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Critical Cleaning ExpertsSM

AQUEOUS CRITICAL CLEANING: A WHITE PAPER

Cleaning and Monitoring Procedures

Optimizing Your Critical Cleaning Processes Begins With Using the
Right Procedures — Then Monitoring Performance to Ensure Results
Getting the best results from any cleaner requires proper mixing and cleaning
procedures. This whitepaper includes mixing directions for each type of
Alconox, Inc. aqueous cleaning detergent. It also describes methods for
monitoring cleaner performance.

Mixing Directions 1 In any industrial cleaning application, “clean” especially for presoak. For diffi cult soils, use very
Soaking means clean enough to avoid later problems. The key hot water (above 150ºF or 65ºC) and double the
Manual Cleaning 2 questions are: recommended amount of detergent. When cleaning
Ultrasonic Cleaning • What will happen if the surface isn’t clean? solution may be reused, make up fresh solutions
Clean-In-Place 3 frequently, as needed.
• How can you ensure that cleaning standards
Machine Washers
are maintained?
Automatic Syphon 2. Soaking
Pipette Washing Whether or not cleaning validation is mandated in
your operation, it is useful to understand the testing Recommended Products: ALCONOX,
Rinsing
methods commonly used for determining cleanliness TERGAZYME, LIQUINOX, CITRANOX, DETERGENT 8,
Drying 4
of industrial, medical, pharmaceutical, food and other LUMINOX, ALCOJET, DETOJET, CITRAJET, TERGAJET,
Bath Life Monitoring,
Extension and types of processing equipment. SOLUJET, DETONOX, KEYLAJET
Control Typical Uses:
Corrosion Inhibition
1. Mixing Directions for Alconox, Inc. • Cleaning small items (e.g., hospital catheters
Cleaning Detergents
Measurement and tubes, small metal parts) and large tank
Procedures 5 Dilute detergent using warm (about 120ºF or 50ºC) interiors, including pharmaceutical and other
Get Validation or hot (about 140ºF or 60ºC) water per Table 1. blending tanks
Support 8 Ambient temperature water may be acceptable,

