PN AR.01033 Test Methods For Monitoring of Cleaning Processes

Test Standard PN AR.
01033
May 2005
Replacement for BEHR-PN V AR.01033 : 2003-08
Translation
No liability can be accepted for the correctness of the translation
It is in all instances the latest version of the document in its original language that is binding
Original language: German
Brazed Aluminum Heat Exchangers – General

Test Methods for Monitoring of Cleaning Processes
BEHR Laboratory Standards
Contents
1 Purpose ...................................................................................................................4
2 Scope .......................................................................................................................4
3 Special Notes ..........................................................................................................4

3.1 Monitoring of test equipment ............................................................................................................ 4
3.2 Deviations............................................................................................................................................ 4
4 Occupational Safety and Health and Environmental Protection ........................4

4.1 Occuational safety and health .......................................................................................................... 4
4.2 Environmental protection .................................................................................................................. 4
5 General Test Methods ............................................................................................4

5.1 Using test inks to determine the surface tension of the components.......................................... 4
5.1.1 Test conditions ............................................................................................................................. 4
5.1.1.1 Information on the use of test inks................................................................................................... 4
5.1.2 Apparatus ..................................................................................................................................... 5
5.1.2.1 Information on the apparatus to be used......................................................................................... 5
5.1.3 Test Sequence ............................................................................................................................. 5
5.1.3.1 Preliminary remarks on the application of test inks ......................................................................... 5
5.1.3.2 Test steps ........................................................................................................................................ 5
5.1.4 Test evaluation ............................................................................................................................. 5
Continued to page 16
Author: Mr. Trautwein, EA-71 Editor: G-Q1 Specialized responsibility: Mr. Dr. Mamber, EA-7
Management Systems
Technical Documents Service
Observe copyright in accordance with ISO 16016  BEHR GmbH & Co. Date of Translation: 9th August 2005
Page 2
PN AR.01033 : 2005-05
5.1.5 Specified values ........................................................................................................................... 5

5.2 Determining the residual lubricant content on the part by means of IR spectroscopy.............. 6
5.2.1 Test conditions ............................................................................................................................. 6
5.2.2 Test sequence.............................................................................................................................. 6
5.2.3 Test results and test evaluation ................................................................................................... 6
5.2.3.1 Specified values............................................................................................................................... 6
5.3 Determining the residual lubricant content on the part by means of extraction and gravimetric
analysis................................................................................................................................................ 6
5.3.1 Test conditions ............................................................................................................................. 6
5.3.2 Apparatus ..................................................................................................................................... 6
5.3.2.1 Tools and equipment ....................................................................................................................... 6
5.3.3 Test sequence.............................................................................................................................. 6
5.3.4 Calculation.................................................................................................................................... 7
6 Test Methods for Aqueous Processes..................................................................7
6.1 Determining the residual lubricant content in the cleaning bath by means of extraction and
gravimetric analysis ........................................................................................................................... 7
6.1.1 Test conditions ............................................................................................................................. 7
6.1.2 Apparatus ..................................................................................................................................... 7
6.1.3 Test sequence.............................................................................................................................. 7
6.1.4 Calculation.................................................................................................................................... 8
6.2 Determining the residual lubricant content in a cleaning bath by means of acid cleavage....... 8
6.2.1 Test conditions ............................................................................................................................. 8
6.2.2 Apparatus ..................................................................................................................................... 8
6.2.3 Test sequence.............................................................................................................................. 8
6.3 Determining the cleaner concentration in the bath by means of titration.................................... 9
6.3.1 Test conditions ............................................................................................................................. 9
6.4 Determining the conductivity in the purging water ........................................................................ 9
6.4.1 Test sequence.............................................................................................................................. 9
6.4.2 Test results and test evaluation ................................................................................................. 10
6.4.2.1 Specified values............................................................................................................................. 10
6.5 Determining the evaporation residues in purging baths by means of differential weighing ... 10
6.5.1 Apparatus ................................................................................................................................... 10
6.5.1.1 Tools and equipment ..................................................................................................................... 10
6.5.2 Test sequence............................................................................................................................ 10
6.5.2.1 Sampling ........................................................................................................................................ 10
6.5.2.2 Test steps ...................................................................................................................................... 10
6.5.3 Calculation.................................................................................................................................. 10
Table 1 11
7 Test Instructions for Solvent-Based Processes.................................................11
7.1 Determining the residual lubricant content in the solvent by means of gravimetric analysis. 11
7.1.1 Test conditions ........................................................................................................................... 11
7.1.2 Apparatus ................................................................................................................................... 11
Observe copyright in accordance with ISO 16016  BEHR GmbH & Co.
Page 3
PN AR.01033 : 2005-05

