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Spectro Quick User Guide PDF
Spectro Quick User Guide PDF
The following guidelines are written to provide the user with a convenient reference document
and to familiarise the user with the sometimes unique responses that this spectrophotometer can
provide. This guide should not be used in place of the manufacturer’s instrument manual or in
place of the method cards provided to determine various Wall Wash Test parameters.
This instrument can be run on either 120 or 240V mains supply and is supplied with US and EU
mains cables. The instrument should be sited on a dry, flat surface. Due to its mode of operation,
its readings are stable, even in relatively rough seas.
Instrument start-up
After switching the instrument on, a series of rapid self-calibration tests are performed. During
this switch on, the cell holder area should be free from sample cells. If there are any problems
during the switch on, the faults will be displayed by the instrument and the user advised how to
remedy the problem. After successful switch on, the instrument is calibrated and ready for use
and the display will show 4 optional files.
Sample Cells There are two sets of sample cells with this instrument. Always ensure
the cell windows are clean, dry and free from visible contamination.
For UV work, the 10mm quartz glass sample cell should be used.
Quartz glass cells are invisible to UV light, but they are very
delicate and should be handled with great care. When using this
cell the clear sides should be exposed to the light path, and the
cell should be placed at the far right hand side of the cell holder.
Due to the unique light path and optical arrangements of this instrument, it is not necessary to
cover the sample cells in order to obtain a reading on this instrument.
The operation of this instrument is by simple file driven menus. Navigation through the screens
and methods is performed by pressing appropriate numerical keys and by the GREEN ‘accept’ or
the RED ‘cancel’ key.
Pressing the RED key also takes the user back one step/page or aborts the current
operation.
The blue 0A/100%T key is for zeroing the instrument (preparing a reference)
The GREEN key takes a measurement or accepts the current option.
Running a Method
Once selected, the method screen will display the Method number and name, the wavelength
and units.
The instrument operates by passing a light beam of known wavelength through a liquid test
sample and measuring the amount of light that is absorbed by the sample. By comparing the
amount of light absorbed in a reference sample with the amount of light absorbed in a test
sample, it is possible to accurately detect the concentration of contamination in the test sample.
Applications in the visible region of the light spectra usually involve a colour change and can be
seen by the operator. But applications in the UV region are invisible to the naked eye.
Pressing blue 0A/100%T (with the appropriate blank reference sample installed in the
instrument) will zero the instrument and the sample box will show reference. During the
scanning, a rapid ticking noise is heard, this is normal.
Pressing the GREEN button (with the appropriate working sample installed in the instrument) will
take a measurement; the value obtained will be shown in the concentration box.
At start up, to allow the optical and electrical components to stabilise, it is recommended to carry
out the following process:
i.) Select any test method from the L I Maritime Programs menu
ii.) Without inserting a test sample into the sample holder, press the blue 0A/100%T button
iii.) Press the GREEN button 5 – 10 times in quick succession
Connection to a PC
The spectrophotometer has a built in USB communications port that can be used to connect to a
dedicated manufacturers’ printer, manufacturers Bluetooth device or to a PC, but it is pre-set to
communicate with a PC via the enclosed USB cable and software.
The instrument can be used for more sophisticated analytical determinations (UV scanning) and
the connection to a PC enables operators to send spectral data via email for evaluation. It will
also enable software updates to be uploaded remotely.
Range For scanning wall wash / cargo / washing water samples in the UV region of the
spectrum either in absorbance units or in the units of % Transmission (generally
for the measurement of MEG FG purity)
i.) To measure the purity of a chemical product when there is no reference. This usually
refers to the purity of a first foot / final loaded cargo sample or to measure the purity
of a chemical product used in the laboratory or for tank cleaning
ii.) To identify the level of contamination in a wall wash sample compared to the pure
laboratory grade methanol (or ethanol)
This procedure is carried out in the UV region of the light spectrum and a quartz sample cell
(labeled with a “Q” on the cell window) must be used.
Procedure
1. Switch the L&I Wave II instrument on. After a few seconds and if all self checks are
accepted, the instrument is calibrated and ready for use. A screen showing four files is
shown
3. Now press the button entitled Wavescan to scan in absorbance units or Wavescan
(Transmission) to scan in % Transmission.
i.) For measuring the purity of a chemical product when there is no given reference.