Cleaning and Monitoring Procedures | Alconox, Inc. 1

 • Pre-treatment to loosen soils and prevent Directions: Make up cleaning solution per mixing
drying — especially for labware or medical directions, or use undiluted detergent on a warm wet
instruments prior to further cleaning cloth or sponge for non-abrasive scouring. Clean as
Advantages: Very little physical effort or expense. follows: Wet the article with solution by dunking or
using a soaked cloth or sponge. Clean with a cloth,
Concerns: Extremely dirty articles or difficult soils
sponge, cotton swab, brush or pad that agitates
may require further cleaning.
surface soils without marring the surface. Rinse
Directions: Soak completely submerged in solution thoroughly (see Rinsing). Wear gloves, eye protection
until clean. This may take several hours, depending and other safety equipment if recommended.
on the type of soil. Remove and rinse thoroughly (see
Rinsing).
4. Ultrasonic Cleaning
Recommended Products: ALCONOX,
3. Manual Cleaning
TERGAZYME, LIQUINOX, CITRANOX, DETERGENT 8,
Recommended Products: ALCONOX, LUMINOX, ALCOJET, DETOJET, CITRAJET, TERGAJET,
TERGAZYME, LIQUINOX, CITRANOX, DETERGENT 8, SOLUJET, DETONOX, KEYLAJET
In any industrial LUMINOX, ALCOJET, DETOJET, CITRAJET, TERGAJET,
cleaning Typical Use: Cleaning large batches of articles or for
SOLUJET, DETONOX, KEYLAJET
fast, convenient cleaning.
application, Typical Use: Cleaning small articles such as medical
Advantages: Fast, effective, penetrating cleaning.
“clean” means examination instruments, labware or circuit boards,
and large articles such as process equipment. Concerns: Capital cost; material tolerance for
clean enough ultrasonic agitation.
to avoid later Advantages: Versatile, inexpensive, effective.
Directions: Make up detergent solution in a
problems. The key Concerns: Time consuming and labor intensive. May
separate container. Add cleaning solution, run
not be effective on hard-to-reach areas requiring pre-
question is, What soak, ultrasonic or machine cleaning.
machine for several minutes to degas solution and
will happen if allow heater to come up to temperature. Place groups
the surface isn’t TABLE 1: DILUTION INSTRUCTIONS FOR ALCONOX, INC. DETERGENTS
clean? Dilution Recommended Amount: Min Usual
Product Form (%) A: oz/gal, B: gram/l, C: ml/l Wash Temp Wash Temp
ALCONOX powder 1 A: 1 1/4, B: 10 Ambient Warm
TERGAZYME powder 1 A: 1 1/4, B:10 Ambient Max 130ºF
LIQUINOX liquid 1 A: 1 1/4, C: 10 Ambient Warm
CITRANOX liquid 1–2 A: 1–3, C: 10–20 Ambient Hot
DETERGENT 8 liquid 2–5 A: 2–6, C: 20–50 Ambient Hot
LUMINOX liquid 2–5 A: 2–6, C: 20–50 Ambient Hot
ALCOJET powder 1/2–1 A: 1/2–1 1/4, B: 5–10 Warm Hot
DETOJET liquid 1/2–1 A: 1/2–1, C: 5–10 Ambient Hot
ALCOTABS tablet – (1 tablet per use) Ambient Ambient
CITRAJET liquid 1–2 A: 1–3, C: 10–20 Ambient Hot
TERGAJET powder 1/2–1 A: 1/2–1 1/4, B: 5–10 Warm Hot
SOLUJET liquid 1/2–1 A: 1/2–1 1/4, B: 5–10 Ambient Hot
DETONOX liquid 1–5 A: 1–4, B: 10–30 Ambient Hot
KEYLAJET liquid 5 A: 1–6, C: 10–50 Ambient Hot
Directions: Dilute detergent (see chart) using warm (about 120° F or 50° C) or hot (about 140° F or 60° C) water. Ambient temperature water may be
acceptable, especially for pre-soak. For difficult soils, use very hot water (above 150° F or 65° C) and double the recommended amount of detergent. When
cleaning solution may be reused, make up fresh solutions frequently, as needed.