7.1.3 Test sequence............................................................................................................................ 11
7.1.3.1 Test steps ...................................................................................................................................... 11
7.1.4 Calculation.................................................................................................................................. 12
7.2 Determining the residual lubricant content in the solvent by means of IR spectroscopic
analysis.............................................................................................................................................. 12
7.2.1 Test conditions ........................................................................................................................... 12
7.2.1.1 Introductory remark........................................................................................................................ 12
7.2.2 Test sequence............................................................................................................................ 12
7.2.2.1 Test steps ...................................................................................................................................... 12
7.2.2.2 Detection of very low oil content .................................................................................................... 12
7.2.3 Calculation.................................................................................................................................. 12
7.3 Determining the total acid take-up capability of the solvent ....................................................... 13
7.3.1 Test conditions ........................................................................................................................... 13
7.3.2 Apparatus ................................................................................................................................... 13
7.3.2.2 Hydrochlorinating reagent.............................................................................................................. 13
7.3.3 Test sequence............................................................................................................................ 13
7.3.3.1 Test steps ...................................................................................................................................... 13
7.3.4 Calculation.................................................................................................................................. 14
7.4 Determining the pH value in the solvent........................................................................................ 14
7.4.1 Test conditions ........................................................................................................................... 14
7.4.1.1 Servicing and checking the pH probe............................................................................................ 14
7.4.2 Test sequence............................................................................................................................ 14
7.4.2.1 Test steps ...................................................................................................................................... 14
7.5 Detection of chloride ions in the solvent ....................................................................................... 14
7.5.1 Test requirements ...................................................................................................................... 14
7.5.2 Test sequence............................................................................................................................ 14
7.5.2.1 Test steps ...................................................................................................................................... 14
Referenced Standards.....................................................................................................15
Previous Issues ...............................................................................................................15
Amendments ....................................................................................................................15
Page 4
PN AR.01033 : 2005-05
1 Purpose
This Test Standard defines various analytical and test methods that are used to test the quality of cleaning
processes and the surface condition of the cleaned parts.
It is used as a basis to enable the process managers or the suppliers draw up detailed test instructions for
the laboratory and operating personnel.
Scope, test frequencies and the binding character of the tests to be performed at the respective site are
defined in the respective BEHR process standards BEHR VN V AR.01036 (aqueous processes), BEHR
VN V AR.01035 (solvents) and BEHR VN V AR.01034 (thermal degreasing) and/or in the work instructions
drawn up by the production department on the basis of the referenced process standards.
2 Scope
This Test Standard is applicable to all sites of the Behr Group and to all suppliers wherever individual
components for BEHR aluminum heat exchangers are cleaned.
3 Special Notes
3.1 Monitoring of test equipment
The test equipment used is subject to the requirements of test equipment monitoring in accordance with
QS 9001 (DIN EN ISO 9001).
3.2 Deviations
Deviations from the methods described in this test standard are permissible in accordance with site-specific
requirements if the modified process is demonstrated by the modifying party to be equivalent with the
abovementioned methods and is documented accordingly.
The department for Advanced Engineering of chemical processes at BEHR Stuttgart shall be informed of any
modifications made.
The quality control measures implemented by the supplier or by the process are to be approved by the
responsible BEHR quality control department prior to commencing series production.
In the event of complaints, the test methods defined in this test standard shall be decisive for quality evalua-
tion.
4 Occupational Safety and Health and Environmental Protection

4.1 Occuational safety and health
For technical safety data pf chlorinated solvents and acids, please refer to the applicable safety data sheets
as per TRGD 220 (91/155/EC).
4.2 Environmental protection

Any remaining residual quantities of solvents and acids shall be disposed of using appropriately marked
containers via the waste material storage area.
5 General Test Methods