4. Fill the 10mm quartz glass cell with laboratory grade distilled or de-ionised water and
insert into the far right hand side of the sample cell holder. The cell is held in place by a
small spring mounted fixing screw inside the cell holder. This represents the reference or
blank sample against which all test samples are compared
5. Press the dark blue 0A/100%T button to set the instrument to zero. A blank graph will
now be seen with wavelength in nm across the “x” axis (from 200 – 350nm) and light
absorbance or transmission up the “y” axis (from 0 – 2.5 A or 0 – 100% T)
6. Remove the quartz sample cell and dispose of the water reference
7. Refill the quartz sample cell with the test sample (methanol, ethanol, mono ethylene
glycol, washing water etc.) and replace in the sample cell holder in the same place that
the reference was located
Interpretation of Results
In absorbance mode, a good sample with little or no contamination will show a characteristic
“smooth” curve:
pure methanol
2.5
2
absorbance
1.5
pure
methanol
1
0.5
0
200 220 240 260 280 300 320 340
wavelength (nm)
By using the left and right arrow keys it is possible to identify the actual absorbance reading at
specific wavelengths. Pure methanol typically has an absorbance reading of less than 0.3 and
220nm and this is a very good indicator of the purity of methanol samples in general,
Any deviation from the smooth curve (typically in the form of peaks) indicates contamination.
The position of the peaks indicates the chemical nature of the contamination. The area
underneath the peaks directly corresponds to the concentration of these contaminants which
means in some instances, this technique can also be used to quantify the contamination
concentration.
benzene in methanol
100 mg / l
1.0 benzene in
meoh
0.8
absorbance
0.6 10 mg / l
benzene in
0.4 meoh
0.2
1mg / l
0.0 benzene in
200.0 220.0 240.0 260.0 280.0 300.0 320.0 340.0 meoh
wavelength (nm)
Copyright L&I Maritime Ltd. October 2016. All Rights Reserved.
L&I Maritime Ltd., Unit 4 First Floor, Old Brewery Yard, Worksop, Nottinghamshire, S80 2DE, UK.
Tel. +44 (0) 1909 532 003 Fax. +44 (0) 1909 500 945 Email. operations@limaritime.com
Page 4 of 20
demo L& I
ii.) To identify the level of contamination in a wall wash or washing water sample
compared to an uncontaminated sample of the same wall wash or water.
9. Fill the 10mm quartz glass cell with pure laboratory grade methanol (or ethanol) or clean
washing water sample (fresh or sea) and insert into the far right hand side of the sample
cell holder. The cell is held in place by a small spring mounted fixing screw inside the cell
holder. This represents the reference or blank sample against which all test samples are
compared
10. Press the dark blue 0A/100%T button to set the instrument to zero. A blank graph will
now be seen with wavelength in nm across the “x”axis (from 200 – 350nm) and light
absorbance or transmission up the “y” axis (from 0 – 2.5 A or 0 – 100% T).
11. Remove the quartz sample cell and dispose of the reference
12. Refill the quartz sample cell with the wall wash or washing water sample and replace in
the sample cell holder in the same place that the reference was located
13. Press the GREEN button which starts the scan. A graph will now be seen on the display
which represents the completed UV scan
Interpretation of Results
The closer the graph is to a flat line, the closer the wall wash or washing water sample is to the
pure methanol (or ethanol) or clean water. Any contamination in the test sample will show up as
a deviation (in the form of peaks) from the flat line. The position of the peaks is specific to the
nature of the contamination and the area underneath the peaks directly corresponds to the
concentration of these contaminants which means in some instances, this technique can also be
used to quantify the contamination concentration.
The following graph also shows that the same concentration of different cargoes does not
produce peaks that are the same size and area. Different cargoes do have different responses.
There is a library of UV traces on the MCIS tank cleaning database (www.milbros.com)
1.5
absorbance
10 mg / l
1.0 phenol in
meoh
0.5
10mg / l
0.0 benzene
200.0 220.0 240.0 260.0 280.0 300.0 320.0 340.0 in meoh
wavelength (nm)
Procedure
1. Ensure that the PVC (print via computer) program is loaded onto the computer that is
intended to accept the data, following the on screen instructions after the CD ROM is
installed. Set up the computer following the detailed instructions that are included in the
PVC CD ROM
2. Switch the L&I Wave II instrument on and after the self-checks are completed, the
instrument is calibrated and ready for use. A screen showing four files is shown
3. Press button 4 marked Utilities followed by button 3 marked Printer. The box marked
Autoprint should be On; use the horizontal arrow keys to do this. Press the RED button
twice to go back to the main menu
4. Now connect the computer and the L&I Wave II instrument using the USB connector and
open the PVC programme on the computer. You will see a text box that says:
Searching .. looking for units on ports whilst the computer finds the instrument, then
Checking if Excel is present whilst the computer locates the Microsoft Excel programme.