Cleaning and Monitoring Procedures | Alconox, Inc. 2

 of small articles in racks or baskets. Align irregularly water (above 140ºF or 60ºC). Most machines have
shaped articles so the long axis of any part faces the at least three rinse cycles (see Rinsing). Refer to
ultrasonic transducer (usually the bottom). Immerse machine manufacturer’s directions.
articles to be cleaned for 2–10 minutes or longer, as
needed. Remove and rinse thoroughly (see Rinsing). 7. Automatic Syphon Pipette Washing
Recommended Products: ALCOTABS
5. Clean-in-Place
Typical Use: Washing pipettes in laboratories.
Recommended Products: ALCONOX,
Advantages: Effective batch pipette cleaning.
TERGAZYME, LIQUINOX, CITRANOX, DETERGENT 8,
Concerns: Pre-soak pipettes for best results.
LUMINOX, ALCOJET, DETOJET, CITRAJET, TERGAJET,
SOLUJET, DETONOX, KEYLAJET Directions: Completely immerse pipettes
immediately after use in a pre-soak solution. When
Typical Use: Pipe, tank and filtration systems.
ready to clean: Drop an ALCOTAB into bottom of
Advantages: Assures clean systems without washer. Place pipettes in holder into the washer.
disassembly. Turn on cold or warm water at a rate that will fill
Don’t neglect Concerns: Good circulation in system. the washer and completely cover all pipettes, then
the rinse! Use Directions: Make up cleaning solution per mixing drain to the bottom during each cycle. Run water
ambient, warm, directions. Circulate solution slowly for at least 1/2 until ALCOTAB has completely dissolved; continue
or hot water. A hour. Allow several hours for large systems (1000s of running water to rinse thoroughly (may take an hour
gallons), especially with ambient temperature water. to complete washing and rinsing). For analytical or
running water
Drain by pumping in one full system capacity of water. tissue culture work, use distilled or deionized water
rinse directly Rinse by circulating and draining at least two times for final rinse.
contacting all the system’s water capacity. Some filtration units may
surfaces for at require more rinsing. 8. Rinsing
least 10 seconds Don’t neglect the rinse! Use ambient, warm, or hot
on each surface 6. Machine Washers water. A running water rinse directly contacting all
Recommended Products: DETERGENT 8, surfaces for at least 10 seconds on each surface
is desirable.
ALCOJET, DETOJET, CITRAJET, TERGAJET, SOLUJET, is desirable. If not practical, use a series of three or
KEYLAJET more agitated soak tanks or at least two counter-flow
cascade tanks to rinse instead.
Typical Use: High-volume cleaning using washer-
sanitizers, ware-washers, conveyor-washers, or spray Specific Cases:
and pressure washers. • Large surfaces — Several passes with a
Advantages: Fast, effective, high volume cleaning. clean cloth or sponge soaked with rinse water
Concerns: Capital cost; article’s ability to withstand followed by a clean, dry, absorbent wipe can
machine washing conditions. work.
Directions: Load articles into racks so that open • Machine cleaning — After washing there
ends face toward spray nozzles. Place difficult-to- should be at least three rinse cycles. Tap water
clean articles with narrow necks and openings near is suitable for many rinsing applications.
the center of the rack, open side down, preferably • Medical and surgical instruments —
on special racks with spray nozzles pointing directly Give a final rinse in distilled or deionized water.
into them. Minimize touching between articles. • Laboratories — Rinse tissue culture and
Group small articles in baskets to prevent dislodging analytical ware with deionized or distilled
by spray action. Use only low-foaming detergent water. Rinse trace organic analytical ware in
per machine manufacturer dose instructions. If no distilled or organic-free water. Give trace metal
instructions, use a 1% solution or 1 oz. per gallon of or inorganic analytical ware a final rinse with
wash water. Use more or less as needed. Use hot deionized water.