5.1 Using test inks to determine the surface tension of the components
5.1.1 Test conditions
5.1.1.1 Information on the use of test inks
As the test inks may contain substances that are detrimental to health (e.g. formamide), the procedure
described below must only be performed by specialist personnel that has completed appropriate training
Page 5
PN AR.01033 : 2005-05
(e.g. in the plant laboratory). Make sure the personal protective measures described in the relevant safety
data sheet/operating instructions of the test ink are observed.
5.1.2 Apparatus
5.1.2.1 Information on the apparatus to be used
A standard portable test set with test inks (as manufactured by AHLBRANDT, ARCOTEC or equivalent
suppliers) is used. This test set consists of 8 bottles with test inks of different surface tensions that cover a
range of 38 to 52 mN/m. Test pens may alternatively be used. The below instructions shall apply both to test
pens and inks as applicable in each case.
It is recommended, however, to use test inks instead of test pens as pens may dry up when stored in an
inappropriate manner and may become contaminated when used improperly. This may in turn lead to
incorrect values being displayed.
5.1.3 Test Sequence
5.1.3.1 Preliminary remarks on the application of test inks
It is recommended to use a cotton swab to apply the ink on the component. This helps prevent the test ink
from being contaminated with oil residues that may be present on the paint brush. The ink bottle used for this
process should be emptied every 4 to 8 weeks and refilled with the required ink from a storage container.
The manufacturer’s shelf life specifications shall be observed at all times.
5.1.3.2 Test steps
Step 1
Using a test ink of the medium range (e.g. 38 mN/m) and a cotton swab, draw three approx. 2 cm long ink
lines on the component to be tested.
Step 2
If it is observed in Step 1 that one of the three ink lines that have been drawn contracts within 3 seconds, the
surface tension on the part surface is lower than that of the test ink applied in Step 1. Now repeat Step 1
using the next lower ink graduations until all three ink lines remain on the surface for three seconds
without contracting in any way.
Step 3
If no contraction of any of the ink lines drawn in Step 1 is observed within 3 seconds, the surface tension of
the part surface is higher than that of the test ink applied in Step 1.
Now repeat Step 1 using the next higher ink graduations until one of the three ink lines contracts within
3 seconds.
5.1.4 Test evaluation

If the ink line that has been drawn remains unchanged for at least 3 seconds without contracting, the
following statement applies:
The surface tension on the part is equal to or higher than that of the test ink applied
If the ink line that has been drawn contracts within 3 seconds, the following statement applies:
The surface tension on the part is lower than that of the test ink applied
5.1.5 Specified values

See BEHR GN AR.01024
Page 6
PN AR.01033 : 2005-05
5.2 Determining the residual lubricant content on the part by means of IR

spectroscopy

The method quoted below in accordance with BEHR PN AR.01042 is not suitable for silicon oil lubricants as
silicon oils do not show any absorption bands in the IR wavelengths used here.
5.2.2 Test sequence

See BEHR PN AR.01042
5.2.3 Test results and test evaluation
5.2.3.1 Specified values

See BEHR PN AR.01042
5.3 Determining the residual lubricant content on the part by means of

extraction and gravimetric analysis

Note: Inhalation of chlorinated solvent vapors is detrimental to health; the procedure described below
must therefore only be performed by specialist personnel that has completed appropriate training
(e.g. in the plant laboratory). Make sure the personal protective measures described in the relevant
safety data sheet of the solvent to be used are observed. Always operate an extraction system
when handling tetrachloroethylenes.
5.3.2 Apparatus
5.3.2.1 Tools and equipment
− Analytical scales, accuracy ±1 mg

− Rotary evaporator
− Vacuum pump (rotary or water jet)
− Water bath, vacuum gauge (pressure gauge, etc.)
− Electrical heating plate
− 1-liter round-bottom flask with ground joint NS29
− Stainless-steel photographic dish, approx. 30 x 20 cm, edge height 5 cm, or beaker
− Beakers, 500 / 1000 / 2000 ml volume, low type
5.3.3 Test sequence

Extracting the residual lubricant from the part
Heat approx. 500 ml pure tetrachloroethylene in a photographic dish or a beaker to approx. 60 to 80 °C. Use
a pair of pliers to completely immerse the samples to be tested for approx. 1 minute, moving them to and
from time to time, and remove and allow them to drip off. In order to achieve sufficiently accurate analytical
results at expected residual lubricant contents of approx. 20 mg/m², the total surface area of the parts to be
treated in this manner must be approx. 1.5 m². Any evaporation losses during the extraction process are
compensated by the solvent. The solvent is cooled to below 50 °C.
Filling the evaporator flask