5. When the computer finds the instrument and connects to Excel you will see another text
box that says Running .. waiting for input followed by this screen, which shows the serial
number of the instrument and the fact that it is connected.
6. If you cannot see this, exit the PVC programme and try again, making sure the computer
and instrument are connected by the USB connection before the PVC is opened.
7. Double click this icon, which opens the PVC Instrument configuration window as follows:
8. Go down to the fourth paragraph called When report received and carry
out the following:
10. Print_Report. To save data just to the computer, double click and set to No.
11. Save_Report. To save data to the computer, double click and set to Yes.
13. Create a file on the desktop of the computer called “spectro downloads” and instruct the
computer to save all data into that file, by updating this directory.
17. Saved Excel files are typically 25-50kb in size and these can be transferred via email as
and when required
- Dissolve 10 g of silver nitrate in 500 ml of 20% nitric acid. Store this solution in a dark bottle.
- Alternatively, separate solutions of 2% silver nitrate and 20% nitric acid can also be used just as
successfully.
Procedure
1. Switch the L&I Wave II instrument on. After a few seconds and if all self checks are accepted,
the unit is calibrated and ready for use. A screen showing four files is shown
2. Press the button relating to the L I Maritime Programs, file number 2
3. Press the button (number 1) relating to 950 Chloride in MeOH. The test can now be
performed
4. Transfer 25 ml of test sample into an appropriate sample tube
5. Add 5 drops of the acidified silver nitrate reagent, or 5 drops each of 2% silver nitrate and
20% nitric acid
6. Prepare a reference sample to run concurrently, by following steps 4 and 5 using pure
methanol. Leave to stand for 15 minutes
7. After 15 minutes, follow these instructions
8. Fill one 40mm rectangular glass sample cell with the prepared reference sample and insert
into the sample cell holder, ensuring the cell is fully seated in the cell holder
9. Press the blue 0A/100%T button to set the instrument to read zero. Once the instrument is
zeroed, it does not display any result, but 0.000 can be seen in the Absorbance box
10. Remove the reference sample from the instrument and pour it back into the reference
sample tube
11. Rinse first and then fill the same glass sample cell with the test sample before inserting into
the instrument. Press the GREEN button and read the chloride concentration of the test
sample directly in ppm from the Concentration box
12. At low concentration levels, it is suggested to take 2 or 3 readings for each sample and use an
average as the result
13. It is recommended to regularly check that the reference sample still reads zero. If the reading
shows any significant drift, reset the reference by repeating steps 8 and 9
Interpretation of Results
The chloride content of the test sample in ppm is read directly from the instrument.
Interferences
1. Hazy and / or excessively coloured test samples
2. The presence of excessive detergents
3. The presence of excessive phosphates
4. The presence of excessive water immiscible contaminants (hydrocarbons)
Copyright L&I Maritime Ltd. October 2016. All Rights Reserved.
L&I Maritime Ltd., Unit 4 First Floor, Old Brewery Yard, Worksop, Nottinghamshire, S80 2DE, UK.
Tel. +44 (0) 1909 532 003 Fax. +44 (0) 1909 500 945 Email. operations@limaritime.com
Page 9 of 20
demo L& I
951 Permanganate Time Test
Range Pass or Fail in line with ASTM D 1363.
Procedure
1. Switch the L&I Wave II instrument on. After a few seconds and if all self checks are accepted,
the unit is calibrated and ready for use. A screen showing four files is shown
2. Press the button relating to the L I Maritime programs, file number 2
3. Press the button (number 2) relating to 951 Permanganate Time. The test can now be
performed
4. Prepare a water bath at 15oC 1oC
5. Fill a sample tube with 25 ml of the test sample and place it in the bath for at least 10
minutes to allow it to cool down to 15oC
6. Now add 1 ml of the potassium permanganate reagent to the sample tube, mix the contents
well and replace in the bath. Note the time
7. Leave the sample tube in the bath for 50 minutes, or whatever length of time the potassium
permanganate time test specification is set at
8. Fill one 40mm rectangular glass sample cell with pure methanol, with no potassium
permanganate solution added (reference sample) and insert into the sample cell holder,
ensuring the cell is fully seated in the cell holder
9. Press the blue 0A/100%T button to set the instrument to read zero. Once the instrument is
zeroed, it does not display any result, but 0.000 can be seen in the Absorbance box
10. Remove the reference sample from the instrument
11. Rinse first and then fill the same glass sample cell with the test sample before inserting into
the instrument. Press the GREEN button and note the % reading from the Concentration box
12. At low concentration levels, it is suggested to take 2 or 3 readings for each sample and use an
average as the result
13. It is recommended to regularly check that the reference sample still reads zero. If the reading
shows any significant drift, reset the reference by following steps 8 and 9
Interpretation of Results
A reading greater than 32.0 % by this procedure, will still show a pink colour, and pass the test
A reading less than 32.0 % by this procedure will appear to be brown in colour, and fail the test
Interferences
1. Hazy and / or excessively coloured test samples
2. The presence of extremes of pH
Range APHA 5 – 500 in line with ASTM D 1209 on the Platinum - Cobalt scale.