Cleaning and Monitoring Procedures | Alconox, Inc. 3

 • Pharmaceutical equipment — Rinse indicates an exhausted cleaning solution. Under
according to good manufacturing practice frequent daily use, detergent solutions can rarely be
with whichever is required: potable, deionized, used more than a week, even when being extended.
distilled, sterile, pyrogen-free or injectable Free-alkalinity titration can be used to extend bath
water. life where the soils deplete free alkalinity, as follows:
• Electronic circuit boards and non- • Titrate a fresh solution to determine free alkalinity
conducting electronic devices — Rinse
• Titrate the used solution to determine the percent
with deionized water.
drop in free alkalinity
• Sensitive optical or precision
• Add detergent to the used bath to bring the free
manufactured parts — May require final
alkalinity back to the new-solution level
rinses in deionized or distilled water.
For example if your initial solution contains 100 ml
• Food processing equipment — Rinse with
of cleaner concentrate and there is a 25% drop in
potable water.
free alkalinity, try adding 25 ml of cleaner concentrate
to recharge the solution. Perform a new free-
For the highest 9. Drying alkalinity titration the first few times to confirm that
levels of critical Drying can effect residues and corrosion. Impurities the detergent is linear with respect to free-alkalinity
cleaning only from rinse water can be deposited during evaporation. depletion. This bath-life extension cannot be repeated
freshly made To minimize this, dry with techniques that physically indefinitely: sludge will eventually form, requiring a
remove rinse water from the substrate: absorbent fresh solution.
up solutions wiping, forced air or air knives, azeotropic solvent
should be used drying such as isopropyl alcohol final rinse and dry, or 11. Corrosion Inhibition
for cleaning vacuum drying, which may also evaporate residues.
Corrosion during cleaning is accelerated by the same
to avoid any Water — particularly high purity rinse water — can
things that accelerate cleaning: heat, aggressive
be corrosive to metal substrates during heated
potential for cross chemicals, time, and agitation. To reduce metal
and air-drying. The use of physical removal drying
contamination. corrosion, in approximate order of effect, use less
techniques or the addition of corrosion inhibitors (with
heat, corrosion inhibited detergents, lower pH or pH
the tolerance of corrosion inhibitor residues) to the
appropriate detergents, shorter cleaning time, and
rinse water can help minimize corrosion.
less agitation. Avoid mixed metals in the same bath
that form batteries and deposit galvanic oxides. The
10. Bath Life Extension and Control following techniques may work to limit corrosion,
For the highest levels of critical cleaning, especially based on the material and/or process involved:
to avoid cross contamination, only freshly prepared • Metal: Use the mildest pH detergent and avoid
solutions should be used. For industrial cleaning mixed metals in the same bath.
applications, however, bath life can be extended while
• Aluminum: After abrasion exposes pure
still achieving high levels of cleaning.
metal surface, allow air passivation time prior
Bath life extension techniques: to cleaning. Use mild acid cleaners such as
• Filtering particulates CITRANOX or CITRAJET to avoid alkaline attack.
• Cooling and settling of sludge • Plastic: Use less aggressive cleaners,
• Cooling and skimming oils containing less solvent or surfactant character.
• Adding half again as much detergent as the Or use lower concentrations of those cleaners,
initial load after partially depleting the cleaning lower cleaning temperatures, less contact time,
life of a bath and less agitation. For stressed polycarbonate
and acrylic use surfactant-free DETOJET for
Conductivity, pH and % solids by refractometer can
cleaning. Unstressed material is not a concern.
be used to measure bath detergent concentration.
Avoid alkaline cleaners on polyurethane.
In general, a pH change of 1 unit toward neutral

Cleaning and Monitoring Procedures | Alconox, Inc. 4

 • Mild sensitive steel: Avoid “flash rusting” by observing whether a gently sprayed water mist
rinsing with cold water and using rapid water- deposits uniformly or whether water repulsion occurs
removing drying techniques such as dipping (usually due to a hydrophobic soil). The atomizer
in isopropyl alcohol to form an evaporating test is slightly more sensitive to hydrophobic soils
azeotrope that removes water safely, centrifuge than the water break test. In the water break test the
drying, wipe drying, air knives, and drying with kinetic energy of the flowing water may overcome a
oxygen-free gas such as dry nitrogen. Or add hydrophobic residue, whereas in the atomizer test
a suitable corrosion inhibitor to the rinse water, you may be able to see the results of a little droplet of
as long as you can tolerate corrosion-inhibitor water being repelled by a hydrophobic contaminant.
residues. Do not use evaporative drying such Oil-soluble fluorescence (mg/cm2 level)
as air drying or oven drying. In this test the cleaned part is dipped into a
• Sensitive steel: Clean with an inhibited fluorescent oil. If oily residues are present, they will
cleaner and isopropyl alcohol rinse (or add a be extracted into the florescent oil that can be easily
corrosion inhibitor to the rinse water). observed under ultraviolet light. Of course, using
• Galvanic corrosion: Avoid mixed metals oil-soluble fluorescence requires cleaning the part
Depending upon the again after each test. Oil-soluble florescence is a
in the same bath that can form a battery
method selected, and deposit oxides on one of the metals. For highly sensitive method and can give very dramatic
cleanliness can be example, many metals will plate out their oxides visible results of oil residue. The problem with this
detected within on aluminum if the two metals are cleaned test is that it really only shows how well your process
in the same bath. Intact stainless steel is removed oily soils; it does not reveal particulate or
three ranges:
generally OK as a mixed metal, but iron, steel, inorganic soils.
Greater than or
brass, aluminum, bronze and other metals can Non-volatile residue (10s of mg/cm2 level)
equal to 0.01 be a problem mixed with other metals. Extract contaminants from a part using a volatile
grams per square solvent and evaporate the solvent in a pre-weighed
centimeter (g/cm2), 12. Cleaning Measurement Procedures container. Weigh again after evaporation to detect the
between 0.01 and Depending upon the method selected, cleanliness weight of volatile residues.
.001 g/cm2, and can be detected to varying degrees within three Extraction (mg/cm2 level)
ranges: Greater than or equal to 0.01 grams per An excellent method for detecting detergent residues.
below 1 microgram
square centimeter (≥ 0.01 g/cm2), 0.01–.001 g/cm2, Use a solvent-soaked glass filter paper or polyester
per square swab to wipe surface. Extract or digest filter paper.
and — the highest level of cleanliness measurement
centimeter. — below 1 microgram per square centimeter (<1 Use trace analysis on the extract. Can be quantitative
µg/cm2). The sensitivity of each method appears in if you wipe a known area. Extraction method can
parentheses after its name. be highly sensitive to a wide range of possible soils
Water-break (10s of mg/cm2 level) and residues. The limitations of this method are that
Use running water and let it sheet across the surface. an appropriate solvent has to be used to extract
Observe if any breaks in the water occur due to whatever type of soil might be there. For example,
hydrophobic (water-fearing) residues. (See “The trace analysis for detergent residues would require
Hydrophobic Surface Film by the Water Break Test,” water as the solvent. The sensitivity of an extraction
ASTM Method F 22–65, at www.astm.org.) The test depends on your method of trace analysis. The
water break test is a fairly crude method, suitable for types of trace analysis often used are UV visible
detecting films of process oils and heavy fingerprints. spectrophotometry, total organic carbon (TOC)
It will not readily detect non-hydrophobic residues. analysis, high performance liquid chromotography
This test is often used for parts washing; it may not (HPLC), atomic absorption (AA) or inorganic residues,
always be suitable for precision cleaning applications. and liquid chromotography (LC) and filtration with
microscopic filter examination.
Atomizer (10s of mg/cm2 level)
A variation of the water-break test, this requires Oil evaporation (10s of mg/cm2)
For filmy residues, a few drops of organic solvent