The 1-liter round flask dried in a drying cabinet at 120 °C for 2 hours is cooled, weighed and the empty
weight is determined with an accuracy of ±0.001 g. The value in [mg] is recorded (value “E“). The solvent is
transferred from the extraction into the flask.
Page 7
PN AR.01033 : 2005-05
Evaporation of the solvent

The round flask is connected to the evaporator and rotation is started. Then the vacuum pump is switched
on. The rotational speed is approx. 50 rpm. At a water bath temprature of approx. 60 °C, the pressure will
settle at a level of approx. 150 mbar. Be sure to wait until the entire volume of the solvent has evaporated
and the inside of the flask appears to be dry. Then the purge air tap is opened completely and external air is
aspirated for approx. 5 minutes in order to purge any remaining gaseous solvent residues and to prevent
recondensation. The flask is then removed and its outside is wiped dry with a paper towel or tissue. Next it is
wiped dry with paper or tissue soaked with alcohol until the outside is completely dry. Allow the flask to cool
off, determine the weight once more and record the value in [mg] (value “F“).
5.3.4 Calculation
R = Residual oil content in [mg/m²)
R=
(F − E ) F = Weight of flask after evaporation
A Parts E = Weight of empty flask
AParts = Surface of extracted parts in [m²]
Test results and test evaluation

See BEHR GN AR.001024
6 Test Methods for Aqueous Processes

6.1 Determining the residual lubricant content in the cleaning bath by means of
extraction and gravimetric analysis

6.1.2 Apparatus

− Analytical scales, accuracy ±0.001 mg
− Water bath, vacuum gauge (pressure gauge, etc.)
− Electrical heating plate
− 200 ml round-bottom flask with ground joint NS29
− Separating funnel
− Beakers, 500 / 1000 / 2000 ml volume, low type
6.1.3 Test sequence

Extracting the residual lubricant from the bath
Filll 500 ml of the bath sample (±10 ml) and approx. 50 ml (±5 ml) tetrachloroethylene into a separating
funnel. Shake the mixture for approx. 2 minutes (±10 seconds) and place the separating funnel into a rack to
allow the phases to separate. If no clearly discernible separation into 2 phases is visible after approx.
10 minutes, add approx. 10 to 20 g common salt (NaCl) or magnesium sulphate (MgSO4) to the contents of
the funnel and shake the funnel briefly again until the salt has dissolved (instead of adding solid salt, an
Page 8
PN AR.01033 : 2005-05
equivalent quantity (approx. 50 ml) of concentrated common salt solution (approx. 300 g/l) may also be
added).
The 1-liter round flask dried in a drying cabinet at 120°C for 2 hours is cooled, weighed and the empty weight
is determined with an accuracy of ±0.001 g. The value in [g] is recorded (value “E“).
After the phases have separated, the lower, clear solvent phase is routed into the 200 ml round flask across
a pleated filter.
Make sure that no water enters the flask (for this purpose, approx. 5 to 10 g dried calcium chloride (CaCl2)
may be added to the filter in order to bind any water residues).
The round flask is connected to the evaporator. Rotation is started and the vacuum pump is switched on.
The rotational speed is approx. 50 rpm. At a water bath temprature of approx. 60°C, pressure will settle at a
level of approx. 150 mbar.
Wait until the entire volume of the solvent has evaporated and the inside of the flask appears to be dry. Then
the purge air tap is opened completely and external air is aspirated for approx. 5 minutes in order to purge
any remaining gaseous solvent residues and to prevent recondensation. The flask is then removed and its
outside is wiped dry with a paper towel or tissue. Next it is wiped with paper or tissue soaked with alcohol
until the outside is completely dry. Allow the flask to cool off, determine the weight once more and record the
value in [g] (value “F“).
6.1.4 Calculation
R = Residual lubricant content in [mg/kg]
R=
(F − E ) F = Weight of flask after evaporation
0.500 E = Weight of empty flask