Procedure
1. Switch the L&I Wave II instrument on. After a few seconds and if all self checks are accepted,
the unit is calibrated and ready for use. A screen showing four files is shown
3. Press the button (number 3) relating to 952 APHA Colour. The test can now be performed
4. Fill one 40mm rectangular glass sample cell with pure methanol (reference sample) and insert
into the sample cell holder, ensuring the cell is fully seated in the cell holder
5. Press the blue 0A/100%T button to set the instrument to read zero. Once the instrument is
zeroed, it does not display any result, but 0.000 can be seen in the Absorbance box
7. Rinse first and then fill the same glass sample cell with the test sample before inserting into
the instrument. Press the GREEN button and read the colour of the test sample directly in
APHA from the Concentration box
8. At low concentration levels, it is suggested to take 2 or 3 readings for each sample and use an
average as the result
9. It is recommended to regularly check that the reference sample still reads zero. If the reading
shows any significant drift, reset the reference by following steps 4 and 5.
Interpretation of Results
The colour of the test sample in APHA is read directly from the instrument
According to the ASTM reference the colour should be reported either as an exact multiple of 5
or “lighter than” the next highest multiple of 5 whichever is the most appropriate
Interferences
Procedure
1. Switch the L&I Wave II instrument on. After a few seconds and if all self checks are accepted, the
unit is calibrated and ready for use. A screen showing four files is shown
2. Press the button relating to the L I Maritime programs, file number 2
3. Press the button (number 4) relating to 953 Hydrocarbons. The test can now be performed
4. Add 10ml of the methanol test sample to 90 ml of distilled water, in a suitable sample tube
Note: By adding more methanol to the distilled water (25:75 / 33:67 / 50:50), makes the
hydrocarbon test progressively stricter. This deviates from ASTM, but may be required at the
loadport. The test result is appropriate whatever the methanol to distilled water dilution ratio.
5. Invert the tube once or twice to mix the water and methanol
6. Prepare a reference sample to run concurrently, by following steps 4 and 5 using pure methanol
instead of the test sample
7. After 20 minutes follow these instructions
NOTE: To avoid the formation of air bubbles in the sample cell, samples should be transferred very
carefully. The sample tube should not be re-inverted after the initial mixing. If air bubbles are
present in the sample cell at the time of analysis, inconsistent results may be observed.
9. Fill one 40mm rectangular glass sample cell with the prepared reference sample and insert into
the sample cell holder, ensuring the cell is fully seated in the cell holder
10. Press the blue 0A/100%T button to set the instrument to read zero. Once the instrument is
zeroed, it does not display any result, but 0.000 can be seen in the Absorbance box
11. Remove the reference sample from the instrument and pour it back into the reference sample
tube
12. Rinse first and then fill the same glass sample cell with the test sample before inserting into the
instrument. Press the GREEN button and read the hydrocarbon content of the test sample in FTU
directly from the Concentration box
13. At low concentration levels, it is suggested to take 2 or 3 readings for each sample and use an
average as the result
14. It is advisable to regularly check that the reference sample still reads zero. If the reading shows
any significant drift, reset the reference by following steps 9 and 10
Interpretation of Results – All results are relative to the reference sample. The results are quoted in
formazin turbidity units (FTU), but they are not a specific hydrocarbon concentration.
Samples having a reading greater than 0 by this procedure fail the test
Known Interferences
1. Hazy test samples.
2. The presence of excessive detergents
Copyright L&I Maritime Ltd. October 2016. All Rights Reserved.
