission or attenuated total reflectance (ATR).
Both may be applied in IR microscopes and IR spectrome-
ters. In general, the use of IR spectrometer is limited to
particles than can be removed from the filter (for example
Fig. 7. Comparison of particle view from light microscopy (upper left) and
with tweezers) and transferred to IR spectrometer. In case
SEM-EDX (upper right and bottom) of ATR technique, the particle is then pressed against the
crystal (diamond crystal is common example) allowing
Other method allowing to obtain information about par- transfer of IR irradiation to the analyzed sample and back
ticle elemental composition, and hence it’s physical charac- to the detector. In case of transmission technique, which is
teristic, is laser induced breakdown spectroscopy usually more sensitive and provides better quality spectra,
(LIBS). In this case high energetic laser pulse vaporizes IR radiation is passing through the particle pressed by two
particle and generates plasma, which spectrum is analyzed. crystals.
This method allows much faster (less than second) ele-
3. Quality control and quality assurance
mental composition analysis than SEM-EDX which meas-
In order to confirm correctness of cleanliness test per-
urement quality is dependent on time. Moreover, SEM-
formance, quality control and assurance (QC&QA) need to
EDX requires multiple-point analysis on particles to gather
be implemented. It is not easy aspect because although
quality results what takes from one to few seconds per
component cleaning procedure is not destructive activity, it
particle. LIBS is generally nearly non-destructive method
cannot be repeated for the same test component, because
as only small portion of material is ablated from the ana-
particles are removed from the component and the present
lyzed surface [22]. However, with high energies and very
state of component cleanliness has been changed [3]. So, in
small particles, some of them may be destroyed during
fact, other elements of QC&QA need to be performed.
analysis and this do not allow repeated analysis or any
Some of them are described in ISO 16232 [3], and the oth-
additional measurement as impact craters with diameter of
ers result from good laboratory practice.
20 µm and depth of 10 µm are analyzed for each particle
Elements of QC&QA include, but are not limited to:
[3]. Therefore, this method allows gathering precise results
– blank value control,
very fast, what is important in many areas when decision
– validation of cleaning procedure (declining curve),
needs to be taken as fast as possible. However, in case of
– cleaning procedure control (double inspection),
disputes possibility of losing some evidence collected dur-
– balance control,
ing cleanliness inspection may be risk that is not acceptable
– microscope control and calibration,
by the independent laboratory. LIBS, as the previously
– check of length standard,
described methods, requires proper particles separation on
– analysis of particles standard,

48 COMBUSTION ENGINES, 2021, 186(3)

 Understanding technical cleanliness: importance, assessment, maintenance

– microscopic analysis of repeated sample (reproducibi- ed contaminants is less than 10% of the total amount of
lity test), contaminants extracted in all previous extraction steps,
– personnel training. including the current step, according to Equation 1 [3]:
One of the most important things in cleanliness inspec-
Cn ≤ 0.10 ∑ni=1 Ci n ≤ 6 (1)
tion is blank value control. This parameter check is re-
quired by all standards and specifications in cleanliness The validation procedure together with blank value
field, and is defined as a maximum value that may not be check is carried out at least once for each component or
exceeded (usually maximum 10% of measured or expected family of components. However, it should be noticed that if
value of total particle mass and number for component any design change or change in the manufacturing process
tested). It is not required before each routine test, but is introduced, the qualification test should be repeated.
should be checked regularly, especially in case of high Double inspection is another procedure for cleaning
CCC requirements or when equipment was not used for performance check, and is performed for routine check of
some time. selected parameters. In this test one component is cleaned
Blank value check is proof for: twice, and after second cleaning total amount of particles
– high purity of external environment in cleanroom, extracted should not be higher than 30% of the sum of
– purity of extraction liquid, particles from first and second cleaning, according to Equa-
– purity of equipment used, tion 2 [3]:
– proper control of cleaning procedure.
It is worth to mention, that the cleanliness test does not C2 ≤ 0.30 (C1 + C2 ) (2)
always have to be performed in cleanrooms, with defined Example of double inspection results are presented in
cleanliness class according to ISO 14644-1 [15]. It may Fig. 9.
also be carried out in separated areas. For that reason the
blank value check is very important as this will reflect pos-
sible environmental effects, that means if external contami-
nants are not introduced into the component under test.
Another required by the standard activity is validation
of cleaning procedure (qualification test). The aim of this
procedure is to select:
– proper extraction liquid quantity,
– proper extraction time,
– proper extraction procedure,
– proper extraction parameters.
The aim of validation procedure is also to check if maxi-
mum amount of particles was extracted from component,
which means that effectiveness of particle extraction is eval-
uated. As a result, extraction (declining or decay) curve is Fig. 9. Example of double inspection results
determined (example of such curve is presented in Fig. 8).
One of the most important things in technical cleanli-
ness inspection, especially emphasized in ISO standard, is
staff skills and training. The procedure of staff training
includes many aspects, from understanding the importance
of technical cleanliness and requirements, having
knowledge of procedures and standards, being aware of all
steps in cleanliness inspection, to choosing the test liquid
and extraction parameters and interpretation of results ob-
tained and so on. Because technical cleanliness is a com-
plex and complicated topic, well-educated and motivated
staff is crucial.
4. Conclusions
The development of the automotive industry entails in-
creasing demands in scope of technical cleanliness of vari-
Fig. 8. Example of declining curve ous components. In-depth analysis of contaminations is
required more and more frequently, with simple gravimetric
Validation procedure is usually performed on one com- analysis being too scarce.
ponent, sometimes on i.e. 5 different components. During Reduction of particulates presence on components’ sur-
this procedure, component is cleaned minimum 3 times, but faces is costly and only understanding of their sources,
usually 6 times, and particles extracted are collected on 6 processes required for their removal and cleanliness testing
different filters. If extraction procedure is performed cor- methodology can lead to cost minimization. Even though
rectly, total amount of particles extracted should decrease the pursuit for the best cleanliness is not wrong, it should be
successively, reaching a point where the amount of extract- always taken into account that the components should be as

COMBUSTION ENGINES, 2021, 186(3) 49

Understanding technical cleanliness: importance, assessment, maintenance

clean as required and not necessarily as clean as possible. In inspection are always required to serve as the best source of
each case the independent and reliable results of cleanliness information regarding the surface preparation.

Nomenclature
CCC component cleanliness code HPLC high performance liquid chromatography
SEM scanning electron microscope GC gas chromatography
EDX energy dispersive spectroscopy IC ionic chromatography
FTIR Fourier transform infrared spectroscopy QC quality control
LIBS laser induced breakdown spectroscopy QA quality assurance
IR infrared spectroscopy

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Joanna Faber, DEng. – Materials Testing Depart- Marta Nycz, MEng. – Materials Testing Department,
ment, BOSMAL Automotive Research and Devel- BOSMAL Automotive Research and Development
opment Institute Ltd, Bielsko-Biała, Poland. Institute Ltd, Bielsko-Biała, Poland.
e-mail: joanna.faber@bosmal.com.pl e-mail: marta.nycz@bosmal.com.pl

Krzysztof Brodzik, DEng. – Materials Testing

Department, BOSMAL Automotive Research and
Development Institute Ltd, Bielsko-Biała, Poland.
e-mail: krzysztof.brodzik@bosmal.com.pl

50 COMBUSTION ENGINES, 2021, 186(3)