See BEHR VN V AR.01036
6.2 Determining the residual lubricant content in a cleaning bath by means of

acid cleavage

Note: Concentrated hydrochloric acid is extremely caustic; inhalation of its vapors is detrimental to health.
For this reason the procedure described below must only be performed by specialist personnel that
has completed appropriate training (e.g. in the plant laboratory). Make sure the personal protective
measures described for 36 % hydrochloric acid in the relevant safety data sheet are observed.
Always operate an extraction system when handling concentrated hydrochloric acid.
6.2.2 Apparatus

Acid cleavage flask (refer to 6.2.4 for a schematic diagram)
6.2.3 Test sequence

The flask is filled with the bath sample to be tested up to to the bottom mark. Then 36% hydrochloric acid is
filled up to the top mark. The flask is closed and its contents are mixed. Then the flask is stored in the
laboratory drying cabinet for approx. 4 to 8 hours at 50 to 60°C. At certain intervals, remove the flask and
separate any oil drops adhering to the wall of the flask by tapping with the fingers against the neck of the
flask.
Page 9
PN AR.01033 : 2005-05

If no further oil separation occurs, the oil content in [% by vol.] is read off on the graduation of the flask. Any
accumulations of solids between the water and oil phase should be added to the reading with 50% of their
height.
Acid filling
height
Oil phase Correct reading:

Oil phase + ½ solids
Solids
10% reading mark
Water phase
30% reading mark
Filling height
100 ml sample

6.3 Determining the cleaner concentration in the bath by means of titration

As different cleaner systems are permissible in accordance with BEHR VN V AR.01036, reference is here-
with made to the bath testing specifications of the respective suppliers of the cleaning chemicals.

6.4 Determining the conductivity in the purging water
6.4.1 Test sequence

The conductivity electrode (measuring range 0 µS/cm to 2000 µS/cm) is either immersed directly into the
bath and moved to and fro or is immersed in the bath sample in a beaker, stirring the contents during
immersion. If the measuring instrument does not have an automatic temperature compensation device,
determine the sample temperature and correct the measurement in accordance with the indications of the
measuring device manufacturer.
Page 10
PN AR.01033 : 2005-05

6.5 Determining the evaporation residues in purging baths by means of

differential weighing
6.5.1 Apparatus

− Analytical scales, accuracy ± 1 mg
− Laboratory scales, accuracy ± 0.1 g
− Heating plate
− Recirculating air drying cabinet
− Crystallization dishes, 300 ml content, approx. 15 cm dia.
6.5.2 Test sequence
6.5.2.1 Sampling
The sample is taken directly above the bottom of the bath with a siphoning filler pump with a sufficiently long
lifting tube.
6.5.2.2 Test steps

1. A dried crystallizing dish is cooled (for 2 h at 130 °C), weighed and the empty weight is determined with
an accuracy of ± 1 mg. The value in [mg] is recorded (value “E“).
2. Fill approx. 200 g of the purging bath to be tested into the crystallizing dish placed on the laboratory
scales and determine the weight with an accuracy of ± 0.1 g. Record the value in [g] (=> value “M“).
3. Heat the dishes carefully on the heating plate and allow the content to evaporate slowly down to approx.
5 ml.
4. Leave the crystallizing dish in the drying cabinet at 130 °C until the entire water has evaporated and a
constant weight is obtained.
5. Remove the dish, allow it to cool off, determine the weight on the analytical scales once more and record
the value in [mg] (=> value “F“).
6.5.3 Calculation
R = Evaporation residue, [mg/kg]
R=
(F − E ) F = Weight of dish after evaporation
(M - E ) • 1000 E = Weight of empty dish
M = Weight of dish + weighed portion of water sample, [g]
Page 11
PN AR.01033 : 2005-05
Table 1
Max. permissible evaporation residues
Purging bath 1: 1500 mg/kg Note: The values given here are based
on experience; deviating values, e.g.
Purging bath 2: 500 mg/kg
within the scope of work instructions or
Purging bath 3 150 mg/kg process (VN) standards, are possible
7 Test Instructions for Solvent-Based Processes

7.1 Determining the residual lubricant content in the solvent by means of
gravimetric analysis

7.1.2 Apparatus
− Analytical scales, accuracy ±0.001 mg

− Vacuum gauge (pressure gauge, etc.)
− Water bath
− 1000-ml round-bottom flask with ground joint NS29
7.1.3 Test sequence
7.1.3.1 Test steps