L&I Maritime Ltd., Unit 4 First Floor, Old Brewery Yard, Worksop, Nottinghamshire, S80 2DE, UK.
Tel. +44 (0) 1909 532 003 Fax. +44 (0) 1909 500 945 Email. operations@limaritime.com
Page 12 of 20
demo L& I
954 Chloride in H2O
- Dissolve 10 g of silver nitrate in 500 ml of 20% nitric acid. Store this solution in a dark bottle.
- Alternatively, separate solutions of 2% silver nitrate and 20% nitric acid can also be used just as
successfully.
Procedure
1. Switch the L&I Wave II instrument on. After a few seconds and if all self checks are
accepted, the unit is calibrated and ready for use. A screen showing four files is shown
2. Press the button relating to the L I Maritime programs, file number 2
3. Press the button (number 5) relating to 954 Chloride in H2O. The test can now be
performed
4. Transfer 25 ml of test sample into an appropriate sample tube
5. Add 5 drops of the acidified silver nitrate reagent, or 5 drops each of 2% silver nitrate and
20% nitric acid
6. Prepare a reference sample to run concurrently, by following steps 4 and 5 using pure DI
water. Leave to stand for 15 minutes
7. Fill one 40mm rectangular glass sample cell with the prepared reference sample and
insert into the sample cell holder, ensuring the cell is fully seated in the cell holder
8. Press the blue 0A/100%T button to set the instrument to read zero. Once the instrument
is zeroed, it does not display any result, but 0.000 can be seen in the Absorbance box
9. Remove the reference sample from the instrument and pour it back into the reference
sample tube
10. Rinse first and then fill the same glass sample cell with the test sample before inserting
into the instrument. Press the GREEN button and read the chloride concentration of the
test sample directly in ppm from the Concentration box
11. At low concentration levels, it is suggested to take 2 or 3 readings for each sample and
use an average as the result
12. It is recommended to regularly check that the reference sample still reads zero. If the
reading shows any significant drift, reset the reference by repeating steps 8 and 9
Interpretation of Results
The chloride content of the test sample in ppm, is read directly from the instrument.
Interferences
1. Hazy and / or coloured test samples
2. The presence of excessive detergents
3. The presence of excessive phosphates
4. The presence of excessive water immiscible contaminants (hydrocarbons)
The following guidelines are written to provide a starting point for the analysis of washing water
using the L&I Wave II Spectrophotometer.
Introduction
Washing water analysis is the opposite of wall wash analysis, in so much that it is designed to
identify what has been removed from the cargo tanks during the tank cleaning process, rather
than identifying what has been left behind after tank cleaning. Very simply, when there are no
longer any traces of the previous cargo in the washing water, tank cleaning can be stopped, as
observed in the following graph:
In all cases, a valid reference sample must be used to set the instrument to zero prior to the start
of analysis. This is generally a sample of the washing water (seawater or freshwater) taken
directly from the tank cleaning line, before it enters the cargo tank; the theory being that the
quality of the washing water leaving the cargo tank can at best be the same quality as the
washing water entering the tank (in which case the analysis results will show no significant
activity). If the washing water removed from the cargo tank does contain previous cargo residues,
it will show up as positive activity on the instrument display.
It is very important to take multiple samples in order to follow the progress of the cleaning. One
sample taken at the end of a scheduled cleaning plan does not provide scope for optimising tank
cleaning procedures, which is one of the most significant benefits of this process.
Washing water samples should ideally be taken from the vessel’s manifold in order to confirm
that both the cargo tanks and cargo lines are clean.
Washing water analysis is carried out in the UV region of the light spectrum, meaning the 10mm
path length must be used for this procedure.
4. Press the dark blue 0A/100%T button to set the instrument to zero. A blank graph will now be
seen with wavelength in nm across the “x”axis (from 200 – 350nm) and light absorbance up the
“y” axis (from 0 – 2.5 absorbance units)
Unlike other test procedures, the data generated by the instrument provides scope to identify the
precise nature of the contaminants found in the washing water samples; not just a “hydrocarbon”
or “PTT” fail. Different chemical groups generally show up in the same place on the graph, which
allows the user to quickly relate the quality of the washing water with the previous cargo.
The following graph shows the most common chemical groups and where they appear in the UV
spectrum:
• In general, the wider the peak the longer the hydrocarbon chain
• Peak width / height is also related to concentration of the hydrocarbon
• Methanol (one carbon) has the smallest peak
• Lube / mineral oils and vegetable oils can produce very wide peaks