Cleaning and Monitoring Procedures | Alconox, Inc. 5

 can be deposited on the surface and then removed especially suited to manufacturing operations that
via pipete and placed on a watch glass. If any require a nondestructive cleanliness test.
filmy residues are present, you should observe a For example, LCD panel surfaces contaminated
characteristic ring of organic-material deposits. with organic matter will be less accepting of films
Gravimetric (mg/cm2 level) such as metals and protective layers, resulting in poor
With small parts of known weight, the amount of manufacturing yields. Contaminant sources include
excess weight indicates the amount of soil present. the vapor of process materials, chemicals, and
Surface energy (mg/cm2 level) human perspiration.
Any hard, flat material has a characteristic surface Very thin organic contaminants several monolayers
energy. As a result, depositing a known volume of in thickness (greater than 10 angstroms) can be
pure liquid (typically deionized water) will form a evaluated using the contact angle technique. In fact, it
droplet of predictable size based on the amount of is generally agreed that the wetting behavior involves
that energy, and measuring that droplet size will only the last layer or two atoms on either side of a
determine surface cleanliness. Generally, hydrophobic solid’s interface. The water contact angle correlates
Since the properties soils create smaller droplets; hydrophilic soils, larger the cleanliness of the surface to the adhesion of the
ones. The surface-energy test is far more sensitive copper deposited onto the surface of the LCD.
of various than the atomizer or water-break test and has the Accepted methods of measuring contact angles
contaminated advantage of being able to detect both hydrophilic to determine surface characteristics include the
surfaces are and hydrophobic soils. The problem with the surface inverted bubble, Wilhelmy Plate, and sessile drop
reflected by different energy test is it only tests the surface directly techniques. The latter is the most widely practiced
underneath the droplet where you are measuring. If quality control technique, as it is relatively quick and
contact angles,
you have a broad, large surface where measuring one requires minimal investment in time and financial
contact angle testing small area would be representative of the cleaning resources.
can be used in a done over the entire surface, this can be an excellent
Follow these tips from Precision Cleaning
range of processes and highly sensitive method. If you have a part with
magazine, (Oct. 97, p. 23) to increase the
to determine cracks, crevices and holes, the accessible surfaces
repeatability and validity of contact angle
may not be representative of soils hidden in the
cleanliness. measurement results:
various cavities.
• Use gloves when handling the measurement
Contact angle
samples. Organics such as finger oils,
A variation on surface energy testing, contact angle
cosmetics, and other contaminants will skew
is defined simply as the relationship of certain forces
contact angle results.
when a liquid stabilizes on a part’s surface. Since
the properties of various contaminated surfaces • Note the nature of the droplet after applying it
are reflected by different contact angles, contact to the surface. Wait until the droplet ceases its
angle testing can be used in a range of processes to advancement and change in lateral movement
determine contamination levels, predict cleanliness stops. Measure this time interval and make
and adhesive bond strengths, and monitor cleaning sure to wait the same period of time after every
operations. measurement. Retain consistent time intervals
between the placement of the droplet and its
Whether you are checking the moisture effects
measurement.
on silicon wafers or LCD quartz panel glass/metal
adhesion, all that is needed is an understanding of • Use a consistent measuring liquid — ideally,
the basic theory involved and proper measurement medical-grade, ultra-purified deionized water
techniques. Contaminants that can be detected from a laboratory supply house. This will limit
by changes in the contact angle include vapors the number of measurement variables.
from the process itself (e.g., vacuum or diffusion • Use test liquids of larger surface tension than
pump oils), various process chemicals, and even the solid’s surface energy in order to obtain
human perspiration. Contact-angle measurement is easy-to-read results.