The 1-liter round flask dried in a drying cabinet at 120 °C for 2 hours is cooled, weighed and the empty
weight is determined with an accuracy of ±0.001 g. The value in [g] is recorded (value “E“). Fill approx. 620
ml ±5 ml of the bath sample to be tested into the flask.
The round flask is connected to the evaporator. Rotation is started and the vacuum pump is switched on.
The rotational speed is approx. 50 rpm. At a water bath temperature of approx. 60 °C, pressure will settle at
a level of approx. 150 mbar.
Wait until the entire volume of the solvent has evaporated and the inside of the flask appears to be dry. Then
the purge air tap is opened completely. External air is aspirated for approx. 5 minutes in order to purge any
solvent residues. The flask is removed and its outside is wiped dry with a paper towel or tissue. Then it is
wiped with paper or tissue soaked with alcohol until the outside is completely dry. Allow the flask to cool off,
determine the weight once more and record the value in [g] (value “F“).
Page 12
PN AR.01033 : 2005-05
7.1.4 Calculation
R = Residual lubricant content in [g/kg]
R = F−E F = Weight of flask after evaporation

E = Weight of empty flask

7.2 Determining the residual lubricant content in the solvent by means of IR

spectroscopic analysis
7.2.1.1 Introductory remark
The method described below is not suitable for silicon oil lubricants as they do not show any absorption
bands in the IR wavelengths used here.
7.2.2 Test sequence
7.2.2.1 Test steps
Allow 10 ml of the solvent to be tested to evaporate for approx. 30 minutes in a crystallization dish at 50°C in
a laboratory drying cabinet until the dish is dry. The contents of the dish must no longer smell of tetrachloro-
ethylene, otherwise the dish must be placed in the drying cabinet for another 10 minutes. After the dish has
cooled to room temperature, 10 ml tetrachloroethylene of UVASOL quality or “highly pure“ quality are added
into the dish using a pipet and the dish is moved to and fro carefully in order to dissolve the oil residues
present.
Now a spectrum of the sample with a wavenumber of 2500 to 3500 is taken in a 10 mm quartz cell in the IR
spectrometer. Tetrachloroethylene of UVASOL quality or “highly pure“ quality is used as a reference. The
absorbance values “E“ at wavenumber 2958 and 2924 are recorded.
7.2.2.2 Detection of very low oil content
If the oil content in the solvent is very low, 20 ml or 30 ml may be used instead of the 10 ml sample de-
scribed under Section 7.2.2.1. The result in accordance with Section 7.2.3 must always be multiplied with a
factor F = 10ml / X ml, with “X“ being the actually used solvent quantity in [ml].
7.2.3 Calculation
 1   E   E 
CR = 1.3 •   •  CH3  +  CH2 
 d   ε CH3   ε CH2 
CR = Concentration of residual lubricant in the solvent in mg/cm³

ECH3 = Measured absorbance of CH3 group at wavenumber 2958
ECH2 = Measured absorbance of CH2 group at wavenumber 2924
Page 13
PN AR.01033 : 2005-05
.
εCH3 = Absorbance coefficient of CH3 group = 8.3 cm³ / mg cm
.
εCH2 = Absorbance coefficient of CH2 group = 5.4 cm³ / mg cm
d = Length of cell in [cm]
Conversion of [mg/cm³] into [mg/kg]:
CR
CR(mg) = 1000 •
1.62
CR(mg)= Concentration of residual lubricant in solvent in [mg/kg]

7.3 Determining the total acid take-up capability of the solvent

Note: Inhalation of vapors of chlorinated solvents or of hydrochloric acid is detrimental to health. For this
reason the procedure described below must only be performed by specialist personnel that has
completed appropriate training (e.g. in the plant laboratory). Concentrated 36% hydrochloric acid is
extremely caustic; inhalation of acid fumes is detrimental to health. Make sure the personal protec-
tive measures described for tetrachloroethylene and 36 % hydrochloric acid in the relevant safety
data sheet are observed. Always operate an extraction system when handling hydrochloric acid
and tetrachloroethylene.
7.3.2 Apparatus
− Buret, accuracy ± 0.1 ml

− Full pipet 50 ml, accuracy class 0.2%
− Full pipet 10 ml, accuracy class 0.2%
− Measuring flask 2000 ml
− Erlenmeyer flask 250 ml, narrow-neck type
7.3.2.2 Hydrochlorinating reagent
5 ml 36% HCl are topped up with isopropyl alcohol to a total of approx. 1.8 liters. 5 ml of a 0.1% solution of
bromophenol blue in isopropyl alcohol are added to this mixture.
Then isopropyl alcohol is added up to the 2 l mark and the contents are mixed agian.
7.3.3 Test sequence
7.3.3.1 Test steps
Blank value:
Using a Peleus ball, 50 ml of hydrochlorinating reagent are pipetted into the Erlenmeyer flask. Then the
titration is performed with 0.1N NaOH until the color changes from yellow through blue-green to a deep blue.
The NaOH consumption is recorded as value “A“.
Solvent test:
Page 14
PN AR.01033 : 2005-05
10 ml of the solvent to be tested are pipeted into the Erlenmeyer flask using a Peleus ball. Then 50 ml of the
hydrochlorinating reagent are added by pipeting using a Peleus ball and the contents of the flask are mixed
thoroughly. The mixture is now covered with a watchglass at room temperature and is allowed to sit for 10
minutes. Then titration is performed with 0.1N NaOH until the color changes from yellow through blue-green
to a deep blue. The NaOH consumption is recorded as value “B“.
7.3.4 Calculation
TSA = Total acid take-up capability in [% NaOH]
TSA = (A − B ) • 0.0246 A = NaOH consumption, blank value
B = NaOH consumption, solvent test

7.4 Determining the pH value in the solvent

when handling chlorinated solvents.
7.4.1.1 Servicing and checking the pH probe
The pH meter used and the matching electrode must be calibrated at least once a week with buffer solutions
of pH values 4.00 and 7.00. Additionally the calibration must be checked daily before commencing work by
immersing the electrode in a buffer solution (e.g. pH 4.00).
Caution: Make sure that the age of this buffer solution remains within the manufacturer’s specifications for
the maximum storage life. For this reason, the manufacturing date must always be indicated on the buffer
solutions.
If the value displayed deviates from the setpoint of the buffer solution by more than 0.1 pH units a new
calibration is required (regardless of the date of the previous calibration).
If it takes more than 2 minutes to adjust a stable reading (measurement drift < 0.1 pH/min), the electrode
must be checked and serviced and/or replaced if required.
7.4.2 Test sequence
7.4.2.1 Test steps
Mix 20 ml of the solvent to be tested with 60 ml demineralized water (conductivity < 10 µS/cm, pH 6.5 to 7.5)
in a 100-ml bottle with ground joint plug and shake the mixture for approx. 1 minute. Wait for the phases to
separate (approx. 5 min).
Insert the calibrated pH probe through the neck of the bottle and locate it with a laboratory tripod and a
clamp, for example, so that its tip is approx. 3 to 5 mm above the solvent phase.

Read off the value displayed on the pH meter after approx. 3 minutes.

Page 15
PN AR.01033 : 2005-05
7.5 Detection of chloride ions in the solvent
7.5.1 Test requirements

Note: Inhalation of vapors of nitric acid is detrimental to health. The procedure described below must
therefore only be performed by specialist personnel that has completed appropriate training (e.g. in
the plant laboratory). 10% nitric acid is extremely caustic. Silver nitrate and aqueous solutions
thereof are toxic when swallowed as well as caustic and will leave black spots when skin contact is
made. Make sure the personal protective measures described in the relevant safety data sheets
are observed. Always operate an extraction system when handling nitric acid.
7.5.2 Test sequence
7.5.2.1 Test steps
Mix 60 ml of the solvent to be tested with 20 ml fully demineralized water (conductivity < 10 µS/cm, pH 6.5 to
7.5) in a 100-ml bottle with a ground joint plug and shake the mixture for approx. 1 minute. Wait for the
phases to separate (approx. 5 min).
Using a pipet, take 10 ml from the water phase and add them into a test tube.
Add 1 ml of 10% nitric acid to this solution. Now add approx. 1 ml of a 50 g/l silver nitrate solution. Mix the
ingredients briefly and wait for approx. 1 minute.

Observe the test tube under backlighting conditions against a black background.