Cleaning and Monitoring Procedures | Alconox, Inc. 6

 • Neutralize the effects of static charges on diameter needle) to deposit very small droplets
substrates. Substrates that are electrostatically onto the sample.
charged can skew contact angle readings up to • Other methods such as visual examination
5 degrees. using a stereomicroscope, fi beroptic light, or
• Accurately control liquid droplets so that they black light are also useful in determining the
are repeatedly deposited onto the sample. existence of cleaning process residues.
Gently move the sample to the liquid droplet
formed at the end of the syringe/dispenser in
For extreme low level residue detection at the
order to minimize gravitational effects.
many µg/cm2 level, surface analysis techniques
• In the case of very high contact angles, you such as Auger electron spectroscopy (AES), electron
may fi nd it diffi cult to adhere the droplet from spectroscopy for chemical analysis (ESCA), fourier
the needle to the solid sample. Use a PTFE- transform infrared (FTIR), secondary ion mass
coated needle of a higher gauge (smaller inner spectroscopy (SIMS) and optically stimulated electron
diameter). emission (OSEE) are used.
Whether you are • In case of very low contact angles, use the
checking the highest possible needle gauge (smallest inner
moisture effects
on silicon wafers
or LCD quartz
panel glass/metal
adhesion, all that
is needed is an
understanding of
the basic theory
involved and proper
measurement
techniques.

Cleaning and Monitoring Procedures | Alconox, Inc. 7

Critical Cleaning ExpertsSM
3 0 Glenn Street, Suite 309
White Plains, NY 10603 • USA

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Critical Cleaning Challenge
Alconox, Inc. has more than 70 years’ experience developing
aqueous cleaning solutions for pharmaceutical manufacturing.
Let us help solve your next critical cleaning challenge.
Please contact Alconox, Inc. for expert validation support or
verifi cation laboratory services:
[email protected]

Learn More About Critical Cleaning

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The Aqueous Cleaning Handbook
or
Critical Cleaning Guide

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Use our sample request form at alconox.com. Or call:
++914-948-4040

For questions or comments about this white paper,

please contact Alconox, Inc. Technical Support at
914.948.4040 or [email protected]

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Cleaning and Monitoring Procedures | Alconox, Inc. 8