There must be neither white precipitate nor any turbidity. If these symptoms are found, however, this means
that the solvent contains chloride ions; this indicates incipient or advanced decomposition of the chlorinated
solvent. Countermeasures must be taken at once, e.g. by adding acid neutralisators or by neutralisation of
the solvent.
Page 16
PN AR.01033 : 2005-05
Referenced Standards
DIN EN ISO 9001 Quality management systems – Requirements
BEHR GN AR.01024 Requirements on the degreasing quality of bought-in parts for aluminum brazing
BEHR PN AR.01042 Production of heat exchangers – General; Determining the residual lubricant
content on metallic surfaces
BEHR VN V AR.01034 NOCOLOK-brazed heat exchangers; Thermal degreasing of individual parts prior
to NOCOLOK brazing – BEHR process and plant standard
BEHR VN V AR.01035 NOCOLOK-brazed heat exchangers; Solvent degreasing of individual parts prior
BEHR VN V AR.01036 NOCOLOK-brazed heat exchangers; Aqueous degreasing of individual parts prior
TRGS 220 Safety data sheet for hazardous substances and preparations
Previous Issues
AA 03330 : 2002-12; AA 03977 : 2000-08
BEHR PN V AR.01033 : 2003-08
Amendments
The following amendments were made compared to BEHR PN V AR.01033 : 2003-08:
a) Preliminary Standard status cancelled.
b) Section 3.1: Standard DIN EN ISO 9002 replaced by DIN EN ISO 9001.
c) Section 4 added.
d) Section 5.2: Works Standard BEHR PN 043 061 replaced by BEHR PN AR.01042
e) Section 5.1.1.1: “Operating instructions” added.
f) Layout and contents of Standard revised.

PN AR.01033 Test Methods For Monitoring of Cleaning Processes

Uploaded by

Document Information

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

PN AR.01033 Test Methods For Monitoring of Cleaning Processes

Uploaded by

Copyright:

Available Formats

Test Standard PN AR.

Original language: German

Brazed Aluminum Heat Exchangers – General

3 Special Notes ..........................................................................................................4

4 Occupational Safety and Health and Environmental Protection ........................4

4.2 Environmental protection .................................................................................................................. 4

5 General Test Methods ............................................................................................4

5.1.5 Specified values ........................................................................................................................... 5

7.1.2.1 Tools and equipment ..................................................................................................................... 11

Previous Issues ...............................................................................................................15

4 Occupational Safety and Health and Environmental Protection

4.2 Environmental protection

5 General Test Methods

5.1.1 Test conditions

5.1.1.1 Information on the use of test inks

5.1.2.1 Information on the apparatus to be used

5.1.3 Test Sequence

5.1.3.1 Preliminary remarks on the application of test inks

5.1.3.2 Test steps

5.1.4 Test evaluation

5.1.5 Specified values

5.2 Determining the residual lubricant content on the part by means of IR

5.2.1 Test conditions

5.2.2 Test sequence

5.2.3 Test results and test evaluation

5.2.3.1 Specified values

5.3 Determining the residual lubricant content on the part by means of

5.3.1 Test conditions

5.3.2.1 Tools and equipment

− Analytical scales, accuracy ±1 mg

5.3.3 Test sequence

Filling the evaporator flask

Evaporation of the solvent

5.3.4.1 Specified values

6 Test Methods for Aqueous Processes

6.1.1 Test conditions

6.1.2.1 Tools and equipment

6.1.3 Test sequence

6.1.5 Test results and test evaluation

6.1.5.1 Specified values

6.2 Determining the residual lubricant content in a cleaning bath by means of

6.2.1 Test conditions

6.2.2.1 Tools and equipment

6.2.3 Test sequence

6.2.4 Test results and test evaluation

Oil phase Correct reading:

30% reading mark

6.2.4.1 Specified values

6.3 Determining the cleaner concentration in the bath by means of titration

6.3.1 Test conditions

6.3.2 Test results and test evaluation

6.3.2.1 Specified values

6.4 Determining the conductivity in the purging water

6.4.1 Test sequence

6.4.2 Test results and test evaluation

6.4.2.1 Specified values

6.5 Determining the evaporation residues in purging baths by means of

6.5.1.1 Tools and equipment

6.5.2 Test sequence

6.5.2.2 Test steps

6.5.4 Test results and test evaluation

6.5.4.1 Specified values

7 Test Instructions for Solvent-Based Processes